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Development of a monitor to quantify lead-based aerosols

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Title:
Development of a monitor to quantify lead-based aerosols
Creator:
Vanderpool, Robert William, 1955-
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Language:
English
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xiv, 224 leaves : ill. ; 28 cm.

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Subjects / Keywords:
Aerosols ( jstor )
Diameters ( jstor )
Inlets ( jstor )
Lead ( jstor )
Liquids ( jstor )
Nitrogen ( jstor )
Nozzles ( jstor )
Polarography ( jstor )
Pumps ( jstor )
Velocity ( jstor )
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bibliography ( marcgt )
theses ( marcgt )
non-fiction ( marcgt )

Notes

Thesis:
Thesis (Ph. D.)--University of Florida, 1991.
Bibliography:
Includes bibliographical references (leaves 223-224).
General Note:
Typescript.
General Note:
Vita.
Statement of Responsibility:
by Robert William Vanderpool.

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University of Florida
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University of Florida
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Copyright [name of dissertation author]. Permission granted to the University of Florida to digitize, archive and distribute this item for non-profit research and educational purposes. Any reuse of this item in excess of fair use or other copyright exemptions requires permission of the copyright holder.
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AJD5025 ( NOTIS )
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DEVELOPMENT OF A MONITOR TO QUANTIFY LEAD-BASED AEROSOLS


By

ROBERT WILLIAM VANDERPOOL













A DISSERTATION PRESENTED TO THE GRADUATE SCHOOL
OF THE UNIVERSITY OF FLORIDA IN PARTIAL FULFILLMENT
OF THE REQUIREMENTS FOR THE DEGREE OF
DOCTOR OF PHILOSOPHY

UNIVERSITY OF FLORIDA


1991





























This dissertation is dedicated to the memory of my parents.












ACKNOWLEDGEMENTS


I would first like to thank Ken Reed for his assistance in machining

several pieces of the experimental apparatus. His expertise is most

appreciated.

The useful discussions with John Applewhite concerning the capabilities

and limitations of the polarograph are appreciated.

I would also like to acknowledge the assistance of Tom Peters during the

field evaluation of the prototype monitor. The successful demonstration of the

instrument's capabilities would not have been possible without his effort.

I also wish to thank the members of my doctoral committee for their time

and effort required to serve in this capacity. Each member, in his own way, has

served as a source of inspiration during the course of my studies at the

University of Florida. I am particularly appreciative of Dr. Lundgren for his

guidance, encouragement, and confidence. He has provided me with

opportunities for laboratory, teaching, and field experience that contributed

greatly to my professional development.

Finally, I would like to thank my wife, P.J., for her patience and support

during the last three years.


iii
















TABLE OF CONTENTS


ACKNOWLEDGEMENTS ...........................

LIST OF TABLES .................................

LIST OF FIGURES ................................

KEY TO SYMBOLS ...............................

ABSTRACT .....................................

CHAPTERS

1 INTRODUCTION .............................

Background .................................
Description of Battery Production Process ...........
Instrument Design Criteria .......................
Summary of Design Approach ....................

2 REVIEW OF UTERATURE ......................

3 DESIGN AND CALIBRATION OF PARTICLE COLLECTION

Design Theory ...............................
Prediction of Impactor Performance ................
Calibration of the Particle Collection Section ..........

4 DESIGN OF AIR SAMPLING SYSTEM ..............

Introduction .................................
Description of Air Sampling System ................
Prediction of Particle Sampling and Transport
Efficiency ..................................


.......

........







SECTION


....=...
. .

. .. =..

. o. ,

........

. ..







5 DESCRIPTION OF LEAD ANALYSIS SYSTEM .................

Introduction .......................................
Design Criteria ................ ............. ........
Description of Polarographic Analysis ...........................
Analysis of Field Bulk Samples .................. ... .......
Description of Modifications to the Polarograph ...............

6 DESCRIPTION OF FLUID HANDLING SYSTEM ...............

7 PROGRAM DESCRIPTION AND OPERATION .................

8 FIELD EVALUATION OF PROTOTYPE INSTRUMENT ...........

Introduction .........................................
Experimental Methods .................................
Experimental Results ...................................

9 SUMMARY AND RECOMMENDATIONS .....................


70

70
70
72
82
88

110

124

132

132
132
139

151


APPENDICES

A IMPACTOR DESIGN DRAWINGS .......................... 155

B IMPACTOR CALIBRATION RESULTS ...................... 160

C CONFIGURATION OF KIETHLEY 575 CHANNELS ............. 162

D LISTING OF PROGRAM ................................ 165

E OPERATING MANUAL FOR THE LEAD-IN-AIR MONITOR ........ 185

REFERENCE LIST ........................................ 223

BIOGRAPHICAL SKETCH .................................. 225














LIST OF TABLES


Table 3-1


Table 4-1

Table 4-2

Table 4-3


Table 4-4

Table 5-1


Table 5-2

Table 5-3


Predicted Operating Characteristics of Teflon
Impactor ...............................

Description of Module 1 Air Flow Components ......

Description of Module 2 Air Flow Components ......

Module 2 Electrical Component Listing and
Description ..............................

Module 2 Electrical Connector Pin Descriptions .....

Polarograph Response Using Copper Internal
Standard ................................

Comparison Tests Between Polarograph and GFAA ..

Component Listing and Description of RUN/STOP
Board ..................................

RUN/STOP Board Connector Pin Functions ........

Component Listing and Description of PCM3 Board ..

Description of Various PCM3 Channels ...........

Component Listing and Description of Decade
Resistance Board ..........................

Decade Resistance Board Connector Pin Functions ..

Component Listing and Description of Model 264A ...

Model 264A Connector Pin Descriptions ..........


28

46

50


54

55


84

87


91

92

94

95


98

99

102

103


Table

Table

Table

Table


Table

Table

Table


5-4

5-5

5-6

5-7


5-8

5-9

5-10








Table 5-11


Table 5-12

Table 6-1


Table 6-2


Table 6-3


Table 6-4

Table 8-1

Table 8-2

Table 8-3


Table 8-4


Table 8-5


Table 8-6


Table 8-7


Component Listing and Description of Digital
Board ......... .........................

Digital Logic Board Connector Pin Descriptions .....

Listing and Description of Liquid Handling
Components .............................

Listing and Description of Nitrogen Handling
Handling Components ......................

Module 1 Electrical Component Listing and
Description ..............................

Module 1 Electrical Connector Pin Descriptions .....

Analysis of Laboratory Lead Standards ...........

Analysis of Field Control Lead Standards ..........

Results of Collocated Sampling Performed at Plate
Offbearing Operation .......................

Results of Unattended Sampling Performed at Plate
Offbearing Operation .......................

Results of Collocated Sampling Performed at Paste
Drying Operation ..........................

Results of Unattended Sampling Performed at Paste
Drying Operation ..........................

Results of Collocated Sampling Performed at Plate
Stacking Operation .........................


vii


106

107


112


120


122

123

140

141


143


145


146


147


149













UST OF FIGURES


Figure 1-1


Figure 1-2


Figure 3-1


Figure 3-2


Figure 3-3



Figure 3-4


Figure 3-5



Figure 3-6


Figure 4-1

Figure 4-2

Figure 4-3

Figure 4-4


Fow chart of lead-acid battery production
process ................................

Summary of prototype lead-in-air monitor design
approach .. ...........................

Measured particle size distributions at a
battery plant .............................

Schematic of single-stage impactor used for
particle collection ............... ..........

Schematic of generation system used for production
of calibration aerosols greater than 0.5 micrometers
aerodynamic diameter ......................

Scanning electron photomicrograph of ammonium
fluorescein calibration aerosols produced by VOAG

Schematic of generation system used for production
of calibration aerosols less than 0.5 micrometers
aerodynamic diameter ......................

Measured particle size collection efficiency curves
for single stage impactor ....................

Schematic of Module 1 air flow system ...........

Schematic of Module 2 air flow system ...........

Wiring diagram of Module 2 electrical components ...

Measured performance of Module 2 mass flow
controller ................................


viii








Figure 4-5


Figure 4-6


Figure 5-1


Figure 5-2


Figure 5-3


Figure 5-4


Figure 5-5


Figure 5-6

Figure 5-7


Figure 5-8


Figure 5-9



Figure 6-1

Figure 6-2


Figure 6-3

Figure 6-4


Theoretical particle transport efficiency through the
sampling probe's horizontal section .............

Theoretical particle transport efficiency through the
probe's 900 bend ..........................

Polarographic response to 40 ppm concentrations of
lead, cadmium, and copper in 0.1 N HNO3 .........

Typical polarographic response as a function of lead
concentration .............................

Polarographic response to 0-200 ppb lead
concentration using 200 ppb internal copper standard

Polarographic response to 0-8000 ppb lead
concentration using 200 ppb internal copper standard

Schematic of printed circuit board which provides
run/stop functions .........................

Wiring diagram of Keithley PCM3 power control module

Schematic of printed circuit board which provides
decade resistance ranging functions ............

Schematic of Model 264A showing recommended
locations for auxiliary circuit boards ..............

Schematic of printed circuit board which provides
logical switching of stir, purge, and drop
dispense/dislodge functions ...................

Schematic of Module 1 liquid handling system ......

Detail drawing of flow-through cell designed for the
polarograph ..............................

Schematic of Module 1 nitrogen handling system ....

Wiring diagram of Module 1 electrical components ...


64


66


76


78


81


83


89

93


97


101



105

111


116

119

121







Photograph of lead-in-air monitor during tests
conducted at plate offbearing process ............

Photograph of Module 1 inlet section showing position
of collocated filter holder relative to Module 1
inlet ....................................


Figure 8-1


Figure 8-2


136



137












KEY TO SYMBOLS


C particle concentration

C, slip correction factor

D particle diffusion coefficient

Dp0 impactor cutpoint

D, tube diameter

g gravitational constant

L tube length

M gas molecular weight

n number of impaction jets

P fractional penetration

P, stack pressure

Q volumetric flowrate

R bubble radius

STK particle Stokes number

T gas temperature

V gas velocity

Vb bubble velocity

V, gas velocity pressure








V, particle settling velocity

W jet width

ad coefficient of diffusional deposition

a, coefficient of inertial deposition

a, coefficient of gravitational deposition

p, gas density

p gas dynamic viscosity

T particle relaxation time


xii












Abstract of Dissertation Presented to the Graduate School
of the University of Florida in Partial Fulfillment of the
Requirements for the Degree of Doctor of Philosophy

DEVELOPMENT OF A MONITOR TO QUANTIFY LEAD-BASED AEROSOLS

By

Robert William Vanderpool

December 1991


Chairperson: Dale A. Lundgren
Major Department: Environmental Engineering Sciences


Manufacture of lead-acid batteries results in the advertent formation of

gas-borne particles containing lead. Since the adverse health effects of

significant lead exposure are well documented, the battery industry is required

to undergo periodic monitoring to demonstrate compliance with existing lead-in-

air regulations.

A prototype instrument has been developed to quantify lead-based

particulates on a near real-time basis. Aerosol samples can be obtained from

high velocity, flowing airstreams as well as from static airstreams. The

instrument thus has potential as an emissions monitor, a recirculation air

monitor, or a monitor of workplace environments. The prototype instrument

contains an air sampling and transport system, a particle collection section, and


xiii








a lead analysis section. Proper sequencing of the system's components and

archival of the experimental test results are provided by an IBM-compatible

computer interfaced with a data acquisition and control system. The prototype

monitor may be operated either in attended or automated sampling and

analysis mode. The details of the instrument design will be presented along

with results of its laboratory and field evaluation.


xiv












CHAPTER 1
INTRODUCTION


Background


Industrial manufacturing processes often result in the formation of gas-

borne particles (aerosols) containing hazardous metals such as lead, cadmium,

and copper. Since the adverse environmental and occupational health effects

of these substances are well documented, periodic air monitoring of

manufacturing processes involving their use is required to demonstrate

compliance with existing federal and local regulations.

The lead acid battery industry, which accounts for 72% of all domestic

lead usage (Environmental Protection Agency, 1986), is a potential source of

significant lead-based aerosol production. Monitoring of lead emissions in the

battery industry typically requires a separate aerosol sampling and analysis

technique. First, a representative aerosol sample is obtained from the process

using approved sampling techniques. This procedure typically involves aerosol

collection through a high efficiency filter to remove particles from the airstream.

The collected aerosol sample must then be extracted from the collection

substrate and analyzed using an appropriate analytical technique. However, the

time delay between sample collection and analysis is typically on the order of









days to weeks. Moreover, improper handling and extraction of the collected

sample can result in significant errors in estimation of the total lead

concentration. Positive sample bias is a particular problem during

measurement of trace lead levels common during evaluation of occupational or

recirculation air monitoring. Finally, specially approved equipment, sampling

and analysis techniques, and trained personnel are necessary to achieve

accurate results. The need existed, therefore, for an instrument capable of

providing both aerosol sampling and analysis of lead-based particles on a near

real-time basis.

The advantages of an automated air sampling and analysis instrument for

lead measurement tests are obvious. Such a device could be used both for

occupational and emission measurements and would significantly reduce the

cost of each test. Such an instrument would report test results within minutes

of the air sampling. Finally, by proper design and construction of the

instrument, the sources of measurement error inherent to the current

methodology could be significantly reduced. Compliance with existing emission

and occupational regulations could be routinely demonstrated. This report

details the design, construction, calibration, and field evaluation of such an


instrument designed for use by the lead-acid battery industry.









Description of Battery Production Process


The design criteria for the lead-in-air monitor was based on careful review

of the various operations involved in the manufacture of lead-acid batteries. Of

particular importance was consideration of the concentration, size distribution,

and chemical composition of the lead-based aerosols produced at each of the

process points. Figure 1-1 is a flow chart of the various operations involved in

the battery production. Not shown in the figure are various paths involving the

reclaim and reuse of lead scrap which occurs at several of the process points.

Battery manufacture first begins with the production of lead monoxide

powder by grinding solid lead metal in the presence of air at elevated

temperatures. Lead oxide paste is then produced by combining the lead oxide

powder with water and dilute sulfuric acid along with small amounts of

proprietary materials.

Battery plate grids are cast from molten lead-based alloys which consist

primarily of lead but also contain various trace metals to improve the plate's

mechanical properties. Following a specified curing time, the grids are

transported to the pasting operation where they are pasted and flash dried prior

to being off-loaded from the assembly line. The pasted plates undergo another

curing process before use. Plate stacking then occurs which involves alternate

stacking of plates with paper separators. The stacked plates are then loaded

into plastic cases and the appropriate cells connected together during the cast-

on-strap operation. The case cover is then installed, cells filled with sulfuric












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acid, and the batteries electrically charged prior to the packaging and shipping

operation.

The characteristics of the lead-based aerosol produced at each step of

the production process depends primarily on the composition of the material

handled and the mechanism by which the aerosol is produced. The aerosol

produced during the grid casting operation tends to be relatively small in size

and may contain only 5% to 20% lead by mass. Lead mass concentrations of

aerosol produced at the grid casting operation typically meet allowable emission

limits and are therefore ducted to the environment without the need for any

control measures.

Conversely, production and handling of lead oxide powder, paste and

pasted plates tends to form dispersion-type aerosols relatively large in diameter

and contain 95% to 99% lead by mass. Aerosols from these processes also

tend to be of much higher lead mass concentrations and are therefore ducted

to control equipment (typically baghouses) prior to the airstream's exhaust to

the environment.

With the exception of the acid fill, charging and packaging operations, all

the steps in the battery production process are sources of elevated lead

exposure to the battery plant workers. These processes, therefore, all possess

ventilation systems designed to remove the majority of the lead-based aerosols

and transport them to the particulate control equipment. Since these airstreams

are ultimately exhausted to the environment, an equivalent supply of makeup air









is required to maintain a flow balance. Battery plants in colder climates have

incorporated recirculation air systems to reduce heating costs associated with

heating the makeup air to plant temperature. This recirculation air is typically

obtained from grid pasting, drying, plate offbearing, cast-on-strap, and plate

stacking operations and is cleaned through a system of two high efficiency

particulate air filters (HEPA) in series with one another. This clean recirculation

air is then supplied to various process points as a source of makeup air.

The Occupational Safety and Health Administration has approved use of

this type of recirculation air system but requires continuous monitoring of the

recirculation air to ensure that the airborne lead content not exceed the

regulated 50 micrograms/m3 permissible exposure limit concentration.

Experience has shown that if the double HEPA filter system is installed and

maintained correctly, concentrations much lower than 5 micrograms/m3 can be

routinely obtained.

It is primarily for the purpose of monitoring recirculation air quality that

the lead-in-air monitor was developed. Other potential applications to the

battery industry will be discussed.

Instrument Design Criteria


The development of a lead-in-air monitor must be based on the sampling

and analysis requirements specific to the lead-acid battery industry. First, the

instrument must be capable of obtaining representative aerosol samples from









both flowing airstreams (stack or duct sampling) as well as from static

airstreams (room sampling). Particle size distribution measurements have

shown that efficient particle collection must take place over a fairly wide range

of particle sizes.

Accurate quantitation of the particulate lead content is also essential.

The analytical technique chosen must be specific for elemental lead and

possess minimum physical and chemical interference from other particulate

and gaseous components. Analytical accuracy and repeatability must exist over

the measurement range of interest. The analytical technique must possess low

blank and background response for the lead measurement.

Sampling should be performed over a 10 to 20 minute time period.

Instantaneous measurements are neither technologically feasible nor particularly

desirable because variations in lead handling processes and activities result in

considerable concentration variability with time. Time averaged measurements,

therefore, are more appropriate indicators of average process emissions. In

conjunction with a 15 minute analysis time, a 15 minute air sampling period

would allow a complete sampling and analysis cycle to be repeated

approximately every 30 minutes.

The instrument must also be capable of quantifying lead levels over a

wide range of concentrations. These concentrations range from recirculation

system alarm levels of 10 micrograms/m3 to levels of greater than

1000 micrograms/m3 for emissions from paste mixing facilities and other three-

part operations.









Instrument reliability and ease of use was also a design consideration.

Cleaning, maintenance, and external calibration of the instrument should be

minimized. The working instrument must be at least semi-automated, fairly

portable, and operate on standard 110 VAC, 60 hz power sources.

Finally, it was desired that the instrument's development and construction

costs be kept to a minimum. Once a final instrument design had been

completed and its capability demonstrated, it was desired that duplication costs

be limited to approximately $10,000.


Summary of Design Approach


Development of an automated sampling instrument for the specific

quantitation of lead involved careful consideration of the design criteria outlined

in the previous section. Ideally, the developed instrument would satisfy all of

the listed criteria although certain design and operational tradeoffs could have

been made if necessary. Of primary concern, however, was the instrument's

ability to obtain representative particulate samples from particle-laden airstreams

and accurately quantify lead levels over a reasonable concentration range.

Design of the instrument can be conveniently divided into three separate

sections: the air sampling system, the particulate sampling system, and the lead

analysis system. The sampling system must efficiently capture particles over a

range of sizes and effectively deliver them to the lead analysis section.

Representative sampling in flowing airstreams requires that isokinetic conditions









be achieved (nozzle velocity equal to freestream velocity) through proper

combination of nozzle inlet area and sampling flowrate. It was envisioned that

the sampling system contain several nozzles of varying inlet areas in

conjunction with a 60 to 90 liter per minute (Ipm) capacity sampling pump

whose sampling rate could be controlled and monitored by the user. The range

of operating flowrates was selected to be 10 to 30 Ipm. Following consideration

of available particle collection techniques (filtration, electrostatics, etc.), inertial

impaction was chosen as the mechanism to be employed in the instrument's

particle collection section. Subsequent calibration of the impactor showed that

it would collect 95% to 100% of the lead-based particles present in the in-plant

processes of interest.

Design of the instrument's analytical section required careful

consideration of its specific operating requirements. Of primary concern was

the ability to accurately quantify collected lead in amounts which were expected

at the various in-plant operations. Considering a 15 minute sampling time and

a nominal 15 Ipm sampling flowrate, approximately 0.23 m3 of air would be

sampled. For expected concentrations ranging from 10 micrograms/m3 to

2000 micrograms/m3 at the various in-plant processes, lead deposits of

2.3 micrograms to 460 micrograms would result. If these deposits were placed

in liquid solution (50 ml, for example), lead concentrations of 46 micrograms per

liter (ppb) to 9 milligrams per liter (ppm) by mass would be expected.

A wide variety of analytical techniques was considered during design of

the instrument's analytical section. Most of these techniques were eliminated









from consideration either due to their high cost, level of complexity, lead

detection capability, or failure to lend themselves to convenient automation.

Ultimately, an electrochemical technique was chosen for the quantitation of lead

in liquid solution. A commercially available polarograph was purchased and

adapted for automation.

A schematic of the completed instrument is shown in Figure 1-2. Air flow

through the system's particle collection section is provided by a 90 Ipm capacity

air pump with flow controlled and monitored using a commercially available

mass flow controller. Deposition of the lead-based particles takes place

primarily by inertial impaction into 50 ml of 0.5M nitric acid which is supplied

from a 5 liter capacity reservoir. Following a sufficient sampling time, an aliquot

of the solution is transferred to a flow-through cell in the polarograph for lead

analysis. The lead-in-air concentration can then be calculated from the

sampling time, sampling flowrate, solution volume, and the measured liquid lead

concentration.

Automated control of the system's components takes place using a data

acquisition and control system (Kiethley Instruments, Inc., Model 575) interfaced

with an IBM-compatible computer. Computer control not only allows for proper

sequencing of the various components but also allows for data reduction and

automatic storage and retrieval of the test results. The Keithley 575 data

acquisition and control system receives necessary power from the computer

and provides both digital and analog input/output capabilities. A Keithley Model

AMM1 analog measurement module provides eight separate analog input









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channels with a range of 10V, an input rate of 50 khz, and 12 bit

measurement resolution. The Kiethley 575 contains two analog output channels

with similar capabilities. At power up, the Model 575 self-calibrates the analog

channels with an accuracy of 2%.

Digital control is provided by 32 digital input/output channels with signals

which are transistor-to-transistor (TTL) compatible. A separate 16 channel

module (Kiethley, Model PCM3) provides external AC or DC power control

using TTL activated solid-state relays.

In the 575 system, the user can access the various module channels

using Kiethley KDAC500/I software linked with a GW-BASIC programming

environment. Use of programming logic rather than hard-wired logic allowed

for design flexibility during development of the prototype system.












CHAPTER 2
LITERATURE REVIEW


Design of the proposed lead-in-air monitor was based on a number of

important criteria. The instrument must capture airborne particles in a

representative manner and transfer them effectively to the instrument's lead

analysis section. The analytical technique chosen must be specific for

elemental lead and yield a response that is linearly proportional to mass

concentration. Analytical accuracy and repeatability must exist over the

measurement range of interest and possess minimal interference from the

collection substrate and other particle components.

During the last two decades, considerable progress has been made

towards development of direct reading instruments for aerosol measurement.

These devices include electrical aerosol analyzers, condensation nuclei

counters, aerodynamic particle sizers, optical sizing and counting devices, and

piezoelectric and beta gauge based devices. Note that each of these

techniques measure a different property of airborne particles and thus do not

provide comparable information. Of these devices, only piezoelectric and beta

gauge devices provide direct reading of collected aerosol mass. None of these

techniques provide information in terms of the chemical composition of the

measured aerosol. Typically, devices such as filters, impactors, or electrostatic









collectors are merely used to capture an aerosol for subsequent analysis by a

separate instrument.

Conversely, there exist a wide variety of analytical techniques available

for chemical quantitative analysis. Typically, these techniques require that the

aerosol sample be previously collected in a separate step and manually

transferred to the instrument's analytical section. Some sample pretreatment or

extraction is often required to obtain reliable test results.

Rather limited success has been achieved in integrating these separate

aerosol sampling and analysis techniques in a single, direct reading instrument.

Many of these analytical techniques required for trace level analysis are fairly

sophisticated and do not adapt well to the development of inexpensive, portable

instruments. These sophisticated techniques often require daily calibration and

frequent maintenance to ensure accurate test results. The need for automated

sample transfer and preparation also complicates the instrument design.

Several tape samplers are available which provide combined aerosol

sampling with mass determination. In these automated devices, air flow is

normally directed through a porous tape which acts as the collection medium

for the airborne particles. This technique thus provides an integrated sample

with results time-weighted for the sampling period. In the GCA Model RDM301

sampler, particle matter is deposited by impaction onto a mylar film coated with

an adhesive (Uoy, 1983). At the end of the sampling period, the collected

material is quantified by beta attenuation. For low energy beta radiation, the









attenuation is a function of mass density of the absorber and is largely

independent of chemical composition or the particle's physical properties.

Spagnola (1989) developed an automated sampling instrument based on this

analytical principle. The instrument uses electromechanical devices for

automatic positioning of membrane filters in the sample holder. At the end of

the sampling period, the filter is analyzed and returned to its original position in

the sample holder. Application of beta attenuation has also been applied to a

dichotomous sampler developed by Macius and Husar (1976).

A paper tape sampler was also modified to provide lead analysis by x-ray

fluorescence (Smith et al., 1986). The system samples air at 0 to 10 Ipm and

irradiates the collected aerosol mass with a 10 mCi cadmium 109 radioisotope.

A Nal scintillator in conjunction with a multi-channel analyzer provides counts

versus x-ray energy for the resulting x-rays. The count corresponding to the

x-ray energy characteristic of lead provides a measure of the collected lead

mass. The authors note that the presence of arsenic and zinc positively

interfere with the lead measurement.

Automated mass monitors have also been developed based on the

concept of piezoelectric sensing of changes in aerosol mass. The TSI Inc.

Model 5000 deposits particles onto a piezoelectric crystal by electrostatic

precipitation. The rate of change of the crystal's output frequency is directly

proportional to the deposited mass concentration. Recently, this mass sensing

technique was applied to the development of an instrument which uses a low-

frequency tapered element coupled to a filter collector (Wang, 1985).







16
Successful measurement of aerosol composition "in-situ" has been limited

and has generally not evolved beyond the laboratory. Arnold and Folan (1987)

devised an instrument which levitates a single airborne particle within an

electrostatic field and irradiates the particle with an infrared beam. The

instrument optically detects changes in particle size caused by evaporation of

the particle due to the heat induced by the infrared absorption. The measured

rate of change is proportional to aerosol mass. The instrument is capable of

detecting picogram quantities of material for both organic and inorganic

functional groups such as sulfate and carbonate (Allen and Palen, 1989).

The majority of analytical techniques which have been adapted for trace

aerosol chemical analysis are available only in an "off-line" mode and do not

adapt well to field use. Martinsson and Hansson (1988) have used particle

induced x-ray emission (PIXE) for the multielement analysis of aerosol

previously deposited onto thin aluminum foils. Deposits were stepwise heated

to several hundred degrees centigrade by applying an electric current through

the sample. An ion beam impinged on the sample during the process. Low

atomic weight element information (such as oxygen and carbon) was obtained

by particle elastic scattering analysis while elements with atomic numbers

greater than 14 were determined by PIXE analysis. The chemical composition

of the sample was inferred from noted vaporization temperatures and

stoichiometry. Laboratory tests found the technique useful for quantitation of

ammonium chloride, ammonium nitrate, and ammonium sulfate.







17

Xhoffer et al. (1989) used a transmission electron microscope to analyze

laboratory generated aerosols deposited onto carbon coated electron

microscope grids. The analytical technique of electron energy loss

spectroscopy was used to observe the change in kinetic energy as the electron

passes through the sample. This technique is generally useful only for low

atomic weight elements. The authors also noted that high background signals

can be associated with the substrate and that rapid deterioration of

environmental samples can occur. The technique was also found to possess

limited quantitative application since the particle's absorption of the incident

electron beam was a function of particle size.

Electron spectroscopy for chemical analysis (ESCA) was investigated by

Muller et al. (1987) as a means of characterizing sub-micrometer sodium sulfate

aerosol collected on various filter media. This technique used incident x-rays to

excite photoemission of core level electrons from the sample. The measured

energy of the emitted photoelectrons is characteristic of the emitting element's

oxidation state. ESCA provides only surface analysis and is thus of limited

quantitative analysis. ESCA signals can also be difficult to interpret

quantitatively. Incorporating a similar surface analytical technique, Fletcher

(1983) used a laser microprobe to vaporize and ionize a collected sample for

analysis by a time-of-flight mass spectrometer. Reported limitations of this

technique were similar to those experienced by Muller et al. using ESCA

analysis.









Neutron activation analysis (NAA) has been employed to provide

elemental information of collected aerosol samples. In this technique, the

sample is irradiated with neutrons to produce radionuclides. The activities of

the radionuclide products are then measured and related to the quantities of the

elements present in the sample. Podzimek and Wojnar (1990) used NAA to

quantify masses of laboratory generated titanium oxide particles deposited on

polyester filters. In a related study, Ondov et al. (1990) used NAA to quantify

45 elements in rural sub-micrometer ambient aerosols collected by micro-orifice

impaction. Although this technique was found to be generally useful, the

substrate blank precluded analysis of several elements of interest.

X-ray powder diffraction analysis of collected aerosol deposits was

reported by Tanninen et al. (1985). Powder diffraction allows for direct

determination of crystalline compounds. The authors used the diffraction

technique to analyze fumes generated by metal arc welding of steel. The main

analytical difficulty encountered was low instrument output intensity due to the

small particles analyzed in conjunction with the small quantity of material

present.

Both conventional flame and graphite furnace atomic absorption

spectroscopy have been widely used for the analysis of collected aerosol

samples. Davidson (1979) used graphite furnace techniques to characterize

size fractionated aerosol samples obtained from three national parks. Attempts

to incorporate atomic absorption analysis in an automated monitor have met

with limited success (Smith et al., 1986).












CHAPTER 3
DESIGN AND CALIBRATION OF THE PARTICLE COLLECTION SECTION


Design Theory


Accurate quantitation of lead-in-air concentrations requires efficient

capture of lead-based particles. If an aerosol was only collected with 10%

efficiency, the resulting lead analysis would obviously greatly underestimate the

actual lead-in-air concentration. This would, in turn, result in an underestimation

of the lead exposure hazard. This section describes the design and calibration

of a device capable of sampling and capturing lead-based particles with the

necessary high efficiency to ensure accurate test results.

There currently exist a variety of aerosol samplers and collectors which

offer a basis for the collector design. These devices include inertial devices

(impactors and cyclones), electrostatic precipitators, thermal precipitators,

diffusion devices, and filtration devices. Each of these devices relies on a

particular property of airborne particles to remove the particles from the

airstream in which they are suspended.

Fundamental to the design of any particulate collection section is

understanding the nature of the aerosol to be measured. In predicting

individual particle properties (settling velocity, diffusional behavior, etc) the most







20
important parameter is that of particle size. Since industrial aerosols are always

a collection of particles of varying sizes, it is understanding of the aerosol's size

distribution which is of importance.

Figure 3-1 presents particle size distributions measured at a battery plant

in the southeastern United States. The specific sampling locations represent

sources of aerosols which supply recirculation air. It is believed, therefore, this

size distribution can be assumed to be fairly representative of aerosols which

exist in recirculation air systems. Plotted in the figure for the various process

points are cumulative lead mass distributions versus aerodynamic particle

diameter as measured using a University of Washington cascade impactor. The

aerodynamic diameter is defined as the diameter of a spherical particle of unit

density which has the same settling velocity as the particle under consideration.

Use of an equivalent aerodynamic diameter accounts for the particle's size,

shape, and density.

Inspection of Figure 3-1 reveals that these measured size distributions

are fairly large with half of the lead mass associated with particles greater than

10 micrometers aerodynamic diameter. These results agree well with similar

measurements by Hodgkins et al. (1990) from two different battery

manufacturing plants. Note that only 1% to 5% of the lead mass is associated

with particles less than one micrometer aerodynamic diameter. A device

capable of collecting all particles greater than one micrometer, therefore, would

have an overall mass collection efficiency on this aerosol of 95% to 99%.










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22
Based on a review of these distributions, both thermal and diffusion type

collectors were eliminated as candidates for the collector design. Although

these type collectors can capture submicron aerosols with high efficiency, their

capture efficiencies for particles greater than one micrometer are quite low

(Hinds, 1982).

Filtration probably represents the most common form of aerosol

collection in air sampling. Unlike thermal and diffusion type devices, samplers

which rely on filtration mechanisms possess high collection efficiencies over a

wide range of particle sizes. Aerosols encountered in the battery industry could

be expected to be removed by filtration with virtually 100% efficiency. Despite

these advantages, however, filtration was eliminated from design consideration

primarily for logistic reasons. Due to high particle-substrate attractive forces,

particles collected on high efficiency filters are extremely difficult to remove

efficiently even if wet chemical techniques are employed. Wetting of either

fibrous or porous membrane filters dramatically increases its pressure drop

making the filter difficult to reuse. The alternative to filter reuse is to replace it

after each sampling test. Automated replacement of the filter would have

involved design and cost complications which were considered to be

unacceptably high.

Electrostatic collection was also given consideration during the

instrument's design phase. In these devices, collection relies on the

electrostatic forces which can be exerted on charged particles in an applied







23
electric field. Similar to filtration samplers, electrostatic samplers possess high

collection efficiencies over a wide range of particle sizes. Use of electrostatic

collection would have involved use of a point-to-plane precipitator for deposition

of airborne particles to a liquid surface similar to the design approach adopted

during the design of the LEAP sampler (Andersen Samplers, Inc.).

This design approach was initially investigated during the instrument

development but was ultimately discarded for two primary reasons. First,

preliminary laboratory tests with a design prototype showed that the flow of

electrical current through the electrolyte resulted in the inadvertent plating out of

previously collected lead ions from solution. Loss of collected lead in solution

would have resulted in underestimation of the total lead-in-air concentration and

thus an underestimation of the lead exposure hazard. Use of electrostatics was

also eliminated due its greater complexity and anticipated maintenance

requirements in the corrosive nitric acid atmosphere of the collection region.

Ultimately, the use of inertial impaction was adopted for the final

instrument design. Inertial impactors have been widely used for aerosol

collection and sizing and can efficiently capture particles greater than one

micrometer diameter. Inertial impactors are relatively simple in construction,

contain no moving parts or electrical components, and require little

maintenance.

Impactors rely on the high inertial forces which can be established on

particles in a high velocity airstream. In a typical impactor stage, particle-laden









gas is accelerated through one or more nozzles and directed toward a solid

surface which forces the airstream to change its flow direction. Due to their

inertia, however, particles will be unable to exactly follow their respective

streamlines and will deviate from the airstream by a distance which is a function

of the particle's aerodynamic diameter and the jet velocity. Particles of sufficient

inertia will deviate a sufficient distance to strike the collection surface and be

removed from the airstream. Conventional impactor stages with high jet

velocities can remove particles of 0.3 micrometers aerodynamic diameter and

larger.

Impactor performance is typically described by its Dp, cutpoint which is

the particle size collected with 50% efficiency. Particles larger than the cutpoint

diameter are collected with much higher efficiency. Extensive theoretical and

practical impactor research has shown that the cutpoint can be predicted with

some confidence by



D r=| 9 r I n W3 rS()
Pso Vi 9 i4 pp Q (3-1)



where C, is the Cunningham's slip correction factor determined from the

particle size and the fluid properties, p is the gas dynamic viscosity, n is the

number of jets, W is the jet width, p is the particle density, and Q is the

volumetric flowrate. The Stokes value (STK) can be predicted from knowledge







25
of the jet Reynolds number, ratio of jet width to jet to plate distance, and ratio of

jet throat length to jet width.

Based on these accepted design criteria, an inertial collector was

designed and constructed for use as the instrument collection section.

Figure 3-2 is a schematic of this device showing key components. Complete

detail drawings of each of the unit's components are presented in Appendix A.

In most inertial impactors, the impaction jet is directed onto a preweighed

stationary surface previously coated with a viscous, nonvolatile grease to

minimize particle bounce and losses due to blowoff. Following the sampling

run, the impaction surface is reweighed to quantify the mass of the collected

aerosol deposit. If chemical analysis is to be performed, the aerosol must be

extracted from the grease in an efficient and representative manner.

The collector developed for the lead-in-air monitor does not impact

particles onto a solid surface but into 50 ml of 0.5 M HNO3. Use of the liquid

impaction substrate eliminates the need for greased substrates and provides for

direct transfer of the particles from the gaseous phase to the liquid phase. High

velocity impaction also provides for the liquid turbulence necessary for efficient

particle dissolution so that aqueous lead ions are formed. High liquid

turbulence also tends to homogenize the liquid sample so that only an aliquot of

the sample need be analyzed for accurate lead determination.









Aerosol Inlet


Liquid Inlet


^; ^
11 olo

o ??
/f y Yle
/ f /
/ /,

/ / / /
^ / /
01 0 0
' //

/ //
/ //


Liquid Outlet



Figure 3-2. Schematic of single-stage impactor used for particle collection.


Air Outlet







27

During the sampling run, particle laden air enters the impactor inlet at a

flowrate of 10 to 30 Ipm (depending on the sampling situation) and is

accelerated through a single stage impactor. As shown in Appendix A, the

impaction stage contains 20 circular jets of 0.026 inch diameter. Following its

impingement into the liquid, the airstream then enters an expansion section

which reduces the upward air velocity and thus reduces inadvertent liquid carry

over. Use of a small plug of glass fiber filter at the air outlet has shown to

further minimize the liquid carry over. At the conclusion of the air sampling

period, a liquid outlet provides for transfer of the solution to the instrument's

lead analysis section.


Prediction of Impactor Performance


Inspection of Equation 3-1 allows for the generalized prediction of

impactor performance as a function of sampling air flowrate and the critical

impactor dimensions. Table 3-1 presents a summary of these calculations

assuming standard temperature and pressure conditions for air. Also presented

are actual measured stage pressure drops as a function of the sampling

flowrate. Calculated cutpoints at flowrates of 10, 20, and 30 Ipm are 0.92, 0.63,

and 0.42 micrometers, respectively.

It should be emphasized that these calculations are based primarily on

theoretical and experimental evaluations of impaction onto a solid surface.

However, immersion of an impaction stage and impingement of an airstream










o '3 (
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0. I CM
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2 co5


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00 0
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into a liquid represents an entirely different flow situation. While impaction is

certainly the most dominant collection mechanism involved, the entire process

may more correctly be described as a bubbling phenomenon.

Unlike the extensive studies related to conventional inertial impaction,

there has been relatively limited research devoted to the absorption of aerosols

by bubbling. As a simplified model, some researchers have considered particle

deposition in air bubbles which freely rise through a stationary liquid. As a

further simplification, these studies only consider the motion of bubbles less

than 0.2 cm diameter which have been found to be approximately spherical in

shape. Larger bubbles become flattened as they rise through the liquid and

pulsations in the bubble shape can occur.

Deposition of particles with a buoyantly rising bubble results primarily due

to the relative motion of the bubble with respect to the liquid. Due to the shear

force which exists at the liquid-gas interface, a gas circulation within the bubble

is established and maintained. As a result of this circulation pattern, large

particles may be removed by inertial impaction to the liquid-gas interface.

Gravitational settling of large particles can also occur as well as removal of

submicron particles by molecular diffusion.

The first analytical and experimental treatment of this particle absorption

phenomenon within a freely rising bubble was performed by Davies and Taylor

(1950). This theory was extended by Fuchs (1964), who developed coefficients

of absorption (deposition efficiency per unit cm of bubble rise) for the separate









absorption mechanisms of inertial impaction, sedimentation, and diffusion.

Later, related experimental studies by Melandrie and Prodi (1971) confirmed the

validity of this approach.

The coefficient of absorption due to inertial deposition, a,, is related to

the bubbles upward velocity, Vb, the particle's relaxation time, T, and the radius

of the bubble, R, by

9 Vt
a 9 = 2 (3-2)
2R



Because particle relaxation time increases with the square of the particle

diameter, this inertial mechanism is dominant for large particles.

Similarly, the absorption coefficient due to particle sedimentation, a,, is

expressed as

3 9gT
a 4R Vb (3-3)



For most bubble sizes of interest, inertial deposition is an order of magnitude

greater than that of sedimentation.

Finally, diffusional deposition efficiency per unit path length can be

calculated by accounting for the particle's diffusion coefficient, D










a = 1.8 VD
Vd-b VR (3-4)


Large bubbles (R > 1 cm) rising in a liquid tend to flatten and pulsate

such that their rate of rise is difficult to predict. However, smaller bubbles can

be assumed to be spherical and their upward velocity can be predicted by a

empirical relationship developed by Melandrie and Prodi (1971)

Vb = 3.05 v (3-5)


where the dimensions of Vb and R are m/sec and m, respectively.

For a known bubble size and particle diameter, the overall change in

particle concentration (C) per unit length of bubble rise can be calculated by

dx
= ( as + a, + ad ) C (3-6)



For example, Jonas and Schulz (1991) used this relationship to calculate an

overall collection efficiency of 98.8% of one micrometer radius iron oxide

particles within 0.5 cm radius bubbles buoyantly rising through one meter of

liquid.

Inspection of the absorption equation reveals that for a given particle

size, decreasing the bubble radius results in an increase in absorption

efficiency. The equation also indicates that for a given bubble size, the

dominant collection mechanism depends strongly on particle size. For large

particles (greater than 0.3 micrometers radius) which possess large relaxation









times, inertial and sedimentation forces dominate while diffusive absorption is

negligible. Conversely, particles less than 0.05 micrometers radius are removed

almost entirely by molecular diffusion. Thus, regardless of bubble diameter,

there exists an absorption minimum which exists for particles of approximately

0.2 to 0.4 micrometer diameter. The actual magnitude of the minimum depends

primarily on bubble radius.

Use of these theoretical considerations to exactly predict the

performance of the lead-in-air monitor's impactor proved to be difficult. This

simplified approach assumes bubbles of known size rising through a stable

liquid of constant height. Experimental verification of the theory by other

researchers has been limited and performed at relatively low flow rates using

uniform sized bubbles. However, the dynamics within the teflon impactor

represent a vastly different flow situation. Temporary replacement of the

impactor's opaque housing with a glass enclosure of similar dimensions allowed

for the direct observation of the bubbling phenomenon. This observation

revealed the limitations of the simplified theory to this particular collector. First,

it was evident that the bubbles produced were not uniform in size but existed

over a wide range of sizes. To apply the absorption theory to a distribution of

bubble sizes, the distribution itself must be known and the collection efficiency

equation integrated over the bubble size range. At these high flowrates, it was

also evident that the bubbles themselves experienced considerable oscillation

and occasional breakup due to the high liquid turbulence. Finally, it was







33
observed that the liquid itself underwent considerable turbulence which changes

the nature of the liquid-bubble interface and results in uncertainties in predicting

the path rise of the individual bubbles.

Due to this lack of reliable design theory, no exact predictions of the

impactor's actual performance were made. Preliminary review of conventional

impactor design theory and bubbling theory were used only as a basis for the

impactor design. For accurate evaluation of the impactor's actual performance,

extensive experimental efficiency tests were conducted with the impactor in the

laboratory.


Calibration of the Particle Collection Section


In evaluating the performance of the particle collector, it was understood

that the collection efficiency would depend on the unit's critical dimensions,

liquid solution volume, particle diameter, and the sampling flowrate. Since the

impactor's dimensions and the solution volume were fixed by design, the

particle size and sampling flowrate were normally the only two parameters

varied during the collection efficiency tests.

The particle collection characteristics of the impactor were evaluated in

the laboratory using monodisperse calibration aerosols of solid, spherical

ammonium fluorescein. These calibration aerosols were produced by two

separate generation systems depending upon the size of the particle required.

For the generation of calibration aerosols 0.5 micrometers aerodynamic

diameter and larger, a Thermal Systems Inc. Model 3050 vibrating orifice







34
aerosol generator (VOAG) was used. A schematic of the complete generation

and sampling system is presented in Figure 3-3. The VOAG operates on the

principle of the controlled mechanical breakup of a liquid jet into uniform

droplets of predictable size. Periodic breakup of the liquid jet was achieved by

application of an AC signal at a known frequency to a piezoelectric crystal

which housed the liquid orifice. Since the liquid consisted of a known quantity

of a non-volatile solute dissolved in a volatile solvent, the generated droplets

dried to form uniform particles of predictable size. For the calibration of the

impactor, the liquid solution was prepared by dissolving a fluorescein powder in

aqueous ammonia. After their production, the droplets dried to form spherical

particles of solid ammonium fluorescein. The particles were then mixed with

clean dilution air and charge neutralized by exposure to a "Kr radioactive

source. The particles were then mixed with additional dilution air and sampled

by the impactor for the calibration tests. An optical microscope was used to

verify the size and quality of the generated particles collected on a fibrous or

membrane filter before each test series. Figure 3-4 is a scanning electron

photomicrograph of a monodisperse aerosol generated by this technique.

For calculating the particle's aerodynamic diameter from its physical

diameter, an ammonium fluorescein particle density of 1.35 g/cm3 was

assumed. This value was based on density measurements by Stober and

Flachsbart (1973), John and Wall (1983), Vanderpool and Rubow (1988), and

Chen and Crow (1986).

















E
0
0


c0
er--
so
Q,-
LL


jo
CI
C







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.0






1
4'
CV



Ca






0E

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.0
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0
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N
Ca
0


0.

10r



















































Figure 3-4. Scanning electron photomicrograph of ammonium fluorescein
calibration aerosols produced by VOAG.









Calibration aerosols less than 0.5 micrometers aerodynamic diameter

were generated using a Thermal Systems Inc. Model 3071 electrostatic

classifier. Figure 3-5 is a schematic of this generation setup. Polydisperse

droplets were first generated by air nebulization of fluorescein solutions through

a Collison nebulizer at an operating pressure of 20 psig. The polydisperse

droplets were then dried in a diffusion drier to form a polydisperse aerosol of

solid ammonium fluorescein particles. This aerosol was then passed through a

single stage impactor to reduce the large particle concentration. The pressure

drop across the impactor stage was monitored to verify the magnitude and

stability of the aerosol flowrate. Monodisperse particles of the desired size were

then produced by electrical classification within the classifier. Lastly, the

monodisperse aerosol was diluted to the necessary sampling flowrate using

clean, dry dilution air and sampled by the impactor.

The air exiting the impactor was passed through a filter holder housing a

47 mm diameter glass fiber filter which was used to collect any airborne

particles not collected by the impactor. Flowrate through the sampling system

was provided by a 90 Ipm capacity vacuum pump fitted with a primary valve

and a recirculation air valve. The pressure drop across a calibrated orifice was

used to adjust and monitor the sampling flowrate. A calibrated dry gas meter

measured the total volume of the gas sampled during each sampling run.

The collection efficiency of the impactor was defined as that mass

fraction of particles exiting the impaction jet which was collected in the liquid















o
0


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I -


U-


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-L


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solution. The total mass exiting the.jet was estimated by summing the mass

measured in the solution with that mass measured on the 47 mm after-filter.

Collected aerosol mass deposits were quantified fluorometrically using a

Turner Model 112 fluorometer calibrated for fluorescein concentrations ranging

from one part per billion to 14,000 parts per billion. For the collection efficiency

tests, the impactor's liquid solution consisted of 50 ml of 0.1N NH4OH. At the

conclusion of the sampling run, this solution was analyzed directly. To quantify

the mass of aerosol collected on the after-filter, the filter was placed in a 100 ml

polypropylene container with 50 ml of 0.1N NH4OH and the container placed in

an ultrasonic bath for approximately 20 minutes. Previous analytical tests have

shown that virtually 100% extraction efficiency can be achieved using this

technique.

Run times for the calibration tests varied depending upon the amount of

aerosol mass collected. For the large particle calibration tests, only 10 minute

run times were necessary. For the smallest particles generated, however, three

hour run times were necessary to achieve sufficient mass deposits for reliable

quantitation.

The performance of the impactor was measured as a function of both

particle size and sampling flowrate. Thirteen discrete particle sizes were used

ranging from 0.05 micrometers to 20 micrometers aerodynamic diameter. For

each particle size generated, collection efficiency tests were performed at

flowrates of 10, 20, and 30 Ipm. Each test series combination of particle size









and flowrate consisted of three separate collection efficiency tests performed

under identical test conditions.

Results of the collection efficiency tests are plotted in Figure 3-6.

Individual test results are tabulated in Appendix B. As expected, the impactor's

collection efficiency varies as a function of both aerodynamic particle size and

sampling flowrate. The right hand side of the collection efficiency curves is of

particular importance. Independent of flowrate, the shape of the curves

resemble that of conventional inertial impactors with impaction efficiency

increasing monotonically with increasing particle size. Clearly, inertial impaction

is the predominant collection mechanism for particles in this size range. In

accordance with impaction theory, the collection efficiency also increased with

increasing flowrate. Measured cutpoints in this region at 10, 20, and 30 Ipm

were 0.90, 0.53, and 0.46 micrometers aerodynamic diameter, respectively.

These measured values compare somewhat favorably with those predicted by

standard impactor theory (0.92, 0.63, and 0.42, micrometers).

The overall shape of the complete curves is quite similar to that predicted

by the simplified bubbling theory. Impaction is clearly dominant for large

particles while molecular diffusion accounts for deposition of small submicron

particles. Note also that an absorption minimum occurs in the range of 0.2 to

0.36 micrometers aerodynamic diameter which is approximately the size region

predicted by bubbling theory. The position and magnitude of the absorption

minimum was also noted to be a function of sampling flowrate. Below











I I I I I I I II


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42

0.2 micrometers diameter, molecular diffusion dominates the particle absorption

and efficiency actually decreases with increasing flowrate. This effect is

believed to result as a consequence of the gas' lower residence time within the

liquid column at higher flowrates.

In terms of quantitative chemical analysis, it is the overall mass efficiency

of the collection device on the aerosol which is of importance. Recall from the

measured size distributions in Figure 3-1, that 95% to 99% of the lead-based

mass is associated with particles greater than one micrometer aerodynamic

diameter. Since the impactor's collection efficiency on these particles is high,

integration of the collection efficiency curve over the measured size distribution

predicts that the impactor should collect this aerosol with over 95% mass

efficiency.

Particle losses through the impactor's inlet section were also quantified

during the calibration tests. Following each test series, the impactor was

disassembled and the inlet section carefully rinsed with a known volume of

0.1N NH4OH. Particle mass deposits were quantified by fluorometric analysis of

the collected rinse solution. In general, test results showed that inlet losses

represent only a small fraction of the sampled aerosol mass. Submicron

aerosol deposits were normally below the limit of quantitation of the fluorometric

technique. Large particle losses were found to be more significant with losses

of 2.2%, 3.2%, and 4.0% measured for particles of 6, 10, and 20 micrometers









aerodynamic diameter, respectively. Subsequent evaluation of the impactor

during its actual field use supported these test results.

Based on the calibration tests, it was concluded that the impactor's

design met the criteria outlined for the overall instrument design. For the

aerosols of interest in the battery industry, the impactor is capable of capturing

the aerosols with high collection efficiency. Use of a liquid solution as the

impaction substrate eliminates particle bounce and substrate overloading which

can exist for solid impaction substrates. Turbulence within the fluid during

collection provides for effective dissolution of the lead-based particles as well as

providing for a well mixed, homogeneous solution. Unlike solid impaction

substrates, the liquid is easily replaced after each sampling test and is

compatible with the chosen lead analysis technique. Lastly, the impactor can

be easily constructed, is physically compatible with the corrosive nitric acid, and

requires little periodic maintenance.













CHAPTER 4
DESIGN OF AIR SAMPLING SYSTEM


Introduction


Accurate quantitation of lead-in-air aerosols requires representative

collection and efficient transport of the lead-based particles to the instrument's

lead analysis section. Since it is infeasible to capture and analyze an entire

aerosol, a fraction of the aerosol must be extracted which reflects the aerosol's

particle size distribution, concentration, and chemical composition. Because

sampling flowrates may vary from one test to another, the designed

instrument's sampling flowrate must be controllable and accurately measured.


Description of Air Sampling System


Figure 4-1 is a schematic of the air sampling components associated

with Module 1. A description of these components is given in Table 4-1. In

addition to the components shown, Module 1 contains the system's nitric acid

reservoir, liquid pumps, and lead analysis system. Referring to Figure 4-1, the

vertical orientation of the impactor is compatible with its liquid contents and

minimizes particle transport losses from the Module 1 inlet to the impaction

stage. The Module 1 sampling system consists of a set of sharp-edged





























11


'12


To Module 2
Vacuum Source


Figure 4-1. Schematic of Module 1 air flow system. Component descriptions
are provided in Table 4-1.


1 2














Table 4-1
Description of Module 1 Air Flow Components




Figure 4-1 Code Description


1 3/16, 1/4, or 3/8 in. Diameter SS Nozzle

2 SS Female Connector, 1 in. Tube 1 in. NPT(F)

3 SS Rexible Hose, Teflon Lined
Cajon, Inc. Model SS-16BHT-36

4 SS Bulkhead Union, 1 in. Tube 1 in. Tube

5 SS 3/8 in. O.D. Tube, 4.25 in.

6 SS Male Connector, 1 in. Tube 1 in. NPT(M)

7 SS Male Elbow, 3/8 in. Tube 1/2 NPT(M)

8 SS 3/8 in. O.D. Tube, 3 7/8 in.

9 SS Union Elbow, 3/8 in. Tube

10 SS 3/8 in. O.D. Tube, 7 7/8 in.

11 SS Bulkhead Union, 3/8 in. Tube

12 3/8 in. Polypropylene Tubing, 6 ft.









nozzles, sampling probe, and impactor in addition to their associated tubing

and compression fittings.

Sampling of indoor air (non-ducted airstreams) is used to evaluate

occupational lead exposures. For indoor air measurements, the sampling

nozzles and sampling probe are not needed. Instead, a sharp-edged nozzle

has been fabricated from a one inch diameter stainless steel tube and attaches

to the top of Module 1. Its vertical orientation allows for direct collection and

transfer of airborne particles to the collector with minimal transport losses.

Unlike indoor air sampling, the sampling of ducted airstreams such as

recirculation airstreams requires sampling from a horizontal duct with high

associated air velocities. As will be discussed, accurate particle sampling from

a flowing airstream requires that a thin-walled nozzle be oriented directly into

the airstream. In addition, the sampling flowrate must be controlled such that

the nozzle inlet velocity equals that of the freestream velocity at the point of

sampling. Depending upon the measured freestream velocity, a nozzle of 3/16,

1/4, or 3/8 inch diameter can be used.

Sampling from horizontal ducts requires that the sampled aerosol must

undergo a 90 degree change of direction prior to entering the instrument's

vertical collection section. The sampling system contains a 39 inch long flexible

probe which is used for this purpose. The probe consists of a teflon inner

lining surrounding by a stainless steel braid. The teflon lining is compatible with

elevated temperatures up to 400 OF and is resistant to corrosion. The probe's







48
0.88 inch inner diameter matches that of the impactor inlet tube thus minimizing

particle transition losses due to air expansion or contraction.

Air flow through Module 1 is provided by connection to the vacuum

source located in Module 2. As shown in Figure 4-2, Module 2 contains an air

filter, mass flow controller, and cooling fan. Component descriptions are

presented in Table 4-2. The cartridge filter contains both activated charcoal and

fibrous filters and serves to protect the mass flow controller and sampling pump

from any particles remaining in the airstream. A high capacity vacuum pump

with teflon coated wetted surfaces provides the driving force for air flow through

the sampling system. As shown in Figure 4-2, this pump has been fitted with a

recirculation valve to reduce the load to the pump.

The sampling flowrate in the lead-in-air monitor is controlled using a

surplus Tylan Model FC-262 mass flow controller which has been adapted for

use in the system. The FC-262 is a 0-50 slpm capacity unit with flowrate

controlled by an internal solenoid valve. Selection of the flowrate is normally

provided by manual adjustment of a potentiometer to supply a 0 to 5 VDC

command signal to the flow controller. Feedback circuitry within the flow

controller continually adjusts the valve setting so that the actual air flow equals

the desired flowrate selected by the user. A measure of the actual flowrate is

provided by a corresponding 0 to 5 VDC output signal which is normally read

by the user from a digital panel meter. For adaptation to the prototype monitor,

the potentiometer input circuit and output display were removed and the










From Module 1

Muffler
1 19 //
1 ,18


17
2 7 13





Inlet


Valve Vacuum

Filter 4 15 P Pump

14

Inlet
Outlet Il
12
5 7 13 1
9

6 Mass
Flow 10
Controller


Module 2
(Top View)


Figure 4-2. Schematic of Module 2 air flow system. Component descriptions
are provided in Table 4-2.












Table 4-2
Description of Module 2 Air Flow Components




Figure 4-2 Code Description


1 SS Bulkhead Union, 1/2 in. Tube 1/2 in.
Tube

2 SS 1/2 in. Tube, 2 3/16 in.

3 SS Female Connector, 1/2 Tube 3/8 NPT(F)

4 Disposable Air Filter
Koby Inc., Model "Junior King"

5 SS Female Connector, 3/8 in. Tube 3/8 NPT(F)

6 3/8 in. Polypropylene Tube, 6 5/16 in.

7 SS Elbow, 3/8 in. Tube 3/8 in. Tube

8 SS 3/8 in. Tube, 1 3/4 in.

9 Mass Flow Controller, 0-50 slpm
Tylan Corp., Model FC262

10 SS 3/8 in. Tube, 2 in.

11 3/8 in. Polypropylene Tube, 5 3/8 in.

12 SS Male Tee Run, 3/8 in. Tube 3/8 NPT(M)

13 SS 3/8 in. Tube, 2 5/8 in.





















Table 4-2--continued



Figure 4-2 Code Description


14 SS 3/8 in. Tube, 2 9/16 in.

15 Valve, Swagelok Corp., Model B1RS6

16 Vacuum/Pressure Pump, 1/4 hp, teflon lined
3.2 cfm, 4A at 0 psi
Thomas Industries, Model 727CM39-TFE

17 3/8 in. Polypropylene Tube, 2 1/4 in.

18 SS Bulkhead Female Connector, 3/8 in. Tube
to 3/8 in. NPT(F)

19 Muffler, Koby Inc., Model M-1-N









command signal is now supplied by an analog output channel from the data

acquisition and control system. The flow controller's output signal is read by a

corresponding analog input channel on the data acquisition and control system.

Figure 4-3 is a complete wiring diagram of the Module 2 circuitry.

Component descriptions, functions, and commercial sources are listed in Table

4-3. Table 4-4 provides connector pin descriptions. A standard 120 VAC, 60

hz source supplies power to the mass flow controller power supply, vacuum

pump, and cooling fan. Power to the flow controller is supplied by a 15 VDC,

200 mA power supply. The power supply is protected using a 0.5 amp fuse.

The sampling pump is internally protected against current overload and thus

requires no additional fusing. On/off control of the air pump and the cooling

fan is provided by use of a solid state relay capable of handling load currents

up to 25 amps. The relay itself is activated through application of a 3-32 VDC

signal which is compatible with standard TTL digital command signals. All

Module 2 input and output signals are communicated by a standard 9 pin

ribbon cable to the Kiethley 575 data acquisition and control system.

Prior to its use, the Tylan mass flow controller had been repaired and

recalibrated by the manufacturer. Its condition and calibration were then

verified in the laboratory. At a variety of flowrates and upstream and

downstream pressures, the actual mass flowrate was measured as a function of

selected mass flowrate. For these tests, a National Bureau of Standards

traceable Gillian Model D-80028 bubble flow meter was used as a flow












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0

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C6

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0C
i

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Table 4-3
Module 2 Electrical Comoonent Ustina and Descriotion


Component


Barrier Terminal
Block

Solid State Relay




Appliance Plug


Cooling Fan



Fan Filter Screen(2)


Vacuum/Pressure Pump



Power Supply


Fuse


Fuse Block


Connector KK


Connector MM


Description


3 Contact, Double Row, 20A
Cinch, Inc. type 3-141

SSR Series, 240 VAC/25A
3-32 VDC input
Potter and Brumfield
Type SSR-240D25

250/115 VAC, 10/15A
Feller, Inc. type 6100-31

115 VAC, 0.15A
34 cfm at 0 in H20 S.P.
Comair/Rotron type SV2A1

Anodized, for 3.5 in fan
Fan-S/Qualtek type 06325-B

115 VAC, 1/4 hp, teflon lined
3.2 cfm, 4A at 0 psi
Thomas Industries type 727CM39-TFE

Dual.Voltage (-15/+ 15 VDC), 200 mA
Sola, Inc. type 85-15-2120

1 1/4 X 1/4 in, 0.5A slow-blow
SPC Technology type F-500SS-0.5

Screw termination
SPC Technology type FB1PS

9 pin D-Sub, crimp style plug
SPC Technology type DEC-9P

22 position, card-edge connector













Table 4-4
Module 2 Electrical Connector Pin Descriptions


Color

YEL

GRN

BRN


575
Channel

DIGOUT8

Ground

ANOUT1


RED ANIN1


BLK ANINO


BLK ANINO


RED ANINO


Pin#

KK-1

KK-2

KK-3


KK-4


KK-5


MM-2


MM-3


MM-4

MM-A


MM-C

MM-G


ANOUT1


Connection

Relay


Function

Pump, fan on/off


Ground Ground

LL-A MFC Command Signal
0-5 VDC

LL-3 MFC Output Signal
"High", 0-5 VDC

LL-2 MFC Output Signal
"Low", 0-5 VDC

KK-5 MFC Output Signal
"Low", 0-5 VDC

KK-4 MFC Output Signal
"High", 0-5 VDC

Power +15 VDC Supply

KK-3 MFC Command Signal
0-5 VDC


Power

Power


Common

-15 VDC Supply


WHT

BRN


GRN

BLU









calibration standard. For each operating pressure and flowrate range, six

separate measurements were made. As shown in Figure 4-4, the correlation

between the actual mass flowrate and the desired flowrate was generally good.

In the 10-30 slpm flowrate range of interest, the agreement was within 2%.

Note that conversion from actual to standard flowrate must account for the

fluid's temperature and pressure at the point of sampling. Conversion from

standard temperature as defined by the mass flow controller's manufacturer

(0 C) to standard temperature as defined by occupational regulations (25 OC)

must also be taken into account. In the prototype lead-in-air monitor, these

conversions take place automatically through the instrument's software.


Prediction of Particle Sampling and Transport Efficiency


Accurate measurement of lead-in-air concentrations requires that lead-

based particles be sampled, transported, collected, and analyzed efficiently.

Design of an efficient particle sampling and transport system depends primarily

on the particle size distribution expected, the fluid properties at the point of

sampling (such as temperature and velocity), and the air sampling flowrate

required by the instrument's particle collection section. Efficient design,

calibration, and field testing of a separate sampling system was beyond the

scope of this project. As a preliminary approach, a particle sampling and

transport system was adapted from EPA Reference Method 12, "Determination

of Inorganic Lead Emissions from Stationary Sources." In the forthcoming






















E

CL

0)
.4-I
0
L.
0
*0
o
L-

a)
&_
v,
cO
0,
0)


5 10


15 20 25 30 35


Set Flowrate


(slpm)


Figure 4-4. Measured performance of Module 2 mass flow controller.







58
sections, the sampling and transport efficiencies of this design will be predicted

based on published theoretical and empirical studies. Alternatives to this

sampling and transport system will be discussed.


Sampling from Still Air


Evaluation of occupational exposures to lead-in-air concentrations

represents sampling from an airstream at zero or low velocity. Because

particles possess higher stopping distances at higher velocities, sampling and

transport losses during still air sampling can be negligible when compared to

sampling from ducted, high velocity airstreams. There exist, however, two

types of still air sampling biases which can result particularly with regard to the

large particle distributions characteristic of the battery industry.

Efficient still air sampling requires use of a vertically oriented sampling

tube. When the inlet air velocity is low, a sampling bias can result due to high

settling velocities characteristic of particles with large aerodynamic diameters.

At low sampling velocities, this results in an overestimation of particle

concentrations. An additional bias can result due to the effect of particle inertia

on particle trajectory. For sampling in still air, curved streamlines result as air is

accelerated towards the inlet nozzle. Due to their inertia, particles will be unable

to follow their respective streamlines and will be displaced a distance which may

be large with respect to the dimensions of the inlet. Inertial effects of this type

can result in an underestimation of actual particle mass concentrations.







59
Based on these possible biases, various criteria have been developed for

the design of air samplers. Davies (1968) developed inlet criteria based on

parameters of nozzle inlet diameter, sampling flowrate, and particle

aerodynamic diameter. Agarwal and Lu (1980) predicted less than 10%

sampling losses if the probe diameter (Dt) meets the following criterion

De > 20 r2 g (4-1)


where r is the particle relaxation time and g is the gravitational constant.

Equation 4-1 was used to predict inlet losses of the 0.88 inch nozzle

used for still air sampling of the lead-in-air monitor. Results showed that

particles up to 60 micrometers aerodynamic diameter would be collected

without significant error. Particles greater than 60 micrometers would be

collected with less than 90% efficiency. The equal diameter of the nozzle the

inlet section ensures that particle transport losses should be minimized.


Sampling from Ducted Air Streams


Unlike sampling from still air, sampling from ducted airstreams can result

in significant sampling biases particularly with regard to the high velocity

airstreams and large particle distributions characteristic of the battery industry.

Moreover, the horizontal arrangement of ventilation ducts requires that a

captured aerosol must be transported a short distance to the instrument which

also involves a change in the aerosol's flow direction. As a result, particle









losses within the aerosol transport system may significantly reduce the mass

concentration detected by the lead analysis section. The factors affecting

particle sampling and transport biases will be discussed.

The purpose of the aerosol sampling system is to obtain a representative

aerosol sample from the airstream of interest. In ducted airstreams, this

involves use of a sampling nozzle and probe to extract a representative aerosol

sample and transport it to the instrument's collection section. Sampling bias

can occur, however, due to particles' inertia in flowing airstreams. Similar to the

sampling from still air, sampling criteria have been developed for efficient

sampling from ducted airstreams. These criteria are generally of three types.

First, sharp-edges inlet nozzles must be used to obtain representative air

samples. Blunt-edged orifices can disrupt the airflow entering the nozzle

resulting in nonrepresentative particle collection and high inlet losses (Vincent

and Gibson (1981), Vincent et al. (1982), Vincent et al. (1985), Stevens (1986),

Vincent (1987), Vincent and Gibson (1988)). The second criterion is that the

nozzle must be oriented directly into the oncoming airstream. Changes in the

sampled air direction due to nozzle misalignment are a function of particle

inertia, the misalignment angle, and the probe diameter (Durham and Lundgren,

1980). Lastly, the sampling should be performed under isokinetic conditions

(nozzle inlet velocity equal to freestream velocity). Anisokinetic sampling can

result in significant large particle sampling biases whose magnitude and

direction depend on the velocity ratio and the particle Stokes number. Note







61
that isokinetic sampling requires prior measurement of the airstream's velocity

at each of the desired sampling points. When sampling, achieving desired

nozzle inlet velocities requires proper combination of nozzle diameter and

sampling flowrates.

Achieving representative aerosol sampling does not ensure efficient

transport of the aerosol from the inlet nozzle to the particle collector. Particle

losses can occur both in the inlet nozzle as well as in the transport section.

Deposition can take place due to molecular diffusion, thermophoretic effects,

electrostatic effects, gravitational effects, and inertial effects. For the sampling

of aerosols of interest in the battery industry, only gravitational and inertial

mechanisms will result in significant transport losses.

Numerous theoretical and experimental studies have been conducted in

relation to understanding particle transport in sampling tubes. In general, these

studies agree on the recognized parameters of importance (such as particle

Stokes number, sampler geometry, and fluid conditions) but often vary widely in

terms of their conclusions and recommendations. Theoretical predictions of

transport losses requires extensive mathematical modeling of both fluid flow

fields and particle trajectories within the flow fields. The validity of these models

is often not confirmed. Differences in sampler geometries and flowrates can

result in significantly different predicted losses. Experimental loss

measurements are generally more practical but differences in sampler









geometries, operating flowrates, and particle properties make comparison of

separate studies difficult.

In the lead-in-air monitor's sampling system, particle transport losses

during duct sampling can occur either in the inlet nozzle or in the flexible

sampling probe. To predict nozzle inlet losses, a brief review of pertinent

literature was made. Although the actual loss will depend on nozzle diameter,

sampling flowrate, and particle size, the literature suggests that large particle

losses may exceed 5% by mass. In the lead-in-air monitor, additional nozzle

losses might also be expected due to the airflow's slight expansion from the

nozzle outlet diameter of 0.75 inches to the 0.88 inch diameter of the sampling

probe. The magnitude of the losses in the expansion section will depend on

sampling flowrate and particle size.

Losses in the sampling probe can more accurately be predicted than

those associated with the inlet nozzles. Considering the flexible probe oriented

as in Figure 4-1, the probe can be divided into three main sections for analysis:

an 8 inch long horizontal section, a 23 inch long section with a 14.5 inch radius

of curvature, and a 8 inch long vertical section. The particle losses in these

sections were considered separately. These calculations were simplified by the

fact that laminar flow conditions exist in the 0.88 inch diameter probe even at a

flow of 30 Ipm. Turbulent flow conditions alter the nature of the fluid flow field

and particle trajectories making accurate loss predictions more complex.







63
Particle deposition in the 8 inch long horizontal section occurs primarily

due to the force of gravity. During their transit time within the tube, particles

may settle a distance sufficient to be removed from the airstream. The

magnitude of these losses was predicted based on a study by Thomas (1958)

on sedimentation losses in horizontal cylindrical tubes. For laminar flow

conditions, the transport efficiency (penetration) can be predicted


P = 1 [ 2 [ 2 1- 4 2/3 + arcsin0l/3 4 1/3 /1- 2/3 ] (4-2)



3x L Vs R
8Q


where P is the fractional penetration, L is the tube length, V, is the particle

settling velocity, R is the tube radius, and Q is the volumetric flowrate through

the tube.

This relationship was evaluated for the 8 inch long section as a function

of particle size and sampling flowrate and is presented graphically in Figure 4-5.

Independent of flowrate, particles less than 10 micrometers aerodynamic

diameter can be transported through this section with fairly high efficiency.

Particle penetration above 10 micrometers, however, is predicted to decrease

fairly rapidly as a function of particle size. Note also that the lower sampling

flowrate results in lower transport efficiency due to the gas' longer residence

time within the horizontal tube. Efficient transport through this section,






























































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0 0


O


O
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.O .) .
000000i


U0IIDJIOUgd IDU0!IDJd


'o 0
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65
therefore, would imply the use of high sampling flowrates and tubes of smaller

diameter.

Unlike losses in horizontal sampling tubes, particle losses in 900 bends

are due primarily to inertia and centrifugal forces on the airborne particles. Due

to their inertia, particles will be unable to follow their respective streamlines

directly and may be displaced a sufficient distance to impact on the duct walls.

Air flow around the bend can also establish a rotational flow pattern normal to

the mean direction of flow. This rotational profile can result in additional

particle losses around the bend. Cheng and Wang (1981) developed a

relationship for transport efficiency in a 900 bend as a function of particle Stokes

number

P = 1 STK (4-3)


=1- pp DP2
18 l x R3


This relationship holds for laminar flow conditions and is plotted in Figure 4-6 as

a function of particle size and flowrate. Similar to losses in the horizontal

section, losses around the bend are minimal for particles less than

10 micrometers aerodynamic diameter. Particles greater than 20 micrometers

aerodynamic diameter are difficult to transport efficiently. Note also the effect of

sampling flowrate on transport efficiency. Higher flowrates correspond to larger









66




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4-)
/ 2
S0**


/ G )




co c
r / o 3





1,*
C.
/ .
*/ .O 0-
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00







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S o, ,. o. 0 o .-
o o

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I-
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" 0 0 0 0o 00 0 0 0-- 0
**........

--ooooooooo


UOIIDJ1 GUad JDUO!pODJj







67
stopping distances which would result in greater particle deposition. Inspection

of equation 4-3 would dictate use of low sampling flowrates and large diameter

tubes.

Note that the effects of flowrate and tube diameter on bend losses are

contradictory to those required for efficient horizontal transport. For a given

tube diameter, higher flowrates result in higher horizontal transport efficiency but

lower transport efficiency around the bend. Conversely, lower flowrates

minimize bend losses but maximize losses in the probe's horizontal section.

Combined losses within these two sections are thus relatively independent of

sampling flowrate. The magnitude of these losses depends primarily on

aerodynamic particle size.

Particle losses within the probe's final 8 inch long vertical section are

predicted to be minimal. Since the tube is oriented vertically, no horizontal

deposition is possible. Operation of the probe in the laminar flow regime also

eliminates the possibility of turbulent deposition which can be significant for

particles with high Stokes numbers in turbulent flow fields. This prediction of

low particle losses in this section is supported by the low impactor inlet losses

measured during the impactor's laboratory calibration.

It can be concluded, therefore, that use of the proposed sampling nozzle

and probe may not allow efficient transport of large particles to the lead-in-air

monitor's collection and analysis section. Combined losses within the nozzle,

nozzle outlet, and sampling probe may be prohibitively high. It should be









noted, however, that these loss calculations may significantly overestimate

particle losses. Theoretical loss calculations normally assume that when a

particle contacts a surface, it is removed from the airstream. Use of liquid

aerosols during experimental loss tests would support these calculations. In

reality, solid particles contacting solid surfaces at high velocity may experience

only fractional sticking efficiencies. Reentrainment of deposited particles also

results in higher particle transport efficiency.

It is apparent that special sampling considerations may need to be given

to the on-line measurement of ducted airstreams in the battery industry.

Conventional stack sampling techniques and equipment may not enable

representative sampling and transport of these large aerosols. As possible

alternatives, three sampling approaches could be investigated. First, the

ductwork at the monitoring point of interest could be modified to include a short

vertical section so that the entire flow is directed downward. A sharp-edged

sampling nozzle attached vertically to the lead-in-air monitor could then

isokinetically extract a representative sample with minimal inlet and transport

losses. Alternatively, a small flexible test section attached to a high volume

vacuum source could isokinetically extract a portion of the major duct flow and

direct this secondary airstream downward over the monitor's sampling nozzle.

Aerosol not sampled by the monitor could then be returned to the major

airstream or filtered prior to its exhaust to the atmosphere. This concept is

similar is design by Baron (1988) and Ball and Mitchell (1990) for efficient









transport of coarse aerosols to particle sizing instrumentation. As a final

alternative, the conventional sampling nozzle could be replaced with a

precollector designed to remove all particles greater than 10 micrometers

aerodynamic diameter. The remaining fraction could then be transported

efficiently to the monitor's collection section. In the human respiratory tract,

particles less than 10 micrometers represent the size fraction capable of

penetrating to the alveolar region and thus represent the best measure of the

actual lead exposure hazard. Particles larger than 10 micrometers are

deposited in the upper regions of the respiratory tract and are absorbed in the

bloodstream with much lower efficiency. Recent developments in

10 micrometer size selective inlets indicate that this design approach is feasible.

Use of a precollector to evaluate worker exposure, however, must first meet

with approval by the Occupational Health and Safety Administration.












CHAPTER 5
DESIGN OF LEAD ANALYSIS SECTION


Introduction


As discussed, accurate evaluation of lead-in-air concentrations requires

efficient aerosol sampling, transport, collection, and accurate analysis of the

collected aerosol's lead content. Previous sections have outlined the

techniques required to ensure representative aerosol sampling, transport, and

collection. This chapter will outline design criteria for the lead analysis

section, briefly review available analytical techniques, and describe in detail the

analytical technique chosen for incorporation into the lead-in-air monitor.


Design Criteria


Selection of the instrument's lead analysis technique was based on

careful consideration of several design criteria. First, the technique must be

specific for elemental lead and capable of accurately quantifying lead

concentrations ranging from 50 ppb to 9000 ppb. It was desired that the

technique's response be fairly linear over a wide range of concentrations and

the technique display adequate repeatability. Because the collected aerosol

sample's composition is not entirely lead, the analytical technique should









possess minimal physical and chemical interference from these other

components. The technique must also be physically compatible with the

chosen particle collection substrate. It was important that the selected

analytical technique require little periodic maintenance or recalibration. Finally,

the selected technique must meet cost requirements and be adaptable to

convenient automation.

Based on these criteria, a thorough review of pertinent literature was

made with regard to selection of the instrument's analytical technique. There

exist a wide variety of analytical techniques available for the quantitation of lead

either in solid or liquid phase. These techniques include both conventional and

graphite furnace atomic absorption spectroscopy, ion chromatography,

inductively coupled argon plasma spectroscopy, x-ray and electron techniques,

colorimetry, neutron activation analysis, and electrochemical techniques. For an

automated device, most of these techniques were eliminated from consideration

either due to their high cost, level of complexity, inadequate lead detection

capabilities, or failure to adapt themselves to convenient automation. For

example, conventional atomic absorption is incapable of detecting sub-ppm

levels of lead in solution. Although graphite furnace atomic absorption

possesses the necessary detection capabilities, its use would have greatly

increased the complexity and cost requirements of the monitor. In addition, the

response of both conventional and graphite furnace atomic absorption displays

a fairly limited range of linearity. Other techniques such as colorimetry involve a









number of chemical handling steps which would have been inconvenient to

automate.

Ultimately, an electrochemical method of lead analysis was regarded as

most appropriate for the lead analysis. Because metals display high

electroactivity, their presence is solution can be detected over a wide range of

concentrations. Electrochemical techniques display high linearity and

repeatability. In particular, the electrochemical technique of polarography was

selected as that which best met the outlined design criteria. In forthcoming

sections, the principle of polarography will be reviewed and its application to

lead-in-air monitor described.


Description of Polarographic Analysis


Electrochemical analysis is based on the observed behavior of

electroactive species in solution when subjected to an electric potential gradient.

For the detection of a particular species of interest (such as metals), a varying

potential is applied to the solution through a conductive electrode. If at a

particular potential a species is oxidized or reduced, an electric current will flow

at the electrode. Since the rate of electron transfer is a function of the number

of redox reactions occurring at a given potential, the measured current

produced is proportional to the concentration of that component in solution.

Because electroactive species display characteristic redox potentials, the

observed potential at which the redox reaction occurs can be used to identify







73
the component of interest. By applying a range of potentials to a sample and

noting the potential and resulting current of several redox reactions,

simultaneous quantitation of several solution components is possible. This

analytical technique is commonly referred to as voltametry.

Although the study of voltametry is not new, recent advances have led to

the development of reliable, commercially available instruments suitable for trace

metal detection. Current designs now incorporate mercury drops as the active

working electrode surface. Since a fresh mercury drop is produced for each

separate sample analysis, carry over contamination of the working electrode is

virtually eliminated. Recent advances in microprocessor technology have also

led to increasing measurement sensitivity and instrument capabilities.

Commercially available analyzers allow the user to select from various applied

potential waveforms which optimize detection of the component of interest. For

many metals (including lead) part per billion detection capability is routine.

Based on a review of available electrochemical detectors, an EG&G

Model 303A static mercury drop electrode was purchased along with an

accompanying Model 264A control unit. The Model 303A contains a mercury-

based working electrode, a silver/silver chloride reference electrode, and a

platinum counter electrode which are all immersed in a static cell containing the

solution of interest. The Model 303A also contains a 5 Ib capacity mercury

reservoir and a delivery system for dispensing individual mercury drops of

repeatable size.









Control of the Model 303A electrode system is provided through

communication with the Model 264A control unit. The Model 264A sets the

Model 303A operating parameters, provides for automatic sequencing of the

analysis steps, receives and conditions the resulting output signals, and

communicates the current versus voltage scan results to an x-y recorder. The

user is able to select from a variety of a scan types including normal direct

current, normal pulse, and differential pulse polarography as well as direct

current and differential pulse stripping analysis. Although these techniques

possess varying degrees of capabilities and applications, differential pulse

stripping analysis provides for the most sensitive detection of lead in solution.

This mode, therefore, is used exclusively for lead quantitation in the lead-in-air

monitor.

Quantitation of lead in solution by stripping analysis typically involves the

following sequence of steps. First, high purity nitrogen is bubbled through the

liquid sample at a flowrate of approximately 40 cc per minute for approximately

3 minutes. This deaeration step removes the electroactive interference of any

dissolved oxygen in the solution. The Model 303A then dispenses a single

mercury drop of selectable size which hangs on the tip of a glass capillary

immersed in the solution. A constant electric potential is applied to the mercury

drop whose magnitude is more negative than the half-wave potential of the

analyte of interest. This results in a electro-reduction of the analyte onto the

surface of the mercury drop. To ensure repeatable mass transfer rates during









this step, the solution is stirred and deposition is performed for a fixed time

period (such as 3 minutes). The preconcentration step is responsible for the

technique's low detection limit for many electroactive species.

At the conclusion of the deposition step, the stirrer is turned off and the

electroactive species is stripped from the electrode by making the electrode

more positive and oxidizing the species back into solution. In this stripping

step, varying the potential at a constant rate (such as 10 mV/sec) allow

different species to oxidize at different times. In differential pulse stripping

analysis, the current measured during each species' oxidation reaches a

maximum value that is proportional to the concentration of each species that

was deposited.

As an example, Figure 5-1 presents the results of a typical analysis of

40 ppm lead, cadmium, and copper standards in 0.1N nitric acid. The position

of the peaks (with potentials referenced to the Ag/AgCI electrode) identifies the

species present in solution and the peak height for each species is proportional

to its concentration in solution.

To ensure reliable test results of trace metal analysis, special

experimental techniques were observed during all polarographic analyses. To

minimize sample contamination and species absorption losses, all polarographic

cells were made of teflon and were acid washed with 6M nitric acid prior to use.

Metal standards were prepared from 1000 ppm stock metal standards certified

by the manufacturer to within 1% accuracy. Serial dilutions were performed








76


z
z
00 d



8.
co '




00

C)
o o
S-o.


o *0

I n I


> S


o C .
o c a
0 0 > I
Q I- I-- I cI S



-4-J








(V 90-30 L) -ua-0in
0..
CD
0.
I-





I-









using positive displacement pipettes with disposable tips rated to within 2%

accuracy. Dilute nitric acid solutions were prepared using trace metal grade

concentrated nitric acid diluted with distilled, deionized water with a measured

resistivity of 17 x 106 ohm-cm. Only certified, triple distilled mercury and ultra-

high purity nitrogen were used in the polarograph.

If polarographic stripping analyses are performed under carefully

controlled conditions, repeatable test results can be obtained over a wide range

of concentrations. Figure 5-2 presents the instrument's response as a function

of lead concentration in 0.1N nitric acid. Each data point represents the

average of 6 separate tests performed under identical test conditions. The

technique's precision (as expressed by the relative standard deviation) was

measured to be approximately 2%.

Considerable attention was devoted to identification and subsequent

optimization of the parameters which affect the polarographic's response to

trace lead concentrations in solution. Factors affecting the deposition step were

identified to be initial deposition potential, mercury drop size, deposition time,

and solution stirring dynamics. The instrument's response during the stripping

phase was found to vary with the potential's rate of change (scan rate) and the

height of the differential wave applied to achieve oxidation. The overall

response was also found to vary with the condition of the Ag/AgCL reference

electrode, solution temperature, and the concentration of the nitric acid solution

used.















O
-0
\40)

C
o





0 c
\o -.



00 0



C
0




\.o c


\ 0
o





u CC
\0
o c c


co c
S0


\o 2

\ a ,1


00 .2
\ ^--




o
C, 2o o
o o c a,







79
Within limits, these variables can be controlled by proper selection of the

polarograph's operating parameters. However, complete control of all of these

variables in an automated monitor is impractical to achieve. In stripping

analysis, the instrument's response to a given lead standard was noted to vary

as much as 50% during successive test series. Ultimately, this variability was

virtually eliminated by including an internal standard (200 ppb copper) in the

nitric acid electrolyte.

Use of the internal copper standard was developed based on numerous

observations of the polarograph's response to several species in solution.

During the analysis of equal mass concentrations of lead, copper, and

cadmium, it was noted that the ratios of the resulting peak heights were

essentially constant regardless of the operating parameters of the instrument.

For example, although reducing the deposition time during stripping analysis

reduced the magnitude of each element's peak, the respective peak ratios

remained essentially constant. Similar behavior was noted by changing the

mercury drop size, nitric acid concentration, analysis scan rate, solution

temperature, and solution stirring dynamics. Thus, if the instrument response to

a known concentration of an analyte is measured, the concentration of a

different species can be calculated from its observed peak height and the

known peak ratio. During the course of the project, the instrument's response

to equal lead and copper concentrations was measured as a function of

concentration and instrument's operating parameters. For 156 separate









measurements, the ratio of the copper to lead peak height was measured to

average 2.33 with a relative standard deviation of 1.8%. Assuming the use of a

200 ppb copper internal standard, the concentration of lead in solution can thus

be calculated using the following relationship


Lead Cone. (ppb) = Lead Peak Height X 2.33 X 200 ppb
Copper Peak Height (5-1)


Use of an internal standard in the lead-in-air monitor offers several

advantages. First, the need for periodic calibration of the analytical section is

eliminated since the instrument essentially calibrates itself during each sample

analysis. Analytical accuracy is no longer sensitive to variables which would be

difficult to control within required limits. Lastly, use of the internal copper

standard provides an internal quality control check during each analysis. If the

instrument's response to the copper standard is outside the expected range, it

serves as an indication that either the electrolyte was prepared incorrectly or

that a possible instrument malfunction may exist.

To determine the value of this design approach, lead standards of

concentrations ranging from 0 to 8000 ppb were prepared in 0.5M nitric acid

with a 200 ppb copper internal standard. The instrument's response to these

solutions was then measured and Equation 5-1 used to predict the actual lead

concentration. For each concentration, six separate measurements were

performed under identical test conditions. Figure 5-3 presents the results of the

0 to 200 ppb lead measurements in comparison to the instrument's ideal











































50 100 150 200


Actual Lead Conc.


(ppb)


Figure 5-3. Polarograph response to 0-200 ppb lead concentration using
200 ppb internal copper standard.


200


-D



C
0


O




L-

CD
(,


150





100





50





0







82

response. It can be seen that agreement between the measured and ideal lead

concentration is quite good for lead concentrations greater than or equal to

approximately 20 ppb. The observed response at 0 ppb is due to the presence

of hydronium ions in solution which provide a residual current overlapping the

position of the lead peak. At a 0 ppb lead concentration this interference

typically provides a calculated lead concentration of 5 to 15 ppb. For lead

concentration above 20 ppb, however, the contribution of the hydronium ions is

insignificant. A minimum quantitation limit of 20 ppb lead is thus reported for

the monitor's analytical section.

Figure 5-4 presents the results of the 0 to 8000 ppb lead response tests.

Note that use of the internal copper standard is accurate even over this wide

range of concentrations. A summary of these test results is tabulated in

Table 5-1 including the technique's precision as expressed by the relative

standard deviation. For lead concentrations ranging from 20 ppb to 8000 ppb,

the precision was calculated to be approximately 2%.


Analysis of Field Bulk Samples


In any quantitative chemical analysis, it is important to ensure that the

analytical technique chosen be compatible with the sample to be analyzed.

Physical and chemical interference associated with the sample's measurement

should be noted and effort made to minimize them in order to achieve reliable

test results. In the case of the lead-in-air monitor, it was important to ensure

















8000


7000 Measure
Ideal
6000


5000


4000


3000


2000


1000


0
0 1000 2000


Actual


3000 4000 5000 6000 7000 8000


Lead Conc. (ppb)


Figure 5-4. Polarograph response to 0-8000 ppb lead concentration using
200 ppb internal copper standard.


-0
0Q

CQ
0
0
cO


0
a)
-a


L.
3
W





0
c(
















Table 5-1
Polaroaraph Response Using Copper Internal Standard


Actual Lead Conc. (DDb)


0

5

10

20

40

80

200

400

800

1600

4000

8000


Polarograph Response
Lead Conc. (ppb) RSD(o%)


9

9

12

22

41

81

197

389

783

1546

4037

7900









that the expected aerosol's composition be compatible with polarographic

analysis.

During battery manufacturing, airborne particles are produced primarily

by mechanical breakup (dispersion) of lead oxide powder, lead oxide paste,

and the lead-based plate material. It can thus be expected that the chemical

composition of the aerosol produced from these materials is virtually identical to

that of its parent material. Bulk samples of lead oxide powder, paste, and plate

material were obtained at the battery plant and returned to the laboratory for

analysis in order to identify any potential analytical interference.

During these tests, a known mass of each material was dissolved in nitric

acid solution and analyzed using the polarograph. For comparison purposes,

these samples were also analyzed using a graphite furnace atomic absorption

(GFAA) spectrophotometer manufactured by Perkin-Elmer (Model 5100). The

GFAA is more widely used for trace metal analysis than the polarograph and

thus represents an accepted criterion upon which to base the polarograph's

accuracy. For each test series, the GFAA was calibrated for lead

concentrations in its linear operating range of 0 to 40 ppb by autodilution of a

100 ppb lead stock standard solution. For comparison purposes, the diluent

consisted of 0.5M nitric acid with a 200 ppb copper internal standard. To

minimize matrix effects associated with lead measurement by GFAA analysis, a

fixed quantity of a matrix modifier (0.2 mg NH4H20PO4 + 0.01 mg Mg(NO3)

was injected with each 5 pl sample.









The results of these comparison tests are presented in Table 5-2.

Analysis was first performed on certified laboratory samples of lead nitrate, lead

monoxide, and lead acetate. Based on the known formula weights of these

materials, each sample was prepared to obtain an expected lead concentration

of 100 ppb. As shown in Table 5-2, both the polarograph and the GFAA

measured these solutions with reasonable accuracy. Based on the three

replicate analyses for each material, the polarograph displayed somewhat better

repeatability than did the GFAA.

Similar solutions were prepared from the bulk materials collected at the

battery plant. Although the lead content of the lead monoxide powder can be

assumed with some confidence, its actual percentage in the lead paste can only

be estimated based on discussions with the battery plant personnel. Results

shown in Table 5-2 generally verified these estimates. Similar to the analysis of

the certified laboratory samples, these results indicated fairly good agreement

between the polarograph and the GFAA. More important, no interference was

observed during the polarographic analysis of these battery plant samples. It

was concluded, therefore, that no interference can be expected during analysis

of any airborne particles produced from these bulk materials.




Full Text
DEVELOPMENT OF A MONITOR TO QUANTIFY LEAD-BASED AEROSOLS
By
ROBERT WILLIAM VANDERPOOL
A DISSERTATION PRESENTED TO THE GRADUATE SCHOOL
OF THE UNIVERSITY OF FLORIDA IN PARTIAL FULFILLMENT
OF THE REQUIREMENTS FOR THE DEGREE OF
DOCTOR OF PHILOSOPHY
UNIVERSITY OF FLORIDA
1991

This dissertation is dedicated to the memory of my parents.

ACKNOWLEDGEMENTS
I would first like to thank Ken Reed for his assistance in machining
several pieces of the experimental apparatus. His expertise is most
appreciated.
The useful discussions with John Applewhite concerning the capabilities
and limitations of the polarograph are appreciated.
I would also like to acknowledge the assistance of Tom Peters during the
field evaluation of the prototype monitor. The successful demonstration of the
instrument’s capabilities would not have been possible without his effort.
I also wish to thank the members of my doctoral committee for their time
and effort required to serve in this capacity. Each member, in his own way, has
served as a source of inspiration during the course of my studies at the
University of Florida. I am particularly appreciative of Dr. Lundgren for his
guidance, encouragement, and confidence. He has provided me with
opportunities for laboratory, teaching, and field experience that contributed
greatly to my professional development.
Finally, I would like to thank my wife, P.J., for her patience and support
during the last three years.
iii

TABLE OF CONTENTS
ACKNOWLEDGEMENTS iii
LIST OF TABLES vi
LIST OF FIGURES viii
KEY TO SYMBOLS xi
ABSTRACT xiii
CHAPTERS
1 INTRODUCTION 1
Background 1
Description of Battery Production Process 3
Instrument Design Criteria 6
Summary of Design Approach 8
2 REVIEW OF LITERATURE 13
3 DESIGN AND CALIBRATION OF PARTICLE COLLECTION SECTION 19
Design Theory 19
Prediction of Impactor Performance 27
Calibration of the Particle Collection Section 33
4 DESIGN OF AIR SAMPLING SYSTEM 44
Introduction 44
Description of Air Sampling System 44
Prediction of Particle Sampling and Transport
Efficiency 56
iv

5 DESCRIPTION OF LEAD ANALYSIS SYSTEM 70
Introduction 70
Design Criteria 70
Description of Polarographic Analysis 72
Analysis of Field Bulk Samples 82
Description of Modifications to the Polarograph 88
6 DESCRIPTION OF FLUID HANDLING SYSTEM 110
7 PROGRAM DESCRIPTION AND OPERATION 124
8 FIELD EVALUATION OF PROTOTYPE INSTRUMENT 132
Introduction 132
Experimental Methods 132
Experimental Results 139
9 SUMMARY AND RECOMMENDATIONS 151
APPENDICES
A IMPACTOR DESIGN DRAWINGS 155
B IMPACTOR CALIBRATION RESULTS 160
C CONFIGURATION OF KIETHLEY 575 CHANNELS 162
D LISTING OF PROGRAM 165
E OPERATING MANUAL FOR THE LEAD-IN-AIR MONITOR 185
REFERENCE LIST 223
BIOGRAPHICAL SKETCH 225
v

LIST OF TABLES
Table 3-1 Predicted Operating Characteristics of Teflon
Impactor 28
Table 4-1 Description of Module 1 Air Flow Components 46
Table 4-2 Description of Module 2 Air Flow Components 50
Table 4-3 Module 2 Electrical Component Listing and
Description 54
Table 4-4 Module 2 Electrical Connector Pin Descriptions 55
Table 5-1 Polarograph Response Using Copper Internal
Standard 84
Table 5-2 Comparison Tests Between Polarograph and GFAA . . 87
Table 5-3 Component Listing and Description of RUN/STOP
Board 91
Table 5-4 RUN/STOP Board Connector Pin Functions 92
Table 5-5 Component Listing and Description of PCM3 Board . . 94
Table 5-6 Description of Various PCM3 Channels 95
Table 5-7 Component Listing and Description of Decade
Resistance Board 98
Table 5-8 Decade Resistance Board Connector Pin Functions . . 99
Table 5-9 Component Listing and Description of Model 264A ... 102
Table 5-10 Model 264A Connector Pin Descriptions 103
vi

Table 5-11 Component Listing and Description of Digital
Board 106
Table 5-12 Digital Logic Board Connector Pin Descriptions 107
Table 6-1 Listing and Description of Liquid Handling
Components 112
Table 6-2 Listing and Description of Nitrogen Handling
Handling Components 120
Table 6-3 Module 1 Electrical Component Listing and
Description 122
Table 6-4 Module 1 Electrical Connector Pin Descriptions 123
Table 8-1 Analysis of Laboratory Lead Standards 140
Table 8-2 Analysis of Field Control Lead Standards 141
Table 8-3 Results of Collocated Sampling Performed at Plate
Offbearing Operation 143
Table 8-4 Results of Unattended Sampling Performed at Plate
Offbearing Operation 145
Table 8-5 Results of Collocated Sampling Performed at Paste
Drying Operation 146
Table 8-6 Results of Unattended Sampling Performed at Paste
Drying Operation 147
Table 8-7 Results of Collocated Sampling Performed at Plate
Stacking Operation 149
vii

LIST OF FIGURES
Figure 1-1 Flow chart of lead-acid battery production
process 4
Figure 1-2 Summary of prototype lead-in-air monitor design
approach 11
Figure 3-1 Measured particle size distributions at a
battery plant 21
Figure 3-2 Schematic of single-stage impactor used for
particle collection 26
Figure 3-3 Schematic of generation system used for production
of calibration aerosols greater than 0.5 micrometers
aerodynamic diameter 35
Figure 3-4 Scanning electron photomicrograph of ammonium
fluorescein calibration aerosols produced by VOAG . 36
Figure 3-5 Schematic of generation system used for production
of calibration aerosols less than 0.5 micrometers
aerodynamic diameter 38
Figure 3-6 Measured particle size collection efficiency curves
for single stage impactor 41
Figure 4-1 Schematic of Module 1 air flow system 45
Figure 4-2 Schematic of Module 2 air flow system 49
Figure 4-3 Wiring diagram of Module 2 electrical components ... 53
Figure 4-4 Measured performance of Module 2 mass flow
controller 57
viii

Figure 4-5 Theoretical particle transport efficiency through the
sampling probe’s horizontal section 64
Figure 4-6 Theoretical particle transport efficiency through the
probe’s 90° bend 66
Figure 5-1 Polarographic response to 40 ppm concentrations of
lead, cadmium, and copper in 0.1 N HN03 76
Figure 5-2 Typical polarographic response as a function of lead
concentration 78
Figure 5-3 Polarographic response to 0-200 ppb lead
concentration using 200 ppb internal copper standard 81
Figure 5-4 Polarographic response to 0-8000 ppb lead
concentration using 200 ppb internal copper standard 83
Figure 5-5 Schematic of printed circuit board which provides
run/stop functions 89
Figure 5-6 Wiring diagram of Keithley PCM3 power control module 93
Figure 5-7 Schematic of printed circuit board which provides
decade resistance ranging functions 97
Figure 5-8 Schematic of Model 264A showing recommended
locations for auxiliary circuit boards 101
Figure 5-9 Schematic of printed circuit board which provides
logical switching of stir, purge, and drop
dispense/dislodge functions 105
Figure 6-1 Schematic of Module 1 liquid handling system 111
Figure 6-2 Detail drawing of flow-through cell designed for the
polarograph 116
Figure 6-3 Schematic of Module 1 nitrogen handling system .... 119
Figure 6-4 Wiring diagram of Module 1 electrical components ... 121
ix

Figure 8-1 Photograph of lead-in-air monitor during tests
conducted at plate offbearing process 136
Figure 8-2 Photograph of Module 1 inlet section showing position
of collocated filter holder relative to Module 1
inlet 137
X

KEY TO SYMBOLS
C - particle concentration
Cs - slip correction factor
D - particle diffusion coefficient
DpgQ - impactor cutpoint
Dt - tube diameter
g - gravitational constant
L - tube length
M - gas molecular weight
n - number of impaction jets
P - fractional penetration
Ps - stack pressure
Q - volumetric flowrate
R - bubble radius
STK - particle Stokes number
T - gas temperature
V - gas velocity
Vb - bubble velocity
Vp - gas velocity pressure
xi

Vs - particle settling velocity
W - jet width
ad - coefficient of diffusional deposition
a¡ - coefficient of inertial deposition
as - coefficient of gravitational deposition
Pp - gas density
/l/ - gas dynamic viscosity
t - particle relaxation time
xii

Abstract of Dissertation Presented to the Graduate School
of the University of Florida in Partial Fulfillment of the
Requirements for the Degree of Doctor of Philosophy
DEVELOPMENT OF A MONITOR TO QUANTIFY LEAD-BASED AEROSOLS
By
Robert William Vanderpool
December 1991
Chairperson: Dale A. Lundgren
Major Department: Environmental Engineering Sciences
Manufacture of lead-acid batteries results in the advertent formation of
gas-borne particles containing lead. Since the adverse health effects of
significant lead exposure are well documented, the battery industry is required
to undergo periodic monitoring to demonstrate compliance with existing lead-in¬
air regulations.
A prototype instrument has been developed to quantify lead-based
particulates on a near real-time basis. Aerosol samples can be obtained from
high velocity, flowing airstreams as well as from static airstreams. The
instrument thus has potential as an emissions monitor, a recirculation air
monitor, or a monitor of workplace environments. The prototype instrument
contains an air sampling and transport system, a particle collection section, and
xiii

a lead analysis section. Proper sequencing of the system’s components and
archival of the experimental test results are provided by an IBM-compatible
computer interfaced with a data acquisition and control system. The prototype
monitor may be operated either in attended or automated sampling and
analysis mode. The details of the instrument design will be presented along
with results of its laboratory and field evaluation.
XIV

CHAPTER 1
INTRODUCTION
Background
Industrial manufacturing processes often result in the formation of gas-
borne particles (aerosols) containing hazardous metals such as lead, cadmium,
and copper. Since the adverse environmental and occupational health effects
of these substances are well documented, periodic air monitoring of
manufacturing processes involving their use is required to demonstrate
compliance with existing federal and local regulations.
The lead acid battery industry, which accounts for 72% of all domestic
lead usage (Environmental Protection Agency, 1986), is a potential source of
significant lead-based aerosol production. Monitoring of lead emissions in the
battery industry typically requires a separate aerosol sampling and analysis
technique. First, a representative aerosol sample is obtained from the process
using approved sampling techniques. This procedure typically involves aerosol
collection through a high efficiency filter to remove particles from the airstream.
The collected aerosol sample must then be extracted from the collection
substrate and analyzed using an appropriate analytical technique. However, the
time delay between sample collection and analysis is typically on the order of
1

2
days to weeks. Moreover, improper handling and extraction of the collected
sample can result in significant errors in estimation of the total lead
concentration. Positive sample bias is a particular problem during
measurement of trace lead levels common during evaluation of occupational or
recirculation air monitoring. Finally, specially approved equipment, sampling
and analysis techniques, and trained personnel are necessary to achieve
accurate results. The need existed, therefore, for an instrument capable of
providing both aerosol sampling and analysis of lead-based particles on a near
real-time basis.
The advantages of an automated air sampling and analysis instrument for
lead measurement tests are obvious. Such a device could be used both for
occupational and emission measurements and would significantly reduce the
cost of each test. Such an instrument would report test results within minutes
of the air sampling. Finally, by proper design and construction of the
instrument, the sources of measurement error inherent to the current
methodology could be significantly reduced. Compliance with existing emission
and occupational regulations could be routinely demonstrated. This report
details the design, construction, calibration, and field evaluation of such an
instrument designed for use by the lead-acid battery industry.

3
Description of Battery Production Process
The design criteria for the lead-in-air monitor was based on careful review
of the various operations involved in the manufacture of lead-acid batteries. Of
particular importance was consideration of the concentration, size distribution,
and chemical composition of the lead-based aerosols produced at each of the
process points. Figure 1-1 is a flow chart of the various operations involved in
the battery production. Not shown in the figure are various paths involving the
reclaim and reuse of lead scrap which occurs at several of the process points.
Battery manufacture first begins with the production of lead monoxide
powder by grinding solid lead metal in the presence of air at elevated
temperatures. Lead oxide paste is then produced by combining the lead oxide
powder with water and dilute sulfuric acid along with small amounts of
proprietary materials.
Battery plate grids are cast from molten lead-based alloys which consist
primarily of lead but also contain various trace metals to improve the plate’s
mechanical properties. Following a specified curing time, the grids are
transported to the pasting operation where they are pasted and flash dried prior
to being off-loaded from the assembly line. The pasted plates undergo another
curing process before use. Plate stacking then occurs which involves alternate
stacking of plates with paper separators. The stacked plates are then loaded
into plastic cases and the appropriate cells connected together during the cast-
on-strap operation. The case cover is then installed, cells filled with sulfuric

Lead Oxide
Production
Figure 1-1. Flow chart of lead-acid battery production process.

5
acid, and the batteries electrically charged prior to the packaging and shipping
operation.
The characteristics of the lead-based aerosol produced at each step of
the production process depends primarily on the composition of the material
handled and the mechanism by which the aerosol is produced. The aerosol
produced during the grid casting operation tends to be relatively small in size
and may contain only 5% to 20% lead by mass. Lead mass concentrations of
aerosol produced at the grid casting operation typically meet allowable emission
limits and are therefore ducted to the environment without the need for any
control measures.
Conversely, production and handling of lead oxide powder, paste and
pasted plates tends to form dispersion-type aerosols relatively large in diameter
and contain 95% to 99% lead by mass. Aerosols from these processes also
tend to be of much higher lead mass concentrations and are therefore ducted
to control equipment (typically baghouses) prior to the airstream’s exhaust to
the environment.
With the exception of the acid fill, charging and packaging operations, all
the steps in the battery production process are sources of elevated lead
exposure to the battery plant workers. These processes, therefore, all possess
ventilation systems designed to remove the majority of the lead-based aerosols
and transport them to the particulate control equipment. Since these airstreams
are ultimately exhausted to the environment, an equivalent supply of makeup air

6
is required to maintain a flow balance. Battery plants in colder climates have
incorporated recirculation air systems to reduce heating costs associated with
heating the makeup air to plant temperature. This recirculation air is typically
obtained from grid pasting, drying, plate offbearing, cast-on-strap, and plate
stacking operations and is cleaned through a system of two high efficiency
particulate air filters (HEPA) in series with one another. This clean recirculation
air is then supplied to various process points as a source of makeup air.
The Occupational Safety and Health Administration has approved use of
this type of recirculation air system but requires continuous monitoring of the
recirculation air to ensure that the airborne lead content not exceed the
regulated 50 micrograms/m3 permissible exposure limit concentration.
Experience has shown that if the double HEPA filter system is installed and
maintained correctly, concentrations much lower than 5 micrograms/m3 can be
routinely obtained.
It is primarily for the purpose of monitoring recirculation air quality that
the lead-in-air monitor was developed. Other potential applications to the
battery industry will be discussed.
Instrument Pesian Criteria
The development of a lead-in-air monitor must be based on the sampling
and analysis requirements specific to the lead-acid battery industry. First, the
instrument must be capable of obtaining representative aerosol samples from

7
both flowing airstreams (stack or duct sampling) as well as from static
airstreams (room sampling). Particle size distribution measurements have
shown that efficient particle collection must take place over a fairly wide range
of particle sizes.
Accurate quantitation of the particulate lead content is also essential.
The analytical technique chosen must be specific for elemental lead and
possess minimum physical and chemical interferences from other particulate
and gaseous components. Analytical accuracy and repeatability must exist over
the measurement range of interest. The analytical technique must possess low
blank and background response for the lead measurement.
Sampling should be performed over a 10 to 20 minute time period.
Instantaneous measurements are neither technologically feasible nor particularly
desirable because variations in lead handling processes and activities result in
considerable concentration variability with time. Time averaged measurements,
therefore, are more appropriate indicators of average process emissions. In
conjunction with a 15 minute analysis time, a 15 minute air sampling period
would allow a complete sampling and analysis cycle to be repeated
approximately every 30 minutes.
The instrument must also be capable of quantifying lead levels over a
wide range of concentrations. These concentrations range from recirculation
system alarm levels of 10 micrograms/m3 to levels of greater than
1000 micrograms/m3 for emissions from paste mixing facilities and other three-
part operations.

8
Instrument reliability and ease of use was also a design consideration.
Cleaning, maintenance, and external calibration of the instrument should be
minimized. The working instrument must be at least semi-automated, fairly
portable, and operate on standard 110 VAC, 60 hz power sources.
Finally, it was desired that the instrument’s development and construction
costs be kept to a minimum. Once a final instrument design had been
completed and its capability demonstrated, it was desired that duplication costs
be limited to approximately $10,000.
Summary of Desion Approach
Development of an automated sampling instrument for the specific
quantitation of lead involved careful consideration of the design criteria outlined
in the previous section. Ideally, the developed instrument would satisfy all of
the listed criteria although certain design and operational tradeoffs could have
been made if necessary. Of primary concern, however, was the instrument’s
ability to obtain representative particulate samples from particle-laden airstreams
and accurately quantify lead levels over a reasonable concentration range.
Design of the instrument can be conveniently divided into three separate
sections: the air sampling system, the particulate sampling system, and the lead
analysis system. The sampling system must efficiently capture particles over a
range of sizes and effectively deliver them to the lead analysis section.
Representative sampling in flowing airstreams requires that isokinetic conditions

9
be achieved (nozzle velocity equal to freestream velocity) through proper
combination of nozzle inlet area and sampling flowrate. It was envisioned that
the sampling system contain several nozzles of varying inlet areas in
conjunction with a 60 to 90 liter per minute (Ipm) capacity sampling pump
whose sampling rate could be controlled and monitored by the user. The range
of operating flowrates was selected to be 10 to 30 Ipm. Following consideration
of available particle collection techniques (filtration, electrostatics, etc.), inertial
impaction was chosen as the mechanism to be employed in the instrument’s
particle collection section. Subsequent calibration of the impactor showed that
it would collect 95% to 100% of the lead-based particles present in the in-plant
processes of interest.
Design of the instrument’s analytical section required careful
consideration of its specific operating requirements. Of primary concern was
the ability to accurately quantify collected lead in amounts which were expected
at the various in-plant operations. Considering a 15 minute sampling time and
a nominal 15 Ipm sampling flowrate, approximately 0.23 m3 of air would be
sampled. For expected concentrations ranging from 10 micrograms/m3 to
2000 micrograms/m3 at the various in-plant processes, lead deposits of
2.3 micrograms to 460 micrograms would result. If these deposits were placed
in liquid solution (50 ml, for example), lead concentrations of 46 micrograms per
liter (ppb) to 9 milligrams per liter (ppm) by mass would be expected.
A wide variety of analytical techniques was considered during design of
the instrument’s analytical section. Most of these techniques were eliminated

10
from consideration either due to their high cost, level of complexity, lead
detection capability, or failure to lend themselves to convenient automation.
Ultimately, an electrochemical technique was chosen for the quantitation of lead
in liquid solution. A commercially available polarograph was purchased and
adapted for automation.
A schematic of the completed instrument is shown in Figure 1 -2. Air flow
through the system’s particle collection section is provided by a 90 Ipm capacity
air pump with flow controlled and monitored using a commercially available
mass flow controller. Deposition of the lead-based particles takes place
primarily by inertial impaction into 50 ml of 0.5M nitric acid which is supplied
from a 5 liter capacity reservoir. Following a sufficient sampling time, an aliquot
of the solution is transferred to a flow-through cell in the polarograph for lead
analysis. The lead-in-air concentration can then be calculated from the
sampling time, sampling flowrate, solution volume, and the measured liquid lead
concentration.
Automated control of the system’s components takes place using a data
acquisition and control system (Kiethley Instruments, Inc., Model 575) interfaced
with an IBM-compatible computer. Computer control not only allows for proper
sequencing of the various components but also allows for data reduction and
automatic storage and retrieval of the test results. The Keithley 575 data
acquisition and control system receives necessary power from the computer
and provides both digital and analog input/output capabilities. A Keithley Model
AMM1 analog measurement module provides eight separate analog input

To Waste System
Figure 1-2. Summary of prototype lead-in-air monitor design approach.

12
channels with a range of ±10V, an input rate of 50 khz, and 12 bit
measurement resolution. The Kiethley 575 contains two analog output channels
with similar capabilities. At power up, the Model 575 self-calibrates the analog
channels with an accuracy of ±2%.
Digital control is provided by 32 digital input/output channels with signals
which are transistor-to-transistor (TTL) compatible. A separate 16 channel
module (Kiethley, Model PCM3) provides external AC or DC power control
using TTL activated solid-state relays.
In the 575 system, the user can access the various module channels
using Kiethley KDAC500/I software linked with a GW-BASIC programming
environment. Use of programming logic rather than hard-wired logic allowed
for design flexibility during development of the prototype system.

CHAPTER 2
LITERATURE REVIEW
Design of the proposed lead-in-air monitor was based on a number of
important criteria. The instrument must capture airborne particles in a
representative manner and transfer them effectively to the instrument’s lead
analysis section. The analytical technique chosen must be specific for
elemental lead and yield a response that is linearly proportional to mass
concentration. Analytical accuracy and repeatability must exist over the
measurement range of interest and possess minimal interference from the
collection substrate and other particle components.
During the last two decades, considerable progress has been made
towards development of direct reading instruments for aerosol measurement.
These devices include electrical aerosol analyzers, condensation nuclei
counters, aerodynamic particle sizers, optical sizing and counting devices, and
piezoelectric and beta gauge based devices. Note that each of these
techniques measure a different property of airborne particles and thus do not
provide comparable information. Of these devices, only piezoelectric and beta
gauge devices provide direct reading of collected aerosol mass. None of these
techniques provide information in terms of the chemical composition of the
measured aerosol. Typically, devices such as filters, impactors, or electrostatic
13

14
collectors are merely used to capture an aerosol for subsequent analysis by a
separate Instrument.
Conversely, there exist a wide variety of analytical techniques available
for chemical quantitative analysis. Typically, these techniques require that the
aerosol sample be previously collected in a separate step and manually
transferred to the instrument’s analytical section. Some sample pretreatment or
extraction is often required to obtain reliable test results.
Rather limited success has been achieved in integrating these separate
aerosol sampling and analysis techniques in a single, direct reading instrument.
Many of these analytical techniques required for trace level analysis are fairly
sophisticated and do not adapt well to the development of inexpensive, portable
instruments. These sophisticated techniques often require daily calibration and
frequent maintenance to ensure accurate test results. The need for automated
sample transfer and preparation also complicates the instrument design.
Several tape samplers are available which provide combined aerosol
sampling with mass determination. In these automated devices, air flow is
normally directed through a porous tape which acts as the collection medium
for the airborne particles. This technique thus provides an integrated sample
with results time-weighted for the sampling period. In the GCA Model RDM301
sampler, particle matter is deposited by impaction onto a mylar film coated with
an adhesive (Lioy, 1983). At the end of the sampling period, the collected
material is quantified by beta attenuation. For low energy beta radiation, the

15
attenuation is a function of mass density of the absorber and is largely
independent of chemical composition or the particle’s physical properties.
Spagnola (1989) developed an automated sampling instrument based on this
analytical principle. The instrument uses electromechanical devices for
automatic positioning of membrane filters in the sample holder. At the end of
the sampling period, the filter is analyzed and returned to its original position in
the sample holder. Application of beta attenuation has also been applied to a
dichotomous sampler developed by Macius and Húsar (1976).
A paper tape sampler was also modified to provide lead analysis by x-ray
fluorescence (Smith et al., 1986). The system samples air at 0 to 10 Ipm and
irradiates the collected aerosol mass with a 10 mCi cadmium 109 radioisotope.
A Nal scintillator in conjunction with a multi-channel analyzer provides counts
versus x-ray energy for the resulting x-rays. The count corresponding to the
x-ray energy characteristic of lead provides a measure of the collected lead
mass. The authors note that the presence of arsenic and zinc positively
interfere with the lead measurement.
Automated mass monitors have also been developed based on the
concept of piezoelectric sensing of changes in aerosol mass. The TSI Inc.
Model 5000 deposits particles onto a piezoelectric crystal by electrostatic
precipitation. The rate of change of the crystal’s output frequency is directly
proportional to the deposited mass concentration. Recently, this mass sensing
technique was applied to the development of an instrument which uses a low-
frequency tapered element coupled to a filter collector (Wang, 1985).

16
Successful measurement of aerosol composition "in-situ" has been limited
and has generally not evolved beyond the laboratory. Arnold and Folan (1987)
devised an instrument which levitates a single airborne particle within an
electrostatic field and irradiates the particle with an infrared beam. The
instrument optically detects changes in particle size caused by evaporation of
the particle due to the heat induced by the infrared absorption. The measured
rate of change is proportional to aerosol mass. The instrument is capable of
detecting picogram quantities of material for both organic and inorganic
functional groups such as sulfate and carbonate (Allen and Palen, 1989).
The majority of analytical techniques which have been adapted for trace
aerosol chemical analysis are available only in an "off-line" mode and do not
adapt well to field use. Martinsson and Hansson (1988) have used particle
induced x-ray emission (PIXE) for the multielement analysis of aerosol
previously deposited onto thin aluminum foils. Deposits were stepwise heated
to several hundred degrees centigrade by applying an electric current through
the sample. An ion beam impinged on the sample during the process. Low
atomic weight element information (such as oxygen and carbon) was obtained
by particle elastic scattering analysis while elements with atomic numbers
greater than 14 were determined by PIXE analysis. The chemical composition
of the sample was inferred from noted vaporization temperatures and
stoichiometry. Laboratory tests found the technique useful for quantitation of
ammonium chloride, ammonium nitrate, and ammonium sulfate.

17
Xhoffer et al. (1989) used a transmission electron microscope to analyze
laboratory generated aerosols deposited onto carbon coated electron
microscope grids. The analytical technique of electron energy loss
spectroscopy was used to observe the change in kinetic energy as the electron
passes through the sample. This technique is generally useful only for low
atomic weight elements. The authors also noted that high background signals
can be associated with the substrate and that rapid deterioration of
environmental samples can occur. The technique was also found to possess
limited quantitative application since the particle’s absorption of the incident
electron beam was a function of particle size.
Electron spectroscopy for chemical analysis (ESCA) was investigated by
Muller et al. (1987) as a means of characterizing sub-micrometer sodium sulfate
aerosol collected on various filter media. This technique used incident x-rays to
excite photoemission of core level electrons from the sample. The measured
energy of the emitted photoelectrons is characteristic of the emitting element’s
oxidation state. ESCA provides only surface analysis and is thus of limited
quantitative analysis. ESCA signals can also be difficult to interpret
quantitatively. Incorporating a similar surface analytical technique, Fletcher
(1983) used a laser microprobe to vaporize and ionize a collected sample for
analysis by a time-of-flight mass spectrometer. Reported limitations of this
technique were similar to those experienced by Muller et al. using ESCA
analysis.

18
Neutron activation analysis (NAA) has been employed to provide
elemental information of collected aerosol samples. In this technique, the
sample is irradiated with neutrons to produce radionuclides. The activities of
the radionuclide products are then measured and related to the quantities of the
elements present in the sample. Podzimek and Wojnar (1990) used NAA to
quantify masses of laboratory generated titanium oxide particles deposited on
polyester filters. In a related study, Ondov et al. (1990) used NAA to quantify
45 elements in rural sub-micrometer ambient aerosols collected by micro-orifice
impaction. Although this technique was found to be generally useful, the
substrate blank precluded analysis of several elements of interest.
X-ray powder diffraction analysis of collected aerosol deposits was
reported by Tanninen et al. (1985). Powder diffraction allows for direct
determination of crystalline compounds. The authors used the diffraction
technique to analyze fumes generated by metal arc welding of steel. The main
analytical difficulty encountered was low instrument output intensity due to the
small particles analyzed in conjunction with the small quantity of material
present.
Both conventional flame and graphite furnace atomic absorption
spectroscopy have been widely used for the analysis of collected aerosol
samples. Davidson (1979) used graphite furnace techniques to characterize
size fractionated aerosol samples obtained from three national parks. Attempts
to incorporate atomic absorption analysis in an automated monitor have met
with limited success (Smith et al., 1986).

CHAPTER 3
DESIGN AND CALIBRATION OF THE PARTICLE COLLECTION SECTION
Pesian Theory
Accurate quantitation of lead-in-air concentrations requires efficient
capture of lead-based particles. If an aerosol was only collected with 10%
efficiency, the resulting lead analysis would obviously greatly underestimate the
actual lead-in-air concentration. This would, in turn, result in an underestimation
of the lead exposure hazard. This section describes the design and calibration
of a device capable of sampling and capturing lead-based particles with the
necessary high efficiency to ensure accurate test results.
There currently exist a variety of aerosol samplers and collectors which
offer a basis for the collector design. These devices include inertial devices
(impactors and cyclones), electrostatic precipitators, thermal precipitators,
diffusion devices, and filtration devices. Each of these devices relies on a
particular property of airborne particles to remove the particles from the
airstream in which they are suspended.
Fundamental to the design of any particulate collection section is
understanding the nature of the aerosol to be measured. In predicting
individual particle properties (settling velocity, diffusional behavior, etc) the most
19

20
important parameter is that of particle size. Since industrial aerosols are always
a collection of particles of varying sizes, it is understanding of the aerosol’s size
distribution which is of importance.
Figure 3-1 presents particle size distributions measured at a battery plant
in the southeastern United States. The specific sampling locations represent
sources of aerosols which supply recirculation air. It is believed, therefore, this
size distribution can be assumed to be fairly representative of aerosols which
exist in recirculation air systems. Plotted in the figure for the various process
points are cumulative lead mass distributions versus aerodynamic particle
diameter as measured using a University of Washington cascade impactor. The
aerodynamic diameter is defined as the diameter of a spherical particle of unit
density which has the same settling velocity as the particle under consideration.
Use of an equivalent aerodynamic diameter accounts for the particle’s size,
shape, and density.
Inspection of Figure 3-1 reveals that these measured size distributions
are fairly large with half of the lead mass associated with particles greater than
10 micrometers aerodynamic diameter. These results agree well with similar
measurements by Hodgkins et al. (1990) from two different battery
manufacturing plants. Note that only 1% to 5% of the lead mass is associated
with particles less than one micrometer aerodynamic diameter. A device
capable of collecting all particles greater than one micrometer, therefore, would
have an overall mass collection efficiency on this aerosol of 95% to 99%.

% Lead Mass Less Than Diameter
0.1
1 10
Aerodynamic Diameter (micrometers)
100
Figure 3-1. Measured particle size distributions at a battery plant.

22
Based on a review of these distributions, both thermal and diffusion type
collectors were eliminated as candidates for the collector design. Although
these type collectors can capture submicron aerosols with high efficiency, their
capture efficiencies for particles greater than one micrometer are quite low
(Hinds, 1982).
Filtration probably represents the most common form of aerosol
collection in air sampling. Unlike thermal and diffusion type devices, samplers
which rely on filtration mechanisms possess high collection efficiencies over a
wide range of particle sizes. Aerosols encountered in the battery industry could
be expected to be removed by filtration with virtually 100% efficiency. Despite
these advantages, however, filtration was eliminated from design consideration
primarily for logistic reasons. Due to high particle-substrate attractive forces,
particles collected on high efficiency filters are extremely difficult to remove
efficiently even if wet chemical techniques are employed. Wetting of either
fibrous or porous membrane filters dramatically increases its pressure drop
making the filter difficult to reuse. The alternative to filter reuse is to replace it
after each sampling test. Automated replacement of the filter would have
involved design and cost complications which were considered to be
unacceptably high.
Electrostatic collection was also given consideration during the
instrument’s design phase. In these devices, collection relies on the
electrostatic forces which can be exerted on charged particles in an applied

23
electric field. Similar to filtration samplers, electrostatic samplers possess high
collection efficiencies over a wide range of particle sizes. Use of electrostatic
collection would have involved use of a point-to-plane precipitator for deposition
of airborne particles to a liquid surface similar to the design approach adopted
during the design of the LEAP sampler (Andersen Samplers, Inc.).
This design approach was initially investigated during the instrument
development but was ultimately discarded for two primary reasons. First,
preliminary laboratory tests with a design prototype showed that the flow of
electrical current through the electrolyte resulted in the inadvertent plating out of
previously collected lead ions from solution. Loss of collected lead in solution
would have resulted in underestimation of the total lead-in-air concentration and
thus an underestimation of the lead exposure hazard. Use of electrostatics was
also eliminated due its greater complexity and anticipated maintenance
requirements in the corrosive nitric acid atmosphere of the collection region.
Ultimately, the use of inertial impaction was adopted for the final
instrument design. Inertial impactors have been widely used for aerosol
collection and sizing and can efficiently capture particles greater than one
micrometer diameter. Inertial impactors are relatively simple in construction,
contain no moving parts or electrical components, and require little
maintenance.
Impactors rely on the high inertial forces which can be established on
particles in a high velocity airstream. In a typical impactor stage, particle-laden

24
gas is accelerated through one or more nozzles and directed toward a solid
surface which forces the airstream to change its flow direction. Due to their
inertia, however, particles will be unable to exactly follow their respective
streamlines and will deviate from the airstream by a distance which is a function
of the particle’s aerodynamic diameter and the jet velocity. Particles of sufficient
inertia will deviate a sufficient distance to strike the collection surface and be
removed from the airstream. Conventional impactor stages with high jet
velocities can remove particles of 0.3 micrometers aerodynamic diameter and
larger.
Impactor performance is typically described by its Dp^ cutpoint which is
the particle size collected with 50% efficiency. Particles larger than the cutpoint
diameter are collected with much higher efficiency. Extensive theoretical and
practical impactor research has shown that the cutpoint can be predicted with
some confidence by
flft. V. 9 4 g ^TK
(3-1)
where Cs is the Cunningham’s slip correction factor determined from the
particle size and the fluid properties, ¡j is the gas dynamic viscosity, n is the
number of jets, W is the jet width, p p is the particle density, and Q is the
volumetric flowrate. The Stokes value (STK) can be predicted from knowledge

25
of the jet Reynolds number, ratio of jet width to jet to plate distance, and ratio of
jet throat length to jet width.
Based on these accepted design criteria, an inertial collector was
designed and constructed for use as the instrument collection section.
Figure 3-2 is a schematic of this device showing key components. Complete
detail drawings of each of the unit’s components are presented in Appendix A.
In most inertial impactors, the impaction jet is directed onto a preweighed
stationary surface previously coated with a viscous, nonvolatile grease to
minimize particle bounce and losses due to blowoff. Following the sampling
run, the impaction surface is reweighed to quantify the mass of the collected
aerosol deposit. If chemical analysis is to be performed, the aerosol must be
extracted from the grease in an efficient and representative manner.
The collector developed for the lead-in-air monitor does not impact
particles onto a solid surface but into 50 ml of 0.5 M HN03. Use of the liquid
impaction substrate eliminates the need for greased substrates and provides for
direct transfer of the particles from the gaseous phase to the liquid phase. High
velocity impaction also provides for the liquid turbulence necessary for efficient
particle dissolution so that aqueous lead ions are formed. High liquid
turbulence also tends to homogenize the liquid sample so that only an aliquot of
the sample need be analyzed for accurate lead determination.

Aerosol Inlet
26
Liquid Outlet
Air Outlet
Figure 3-2. Schematic of single-stage impactor used for particle collection.

27
During the sampling run, particle laden air enters the impactor inlet at a
flowrate of 10 to 30 Ipm (depending on the sampling situation) and is
accelerated through a single stage impactor. As shown in Appendix A, the
impaction stage contains 20 circular jets of 0.026 inch diameter. Following its
impingement into the liquid, the airstream then enters an expansion section
which reduces the upward air velocity and thus reduces inadvertent liquid carry
over. Use of a small plug of glass fiber filter at the air outlet has shown to
further minimize the liquid carry over. At the conclusion of the air sampling
period, a liquid outlet provides for transfer of the solution to the instrument’s
lead analysis section.
Prediction of Impactor Performance
Inspection of Equation 3-1 allows for the generalized prediction of
impactor performance as a function of sampling air flowrate and the critical
impactor dimensions. Table 3-1 presents a summary of these calculations
assuming standard temperature and pressure conditions for air. Also presented
are actual measured stage pressure drops as a function of the sampling
flowrate. Calculated cutpoints at flowrates of 10, 20, and 30 Ipm are 0.92, 0.63,
and 0.42 micrometers, respectively.
It should be emphasized that these calculations are based primarily on
theoretical and experimental evaluations of impaction onto a solid surface.
However, immersion of an impaction stage and impingement of an airstream

Table 3-1
Predicted Operating Characteristics of Teflon Impactor
Flow
Hem)
Velocity
(cm/sec}
Reynolds No.
(STK}1/2
10
2440
1070
0.48
20
4880
2150
0.48
30
7310
3220
0.48
Dp (C)1/2
Dp
Measured
A P
(micrometers^
(micrometers}
(mm Ha}
1.00
0.92
10
0.71
0.63
24
0.50
0.42
46
ro
oo

29
into a liquid represents an entirely different flow situation. While impaction is
certainly the most dominant collection mechanism involved, the entire process
may more correctly be described as a bubbling phenomenon.
Unlike the extensive studies related to conventional inertial impaction,
there has been relatively limited research devoted to the absorption of aerosols
by bubbling. As a simplified model, some researchers have considered particle
deposition in air bubbles which freely rise through a stationary liquid. As a
further simplification, these studies only consider the motion of bubbles less
than 0.2 cm diameter which have been found to be approximately spherical in
shape. Larger bubbles become flattened as they rise through the liquid and
pulsations in the bubble shape can occur.
Deposition of particles with a buoyantly rising bubble results primarily due
to the relative motion of the bubble with respect to the liquid. Due to the shear
force which exists at the liquid-gas interface, a gas circulation within the bubble
is established and maintained. As a result of this circulation pattern, large
particles may be removed by inertial impaction to the liquid-gas interface.
Gravitational settling of large particles can also occur as well as removal of
submicron particles by molecular diffusion.
The first analytical and experimental treatment of this particle absorption
phenomenon within a freely rising bubble was performed by Davies and Taylor
(1950). This theory was extended by Fuchs (1964), who developed coefficients
of absorption (deposition efficiency per unit cm of bubble rise) for the separate

30
absorption mechanisms of inertial impaction, sedimentation, and diffusion.
Later, related experimental studies by Melandrie and Prodi (1971) confirmed the
validity of this approach.
The coefficient of absorption due to inertial deposition, a., is related to
the bubbles upward velocity, Vb, the particle’s relaxation time, r, and the radius
of the bubble, R, by
Because particle relaxation time increases with the square of the particle
diameter, this inertial mechanism is dominant for large particles.
Similarly, the absorption coefficient due to particle sedimentation, as, is
expressed as
a = 3 3 T
s 4 R Vh (3“3)
For most bubble sizes of interest, inertial deposition is an order of magnitude
greater than that of sedimentation.
Finally, diffusional deposition efficiency per unit path length can be
calculated by accounting for the particle’s diffusion coefficient, D

31
D
(3-4)
Large bubbles (R > 1 cm) rising in a liquid tend to flatten and pulsate
such that their rate of rise is difficult to predict. However, smaller bubbles can
be assumed to be spherical and their upward velocity can be predicted by a
empirical relationship developed by Melandrie and Prodi (1971)
vb = 3.05 y/R
(3-5)
where the dimensions of Vb and R are m/sec and m, respectively.
For a known bubble size and particle diameter, the overall change in
particle concentration (C) per unit length of bubble rise can be calculated by
= - ( «i + “s + ad ) c
(3-6)
For example, Jonas and Schulz (1991) used this relationship to calculate an
overall collection efficiency of 98.8% of one micrometer radius iron oxide
particles within 0.5 cm radius bubbles buoyantly rising through one meter of
liquid.
Inspection of the absorption equation reveals that for a given particle
size, decreasing the bubble radius results in an increase in absorption
efficiency. The equation also indicates that for a given bubble size, the
dominant collection mechanism depends strongly on particle size. For large
particles (greater than 0.3 micrometers radius) which possess large relaxation

32
times, inertial and sedimentation forces dominate while diffusive absorption is
negligible. Conversely, particles less than 0.05 micrometers radius are removed
almost entirely by molecular diffusion. Thus, regardless of bubble diameter,
there exists an absorption minimum which exists for particles of approximately
0.2 to 0.4 micrometer diameter. The actual magnitude of the minimum depends
primarily on bubble radius.
Use of these theoretical considerations to exactly predict the
performance of the lead-in-air monitor’s impactor proved to be difficult. This
simplified approach assumes bubbles of known size rising through a stable
liquid of constant height. Experimental verification of the theory by other
researchers has been limited and performed at relatively low flow rates using
uniform sized bubbles. However, the dynamics within the teflon impactor
represent a vastly different flow situation. Temporary replacement of the
impactor’s opaque housing with a glass enclosure of similar dimensions allowed
for the direct observation of the bubbling phenomenon. This observation
revealed the limitations of the simplified theory to this particular collector. First,
it was evident that the bubbles produced were not uniform in size but existed
over a wide range of sizes. To apply the absorption theory to a distribution of
bubble sizes, the distribution itself must be known and the collection efficiency
equation integrated over the bubble size range. At these high flowrates, it was
also evident that the bubbles themselves experienced considerable oscillation
and occasional breakup due to the high liquid turbulence. Finally, it was

33
observed that the liquid itself underwent considerable turbulence which changes
the nature of the liquid-bubble interface and results in uncertainties in predicting
the path rise of the individual bubbles.
Due to this lack of reliable design theory, no exact predictions of the
impactor’s actual performance were made. Preliminary review of conventional
impactor design theory and bubbling theory were used only as a basis for the
impactor design. For accurate evaluation of the impactor’s actual performance,
extensive experimental efficiency tests were conducted with the impactor in the
laboratory.
Calibration of the Particle Collection Section
In evaluating the performance of the particle collector, it was understood
that the collection efficiency would depend on the unit’s critical dimensions,
liquid solution volume, particle diameter, and the sampling flowrate. Since the
impactor’s dimensions and the solution volume were fixed by design, the
particle size and sampling flowrate were normally the only two parameters
varied during the collection efficiency tests.
The particle collection characteristics of the impactor were evaluated in
the laboratory using monodisperse calibration aerosols of solid, spherical
ammonium fluorescein. These calibration aerosols were produced by two
separate generation systems depending upon the size of the particle required.
For the generation of calibration aerosols 0.5 micrometers aerodynamic
diameter and larger, a Thermal Systems Inc. Model 3050 vibrating orifice

34
aerosol generator (VOAG) was used. A schematic of the complete generation
and sampling system is presented in Figure 3-3. The VOAG operates on the
principle of the controlled mechanical breakup of a liquid jet into uniform
droplets of predictable size. Periodic breakup of the liquid jet was achieved by
application of an AC signal at a known frequency to a piezoelectric crystal
which housed the liquid orifice. Since the liquid consisted of a known quantity
of a non-volatile solute dissolved in a volatile solvent, the generated droplets
dried to form uniform particles of predictable size. For the calibration of the
impactor, the liquid solution was prepared by dissolving a fluorescein powder in
aqueous ammonia. After their production, the droplets dried to form spherical
particles of solid ammonium fluorescein. The particles were then mixed with
clean dilution air and charge neutralized by exposure to a “Kr radioactive
source. The particles were then mixed with additional dilution air and sampled
by the impactor for the calibration tests. An optical microscope was used to
verify the size and quality of the generated particles collected on a fibrous or
membrane filter before each test series. Figure 3-4 is a scanning electron
photomicrograph of a monodisperse aerosol generated by this technique.
For calculating the particle’s aerodynamic diameter from its physical
diameter, an ammonium fluorescein particle density of 1.35 g/cm3 was
assumed. This value was based on density measurements by Stober and
Flachsbart (1973), John and Wall (1983), Vanderpool and Rubow (1988), and
Chen and Crow (1986).

Signal Generator
Makeup
Air
Impactor
Figure 3-3. Schematic of generation system used for production of calibration aerosols greater than
0.5 micrometers aerodynamic diameter.
CO
cn

36
Figure 3-4. Scanning electron photomicrograph of ammonium fluorescein
calibration aerosols produced by VOAG.

37
Calibration aerosols less than 0.5 micrometers aerodynamic diameter
were generated using a Thermal Systems Inc. Model 3071 electrostatic
classifier. Figure 3-5 is a schematic of this generation setup. Polydisperse
droplets were first generated by air nebulization of fluorescein solutions through
a Collison nebulizer at an operating pressure of 20 psig. The polydisperse
droplets were then dried in a diffusion drier to form a polydisperse aerosol of
solid ammonium fluorescein particles. This aerosol was then passed through a
single stage impactor to reduce the large particle concentration. The pressure
drop across the impactor stage was monitored to verify the magnitude and
stability of the aerosol flowrate. Monodisperse particles of the desired size were
then produced by electrical classification within the classifier. Lastly, the
monodisperse aerosol was diluted to the necessary sampling flowrate using
clean, dry dilution air and sampled by the impactor.
The air exiting the impactor was passed through a filter holder housing a
47 mm diameter glass fiber filter which was used to collect any airborne
particles not collected by the impactor. Flowrate through the sampling system
was provided by a 90 Ipm capacity vacuum pump fitted with a primary valve
and a recirculation air valve. The pressure drop across a calibrated orifice was
used to adjust and monitor the sampling flowrate. A calibrated dry gas meter
measured the total volume of the gas sampled during each sampling run.
The collection efficiency of the impactor was defined as that mass
fraction of particles exiting the impaction jet which was collected in the liquid

-4
Impactor
Sheath
Air,—
Flowmeter
-D^Ch
Collison
3 - Jet
Nebulizer
Diffusion
Drier
Charge
Neutralizer
Total
Filter
7
\
Monodisperse
Aerosol
5
Valve
Negative
HV Supply
Compressed
Air
Total
Filter
Drying Chamber Re9ulator
Valve
Flowmeter
Excess
Air
Flowmeter
-C^Ch
Total
Filter
Valve
Vacuum
Pump
Makeup
Air
Pressure Guage
-0—i
Gas Meter
Teflon
Impactor
Figure 3-5. Schematic of generation system used for production of calibration aerosols less than
0.5 micrometers diameter.

39
solution. The total mass exiting the jet was estimated by summing the mass
measured in the solution with that mass measured on the 47 mm after-filter.
Collected aerosol mass deposits were quantified fluorometrically using a
Turner Model 112 fluorometer calibrated for fluorescein concentrations ranging
from one part per billion to 14,000 parts per billion. For the collection efficiency
tests, the impactor’s liquid solution consisted of 50 ml of 0.1 N NH4OH. At the
conclusion of the sampling run, this solution was analyzed directly. To quantify
the mass of aerosol collected on the after-filter, the filter was placed in a 100 ml
polypropylene container with 50 ml of 0.1 N NH4OH and the container placed in
an ultrasonic bath for approximately 20 minutes. Previous analytical tests have
shown that virtually 100% extraction efficiency can be achieved using this
technique.
Run times for the calibration tests varied depending upon the amount of
aerosol mass collected. For the large particle calibration tests, only 10 minute
run times were necessary. For the smallest particles generated, however, three
hour run times were necessary to achieve sufficient mass deposits for reliable
quantitation.
The performance of the impactor was measured as a function of both
particle size and sampling flowrate. Thirteen discrete particle sizes were used
ranging from 0.05 micrometers to 20 micrometers aerodynamic diameter. For
each particle size generated, collection efficiency tests were performed at
flowrates of 10, 20, and 30 Ipm. Each test series combination of particle size

40
and flowrate consisted of three separate collection efficiency tests performed
under identical test conditions.
Results of the collection efficiency tests are plotted in Figure 3-6.
Individual test results are tabulated in Appendix B. As expected, the impactor’s
collection efficiency varies as a function of both aerodynamic particle size and
sampling flowrate. The right hand side of the collection efficiency curves is of
particular importance. Independent of flowrate, the shape of the curves
resemble that of conventional inertial impactors with impaction efficiency
increasing monotonically with increasing particle size. Clearly, inertial impaction
is the predominant collection mechanism for particles in this size range. In
accordance with impaction theory, the collection efficiency also increased with
increasing flowrate. Measured outpoints in this region at 10, 20, and 30 Ipm
were 0.90, 0.53, and 0.46 micrometers aerodynamic diameter, respectively.
These measured values compare somewhat favorably with those predicted by
standard impactor theory (0.92, 0.63, and 0.42, micrometers).
The overall shape of the complete curves is quite similar to that predicted
by the simplified bubbling theory. Impaction is clearly dominant for large
particles while molecular diffusion accounts for deposition of small submicron
particles. Note also that an absorption minimum occurs in the range of 0.2 to
0.36 micrometers aerodynamic diameter which is approximately the size region
predicted by bubbling theory. The position and magnitude of the absorption
minimum was also noted to be a function of sampling flowrate. Below

00
90
80
70
60
50
40
30
20
10
0
0
6
«■
o
A
_
â–¡
â–¡
A
O
A
A
â–¡
â–¡
O
o
A
S
O
n
-
Symbol
Flowrate
-
A
o
D o
O
10 1pm
é
â–¡
20 1pm
o
A
30 1pm
-
â–  1 , â– 
â–  â–  ..... 1
.1 11
â–  . . . â–  1 L.
1 0.1 1 10
Aerodynamic Diameter (micrometers)
jure 3-6.
Measured particle size collection efficiency curves of single stage impactor.

42
0.2 micrometers diameter, molecular diffusion dominates the particle absorption
and efficiency actually decreases with increasing flowrate. This effect is
believed to result as a consequence of the gas’ lower residence time within the
liquid column at higher flowrates.
In terms of quantitative chemical analysis, it is the overall mass efficiency
of the collection device on the aerosol which is of importance. Recall from the
measured size distributions in Figure 3-1, that 95% to 99% of the lead-based
mass is associated with particles greater than one micrometer aerodynamic
diameter. Since the impactor’s collection efficiency on these particles is high,
integration of the collection efficiency curve over the measured size distribution
predicts that the impactor should collect this aerosol with over 95% mass
efficiency.
Particle losses through the Impactor’s inlet section were also quantified
during the calibration tests. Following each test series, the impactor was
disassembled and the inlet section carefully rinsed with a known volume of
0.1N NH4OH. Particle mass deposits were quantified by fluorometric analysis of
the collected rinse solution. In general, test results showed that inlet losses
represent only a small fraction of the sampled aerosol mass. Submicron
aerosol deposits were normally below the limit of quantitation of the fluorometric
technique. Large particle losses were found to be more significant with losses
of 2.2%, 3.2%, and 4.0% measured for particles of 6, 10, and 20 micrometers

43
aerodynamic diameter, respectively. Subsequent evaluation of the impactor
during its actual field use supported these test results.
Based on the calibration tests, it was concluded that the impactor’s
design met the criteria outlined for the overall instrument design. For the
aerosols of interest in the battery industry, the impactor is capable of capturing
the aerosols with high collection efficiency. Use of a liquid solution as the
impaction substrate eliminates particle bounce and substrate overloading which
can exist for solid impaction substrates. Turbulence within the fluid during
collection provides for effective dissolution of the lead-based particles as well as
providing for a well mixed, homogeneous solution. Unlike solid impaction
substrates, the liquid is easily replaced after each sampling test and is
compatible with the chosen lead analysis technique. Lastly, the impactor can
be easily constructed, is physically compatible with the corrosive nitric acid, and
requires little periodic maintenance.

CHAPTER 4
DESIGN OF AIR SAMPLING SYSTEM
Introduction
Accurate quantitation of lead-in-air aerosols requires representative
collection and efficient transport of the lead-based particles to the instrument’s
lead analysis section. Since it is infeasible to capture and analyze an entire
aerosol, a fraction of the aerosol must be extracted which reflects the aerosol’s
particle size distribution, concentration, and chemical composition. Because
sampling flowrates may vary from one test to another, the designed
instrument’s sampling flowrate must be controllable and accurately measured.
Description of Air Sampling System
Figure 4-1 is a schematic of the air sampling components associated
with Module 1. A description of these components is given in Table 4-1. In
addition to the components shown, Module 1 contains the system’s nitric acid
reservoir, liquid pumps, and lead analysis system. Referring to Figure 4-1, the
vertical orientation of the impactor is compatible with its liquid contents and
minimizes particle transport losses from the Module 1 inlet to the impaction
stage. The Module 1 sampling system consists of a set of sharp-edged
44

45
Figure 4-1. Schematic of Module 1 air flow system. Component descriptions
are provided in Table 4-1.

46
Table 4-1
Description of Module 1 Air Flow Components
Figure 4-1 Code
Description
1
2
3
4
5
6
7
8
9
10
11
12
3/16, 1/4, or 3/8 in. Diameter SS Nozzle
SS Female Connector, 1 in. Tube -1 in. NPT(F)
SS Flexible Hose, Teflon Lined
Cajon, Inc. Model SS-16BHT-36
SS Bulkhead Union, 1 in. Tube - 1 in. Tube
SS 3/8 in. O.D. Tube, 4.25 in.
SS Male Connector, 1 in. Tube - 1 in. NPT(M)
SS Male Elbow, 3/8 in. Tube - 1 /2 NPT(M)
SS 3/8 in. O.D. Tube, 3 7/8 in.
SS Union Elbow, 3/8 in. Tube
SS 3/8 in. O.D. Tube, 7 7/8 in.
SS Bulkhead Union, 3/8 in. Tube
3/8 in. Polypropylene Tubing, 6 ft.

47
nozzles, sampling probe, and Impactor in addition to their associated tubing
and compression fittings.
Sampling of indoor air (non-ducted airstreams) is used to evaluate
occupational lead exposures. For indoor air measurements, the sampling
nozzles and sampling probe are not needed. Instead, a sharp-edged nozzle
has been fabricated from a one inch diameter stainless steel tube and attaches
to the top of Module 1. Its vertical orientation allows for direct collection and
transfer of airborne particles to the collector with minimal transport losses.
Unlike indoor air sampling, the sampling of ducted airstreams such as
recirculation airstreams requires sampling from a horizontal duct with high
associated air velocities. As will be discussed, accurate particle sampling from
a flowing airstream requires that a thin-walled nozzle be oriented directly into
the airstream. In addition, the sampling flowrate must be controlled such that
the nozzle inlet velocity equals that of the freestream velocity at the point of
sampling. Depending upon the measured freestream velocity, a nozzle of 3/16,
1 /4, or 3/8 inch diameter can be used.
Sampling from horizontal ducts requires that the sampled aerosol must
undergo a 90 degree change of direction prior to entering the instrument’s
vertical collection section. The sampling system contains a 39 inch long flexible
probe which is used for this purpose. The probe consists of a teflon inner
lining surrounding by a stainless steel braid. The teflon lining is compatible with
elevated temperatures up to 400 °F and is resistant to corrosion. The probe’s

48
0.88 inch inner diameter matches that of the impactor inlet tube thus minimizing
particle transition losses due to air expansion or contraction.
Air flow through Module 1 is provided by connection to the vacuum
source located in Module 2. As shown in Figure 4-2, Module 2 contains an air
filter, mass flow controller, and cooling fan. Component descriptions are
presented in Table 4-2. The cartridge filter contains both activated charcoal and
fibrous filters and serves to protect the mass flow controller and sampling pump
from any particles remaining in the airstream. A high capacity vacuum pump
with teflon coated wetted surfaces provides the driving force for air flow through
the sampling system. As shown in Figure 4-2, this pump has been fitted with a
recirculation valve to reduce the load to the pump.
The sampling flowrate in the lead-in-air monitor is controlled using a
surplus Tylan Model FC-262 mass flow controller which has been adapted for
use in the system. The FC-262 is a 0-50 slpm capacity unit with flowrate
controlled by an internal solenoid valve. Selection of the flowrate is normally
provided by manual adjustment of a potentiometer to supply a 0 to 5 VDC
command signal to the flow controller. Feedback circuitry within the flow
controller continually adjusts the valve setting so that the actual air flow equals
the desired flowrate selected by the user. A measure of the actual flowrate is
provided by a corresponding 0 to 5 VDC output signal which is normally read
by the user from a digital panel meter. For adaptation to the prototype monitor,
the potentiometer input circuit and output display were removed and the

49
Module 2
(Top View)
Figure 4-2. Schematic of Module 2 air flow system. Component descriptions
are provided in Table 4-2.

50
Table 4-2
Description of Module 2 Air Flow Components
Figure 4-2 Code
Description
1
2
3
4
5
6
7
8
9
10
11
12
13
SS Bulkhead Union, 1/2 in. Tube - 1/2 in.
Tube
SS 1/2 in. Tube, 2 3/16 in.
SS Female Connector, 1/2 Tube - 3/8 NPT(F)
Disposable Air Filter
Koby Inc., Model "Junior King"
SS Female Connector, 3/8 in. Tube - 3/8 NPT(F)
3/8 in. Polypropylene Tube, 6 5/16 in.
SS Elbow, 3/8 in. Tube - 3/8 in. Tube
SS 3/8 in. Tube, 1 3/4 in.
Mass Flow Controller, 0-50 slpm
Tylan Corp., Model FC262
SS 3/8 in. Tube, 2 in.
3/8 in. Polypropylene Tube, 5 3/8 in.
SS Male Tee Run, 3/8 in. Tube - 3/8 NPT(M)
SS 3/8 in. Tube, 2 5/8 in.

51
Figure 4-2 Code
14
15
16
17
18
19
Table 4-2--continued
Description
SS 3/8 in. Tube, 2 9/16 in.
Valve, Swagelok Corp., Model B1RS6
Vacuum/Pressure Pump, 1/4 hp, teflon lined
3.2 cfm, 4A at 0 psi
Thomas Industries, Model 727CM39-TFE
3/8 in. Polypropylene Tube, 2 1/4 in.
SS Bulkhead Female Connector, 3/8 in. Tube
to 3/8 in. NPT(F)
Muffler, Koby Inc., Model M-1-N

52
command signal is now supplied by an analog output channel from the data
acquisition and control system. The flow controller’s output signal is read by a
corresponding analog input channel on the data acquisition and control system.
Figure 4-3 is a complete wiring diagram of the Module 2 circuitry.
Component descriptions, functions, and commercial sources are listed in Table
4-3. Table 4-4 provides connector pin descriptions. A standard 120 VAC, 60
hz source supplies power to the mass flow controller power supply, vacuum
pump, and cooling fan. Power to the flow controller is supplied by a 15 VDC,
200 mA power supply. The power supply is protected using a 0.5 amp fuse.
The sampling pump is internally protected against current overload and thus
requires no additional fusing. On/off control of the air pump and the cooling
fan is provided by use of a solid state relay capable of handling load currents
up to 25 amps. The relay itself is activated through application of a 3-32 VDC
signal which is compatible with standard TTL digital command signals. All
Module 2 input and output signals are communicated by a standard 9 pin
ribbon cable to the Kiethley 575 data acquisition and control system.
Prior to its use, the Tylan mass flow controller had been repaired and
recalibrated by the manufacturer. Its condition and calibration were then
verified in the laboratory. At a variety of flowrates and upstream and
downstream pressures, the actual mass flowrate was measured as a function of
selected mass flowrate. For these tests, a National Bureau of Standards
traceable Gillian Model D-80028 bubble flow meter was used as a flow

Figure 4-3. Wiring diagram of Module 2 electrical components. Component descriptions are provided in
Table 4-3. Connector pin functions are presented in Table 4-4.

Table 4-3
Module 2 Electrical Component Listing and Description
54
ComDonent
DescriDtion
Barrier Terminal
Block
3 Contact, Double Row, 20A
Cinch, Inc. type 3-141
Solid State Relay
SSR Series, 240 VAC/25A
3-32 VDC input
Potter and Brumfield
Type SSR-240D25
Appliance Plug
250/115 VAC, 10/15A
Feller, Inc. type 6100-31
Cooling Fan
115 VAC, 0.15A
34 cfm at 0 in H20 S.P.
Comair/Rotron type SV2A1
Fan Filter Screen(2)
Anodized, for 3.5 in fan
Fan-S/Qualtek type 06325-B
Vacuum/Pressure Pump
115 VAC, 1/4 hp, teflon lined
3.2 cfm, 4A at 0 psi
Thomas Industries type 727CM39-TFE
Power Supply
Dual Voltage (-15/ +15 VDC), 200 mA
Sola, Inc. type 85-15-2120
Fuse
1 1/4X 1/4 in, 0.5A slow-blow
SPC Technology type F-500SS-0.5
Fuse Block
Screw termination
SPC Technology type FB1PS
Connector KK
9 pin D-Sub, crimp style plug
SPC Technology type DEC-9P
Connector MM
22 position, card-edge connector

55
Table 4-4
Module 2 Electrical Connector Pin Descriptions
Pin#
Color
575
Channel
Connection
Function
KK-1
YEL
DIGOUT8
Relay
Pump, fan on/off
KK-2
GRN
Ground
Ground
Ground
KK-3
BRN
ANOUT1
LL-A
MFC Command Signal
0-5 VDC
KK-4
RED
ANIN1
LL-3
MFC Output Signal
"High", 0-5 VDC
KK-5
BLK
ANINO
LL-2
MFC Output Signal
"Low", 0-5 VDC
MM-2
BLK
ANINO
KK-5
MFC Output Signal
"Low", 0-5 VDC
MM-3
RED
ANINO
KK-4
MFC Output Signal
"High", 0-5 VDC
MM-4
WHT
—
Power
+ 15 VDC Supply
MM-A
BRN
ANOUT1
KK-3
MFC Command Signal
0-5 VDC
MM-C
GRN
—
Power
Common
MM-G
BLU
—
Power
-15 VDC Supply

56
calibration standard. For each operating pressure and flowrate range, six
separate measurements were made. As shown in Figure 4-4, the correlation
between the actual mass flowrate and the desired flowrate was generally good.
In the 10-30 slpm flowrate range of interest, the agreement was within 2%.
Note that conversion from actual to standard flowrate must account for the
fluid’s temperature and pressure at the point of sampling. Conversion from
standard temperature as defined by the mass flow controller’s manufacturer
(0 °C) to standard temperature as defined by occupational regulations (25 °C)
must also be taken into account. In the prototype lead-in-air monitor, these
conversions take place automatically through the instrument’s software.
Prediction of Particle Sampling and Transport Efficiency
Accurate measurement of lead-in-air concentrations requires that lead-
based particles be sampled, transported, collected, and analyzed efficiently.
Design of an efficient particle sampling and transport system depends primarily
on the particle size distribution expected, the fluid properties at the point of
sampling (such as temperature and velocity), and the air sampling flowrate
required by the instrument’s particle collection section. Efficient design,
calibration, and field testing of a separate sampling system was beyond the
scope of this project. As a preliminary approach, a particle sampling and
transport system was adapted from EPA Reference Method 12, "Determination
of Inorganic Lead Emissions from Stationary Sources." In the forthcoming

Measured Flowrate (slpm)
57
Set Flowrate (slpm)
Figure 4-4. Measured performance of Module 2 mass flow controller.

58
sections, the sampling and transport efficiencies of this design will be predicted
based on published theoretical and empirical studies. Alternatives to this
sampling and transport system will be discussed.
Sampling from Still Air
Evaluation of occupational exposures to lead-in-air concentrations
represents sampling from an airstream at zero or low velocity. Because
particles possess higher stopping distances at higher velocities, sampling and
transport losses during still air sampling can be negligible when compared to
sampling from ducted, high velocity airstreams. There exist, however, two
types of still air sampling biases which can result particularly with regard to the
large particle distributions characteristic of the battery industry.
Efficient still air sampling requires use of a vertically oriented sampling
tube. When the inlet air velocity is low, a sampling bias can result due to high
settling velocities characteristic of particles with large aerodynamic diameters.
At low sampling velocities, this results in an overestimation of particle
concentrations. An additional bias can result due to the effect of particle inertia
on particle trajectory. For sampling in still air, curved streamlines result as air is
accelerated towards the inlet nozzle. Due to their inertia, particles will be unable
to follow their respective streamlines and will be displaced a distance which may
be large with respect to the dimensions of the inlet. Inertial effects of this type
can result in an underestimation of actual particle mass concentrations.

59
Based on these possible biases, various criteria have been developed for
the design of air samplers. Davies (1968) developed inlet criteria based on
parameters of nozzle inlet diameter, sampling flowrate, and particle
aerodynamic diameter. Agarwal and Liu (1980) predicted less than 10%
sampling losses if the probe diameter (Dt) meets the following criterion
Dt > 20 T2 g (4-3.)
where r is the particle relaxation time and g is the gravitational constant.
Equation 4-1 was used to predict inlet losses of the 0.88 inch nozzle
used for still air sampling of the lead-in-air monitor. Results showed that
particles up to 60 micrometers aerodynamic diameter would be collected
without significant error. Particles greater than 60 micrometers would be
collected with less than 90% efficiency. The equal diameter of the nozzle the
inlet section ensures that particle transport losses should be minimized.
Sampling from Ducted Air Streams
Unlike sampling from still air, sampling from ducted airstreams can result
in significant sampling biases particularly with regard to the high velocity
airstreams and large particle distributions characteristic of the battery industry.
Moreover, the horizontal arrangement of ventilation ducts requires that a
captured aerosol must be transported a short distance to the instrument which
also involves a change in the aerosol’s flow direction. As a result, particle

60
losses within the aerosol transport system may significantly reduce the mass
concentration detected by the lead analysis section. The factors affecting
particle sampling and transport biases will be discussed.
The purpose of the aerosol sampling system is to obtain a representative
aerosol sample from the airstream of interest. In ducted airstreams, this
involves use of a sampling nozzle and probe to extract a representative aerosol
sample and transport it to the instrument’s collection section. Sampling bias
can occur, however, due to particles’ inertia in flowing airstreams. Similar to the
sampling from still air, sampling criteria have been developed for efficient
sampling from ducted airstreams. These criteria are generally of three types.
First, sharp-edges inlet nozzles must be used to obtain representative air
samples. Blunt-edged orifices can disrupt the airflow entering the nozzle
resulting in nonrepresentative particle collection and high inlet losses (Vincent
and Gibson (1981), Vincent et al. (1982), Vincent et al. (1985), Stevens (1986),
Vincent (1987), Vincent and Gibson (1988)). The second criterion is that the
nozzle must be oriented directly into the oncoming airstream. Changes in the
sampled air direction due to nozzle misalignment are a function of particle
inertia, the misalignment angle, and the probe diameter (Durham and Lundgren,
1980). Lastly, the sampling should be performed under isokinetic conditions
(nozzle inlet velocity equal to freestream velocity). Anisokinetic sampling can
result in significant large particle sampling biases whose magnitude and
direction depend on the velocity ratio and the particle Stokes number. Note

61
that isokinetic sampling requires prior measurement of the airstream’s velocity
at each of the desired sampling points. When sampling, achieving desired
nozzle inlet velocities requires proper combination of nozzle diameter and
sampling flowrates.
Achieving representative aerosol sampling does not ensure efficient
transport of the aerosol from the inlet nozzle to the particle collector. Particle
losses can occur both in the inlet nozzle as well as in the transport section.
Deposition can take place due to molecular diffusion, thermophoretic effects,
electrostatic effects, gravitational effects, and inertial effects. For the sampling
of aerosols of interest in the battery industry, only gravitational and inertial
mechanisms will result in significant transport losses.
Numerous theoretical and experimental studies have been conducted in
relation to understanding particle transport in sampling tubes. In general, these
studies agree on the recognized parameters of importance (such as particle
Stokes number, sampler geometry, and fluid conditions) but often vary widely in
terms of their conclusions and recommendations. Theoretical predictions of
transport losses requires extensive mathematical modeling of both fluid flow
fields and particle trajectories within the flow fields. The validity of these models
is often not confirmed. Differences in sampler geometries and flowrates can
result in significantly different predicted losses. Experimental loss
measurements are generally more practical but differences in sampler

62
geometries, operating flowrates, and particle properties make comparison of
separate studies difficult.
In the lead-in-air monitor’s sampling system, particle transport losses
during duct sampling can occur either in the inlet nozzle or in the flexible
sampling probe. To predict nozzle inlet losses, a brief review of pertinent
literature was made. Although the actual loss will depend on nozzle diameter,
sampling flowrate, and particle size, the literature suggests that large particle
losses may exceed 5% by mass. In the lead-in-air monitor, additional nozzle
losses might also be expected due to the airflow’s slight expansion from the
nozzle outlet diameter of 0.75 inches to the 0.88 inch diameter of the sampling
probe. The magnitude of the losses in the expansion section will depend on
sampling flowrate and particle size.
Losses in the sampling probe can more accurately be predicted than
those associated with the inlet nozzles. Considering the flexible probe oriented
as in Figure 4-1, the probe can be divided into three main sections for analysis:
an 8 inch long horizontal section, a 23 inch long section with a 14.5 inch radius
of curvature, and a 8 inch long vertical section. The particle losses in these
sections were considered separately. These calculations were simplified by the
fact that laminar flow conditions exist in the 0.88 inch diameter probe even at a
flow of 30 Ipm. Turbulent flow conditions alter the nature of the fluid flow field
and particle trajectories making accurate loss predictions more complex.

63
Particle deposition in the 8 inch long horizontal section occurs primarily
due to the force of gravity. During their transit time within the tube, particles
may settle a distance sufficient to be removed from the airstream. The
magnitude of these losses was predicted based on a study by Thomas (1958)
on sedimentation losses in horizontal cylindrical tubes. For laminar flow
conditions, the transport efficiency (penetration) can be predicted
P = 1 - — [ 2 <|> \Jl~ 2/3 + arcsin1/3 - 1/3 \Jl- 2/3 1 (4-2)
Tl
. 3 ic L Vs R
4> = —
8 Q
where P is the fractional penetration, L is the tube length, Vs is the particle
settling velocity, R is the tube radius, and Q is the volumetric flowrate through
the tube.
This relationship was evaluated for the 8 inch long section as a function
of particle size and sampling flowrate and is presented graphically in Figure 4-5.
Independent of flowrate, particles less than 10 micrometers aerodynamic
diameter can be transported through this section with fairly high efficiency.
Particle penetration above 10 micrometers, however, is predicted to decrease
fairly rapidly as a function of particle size. Note also that the lower sampling
flowrate results in lower transport efficiency due to the gas’ longer residence
time within the horizontal tube. Efficient transport through this section,

Fractional Penetration
Aerodynamic Diameter (micrometers)
O)
-&â– 
Figure 4-5. Theoretical particle transport efficiency through the sampling probe’s horizontal section.

65
therefore, would imply the use of high sampling flowrates and tubes of smaller
diameter.
Unlike losses in horizontal sampling tubes, particle losses in 90° bends
are due primarily to inertia and centrifugal forces on the airborne particles. Due
to their inertia, particles will be unable to follow their respective streamlines
directly and may be displaced a sufficient distance to impact on the duct walls.
Air flow around the bend can also establish a rotational flow pattern normal to
the mean direction of flow. This rotational profile can result in additional
particle losses around the bend. Cheng and Wang (1981) developed a
relationship for transport efficiency in a 90° bend as a function of particle Stokes
number
P = 1 - STK (4-3)
= i - P* Dp Q
18 n it R2
This relationship holds for laminar flow conditions and is plotted in Figure 4-6 as
a function of particle size and flowrate. Similar to losses in the horizontal
section, losses around the bend are minimal for particles less than
10 micrometers aerodynamic diameter. Particles greater than 20 micrometers
aerodynamic diameter are difficult to transport efficiently. Note also the effect of
sampling flowrate on transport efficiency. Higher flowrates correspond to larger

Fractional Penetration
Aerodynamic Diameter (micrometers)
Figure 4-6. Theoretical particle transport efficiency through the probe’s 90° bend.

67
stopping distances which would result in greater particle deposition. Inspection
of equation 4-3 would dictate use of low sampling flowrates and large diameter
tubes.
Note that the effects of flowrate and tube diameter on bend losses are
contradictory to those required for efficient horizontal transport. For a given
tube diameter, higher flowrates result in higher horizontal transport efficiency but
lower transport efficiency around the bend. Conversely, lower flowrates
minimize bend losses but maximize losses in the probe’s horizontal section.
Combined losses within these two sections are thus relatively independent of
sampling flowrate. The magnitude of these losses depends primarily on
aerodynamic particle size.
Particle losses within the probe’s final 8 inch long vertical section are
predicted to be minimal. Since the tube is oriented vertically, no horizontal
deposition is possible. Operation of the probe in the laminar flow regime also
eliminates the possibility of turbulent deposition which can be significant for
particles with high Stokes numbers in turbulent flow fields. This prediction of
low particle losses in this section is supported by the low impactor inlet losses
measured during the impactor’s laboratory calibration.
It can be concluded, therefore, that use of the proposed sampling nozzle
and probe may not allow efficient transport of large particles to the lead-in-air
monitor’s collection and analysis section. Combined losses within the nozzle,
nozzle outlet, and sampling probe may be prohibitively high. It should be

68
noted, however, that these loss calculations may significantly overestimate
particle losses. Theoretical loss calculations normally assume that when a
particle contacts a surface, it is removed from the airstream. Use of liquid
aerosols during experimental loss tests would support these calculations. In
reality, solid particles contacting solid surfaces at high velocity may experience
only fractional sticking efficiencies. Reentrainment of deposited particles also
results in higher particle transport efficiency.
It is apparent that special sampling considerations may need to be given
to the on-line measurement of ducted airstreams in the battery industry.
Conventional stack sampling techniques and equipment may not enable
representative sampling and transport of these large aerosols. As possible
alternatives, three sampling approaches could be investigated. First, the
ductwork at the monitoring point of interest could be modified to include a short
vertical section so that the entire flow is directed downward. A sharp-edged
sampling nozzle attached vertically to the lead-in-air monitor could then
isokinetically extract a representative sample with minimal inlet and transport
losses. Alternatively, a small flexible test section attached to a high volume
vacuum source could isokinetically extract a portion of the major duct flow and
direct this secondary airstream downward over the monitor’s sampling nozzle.
Aerosol not sampled by the monitor could then be returned to the major
airstream or filtered prior to its exhaust to the atmosphere. This concept is
similar is design by Baron (1988) and Ball and Mitchell (1990) for efficient

69
transport of coarse aerosols to particle sizing instrumentation. As a final
alternative, the conventional sampling nozzle could be replaced with a
precollector designed to remove all particles greater than 10 micrometers
aerodynamic diameter. The remaining fraction could then be transported
efficiently to the monitor’s collection section. In the human respiratory tract,
particles less than 10 micrometers represent the size fraction capable of
penetrating to the alveolar region and thus represent the best measure of the
actual lead exposure hazard. Particles larger than 10 micrometers are
deposited in the upper regions of the respiratory tract and are absorbed in the
bloodstream with much lower efficiency. Recent developments in
10 micrometer size selective inlets indicate that this design approach is feasible.
Use of a precollector to evaluate worker exposure, however, must first meet
with approval by the Occupational Health and Safety Administration.

CHAPTER 5
DESIGN OF LEAD ANALYSIS SECTION
Introduction
As discussed, accurate evaluation of lead-in-air concentrations requires
efficient aerosol sampling, transport, collection, and accurate analysis of the
collected aerosol’s lead content. Previous sections have outlined the
techniques required to ensure representative aerosol sampling, transport, and
collection. This chapter will outline design criteria for the lead analysis
section, briefly review available analytical techniques, and describe in detail the
analytical technique chosen for incorporation into the lead-in-air monitor.
Pesian Criteria
Selection of the instrument’s lead analysis technique was based on
careful consideration of several design criteria. First, the technique must be
specific for elemental lead and capable of accurately quantifying lead
concentrations ranging from 50 ppb to 9000 ppb. It was desired that the
technique’s response be fairly linear over a wide range of concentrations and
the technique display adequate repeatability. Because the collected aerosol
sample’s composition is not entirely lead, the analytical technique should
70

71
possess minimal physical and chemical interference from these other
components. The technique must also be physically compatible with the
chosen particle collection substrate. It was important that the selected
analytical technique require little periodic maintenance or recalibration. Finally,
the selected technique must meet cost requirements and be adaptable to
convenient automation.
Based on these criteria, a thorough review of pertinent literature was
made with regard to selection of the instrument’s analytical technique. There
exist a wide variety of analytical techniques available for the quantitation of lead
either in solid or liquid phase. These techniques include both conventional and
graphite furnace atomic absorption spectroscopy, ion chromatography,
inductively coupled argon plasma spectroscopy, x-ray and electron techniques,
colorimetry, neutron activation analysis, and electrochemical techniques. For an
automated device, most of these techniques were eliminated from consideration
either due to their high cost, level of complexity, inadequate lead detection
capabilities, or failure to adapt themselves to convenient automation. For
example, conventional atomic absorption is incapable of detecting sub-ppm
levels of lead in solution. Although graphite furnace atomic absorption
possesses the necessary detection capabilities, its use would have greatly
increased the complexity and cost requirements of the monitor. In addition, the
response of both conventional and graphite furnace atomic absorption displays
a fairly limited range of linearity. Other techniques such as colorimetry involve a

72
number of chemical handling steps which would have been inconvenient to
automate.
Ultimately, an electrochemical method of lead analysis was regarded as
most appropriate for the lead analysis. Because metals display high
electroactivity, their presence is solution can be detected over a wide range of
concentrations. Electrochemical techniques display high linearity and
repeatability. In particular, the electrochemical technique of polarography was
selected as that which best met the outlined design criteria. In forthcoming
sections, the principle of polarography will be reviewed and its application to
lead-in-air monitor described.
Description of Polaroaraphic Analysis
Electrochemical analysis is based on the observed behavior of
electroactive species in solution when subjected to an electric potential gradient.
For the detection of a particular species of interest (such as metals), a varying
potential is applied to the solution through a conductive electrode. If at a
particular potential a species is oxidized or reduced, an electric current will flow
at the electrode. Since the rate of electron transfer is a function of the number
of redox reactions occurring at a given potential, the measured current
produced is proportional to the concentration of that component in solution.
Because electroactive species display characteristic redox potentials, the
observed potential at which the redox reaction occurs can be used to identify

73
the component of interest. By applying a range of potentials to a sample and
noting the potential and resulting current of several redox reactions,
simultaneous quantitation of several solution components is possible. This
analytical technique is commonly referred to as voltametry.
Although the study of voltametry is not new, recent advances have led to
the development of reliable, commercially available instruments suitable for trace
metal detection. Current designs now incorporate mercury drops as the active
working electrode surface. Since a fresh mercury drop is produced for each
separate sample analysis, carry over contamination of the working electrode is
virtually eliminated. Recent advances in microprocessor technology have also
led to increasing measurement sensitivity and instrument capabilities.
Commercially available analyzers allow the user to select from various applied
potential waveforms which optimize detection of the component of interest. For
many metals (including lead) part per billion detection capability is routine.
Based on a review of available electrochemical detectors, an EG&G
Model 303A static mercury drop electrode was purchased along with an
accompanying Model 264A control unit. The Model 303A contains a mercury-
based working electrode, a silver/silver chloride reference electrode, and a
platinum counter electrode which are all immersed in a static cell containing the
solution of interest. The Model 303A also contains a 5 lb capacity mercury
reservoir and a delivery system for dispensing individual mercury drops of
repeatable size.

74
Control of the Model 303A electrode system is provided through
communication with the Model 264A control unit. The Model 264A sets the
Model 303A operating parameters, provides for automatic sequencing of the
analysis steps, receives and conditions the resulting output signals, and
communicates the current versus voltage scan results to an x-y recorder. The
user is able to select from a variety of a scan types including normal direct
current, normal pulse, and differential pulse polarography as well as direct
current and differential pulse stripping analysis. Although these techniques
possess varying degrees of capabilities and applications, differential pulse
stripping analysis provides for the most sensitive detection of lead in solution.
This mode, therefore, is used exclusively for lead quantitation in the lead-in-air
monitor.
Quantitation of lead in solution by stripping analysis typically involves the
following sequence of steps. First, high purity nitrogen is bubbled through the
liquid sample at a flowrate of approximately 40 cc per minute for approximately
3 minutes. This deaeration step removes the electroactive interference of any
dissolved oxygen in the solution. The Model 303A then dispenses a single
mercury drop of selectable size which hangs on the tip of a glass capillary
immersed in the solution. A constant electric potential is applied to the mercury
drop whose magnitude is more negative than the half-wave potential of the
analyte of interest. This results in a electro-reduction of the analyte onto the
surface of the mercury drop. To ensure repeatable mass transfer rates during

75
this step, the solution is stirred and deposition is performed for a fixed time
period (such as 3 minutes). The preconcentration step is responsible for the
technique’s low detection limit for many electroactive species.
At the conclusion of the deposition step, the stirrer is turned off and the
electroactive species is stripped from the electrode by making the electrode
more positive and oxidizing the species back into solution. In this stripping
step, varying the potential at a constant rate (such as 10 mV/sec) allow
different species to oxidize at different times. In differential pulse stripping
analysis, the current measured during each species’ oxidation reaches a
maximum value that is proportional to the concentration of each species that
was deposited.
As an example, Figure 5-1 presents the results of a typical analysis of
40 ppm lead, cadmium, and copper standards in 0.1 N nitric acid. The position
of the peaks (with potentials referenced to the Ag/AgCI electrode) identifies the
species present in solution and the peak height for each species is proportional
to its concentration in solution.
To ensure reliable test results of trace metal analysis, special
experimental techniques were observed during all polarographic analyses. To
minimize sample contamination and species absorption losses, all polarographic
cells were made of teflon and were acid washed with 6M nitric acid prior to use.
Metal standards were prepared from 1000 ppm stock metal standards certified
by the manufacturer to within 1% accuracy. Serial dilutions were performed

60
50
40
30
20
10
0
0
T
T
T
T
Cu
4 0.2 0.0 -0.2 -0.4 -0.6 -0.8
Potential vs. Ag/AgCI, V
response to 40 ppm concentrations of lead, cadmium, and copper in 0.1 N HN03.
'si
CD

77
using positive displacement pipettes with disposable tips rated to within 2%
accuracy. Dilute nitric acid solutions were prepared using trace metal grade
concentrated nitric acid diluted with distilled, deionized water with a measured
resistivity of 17 x 106 ohm-cm. Only certified, triple distilled mercury and ultra-
high purity nitrogen were used in the polarograph.
If polarographic stripping analyses are performed under carefully
controlled conditions, repeatable test results can be obtained over a wide range
of concentrations. Figure 5-2 presents the instrument’s response as a function
of lead concentration in 0.1 N nitric acid. Each data point represents the
average of 6 separate tests performed under identical test conditions. The
technique’s precision (as expressed by the relative standard deviation) was
measured to be approximately 2%.
Considerable attention was devoted to identification and subsequent
optimization of the parameters which affect the polarographic’s response to
trace lead concentrations in solution. Factors affecting the deposition step were
identified to be initial deposition potential, mercury drop size, deposition time,
and solution stirring dynamics. The instrument’s response during the stripping
phase was found to vary with the potential’s rate of change (scan rate) and the
height of the differential wave applied to achieve oxidation. The overall
response was also found to vary with the condition of the Ag/AgCL reference
electrode, solution temperature, and the concentration of the nitric acid solution
used.

Current (10E-06A)
~sl
00
Figure 5-2. Typical polarographic response as a function of lead concentration.

79
Within limits, these variables can be controlled by proper selection of the
polarograph’s operating parameters. However, complete control of all of these
variables in an automated monitor is impractical to achieve. In stripping
analysis, the instrument’s response to a given lead standard was noted to vary
as much as 50% during successive test series. Ultimately, this variability was
virtually eliminated by including an internal standard (200 ppb copper) in the
nitric acid electrolyte.
Use of the internal copper standard was developed based on numerous
observations of the polarograph’s response to several species in solution.
During the analysis of equal mass concentrations of lead, copper, and
cadmium, it was noted that the ratios of the resulting peak heights were
essentially constant regardless of the operating parameters of the instrument.
For example, although reducing the deposition time during stripping analysis
reduced the magnitude of each element’s peak, the respective peak ratios
remained essentially constant. Similar behavior was noted by changing the
mercury drop size, nitric acid concentration, analysis scan rate, solution
temperature, and solution stirring dynamics. Thus, if the instrument response to
a known concentration of an analyte is measured, the concentration of a
different species can be calculated from its observed peak height and the
known peak ratio. During the course of the project, the instrument’s response
to equal lead and copper concentrations was measured as a function of
concentration and instrument’s operating parameters. For 156 separate

80
measurements, the ratio of the copper to lead peak height was measured to
average 2.33 with a relative standard deviation of 1.8%. Assuming the use of a
200 ppb copper internal standard, the concentration of lead in solution can thus
be calculated using the following relationship
Lead Cone, (ppb)
Lead Peak Height
Copper Peak Height
X 2.33 X 200 ppb
(5-1)
Use of an internal standard in the lead-in-air monitor offers several
advantages. First, the need for periodic calibration of the analytical section is
eliminated since the instrument essentially calibrates itself during each sample
analysis. Analytical accuracy is no longer sensitive to variables which would be
difficult to control within required limits. Lastly, use of the internal copper
standard provides an internal quality control check during each analysis. If the
instrument’s response to the copper standard is outside the expected range, it
serves as an indication that either the electrolyte was prepared incorrectly or
that a possible instrument malfunction may exist.
To determine the value of this design approach, lead standards of
concentrations ranging from 0 to 8000 ppb were prepared in 0.5M nitric acid
with a 200 ppb copper internal standard. The instrument’s response to these
solutions was then measured and Equation 5-1 used to predict the actual lead
concentration. For each concentration, six separate measurements were
performed under identical test conditions. Figure 5-3 presents the results of the
0 to 200 ppb lead measurements in comparison to the instrument’s ideal

Measured Lead Cone, (ppb)
81
Actual Lead Cone, (ppb)
Figure 5-3. Polarograph response to 0-200 ppb lead concentration using
200 ppb internal copper standard.

82
response. It can be seen that agreement between the measured and ideal lead
concentration is quite good for lead concentrations greater than or equal to
approximately 20 ppb. The observed response at 0 ppb is due to the presence
of hydronium ions in solution which provide a residual current overlapping the
position of the lead peak. At a 0 ppb lead concentration this interference
typically provides a calculated lead concentration of 5 to 15 ppb. For lead
concentration above 20 ppb, however, the contribution of the hydronium ions is
insignificant. A minimum quantitation limit of 20 ppb lead is thus reported for
the monitor’s analytical section.
Figure 5-4 presents the results of the 0 to 8000 ppb lead response tests.
Note that use of the internal copper standard is accurate even over this wide
range of concentrations. A summary of these test results is tabulated in
Table 5-1 including the technique’s precision as expressed by the relative
standard deviation. For lead concentrations ranging from 20 ppb to 8000 ppb,
the precision was calculated to be approximately 2%.
Analysis of Field Bulk Samóles
In any quantitative chemical analysis, it is important to ensure that the
analytical technique chosen be compatible with the sample to be analyzed.
Physical and chemical interferences associated with the sample’s measurement
should be noted and effort made to minimize them in order to achieve reliable
test results. In the case of the lead-in-air monitor, it was important to ensure

Measured Lead Cone, (ppb)
83
Actual Lead Cone, (ppb)
Figure 5-4. Polarograph response to 0-8000 ppb lead concentration using
200 ppb internal copper standard.

Table 5-1
Polaroaraph Response Usina Copper Internal Standard
Polarograph Response
Actual Lead Cone, fppbl Lead Cone, fppbl RSD(%1
0
9
8.3
5
9
7.0
10
12
5.9
20
22
3.1
40
41
0.7
80
81
0.4
200
197
0.8
400
389
0.7
800
783
0.8
1600
1546
1.8
4000
4037
2.1
8000
7900
2.4

85
that the expected aerosol’s composition be compatible with polarographic
analysis.
During battery manufacturing, airborne particles are produced primarily
by mechanical breakup (dispersion) of lead oxide powder, lead oxide paste,
and the lead-based plate material. It can thus be expected that the chemical
composition of the aerosol produced from these materials is virtually identical to
that of its parent material. Bulk samples of lead oxide powder, paste, and plate
material were obtained at the battery plant and returned to the laboratory for
analysis in order to identify any potential analytical interferences.
During these tests, a known mass of each material was dissolved in nitric
acid solution and analyzed using the polarograph. For comparison purposes,
these samples were also analyzed using a graphite furnace atomic absorption
(GFAA) spectrophotometer manufactured by Perkin-Elmer (Model 5100). The
GFAA is more widely used for trace metal analysis than the polarograph and
thus represents an accepted criterion upon which to base the polarograph’s
accuracy. For each test series, the GFAA was calibrated for lead
concentrations in its linear operating range of 0 to 40 ppb by autodilution of a
100 ppb lead stock standard solution. For comparison purposes, the diluent
consisted of 0.5M nitric acid with a 200 ppb copper internal standard. To
minimize matrix effects associated with lead measurement by GFAA analysis, a
fixed quantity of a matrix modifier (0.2 mg NH4H20P04 + 0.01 mg Mg(N03)2)
was injected with each 5 fj\ sample.

86
The results of these comparison tests are presented in Table 5-2.
Analysis was first performed on certified laboratory samples of lead nitrate, lead
monoxide, and lead acetate. Based on the known formula weights of these
materials, each sample was prepared to obtain an expected lead concentration
of 100 ppb. As shown in Table 5-2, both the polarograph and the GFAA
measured these solutions with reasonable accuracy. Based on the three
replicate analyses for each material, the polarograph displayed somewhat better
repeatability than did the GFAA.
Similar solutions were prepared from the bulk materials collected at the
battery plant. Although the lead content of the lead monoxide powder can be
assumed with some confidence, its actual percentage in the lead paste can only
be estimated based on discussions with the battery plant personnel. Results
shown in Table 5-2 generally verified these estimates. Similar to the analysis of
the certified laboratory samples, these results indicated fairly good agreement
between the polarograph and the GFAA. More important, no interference was
observed during the polarographic analysis of these battery plant samples. It
was concluded, therefore, that no interference can be expected during analysis
of any airborne particles produced from these bulk materials.

87
Table 5-2
Comparison Tests Between Polaroaraph and GFAA
Lead Cone, (ppb) (RSD)
Description Expected Polaroaraph GFAA
Laboratory Samples
Blank
0
11 (6.2%)
1
(18.2%)
100 ppb Pb Std
(certified)
100
102 (0.6%)
104
(7.8%)
108 ppb Pb Std
(certified, no Cu)
100
—
98
(4.5%)
108 ppb PbO
(certified)
100
98 (0.0%)
94
(2.8%)
108 ppb Pb-Acetate
(certified)
100
99 (0.6%)
92
(7.1%)
Field Samóles
108 ppb PbO from
battery plant
100
101 (0.0%)
94
(3.8%)
108 ppb Pb-paste
from battery plant
95-100
95 (0.6%)
98
(1.8%)
108 ppb Plate
material from
battery plant
90-95
93 (2.1%)
94
(3.7%)

Description of Modifications to the Polaroaraph
Introduction
In previous sections, the suitability of polarography for the instrument’s
analytical section has been discussed. The polarograph is commercially
available, meets costs requirements, possess the necessary lead detection
limits and measurement range, and displays no analytical interferences from the
aerosols of interest to the battery industry. To achieve the design goals of the
complete lead-in-air monitor, however, several modifications were made to the
polarograph to adapt it to automated control. These modifications were made
primarily to eliminate the need for manual selection of the polarograph’s
operating parameters, manual selection of the proper measurement range, and
manual retrieval and interpretation of test results.
Run/Stop Control of Model 264A
On the Model 264A control unit, initiation of an analysis run is performed
manually using a DPDT momentary contact pushbutton switch (SW1) located
on the main 264A circuit board. Similarly, termination of an analysis is
performed manually using a separate pushbutton switch (SW2). To provide for
remote control of these run/stop functions, a printed circuit board was
designed, constructed, and has been installed within the Model 264A. A wiring
diagram of this circuit is presented in Figure 5-5 along with component

89
264A SWITCHES
RELAY DETAIL
Figure 5-5. Schematic of printed circuit board which provides run/stop
functions. Component descriptions are provided in Table 5-3.
Connector pin functions are described in Table 5-4.

90
descriptions in Table 5-3. Connector pin functions are presented in Table 5-4.
The "run" circuit uses a SPDT electromechanical relay in parallel with SW1 to
provide for initiation of the run function. Activation of the relay’s coil is provided
by a 5 VDC command signal from a Kiethley power control module (PCM3)
which has also been installed within the Model 264A. Software control of the
PCM3 channel releases the relay once the polarographic analysis cycle has
begun. Similarly, the manually operated stop function has been automated
through a separate electromechanical relay activated by a separate PCM3
channel.
Figure 5-6 presents the wiring diagram of the PCM3 control module with
accompanying component descriptions and channel functions listed in
Tables 5-5 and 5-6, respectively. Although the PCM3 is capable of providing
both AC and DC power control for up to 16 separate channels, only 8 channels
providing DC control are required in the lead-in-air monitor. Activation of each
channel is provided through the data acquisition and control system’s software.
Description of Decade Resistance Board
During a polarographic scan, the electrical current produced during a
redox reaction is proportional to the concentration of the species undergoing
the reaction. In the Model 264A, this measured current undergoes a current-to-
voltage conversion using an operational amplifier (U2 on 264A circuit board)
with a maximum output voltage of 5 VDC. Since the current can vary over five

Table 5-3
Component Listing and Description of RUN/STOP Board
ComDonent
DescriDtion
Electromechanical Relays
5 VDC, 72 mA, SPDT DIP
2A at 125 VDC
Radio Shack
Type 275-243
Connector RR
5 pin Pout Header
Friction Lock
Amphenol Type 640456-6
Connector SS
5 pin Pout Header
Friction Lock
Amphenol Type 640456-6

92
Table 5-4
RUN/STOP Board Connector Pin Functions
Pin
Color
PCM Channel
Function
RR-1
PUR
PCM-1
Activates RUN Relay
RR-2
BLK
PCM-GND
Ground
RR-3
GRY
PCM-2
Activates STOP Relay
SS-1
WHT
-
STOP Switch (S2) Contact 1
SS-2
YEL
-
RUN Switch (S1) Contact 1
SS-3
BLU
-
STOP Swich (S2) Contact 2
SS-4
RED
_
RUN Switch (S1) Contact 1

CD
03
Figure 5-6. Wiring diagram of Kiethley PCM3 power control module. Component descriptions are provided
in Table 5-5. Channel functions are listed in Table 5-6.

94
Table 5-5
Component Listing and Description of PCM3 Board
ComDonent
DescriDtion
Solid State Relays
5 VDC Output
3-14 VDC input, 3A at 60 VDC
Potter and Brumfield
Type SSR-ODC5
Power Control Board
Kiethley PCM3 Module

95
Table 5-6
Description of Various PCM3 Channels
PCM3
Channel
Color
Connection
1
PUR
RR-1
2
GRY
RR-3
3
WHT
MM-2
4
RED
MM-3
5
BRN
MM-4
6
GRY
MM-5
7
YEL
MM-6
8
TAN
MM-8
Function
Activates RUN Relay
Activates STOP Relay
Activates Decade PCB Relay 5
Activates Decade PCB Relay 4
Activates Decade PCB Relay 3
Activates Decade PCB Relay 2
Activates Decade PCB Relay 1
Activates Decade PCB Relay 6

96
orders of magnitude, the gain of the amplifier is controlled through a feedback
loop providing five decades of resistance. Varying this feedback resistance is
equivalent to changing the instrument’s measurement range. On the 264A, this
gain switch is selected manually based on the maximum concentration
expected during each sample analysis. If the actual concentration is higher
than expected, however, an over-range condition occurs and no useful results
can be obtained from the analysis. Conversely, if the gain switch is set too low,
the output voltage produced by the amplifier will be too low to produce reliable
test results. In either case, the operator must make the proper adjustment to
the gain switch and repeat the entire analysis cycle.
To automate the ranging function of the polarograph, a decade
resistance circuit board was constructed and installed inside the Model 264A.
Figure 5-7 is a wiring diagram of this circuit with component descriptions and
connector pin functions presented in Tables 5-7 and 5-8, respectively. When
activated, this circuit bypasses the Model 264A current range circuit and
provides for the correct feedback resistance as controlled by the instrument’s
software. Similar to the run/stop circuit, activation of the electromechanical
relays on the decade resistance board is provided by 5 VDC command signals
from the Kiethley PCM3 circuit board. When the decade resistance board is
activated, manually changing the current ranging switch on the 264A front panel
has no effect on the amplifier gain.

flllllill
1
Figure 5-7. Schematic of printed circuit board which provides decade resistance ranging functions. Table 5-7
provides component descriptions and Table 5-8 lists connector pin functions.
CO
III I
L.

98
Table 5-7
Component Listing and Description of Decade Resistance Board
Component
Description
Electromechanical Relays 5 VDC, 72mA, SPDT
2A at 125 VAC
Radio Shack
Type 275-243
Connector NN 8 pin Post Header, Fricton Lock
Amphenol Type 1-640456-0
Connector PP 5 pin Post Header, Friction Lock
Amphenol Type 640456-6
Attaches to J6 on 264A Main Board
Connector QQ
Resistor R1
Resistor R2
Resistor R3
Resistor R4
Resistor R5
5 pin Post Header, Friction Lock
Amphenol Type 640456-6
Attaches to 264A Current Range Board
2M ohm, 1%, 0.5 W
200k ohm, 1%, 0.5 W
20k ohm, 1%, 0.5 W
2k ohm, 1%, 0.5 W
200 ohm, 1%, 0.5 W

Table 5-8
Decade Resistance Board Connector Pin Functions
PiM
Current Ranae
Function
NN-1
—
Not Connected
NN-2
OOnA
Activates Relay 5
NN-3
/ja
Activates Relay 4
NN-4
0/jA
Activates Relay 3
NN-5
00/jA
Activates Relay 2
NN-6
mA
Activates Relay 1

100
Figure 5-8 shows the recommended locations for the run/stop, PCM3,
and decade resistance circuit boards which have been installed within the
Model 264A control unit. Communication between the PCM3 and the data
acquisition and control system is provided by a 50 pin ribbon cable with
appropriate connectors installed in the rear panel of the Model 264A and the
Kiethley 575 system. Component listings and descriptions for these connectors
are presented in Tables 5-9 and 5-10.
Description of Digital Logic Circuit
Communication between the Model 303A polarograph and the Model
264A control unit takes place through a 25 pin D-sub ribbon cable (EG&G
Model C0113). In addition to providing power to the Model 303A, the control
unit sends digital command signals to activate the polarograph’s functions of
stir, mercury drop dispense/dislodge, and nitrogen purge. Polarographic scan
results are returned the control unit through this same cable.
In the Model 303A, mercury flows from the mercury reservoir through a
thin glass capillary (0.006 inch diameter) to form a drop at the capillary tip.
During the electrochemical reaction, the mercury column within the capillary
carries the resulting redox current from the mercury drop to the electrical output
circuit. If a discontinuity should occur in the mercury column, however, no
electrical potential can be applied to the drop and the electrochemical reaction
cannot take place. In this event, reestablishing the mercury column continuity

101
Kiethley 575
(Top View)
Rear Panel
Front Pane!
Figure 5-8. Schematic of Model 264A showing recommended locations for
auxiliary circuit boards. Component descriptions are listed
in Table 5-9. Connector pin functions are provided in Table 5-10.

102
Table 5-9
Component Listing and Description of Model 264A
Figure 5-8 Code Function
Description
1
2
3
Connects CC to II 9 pin D-Sub ribbon cable
with 3M type plug 8209-6000
and socket type 8309-6000
Connects GG to HH 50 pin delta ribbon cable
with 3M F card edge connector
type 3415-0001 and 3M delta
plug type 3564-1000
Connects Kiethley
575 to PCM3
50 pin delta ribbon cable with
3M socket type 3565-1000 and 3M
F card edge connector type
3415-0001

103
Table 5-10
Model 264A Connector Pin Descriptions
Pin#
Color
575
Channel
264A
Connection
Function
11-1
PUR
ANIN1
DPM-6
Reads I "High" in
I vs. V scan
II-2
BLU
ANIN1
DPM-H
Reads I "Low" in
I vs. V scan
II-3
RED
ANIN4
J14-5
Reads scan status
from scan LED
II-4
GRY
ANIN3
l/E monitor
rear panel
Reads V "High" in
I vs. V scan
II-5
GRN
ANIN3
GND
Reads V "Low" in
I vs. V scan

104
requires repeated manual activation of the drop dislodge/dispense function
switches (located on the front panel of the polarograph) until continuity is
regained. Disruption of the mercury column continuity occurs primarily during
movement or excessive vibration of the polarograph. Since the lead-in-air
monitor was intended for portable use, it was anticipated that loss of mercury
column continuity would occasionally take place.
To eliminate the need for manual control, a circuit board was designed to
provide to automatically trigger these dispense/dislodge function switches. In
the Model 303A, a digital TTL logic low signal applied to pin 10 from the Model
264A control unit triggers a single dislodge/dispense sequence. Figure 5-9 is a
schematic of the circuit board designed to provide for external application of
this signal without interfering with the normal operation of the polarograph.
Component descriptions and connector pin functions are provided in
Tables 5-11 and 5-12. The combination of switching diodes and resistors
shown for pin 10 represents a standard digital AND logic gate. The circuit
shown allows a separate digital low TTL signal to be applied when desired by
the data acquisition and control system. Experiments have shown that initiating
the drop dislodge/dispense function through fifteen cycles is sufficient to
reestablish column continuity.
To enable stirring of the flow through polarographic cell during the rinse
cycle, a similar logic gate on the circuit board is applied to pin 8 of the ribbon
cable. External control of the polarograph’s nitrogen purge function is provided

105
Figure 5-9. Schematic of printed circuit board which provides logical switching
of stir, purge, and drop dispense/dislodge functions. Component
descriptions are listed in Table 5-11 and connector pin functions
listed in Table 5-12.

106
Table 5-11
Component Listing and Description of Digital Logic Board
ComDonent
Descriotion
Connector TT
Right Angle D-Sub Header Plug
Dupont Type 71563-325
Connector UU
Right Angle D-Sub Header Socket
' Dupont Type 71564-325
Connector W
4 pin Post Header, Friction Lock
Amphenol Type 640456-4
Switching Diodes
Silicon diode, 1N914
Radio Shack Type 276-1122
Resistors
Metal film, 1k ohm, 1%, 0.5 W
Dale Type RN-65D

107
Table 5-12
Digital Logic Board Connector Pin Descriptions
Pin#
Color
575
Channel
Module 1
Connection
Function
W-1
YEL
ANOUT1
BB-9
Supplies 6 VDC
W-2
ORG
DIGOUT6
BB-11
Initiates STIR
W-3
BLK
DIGOUT7
BB-12
Initiates Hg Drop
Dislodge/Dispense
W-4
PNK
DIGOUT5
BB-10
Initiates Purge

108
by control of pin 24. No modifications were made to the ribbon cable’s other
pin positions.
Measurement of Analysis Results
In polarography, test results are analyzed on the basis of measured
redox current versus the applied scan voltage. Resulting peak heights are
proportional to concentration while peak positions identify the component
undergoing the redox reaction. When using the Model 264A control unit, this
information is typically transmitted to an x-y recorder and the resulting
polarogram is interpreted by the user. As an alternative to use of an x-y
recorder, either measured redox current (converted to voltage) or scan voltage
can be selectively displayed on a 2 VDC digital panel meter (DPM) located on
the front of the 264A. The user may then manually record and interpret the
results displayed during the analysis. Obviously, neither of these output options
lend themselves to convenient automation.
To monitor the redox current produced during a scan, connections were
made to the appropriate pins of the Model 264A panel meter (see Table 5-10)
and signals transmitted to an analog input channel on the data acquisition and
control system through a 9 pin ribbon cable. The scan voltage is monitored by
connection to the electrometer monitor on the rear panel of the 264A,
transmitted through the ribbon cable, and analyzed on a separate analog input
channel.

109
Monitoring these analog signals does not take place continually but only
during the time of the analysis scan (stripping phase). On the Model 264A, the
onset of the scan is signaled to the user by powering a light emitting diode
(LED) located on the unit’s front panel. Monitoring the voltage drop across this
LED provides a convenient means of detecting when a scan has begun. This
signal thus acts as a hardware trigger to notify the lead-in-air monitor’s software
to begin recording the scan results. When the LED is deactivated, recording of
the scan is terminated and the recorded data is analyzed.

CHAPTER 6
DESCRIPTION OF FLUID HANDLING SYSTEM
Design of the lead-in-air monitor’s particle collection and lead analysis
section were based on the use of a liquid collection substrate. Specifically,
lead-based aerosols are deposited in 50 ml of 0.5M nitric acid with a 200 ppb
copper internal standard. Use of liquid substrates dictates the need for a liquid
storage system, an accurate and repeatable liquid delivery system, and a waste
disposal system. In addition, the static type cell of the commercially available
polarograph must be replaced with a flow-through type cell. All system
components must be compatible with the acidic solution and not contaminate
the solution. Ideally, the liquid handling system would represent a closed
system thus minimizing possible contamination from the outside environment.
In this section, the details of the liquid handling system will be discussed.
Figure 6-1 is a schematic of the liquid handling system that was devel¬
oped based on the monitor’s requirements. Component descriptions are
presented in Table 6-1. To minimize fluid contamination, all tubing and com¬
pression fittings used in the liquid handling system are composed of teflon. The
nitric acid electrolyte is stored in a 5 liter capacity teflon reservoir. To ensure
that the existing electrolyte supply is sufficient for a sampling series, a
no

111
To Waste
Container
(18)
Figure 6-1. Schematic of Module 1 liquid handling system.

Table 6-1
Listing and Description of Liquid Handling Components
112
Figure 6-1 Code
1
2
3
4
5
6
7
8
9
10
11
Description
Teflon Bottle, 5 Liter Capacity
Fisher Scientific, Model 02-892-50H
Teflon Bulkhead Union, 1/4 in. Tube
Cole Parmer, Model N-06482-34
Teflon 1/4 in. Tube, 8 1/2 in.
Cole Parmer, Model N-06375-02
Teflon 1/4 in. Tube, 7 7/8 in.
Teflon Male Adaptor Elbow, 1/4 in. Tube
to 1/8 in. NPT(M)
Cole Parmer, Model N-06374-12
Liquid Pump, Positive Displacement
120 VAC, 14.2W
Valcor Scientific, Model SV602C115PV
Nalgene Tube, 5/16 in. O.D., 3/16 in. I.D.,
9 in.
Fisher Scientific, Model 14-176-14
Drying Tube, 4 in. with Glass Wool
Fisher Scientific, Model 09242A
Teflon 1/4 in. Tube, 12 1/2 in.
Teflon Male Adaptor, 1/4 in. Tube to
1/8 in. NPT(M)
Cole Parmer, Model N-06374-02
Teflon Nipple, 1/8 in. NPT(M)
Cole Parmer, Model 06483-00

113
Figure 6-
12
13
14
15
16
17
18
19
Table 6-1--continued
Code
Description
Teflon 1/4 in. Tube, 12 in.
Teflon Flow Through Cell
Machine to Specifications
Teflon 1/4 in. Tube, 5 in.
Teflon 1/4 in. Tube, 2 3/8 in.
Teflon Elbow Panel Mount
Cole Parmer, Model N-06379-69
Teflon 1/4 in. Tube, 22 in.
Nalgene Polypropylene WM Bottle
10 liter Capacity
Fisher Scientific, Model 02-961-65A
Polysulfone Level Switch
Gems Services, Model A76147

114
polysulfone fluid level switch has been installed near the base of the reservoir.
The status of the level switch is monitored through the data acquisition and
control system. At the top of the reservoir, two bulkhead tube fittings have
been installed to provide for the fluid transfer and corresponding vent makeup
air. To avoid possible contamination of the reservoir, this makeup air is filtered
through a drying tube packed with glass wool.
Careful consideration was given to selection of the system’s fluid han¬
dling pumps. Since lead mass is estimated from the product of the measured
lead concentration and the liquid volume, the exact liquid volume dispensed to
the impactor must be known. A liquid pump of selectable delivery rate and
possessing high repeatability was required. The pumps must be self-priming,
be compatible with the acidic solution, meet cost requirements, and be adapt¬
able to computer-based power control.
Given these considerations, three identical fluid metering pumps were
purchased (Valcor Scientific, Model SV602C115PV) and incorporated into the
system. These pumps are solenoid operated, positive displacement types with
polypropylene and glass wetted surfaces. Application of 115 VAC power to the
solenoid coil provides for one-half of the pumping cycle and de-energization of
the coil completes the pumping cycle. The pump may be cycled up to 120
cycles per minute. Digital signals to solid-state power relays establish the
pumping rate. In addition, the pump’s piston stroke length can be selected
using a manual adjustment screw. Thus, the overall fluid delivery rate (up to

115
120 ml/rnin) can be controlled by proper combination of the piston stroke
length and the rate of the applied power cycle. The repeatability of these
pumps has been measured to be within 2%.
Once 50 ml of the electrolyte is dispensed to the impactor and the air
sampling run completed, the solution is transferred to the polarograph for
analysis. In the commercial polarograph, 10 to 15 ml of the solution to be
analyzed is normally placed in a static cup and a teflon coated stirring bar
placed in the cup. The cup is then installed in the polarograph to immerse the
electrodes in the solution. A spring-loaded metal support is then positioned to
support the cell. To provide for solution stirring during the deposition step, an
EG&G Model 305 stirrer is placed under the cell. After each separate analysis,
the cup must be removed, cleaned, filled with a new solution and the installation
and analysis steps repeated. Since these steps would be difficult to automate,
a flow-through cell was designed and machined to replace this static cell
arrangement.
Figure 6-2 is a detail drawing of this flow-through cell. The unit is
cylindrical in cross-section and was machined from teflon. A separate 0.55 inch
diameter disk was machined and is press-fit within the neck of the cell and
supports a star-shaped stirring bar (Fisher Scientific, Model 14-511-96A). The
top section of the cell was machined to seal against the o-ring of the polarogra-
ph’s electrode section when the cell is supported by the Model 305 stirrer.

116
2.00
1.45
1.00
0.55
i
Title
Part No.
Material
Flow-through Cell
DRW-6
Teflon
Date
Scale
Aug. 30, 1991
Approximate
R.W. Vanderpool
Dimensions are in inches. Tolerances plus
or minus 0.01 inches unless otherwise noted
Figure 6-2. Detail drawing of flow-through cell designed for the polarograph.

117
Once installed, the flow-through cell need not be removed except during
periodic maintenance of the electrodes. Fluid is introduced into the cell through
the polarograph’s plastic electrode support block which has been drilled and
tapped to accept a male tubing adaptor. Since the capacity of the flow¬
through cell is approximately 22 ml, the entire 50 ml contents of the impactor
cannot be totally transferred to the cell. Therefore, approximately 35 ml is
rinsed through the cell by simultaneous operation of liquid pumps 2 and 3.
Liquid pump 3 is then deactivated and the remaining 15 ml fills the cell for
analysis. Since the polarograph measures lead concentration rather than
absolute lead mass, the exact volume of solution analyzed is not critical.
Once the analysis in completed, the liquid handling undergoes a
complete acid rinse cycle using 50 ml of the electrolyte. This includes a
n
10 second air sampling period to thoroughly rinse the wetted surfaces of the
teflon impactor. Fifteen milliliters of the electrolyte remains in the flow-through
cell to ensure that the reference electrode does not dry out. Prior to the next
sampling and analysis test, this entire rinse cycle is automatically repeated.
Rinsing the liquid components twice between sampling runs has proved to be
effective in minimizing contamination from one test run to another. Because
each sampling run includes two rinse cycles, 150 ml of electrolyte is consumed
for each test run. The 5 liter container thus has sufficient capacity for
approximately 30 runs before a low level condition is indicated by the reservoir’s
fluid level switch.

118
Recall that nitrogen purging of the cell’s contents Is required to remove
the electroactive influence of any dissolved oxygen. Figure 6-3 is a schematic
of the nitrogen handling system with component descriptions provided in
Table 6-2. Nitrogen is supplied from a disposable cylinder with a capacity of 34
liters at standard temperature and pressure. A 0-500 psig gauge at the cylinder
outlet allows inspection of the cylinder’s current nitrogen supply. A regulator at
the cylinder exit provides a nitrogen output pressure of 20 psig. The gas then
passes through a normally-closed 115 VAC activated solenoid valve. Although
the polarograph itself contains a nitrogen flow solenoid valve, it merely directs
the nitrogen gas either through the cell contents or over the liquid surface.
Without the additional solenoid to supply the nitrogen only when needed, the
limited nitrogen supply would soon become depleted.
Nitrogen flow through the polarograph is adjusted and monitored using a
0 to 100 cc/min capacity rotameter. Although the actual flowrate is not critical,
the nitrogen flowrate should be adjusted to be between 30 and 50 cc/min.
Once the rotameter is set, it does not normally require readjustment until the
nitrogen cylinder need be replaced. Based on the nitrogen purge requirements
of each analysis cycle, the nitrogen cylinder need be replaced only after
approximately 200 separate analyses.
Figure 6-4 is a wiring diagram of the components associated with the
nitrogen handling system. Component descriptions and sources are listed in
Table 6-3. Connector pin descriptions are presented in Table 6-4.

119
Figure 6-3. Schematic of Module 1 nitrogen handling system.

120
Table 6-2
Listing and Description of Nitrogen Handling Components
Figure 6-3 Code
Description
1 Ultra-High Purity Nitrogen
Certified >99.999 mole %
500 psig, 34 liters at 70 °F
Alphagaz, Cylinder Size 7D
2 Regulator, Delivery Pressure = 20 psig
with 0-500 psig Guage, CGA 600 Outlet
Alphagaz, Model 713
3 Norprene Tubing, 5/16 in. O.D., 3/16 in I.D.
Fisher Scientific, Model 14-169-25D
4 Delta Solenoid Valve with Teflon Wetted
Parts, 115 VAC, 0.15A, 1/8 in. Ports
2-Way Normally Closed
Fluorocarbon, Model DV2-122NCA1
5 Rotameter, Brooks Instr. Co., Model 1350
with R-2-65A Tube and Sapphire Float.
Flush Panel Mounted.

K)
Figure 6-4. Wiring diagram of Module 1 electrical components.

Table 6-3
Module 1 Electrical Component Listing and Description
Figure 6-4 Code
1
2
3
4
5
6
Description
Barrier Terminal Block
3 Contact, Double Row, 20A
Cinch, Inc.
Type 3-141
Solid State Relay, 240 VAC/25A
3-32 VDC Input
Potter and Brumfield
Type SSR-240D25
Liquid Pumps, 125 VAC
Valcor Scientific
Type SV602C115PV
Electromechanical Relay, 125 VAC
15mA, DPDT, 10A at 125 VAC
Radio Shack
Type 275-217
Delta Solenoid Valve with Teflon Wetted
Parts, 115 VAC, 0.15A, 1/8 inch Ports
2-Way Normally Closed
Fluorocarbon, Model DV2-122NCA-1
Quick Connector
Amphenol
2 Circuit Pin Housing, type 1-480319-0
2 Circuit Pin Socket, type 1-480318-0
Contacts, 24-18 AWG, types 60618-1
and 60617-1
Polysulfone Fluid Level Switch
Gems Sensor Division Model A76147

123
Table 6-4
Module 1 Electrical Connector Pin Descriptions
Pin
Color
575 Channel
BB-1
RED
DIGOUTO
BB-2
GRN
ANIN2
BB-4
GRN
GROUND
BB-5
BLU
DIGOUT1
BB-6
GRY
DIGOUT2
BB-7
PUR
DIGOUT3
BB-8
WHT
DIGOUT4
BB-9
YEL
ANOUTO
BB-10
PNK
DIGOUT5
BB-11
ORG
DIGOUT6
BB-12
BLK
DIG0UT7
Function
Powers Fluid Level Switch
Reads Fluid Level Switch
Ground
Activates Nitrogen Solenoid
Activates LP1 for Impactor Fill
Activates LP2 for Impactor Empty
Activates LP3 for Cell Empty
6 VDC to Decade Board
Initiates Purge Function
Initiates Stir Function
Initiates Drop Dislodge/Dispense

CHAPTER 7
PROGRAM DESCRIPTION AND OPERATION
In the lead-in-air monitor, automated sequencing of the system’s
components takes place using a Kiethley 575 data acquisition and control
system interfaced with a PC-Brand 286/25 IBM-compatible computer.
Interaction between the computer and the data acquisition and control system
takes place through a Kiethley data acquisition interface card which was
installed inside a vacant 8 bit slot within the computer. The KDAC500 software
package was then installed on the computer’s 20 megabyte hard drive.
In the Kiethley 575 system, the user can access the various input/output
module channels using the Kiethley software linked with a GW-Basic
programming environment. Installation of the KDAC500 software requires the
user to specify configuration options which include channel input/output names
for each module channel. Individual channels are accessed through machine
language call statements which use channel names as arguments. A listing of
the names chosen for the lead-in-air monitor is presented in Table C-1 in
Appendix C. For a complete listing of the configuration settings, the user may
view the contents of the CONFIG.TBL file located on the computer’s hard drive.
Operation of the lead-in-air monitor is controlled through a single GW-
Basic program, "MAIN", which has been written for this purpose. This program
124

125
was installed on the hard drive and automatically loads and executes when the
computer is powered up. A complete listing of this program is provided in
Appendix D.
Program execution begins by initializing program variables (such as
standard pressure, nitrogen purge time, etc.), dimensioning basic arrays, and
initializing the digital logic board to deactivate purge, stir, and dislodge/dispense
functions. The user is then presented with the main program menu of operating
options. This allows selection of either single or continuous sampling analysis,
analysis of contents of polarographic cell, various fluid handling options, view or
print of previous saved results, or an option to exit the program.
The single sampling and analysis option is chosen if the user wishes to
perform single point analysis at various sampling locations within the battery
plant. The unattended sampling and analysis option allows the user to perform
multiple sampling and analyses tests at the same sampling location. In either
case, the user is first prompted to enter pertinent sampling conditions at the
desired point of sampling. These inputs include measured stack gas
temperature and stack gas velocity pressure which are necessary to calculate
the stack gas velocity using the equation
v =
KCpJVp^
Ps M
(7-1)
where V is the stack gas velocity, K the appropriate units constant, Cp is the
pitot tube correction factor, Vp is the measured velocity pressure, and T, Ps, and

126
M are the stack gas temperature, static pressure, and molecular weight,
respectively. In the program, values of stack gas pressure and molecular
weight are assumed for standard air. The value of the pitot tube correction
factor (0.99) assumes use of a standard pitot tube for velocity pressure
measurement. If needed, the appropriate program lines may be rewritten to
modify these assumed values.
Based on the calculated velocity, the program computes the ideal nozzle
diameter necessary to achieve isokinetic sampling. The user is then prompted
to enter the diameter of an available nozzle close to this ideal size. If this
selected diameter requires a flowrate outside the sampling system’s 10 to 30
liters per minute design range, the user is prompted to modify the selection. If
static (still air) sampling is to be performed, the user is prompted to enter a zero
value for the velocity pressure. A fixed 15 actual liters per minute sampling
flowrate is used for all static sampling tests.
Prior to the air sampling, a complete rinse of the liquid handling
components is performed by proper sequencing of the liquid handling pumps.
The status of the electrolyte level switch is also checked at this time to ensure
that the available electrolyte supply is sufficient for a complete sampling cycle.
Once the rinse is completed, 50 ml of the electrolyte is transferred to the
impactor.
Based on the required nozzle volumetric flowrate, the mass flowrate
required by the mass flow controller is calculated. The appropriate analog

127
command voltage is signaled to the mass flow controller to set the position of
the solenoid valve. A one volt command signal is equivalent to 10 liters per
minute at 32 °F. The air pump is then activated and sampling is performed for
15 minutes unless the test is manually aborted by the user. At ten second
intervals during the sampling, the measured sampling flowrate is monitored from
the mass flow controller output and this value stored in an array created for this
purpose. At the end of the sampling period, the air pump is turned off and the
average flowrate computed from the array of measured values.
Once the air sampling is completed, the liquid solution is transferred from
the impactor to the polarograph cell for lead analysis. The cell’s contents are
first purged with nitrogen by activating the normally-closed solenoid for three
minutes. During the purge cycle, activation of the STIR function on the digital
logic board provides for stirring of the solution. The program then activates the
RUN function on the RUN/STOP circuit board to initiate a polarographic
analysis. Following the required deposition step to deposit the aqueous lead
onto the surface of the electrode, the stripping step is initiated to quantify the
lead concentration. Once this scan is detected, the resulting current versus
voltage readings are recorded every 0.2 seconds and stored in separate arrays.
Typically, a full polarographic scan requires 80 seconds to complete. When the
scan is completed, the readings are terminated and the current and voltage
arrays analyzed.

128
In polarography, the position of the scan peaks identifies the analyte
present while its peak height is proportional to its concentration in solution. In
the lead-in-air monitor, two separate primary peaks will be observed, one
corresponding to the collected lead and the other corresponding to the internal
copper standard. The peak heights are determined by examining the contents
of the current and voltage arrays. As discussed, the ratios of the peak heights
rather than their absolute heights are used to quantify the lead concentration in
solution.
Prior to the analysis, the decade resistance board sets the scan range to
the value appropriate for lead concentrations expected during occupational or
recirculation air monitoring. In this range, the response to the 200 ppb copper
internal standard is typically about 1.6 volts but can vary by approximately 50%.
If the response is less than 0.3 volts, however, it signals that either the
electrolyte was improperly prepared or that a discontinuity exists in the mercury
column. In this event, the digital logic board is activated to initiate fifteen
mercury drop dispense/dislodge cycles to reestablish the mercury column
continuity. The lead analysis scan is then repeated. If the problem persists, the
operator is prompted to correct the problem.
Alternatively, if the actual lead concentration is higher than approximately
2000 ppb, an overrange condition will occur and the decade board will
automatically reduce the output amplifier gain by a factor of ten. The analysis
will then be repeated.

129
Once the solution’s lead concentration is quantified, the lead-in-air
concentration is calculated from the average flowrate, sampling time, liquid lead
concentration, and solution volume. Reported lead concentration units of
micrograms per cubic meter are based on a standard temperature of 25 °F.
A summary of the analytical results is presented on the video display for
the user’s inspection. Reported are values of liquid and air lead concentration,
air volume sampled, height of lead and copper peaks, and value of the percent
isokinetic during the sampling run.
Whether operating in single point sampling mode or unattended
operation, the test results are then automatically stored on the computer’s hard
drive for later inspection. Rather than requiring the user to enter a separate
filename for each test run, the program reads the computer’s internal clock and
uses the current date as the filename. For successive runs performed on the
same test date, the program simply adds the new test results to the same
random access file. The information saved for each test run includes the test’s
starting time, test duration, average flowrate, liquid and air lead concentrations,
and a test run description. This description is entered by the user at the start of
the sampling run and may contain up to 30 characters.
Following storage of the test results, the liquid handling system then
undergoes a complete rinse cycle. If single point sampling had been
performed, the user is returned to the main program menu. If the instrument is
currently operating in unattended sampling mode, the complete sampling and

130
analysis cycle is repeated. Unattended operation will continue until manually
aborted or until the electrolyte supply is insufficient for continued operation. In
the latter event, the user is prompted to refill the reservoir to allow for continued
operation.
In the main menu, a fluid handling option exists which presents the user
with a separate menu of various fluid handling options. The user is able to
either perform a main system rinse cycle or operate any of the three liquid
pumps to either fill the impactor, empty the impactor, or empty the
polarographic cell. These latter options are useful if the user wishes to
periodically verify the calibration of the liquid handling pumps. Manual control
of the sampling pumps is also useful should a power outage occur and
interrupt proper sequencing of the fluid handling components.
A separate main menu option enables analysis of the polarographic cell
contents without any air sampling. This option can be used to verify the
polarograph’s response to the internal copper standard. Alternatively, this
option can be used to check the analysis accuracy of a lead standard sample
introduced into the cell.
The final main menu option enable the user the view or print previously
saved test results. All tests results are stored in the subdirectory
"C:\K500\RESULTS" created for this purpose. Using a separate menu, the
user can request a listing of existing file names. The contents of a particular file
may either be viewed on the computer’s monitor or a hard copy listing of the

131
file made. Note that printing previous test results requires the user to connect
the computer to a parallel dot-matrix or letter quality printer.

CHAPTER 8
FIELD EVALUATION OF PROTOTYPE MONITOR
Introduction
Accurate evaluation of lead-in-air concentrations requires accurate air
sampling, particle transport and collection, and lead analysis. In previous
sections, the details of each of these instrument subsystems has been
described in detail. Laboratory evaluation of these subsystems suggested that
they each performed approximately as designed. In order to fully evaluate the
capabilities of the complete instrument, however, field tests were conducted in a
battery plant under conditions of the instrument’s intended use. Although the
primary intent of the field tests was to evaluate the ability of the monitor to
quantify lead-in-air concentrations, the field tests were also designed to evaluate
the instrument’s overall ruggedness, portability, and the extent to which
unattended operation could be expected.
Experimental Methods
Prior to the field tests, all field sampling equipment and sample
containers were prewashed with 6M nitric acid, rinsed in D.l. water, and air
dried. Individual collection vials, filter holders, and sampling nozzles were
132

133
sealed in separate press-lock style plastic bags. Glass fiber filters to be used
for the field tests were preheated at 300 °F for two hours then stored In a
desiccator until the time of their use. Three of these filters were later selected
at random and subjected to extraction procedures to determine their
background lead content. As measured by GFAA, the lead content of these
filters was found to be insignificant compared to the lead mass collected during
the field tests.
As quality control checks, a series of lead standards was prepared in the
laboratory prior to the field tests. These samples consisted of 0, 100, 200, and
300 ppb lead standards prepared in 0.5M nitric acid with a 200 ppb internal
copper standard. All samples were stored in prewashed polypropylene
containers. A separate container of the 100 ppb lead standard was prepared
and was used periodically in the field to verify the accuracy of the monitor’s
analytical section. One set of the 0 to 300 ppb lead standards was stored in
the laboratory at 4 °C and was used as laboratory standards to check the long¬
term stability of lead solutions stored in this manner. A second set of these 0 to
300 ppb standards was used as field control standards which were transported
to the field site but not opened during the week of testing. Use of field
standards was designed to check for any inadvertent container contamination
which might occur at the testing site.
Field evaluation of the lead-in-air monitor occurred during the week of
July 15-19, 1991 at a battery plant in the southeast United States. All sampling

134
equipment preparation and storage took place in a quality control laboratory
within the battery plant. The possibility of sample contamination by trace
quantities of lead required the use of an area as isolated from the battery
production process as possible. Sample contamination within this quality
control laboratory was expected to be minimal.
Upon arrival at the battery plant, an initial check of the monitor’s
condition revealed two key components were inoperable. First, the nitrogen
solenoid valve did not respond when control power was applied. This solenoid
was replaced in the field with a spare unit. The second malfunction
encountered involved the liquid metering pump which dispenses electrolyte to
the impactor prior to air sampling. Inspection of the unit revealed that the
pump’s piston would not move when the pump’s coil was activated. As a
result, no dispensing of the electrolyte could occur. Once the pump was
disassembled, its components cleaned, and reassembled, the problem did not
reoccur during the week of field tests. No additional operating problems with
the lead-in-air monitor were encountered during the remainder of the week’s
testing.
The majority of the field tests were performed at the process site where
the dried, pasted grids are manually off-loaded from the conveyor belt and
stacked onto platens for later transport to the curing ovens. This process site
was chosen because it represented a site of aerosol production similar to that
expected in recirculation air systems in terms of the aerosol’s size distribution

135
and concentration. Unlike some other potential sampling sites, this site allowed
sampling without interfering with the activities of the plant personnel. Figure 8-1
is a photograph of the approximate position of the lead-in-air monitor in relation
to the plate off-bearing process.
In order to determine the accuracy of the lead-in-air monitor, collocated
total filter sampling was performed during the majority of the field tests. As
shown in Figure 8-2, an aluminum filter holder was positioned next to the
monitor’s sampling inlet. The filter holder has a circular inlet with a diameter of
1.375 inches. Glass fiber filters of 47 mm diameter (Gelman, A/E 61631) were
used for these tests and display essentially 100% collection efficiency
independent of particle size or flowrate. The filters were loaded and unloaded
in the battery plant laboratory and the filter holder covered with a plastic bag
until just prior to sampling. During the week of testing, three blank filters were
separately loaded and unloaded into the filter holder without any air sampling in
order to measure possible contamination during the filter handling. Subsequent
lead extraction and analysis of these filters showed that total filter contamination
was not significant.
Flowrate through the total filter was provided by connection to an EPA
Method 5 sampling box which allowed control of the flowrate and measured the
total volume of air sampled during the sampling run. For the static sampling
tests, the total filter flowrate was adjusted to equal that of the lead-in-air monitor.

136
Figure 8-1. Photograph of lead-in-air monitor during tests conducted at plate
offbearing process.

137
Figure 8-2. Photograph of Module 1 inlet section showing position of collocated
filter holder relative to Module 1 inlet nozzle.

138
For the duct sampling tests, the total filter flowrate was adjusted to achieve
isokinetic sampling through a 0.42 inch diameter inlet nozzle.
During the week of field tests, fourteen separate sampling runs with
collocated filter sampling was performed in the region of the plate off-bearing.
To determine the unattended operation capabilities of the monitor, ten
unattended sampling runs were performed in this area. Four collocated static
sampling runs were also performed in the area of the paste drying oven along
with nine unattended tests in this area. Lastly, three collocated sampling runs
were performed inside a 10 inch diameter exhaust duct at a plate stacking site.
After each test series, the sampling equipment was returned to the
battery plant laboratory. To quantify aerosol transport losses, the Module 1
stainless steel inlet nozzle and teflon inlet tube were removed and their inner
surfaces thoroughly rinsed with approximately 100 ml of 0.5M nitric acid with a
200 ppb internal Cu standard. Prior to their reuse, all rinsed components were
dried in an oven at 250 °F. The rinses were transferred to separate 150 ml
capacity screw-capped polypropylene containers which had been previously
cleaned with nitric acid. The particle losses to the total filter nozzle inlet were
quantified in a similar manner. All rinse containers were labeled, placed in a
lock-tight polypropylene container, and stored at 4 °C until the time of their
analysis. Collection filters were placed in separate 150 ml capacity wide-mouth
polypropylene containers previously washed with nitric acid. The containers

139
were labeled and later served as preparation containers during lead extraction
in the laboratory.
Following the week of field testing, all equipment was returned to the
laboratory. The outside surfaces of all rinse and filter containers were wiped
with a 0.5M nitric acid-saturated cloth before the containers were opened. The
collected filter samples were extracted in the following manner. Each filter
container received 10 ml of 2.5M nitric acid, followed by a 15 minute water bath
sonication, followed by a 40 ml addition of D.l. water containing 250 ppm
copper standard. The composition of this resulting solution was thus 0.5M
nitric acid with a 200 ppb internal copper standard. This solution received an
additional 15 minute water bath sonication prior to analysis.
The collected nozzle rinse and extracted filter solutions were analyzed for
their lead content using both polarography and GFAA. Three separate analysis
were performed for each sample using each analytical technique. Laboratory
standards, field standards, and field control samples were also analyzed at this
time.
Experimental Results
Prior to analyzing the collected field samples, the 0 to 300 ppb laboratory
and field standards were analyzed using both GFAA and polarography. For
each technique, three separate analysis were performed for each sample.
Tables 8-1 and 8-2 present measured results of the laboratory standards and

140
Table 8-1
Analysis of Laboratory Lead Standards
Lead Cone. foDbl
Run No.
PolaroaraDhv
GFAA
0
1
9
0
2
7
1
3
6
0
Avg
7
0
100
1
99
110
2
100
106
3
99
109
Avg
99
108
200
1
194
218
2
195
212
3
195
220
Avg
195
217
300
1
298
333
2
295
321
3
296
327
Avg
296
327

141
Table 8-2
Analysis of Field Control Lead Standards
Lead Cone, fppbl Run No. Polaroaraphv GFAA
0
1
11
0
2
12
0
3
9
Avg
11
0
100
1
100
111
2
99
108
3
100
109
Avg
100
109
200
1
192
226
2
195
218
3
194
226
Avg
194
223
300
1
292
336
2
291
324
3
293
324
Avg
292
328

142
field control standards, respectively. As shown in the tables, the two techniques
generally agreed with each other within approximately 10%. The polarography
measurements, however, were generally more accurate and displayed greater
repeatability than the GFAA analysis. The similarity between the laboratory
standards and the field standards indicates that the field containers did not
experience significant contamination during the week of field testing.
Collected field filter blanks and nozzle blanks were also analyzed at this
time. Results showed that the background lead content of the Module 1
stainless steel inlet, the impactor teflon inlet tube, and the 47 mm filter holder
inlet were near the detection limit of the two techniques.
Table 8-3 presents results of the fourteen collocated tests conducted at
the plate offbearing process. Presented are the lead concentrations reported
by the lead-in-air monitor versus that concentration calculated from the
measured filter lead mass and the sampled air volume. Results showed that
the monitor’s reported concentration agreed well with the total filter
measurement. In the measured range of 8 to 30 micrograms/m3, the two
values never differed by more than 13%. All measured values were within the
occupational permissible exposure limit of 50 micrograms/m3. For the fourteen
tests, the average accuracy ratio was 95% with a relative standard deviation of
8.2%. The measured lead mass associated with the inlet rinse represented 4%
of the total aerosol sampled. It thus appears that the lead-in-air monitor and
the total filter sampler aspirated aerosols of similar mass concentrations.

143
Table 8-3
Results of Collocated Sampling Performed at Plate Offbearina Operation
Lead Cone, (micrograms/m3)
Run No.
Lead-in-Air
Monitor
Total Filter
Samóle
Ratio
1
26
28
0.93
2
26
30
0.87
3
21
23
0.91
4
21
22
0.95
5
21
22
0.95
6
9
8
1.13
7
14
15
0.93
8
20
23
0.87
9
19
21
0.90
10
16
16
1.00
11
12
11
1.09
12
13
13
1.00
13
6
7
0.94
14
7
8
0.88

144
An additional ten sampling runs were performed in the area of the plate
offbearing. For these tests, the lead-in-air monitor was setup in unattended
operating mode and run for five hours without input from the operator. No
operational problems were experienced during these tests. Results of these
tests are shown in Table 8-4.
Tests were then conducted in the area of the paste drying oven. In this
area, three separate collocated filter tests were conducted. Results presented
in Table 8-5 again demonstrate the accuracy of the lead-in-air monitor. Note
that the monitor was capable of detecting the 78 micrograms/m3 excursion
which followed a cleaning cycle of the plate pasting equipment. Following these
tests, nine additional tests were performed in this area with the monitor
operating in unattended mode. Results of these tests are presented in
Table 8-6. Following the ninth test, the monitor correctly detected that the
electrolyte supply was insufficient for continued operation and notified the
operator of this condition.
The final test series was conducted in the region of the plate stacking
operation. In this operation, paper separators and pasted plates are manually
loaded into a stacking machine which automatically places the separators
between successive plates. Sampling was performed in a 10 inch diameter
circular duct which exhausts aerosols generated from the process. A sampling
port was installed in a 90° bend located approximately six feet downstream of
the process. The stack gas velocity pressure, static pressure, and temperature

145
Table 8-4
Results of Unattended Sampling Performed at Plate Offbearing Operation
Run No.
1
2
3
4
5
6
7
8
9
10
Lead Cone.
micrograms/m3
17
16
17
11
16
9
18
11
25
22

146
Table 8-5
Results of Collocated Sampling Performed at Paste Drying Operation
Run No.
1
2
Lead Cone, (micrograms/m3)
Lead-in-Air
Total Filter
Monitor
Sample
Ratio
76
78
0.97
24
26
0.92
18
19
0.95
3

147
Table 8-6
Results of Unattended Sampling Performed at Paste Drying Operation
Run No.
1
2
3
4
5
6
7
8
Lead Cone.
mlcroqrams/m3
24
17
23
19
24
21
16
22
9
22

148
were measured to be 0.43 inches of water, 29.91 inches of mercury, and 89 °F,
respectively.
Three collocated filter tests were performed in this area. For the lead-in¬
air monitor, a 0.185 inch diameter stainless steel nozzle was used in conjunction
with a 39 inch long teflon-lined sampling probe of 0.88 inch inside diameter.
For the comparative filter tests, a 0.242 inch diameter stainless steel nozzle was
used in conjunction with an in-stack stainless filter holder. Both nozzles were
located approximately at the duct centroid and were oriented directly into the
airstream. Each of the three tests were conducted for a fifteen minute time
period. At the end of the test series, the nozzles and teflon probes were
carefully rinsed for their lead content.
As shown in Table 8-7, a significant difference was observed between the
monitor’s results and those calculated from the filter’s lead content. Upon first
inspection, it was believed that nozzle and probe losses would explain the lead-
in-air monitor’s observed underestimation of the lead concentration. However,
analysis of the monitor’s nozzle, probe, and inlet section lead deposits following
this test series showed that only 11% of the sampled aerosol was lost to these
surfaces. Probe losses accounted for 7% of the total losses.
It thus appears that the two samplers aspirated significantly different
aerosols during the sampling tests. This difference could be possibly explained
by the fact that the nozzles were not exactly collocated but were separated by
approximately 3 inches. Since the point of sampling was close to the source of

149
Table 8-7
Results of Collocated Sampling Performed at Plate Stacking Operation
Run No.
1
2
Lead Cone, (micrograms/m3)
Lead-ln-AIr
Total Filter
Monitor
Samóle
Ratio
349
697
0.50
1084
2831
0.38
1323
5545
0.24
3

150
aerosol generation, the aerosol may not have been well mixed at the point of
sampling. The noted concentration differences may also have resulted due to
inadvertent anisokinetic sampling. Considering the large size of the particles
produced at this process, anisokinetic sampling could be responsible for a
significant fraction of the observed discrepancy. The total filter measurements,
therefore, do not accurately gauge the performance of the lead-in-air monitor
during these tests. In the absence of an accurate comparison measurement,
the total lead mass balance within the lead-in-air monitor’s sampling system
must be relied upon. For this limited test series, results showed that monitor
quantified 89% of the sampled aerosol. Transport losses in the nozzle, probe,
and impactor inlet tube accounted for the remaining 11% of the sampled
aerosol.

CHAPTER 9
SUMMARY AND RECOMMENDATIONS
A prototype sampling and analysis system has been developed for
quantifying lead-based aerosols in the lead-acid battery industry. Design criteria
for the instrument were based on measured size distributions and chemical
properties specific to aerosols generated during lead-acid battery production.
Separate prototype subsystems of air sampling, particle collection, liquid
handling, and lead analysis were designed and have been described in detail.
Laboratory evaluation of these subsystems verified that they perform essentially
as designed.
Field evaluation of the lead-in-air monitor in a battery plant verified that
the overall design performed well under conditions of its intended use. For the
seventeen collocated static sampling tests performed at two process locations,
the mean accuracy of the monitor was measured to be 95% with a relative
standard deviation of 7%. Analysis of aerosol losses within the sampling nozzle
and impactor inlet tube accounted for the slight deviation from ideal
performance. These tests verify that the instrument’s particle collection section
and lead analysis section perform as designed.
A total of 19 separate static sampling tests were performed at two
process locations with the monitor operated in unattended mode. During these
151

152
tests, the unit’s software provided for automated sequencing of the sample and
analysis cycles without input from the operator. Test results were automatically
stored on the computer’s hard drive for later retrieval and inspection. Mass
balance studies of particle transport losses verified that only 4% to 6% of the
aspirated aerosol is not quantified due to transport losses. No operational
problems were experienced during these unattended tests of the prototype
monitor.
A limited series of tests was performed at a plate stacking operation to
evaluate the monitor’s ability to quantify lead-based particle concentrations in
flowing airstreams. Collocated filter sampling indicated that ducted aerosols
near the point of their generation may not be uniform across the duct’s cross-
section. Anisokinetic sampling of large particles in high velocity airstreams can
also result in significant measurement error. Due to expected particle bounce
and reentrainment within the transport system, actual particle losses were
significantly lower than those predicted from worst-case theoretical
considerations. As described, recommended modifications to the sampling
system may further reduce transport losses with an accompanying increase in
the overall accuracy of the monitor’s reported results.
The prototype monitor was constructed to verify the overall design
approach of an instrument capable of quantifying lead-based particles in the
lead-acid battery industry. Laboratory and field evaluation of the prototype
confirmed the validity of this approach. A number of recommendations can be

153
made, however, to improve the instrument’s overall performance and reliability.
These recommendations should be considered during any future phase of its
development.
The primary intended application of the monitor is to serve as an
unattended on-line monitor of recirculation air quality. As such, the primary
limitation of the prototype instrument is its limited supply of nitric acid electrolyte
and nitrogen purge gas. In the current design, the electrolyte and nitrogen
supply must be replenished after every 30 and 200 separate analysis runs,
respectively. Providing larger available supplies of these two materials would
significantly extend the long-term capabilities of the instrument thus requiring
less periodic attention from the operator.
Due to intermittent problems experienced with the liquid handling pumps,
it is recommended that they be replaced with pumps of greater reliability and
precision. Digitally controlled precision peristaltic pumps should be considered
as possible alternatives. Use of extended-life norprene tubing would minimize
the frequency with which the pump’s tubing need be replaced.
Future development of the instrument could be devoted to reducing its
overall size. If the monitor is intended for static or fixed flowrate sampling, the
air sampling system could be reduced in size and simplified. Lower flow
requirements for static sampling would directly translate to lower pumping
capacities. Perhaps the most significant design simplification could be achieved
by developing custom microprocessor-based control circuitry. The use of

154
dedicated control circuitry would eliminate the need for the polarograph’s
control unit, the data acquisition and control system, and the full-sized computer
with its accompanying display monitor. This modification alone would greatly
improve the portability and reliability of the overall instrument design.
A complete operating manual for the prototype lead-in-air monitor is
presented in Appendix E. Included are instructions for setting up the
instrument, procedures for performing initial system checks, and instructions for
instrument operation during both still air and ducted air field sampling.
Instrument maintenance and troubleshooting sections are included in the
manual.

APPENDIX A
DETAIL DRAWINGS OF TEFLON IMPACTOR

Machine to
Title
Part No.
Material
Housing Body
DRW-5
Teflon
Date
Scale
August 30, 1991
1 inch = 2 inches
Dimensions are in inches. Tolerances plus
n.w. vanoerpooi
or minus 0.01 inches unless otherwise noted
156

1.25
10.625
1.20
i8tpi r •
L
0.500
r
1.08
0.375
Tille
Part No.
Material
Central Tube
DRW-4
Teflon
Date
Scale
August 30, 1991
1 inch = 2 inches
R.W. Vanderpool
Dimensions are in inches. Tolerances plus
or minus 0.01 inches unless otherwise noted

158
20 Holes (#71 drill - 0.026")
Title
Drawing No.
Material
Impactor Stage
DRW-3
Teflon
Date
Scale
August 30, 1991
1 inch =
2 inches
R.W. Vanderpool
Dimensions are in inches. Tolerances plus
or minus 0.01 inches unless otherwise noted

159
Drill and Tap for
One Piece to be Made
Title
Drawing No.
Material
Housing Inlet
DRW-2
Teflon
Date
Scale
August 30, 1991
Approximate
R.W. Vanderpool
Dimensions are in inches. Tolerances plus
or minus 0.01 inches unless otherwise noted

APPENDIX B
RESULTS OF IMPACTOR COLLECTION EFFICIENCY TESTS

Table B-1
Results of Impactor Collection Efficiency Tests
Aerodynamic
Particle Diameter
micrometers
Collection Efficiency (%)
10 bm 20 lorn 30 bm
0.05
91
87
78
0.10
57
78
82
0.20
27
30
31
0.36
22
32
36
0.50
30
47
54
0.70
30
47
54
1.00
66
78
82
1.40
82
87
90
2.0
95
95
97
3.2
98
99
99
6.0
99.8
99.9
99.9
10.0
99.9
99.9
99.9
20.0
99.9
99.9
99.9
161

APPENDIX C
CONFIGURATION OF KEITH LEY 575 CHANNELS

Table C-1
Configuration of Keithley 575 Channels
575
Connection
Channel No.
Name
Color
J1
ChO
ANOUTO
YEL
(Analog Out)
Ch1
ANOUT1
BRN
J12
ChO
DIGOUTO
RED
Ch1
DIGOUT1
BLU
Ch2
DIGOUT2
GRY
Ch3
DIGOUT3
PUR
Ch4
DIGOUT4
WHT
Ch5
DIGOUT5
PNK
Ch6
DIGOUT6
ORG
Ch7
DIGOUT7
BLK
Ch8
DIGOUT8
YEL
Connects to:
Function
DD-7
6 VDC to Decade Board
EE-3
0-5 VDC Command Signal to MFC
DD-1
Powers Fluid Level Switch
DD-5
Activates Nitrogen Solenoid
DD-6
Activates LP1 for Impactor Fill
DD-7
Activates LP2 for Impactor Empty
DD-8
Activates LP3 for Cell Empty
DD-10
Initiates Nitrogen Purge
DD-11
Initiates Stir Function
DD-12
Initiates Drop Dislodge/Dispense
EE-1
On/Off Control for Pump/Fan

Table C-1
575
Connection
Channel No.
Name
Color
J1
(Digital Out)
ChO
ANINO
RED
BLK
Ch1
ANIN1
PUR
BLU
Ch2
ANIN2
RED
GRN
Ch3
ANIN3
GRY
GRN
Ch4
ANIN4
RED
GRN
continued
Connects to:
Function
EE-5
EE-4
Reads MFC Output "High"
Reads MFC Output "Low"
CC-1
CC-2
Reads I in I vs. V Scan "High"
Reads I in I vs. V Scan "Low"
DD-2
GND
Reads Fluid Level Switch "High"
Reads Fluid Level Switch "Low"
CC-4
GND
Reads V in I vs. V Scan "High"
Reads V in I vs. V Scan "Low"
CC-3
GND
Checks Status of Scan "High"
Checks Status of Scan "Low"

APPENDIX D
PROGRAM LISTING

10 ’
20 ’ SET VALUE FOR STANDARD PRESSURE (IN HG)
30 PRESSURE = 29.92
40 ’ SET VALUE FOR COPPER STANDARD (PPB)
50 COPPERSTD= 200
60 ’ SET TIME FOR AIR SAMPLING (SEC)
70 SAMPLETIME=900
80 ’ SET NITROGEN PURGE TIME (SEC)
90 PURGETIME = 180
100 ’ SET PITOT TUBE CORRECTION FACTOR FOR STANDARD PITOT TUBE
110 CP = .99
120 ' CHANGE FROM CURRENT DIRECTORY TO "RESULTS" DIRECTORY
130 CHDIR "\":CHDIR "\K500\RESULTS"
140 ’ DIMENSION BASIC ARRAYS
150 DIM XARRAY(800):DIM YARRAY(800):DIM QARRAY(200):DIM BOX%(2)
160 ’
170 ’
180 CLS
190 ’ INITIALIZE AND CALIBRATE DATA ACQUISITION AND CONTROL SYSTEM
200 CALL KDINIT
210 ’ INITIALIZE MODEL 303A PURGE, STIR, AND DISPENSE FUNCTIONS TO
"OFF"
220 VL! (0) =6!
230 CALL FGWRITE’("anoutO",vl!0,"c.volts","nt")
240 VL%(0) = 1
250 CALL FGWRITE’("digout5",vl%0,"c.raw.int","nt")
260 CALL FGWRITE’("digout6",vl%0;,c.raw.int","nt")
270 CALL FGWRITE’("digout7",vl%0,"c.raw.int","nt")
280 ’ "POWER" LEVEL SWITCH USING DIGITAL HIGH SIGNAL
290 VL%(0) = 0
300 CALL FGWRITE’("DIGOUT2",VL%0,"C.RAW.INT","NT")
310 ’ INITIALIZE ARRAYS FOR CONTROLLING LIQUID PUMPS LP1, LP2, AND
LP3
320 BOX%(1) = 1: BOX%(2) = 0
330 CALL ARMAKE’("LPARRAY",2.,"DIGOUT2")
340 CALL ARPUT’("LPARRAY",1.,2.,"DIGOUT2",1,BOX%0,"C.RAW.INT")
350 CALL ARPUT’("LPARRAY",1.,2.,"DIGOUT3",1,BOX%0,"C.RAW.INT")
360 CALL ARPUT’("LPARRAY",1.,2.,"DIGOUT4",1,BOX%0,"C.RAW.INT')
370 ’ DISABLE NON-FATAL ERROR MESSAGES
380 CALL KDWARN’C'WARNOFF")
390 '
400 ’
410 ’ MAIN MENU
420 CLS:CLOSE:SCAN =0:TIMER OFF:LOCATE 1,1:FOR J = 1 TO 10:PRINT
166

167
■•********»;:NEXT j
430 TITLES = "LEAD-IN-AIR MONITOR"
440 LOCATE 2,1:PRINT TAB(40-LEN(TITLES)/2)TITLE$
450 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
460 TITLES = '"MAIN MENU"
470 LOCATE 9,1:PRINT TAB(40-LEN(TITLES)/2)TITLE$
480 TITLES = " "
490 LOCATE 10,1 :PRINT TAB(40-LEN(TITLES)/2)TITLE$
500 LOCATE 12,1
510 PRINT TAB(25)"(1) PERFORM SINGLE SAMPLING AND ANALYSIS TEST"
520 PRINT TAB(25)"(2) UNATTENDED SAMPLING AND ANALYSIS"
530 PRINT TAB(25)"(3) ANALYZE SOLUTION ONLY"
540 PRINT TAB(25)"(4) VIEW OR PRINT PREVIOUS TEST RESULTS"
550 PRINT TAB(25)"(5) FLUID HANDLING OPTIONS"
560 PRINT TAB(25)"(6) EXIT PROGRAM"
570 LOCATE 21,1: PRINT TAB(9);:INPUT "ENTER YOUR
CHOICE";CHOICE:CHOICE=CINT(CHOICE)
580 ’ ELIMINATE INVALID CHOICES
590 IF CHOICEd OR CHOICE>6 THEN LOCATE 18,1:PRINT TAB(27)"
":GOTO 570
600 ON CHOICE GOTO 620,620,2130,4040,6620,5130
610 ’ CHECK ELECTROLYTE LEVEL, RINSE SYSTEM, AND TRANSFER 50 ML
TO IMPACTOR
620 GOSUB 5140:GOSUB 5290:GOSUB 5800
630 IF CHOICE = 1 GOTO 830
640 ’ INSTRUCTIONS FOR SETTING INSTRUMENT IN UNATTENDED
OPERATING MODE
650 CLS
660 TITLES = "UNATTENDED OPERATION"
670 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
680 LOCATE 2,1 :PRINT TAB(40-LEN(TITLE$)/2)TITLE$:LOCATE 9,1
690 LOCATE 3,1:FOR J = 1 TO 10:PRINT “********";:NEXT J
700 LOCATE 9,1:PRINT "YOU HAVE SELECTED FOR THE INSTRUMENT TO
SAMPLE IN UNATTENDED MODE WITHOUT"
710 PRINT "INPUT FROM THE OPERATOR."
720 PRINT
730 PRINT "THE INSTRUMENT WILL SAMPLE FOR 15 MINUTES AT 30 MINUTE
INTERVALS."
740 PRINT THE TEST RESULTS WILL BE AUTOMATICALLY SAVED TO DISK
FOR LATER INSPECTION."
750 PRINT
760 PRINT "SAMPLING WILL CONTINUE UNTIL MANUALLY ABORTED OR UNTIL
THE ELECTROLYTE-
770 PRINT "SUPPLY IS INSUFFICIENT FOR CONTINUED OPERATION."

168
780 LOCATE 23,23
790 PRINT "PRESS ANY KEY TO CONTINUE "
800 IF INKEY$ = "" GOTO 800
810 ’
820 ’ ENTER PERTINENT STACK CONDITIONS
830 CLS
840 TITLES = "STACK CONDITIONS"
850 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
860 LOCATE 2,1 :PRINT TAB(40-LEN(TITLE$)/2)TITLE$
870 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
880 LOCATE 6,1:PRINT "PRIOR TO SAMPLING, YOU MUST ENTER THE
MEASURED STACK CONDITIONS AT THE POINT OF SAMPLING"
890 LOCATE 9,1
900 INPUT "STACK GAS TEMPERATURE (DEG F)";TF
910 PRINT
920 INPUT "STACK GAS VELOCITY PRESSURE (IN H20). ENTER 0 FOR STATIC
SAMPLING ";VP
930 IF VP=0 THEN QNOZZLE = 15:GOTO 1040
940 ’ CALCULATE ACTUAL STACK GAS VELOCITY
950 VEL=85.49*CP*SQR(VP)*SQR((TF + 460)/(PRESSURE*29))
960 ’ CALCULATE IDEAL NOZZLE SIZE
970 NOZZLE = SQR(4*15000/(3.14*VEL*60*(30.48~3)))*12
980 PRINT:PRINT "FOR THESE CONDITIONS, SELECT A NOZZLE DIAMETER
CLOSE TO "¡USING M.###";NOZZLE;:PRINT " INCHES"
990 LOCATE 15,1
1000 INPUT “ENTER ACTUAL DIAMETER OF AVAILABLE NOZZLE ";DN
1010 ’ CALCULATE ACTUAL NOZZLE FLOWRATE REQUIRED TO ACHIEVE
ISOKINETIC SAMPLING
1020 QNOZZLE = VEL*3.1416*(DN/12)^2*60*28.3/4
1030 ' CONVERT ACTUAL FLOWRATE TO FLOWRATE REQUIRED BY MASS
FLOW CONTROLLER
1040 QMFC = QNOZZLE*(32 + 460)/(TF+460)* PRESSURE/29.92
1050 IF VP=0 THEN GOTO 1160
1060 ’ CHECK THAT FLOWRATE IS WITHIN 8 TO 30 SLPM
1070 IF QMFC<30 AND QMFC>8 THEN GOTO 1160
1080 IF QMFC < 8 THEN LOCATE 17,1 :PRINT:PRINT "THE REQUIRED FLOWRATE
FOR THIS NOZZLE IS TOO LOW. USE A LARGER NOZZLE":BEEP
1090 IF QMFC>30 THEN LOCATE 17,1 :PRINT:PRINT "THE REQUIRED
FLOWRATE FOR THIS NOZZLE IS TOO HIGH. USE A SMALLER
NOZZLE":BEEP
1100 PRINT:PRINT:PRINT:PRINTTAB(18)"PRESS ANY KEYTO CONTINUE "
1110 IF INKEY$ = "" GOTO 1110
1120 FOR J = 15 TO 22
1130 LOCATE J,1:PRINT "

169
1140 NEXT J
1150 LOCATE 15,1:GOTO 1000
1160 PRINT:PRINT "THE REQUIRED ACTUAL FLOWRATE FOR THIS NOZZLE IS
";:PRINT USING "##.#";QNOZZLE;:PRINT " LPM"
1170 PRINT.PRINT.INPUT "ENTER DESCRIPTION FOR THIS TEST
"¡DESCRIPTIONS
1180 KEY(5) OFF
1190 ’
1200 ’
1210 ’ ROUTINE FOR AIR SAMPLING OF STACK GAS
1220 CLS:TITLE$ = "INITIALIZE AIR SAMPLING"
1230 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
1240 LOCATE 2,1:PRINT TAB(40-LEN(TITLE$)/2)TITLE$
1250 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
1260 LOCATE 10,5:PRINT "PRIOR TO SAMPLING, MAKE SURE PROBE IS
PROPERLY POSITIONED AND ALIGNED."
1270 LOCATE 18,18:PRINT "PRESS SPACEBAR TO BEGIN AIR SAMPLING "
1280 IF INKEY$< >CHR$(32) GOTO 1280
1290 ’ READ STARTING TIME FROM COMPUTER
1300 STARTTIMES = LEFTS (TIMES, 5)
1310 ’ SET COMMAND VOLTAGE TO CONTROL MASS FLOW CONTROLLER.
A ONE VOLT COMMAND SIGNAL IS EQUIVALENT TO 10 LPM AT 32 F.
1320 VL!(0) = QMFC/10
1330 CALL FGWRITE’("ANOUT1",VL!0,"C.VOLTS","NT")
1340 ’ TURN ON AIR PUMP AND COOLING FAN
1350 VL%(0) = 1
1360 CALL FGWRITE’("DIGOUT8",VL%0, "C.RAW.INT","NT")
1370 ’ LET REMAIN EQUAL THE SPECIFIED SAMPLING TIME (SEC)
1380 REMAIN = SAMPLETIME:TIMER ON
1390 CLSTITLES = "AIR SAMPLING"
1400 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
1410 LOCATE 2,1:PRINT TAB(40-LEN(TITLES)/2)TITLE$
1420 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
1430 ’ SAMPLING WILL CONTINUE UNTIL ELAPSED TIME = SET TIME OR
UNTIL MANUALLY ABORTED BY THE OPERATOR
1440 ’ ROUTINE IN EVENT OF MANUAL ABORT
1450 ON KEY(5) GOSUB 1610:KEY(5) ON
1460 LOCATE 20,18:PRINT "PRESS F5 TO TERMINATE SAMPLING "
1470 LOCATE 10,20:PRINT "TIME REMAINING =";
1480 ’ MEASURE AND RECORD SAMPLING FLOWRATE AT 10 SECOND
INTERVALS
1490 CALL BGREAD’C'qarray",800.,'"aninO", 1,'"none", 1 ,"nt","TASK10")
1500 CALL INTON’(10,"SEC")

170
1510 CALL BGGO’fNT","")
1520 ’ ROUTINE FOR RESETTING ELAPSED TIME EVERY 1 SECOND
1530 ON TIMER (1) GOSUB 1560
1540 ‘ CHECK IF ELAPSED TIME EQUALS THE DESIRED SAMPLING TIME
1550 IF REMAIN>0 THEN GOTO 1550 ELSE 1770
1560 REMAIN = REMAIN-1
1570 MIN = INT(REMAIN/60):SEC = CINT(REMAIN)-MIN*60
1580 LOCATE 10,38:PRINT MIN;"MINUTES ";SEC;"SECONDS “
1590 ELAPSED=TIME-REMAIN
1600 RETURN
1610 CLS:TIMER OFF:TITLE$ = "SAMPLING ABORTED"
1620 VL%(0)=0
1630 CALL FGWRITE’("DIGOUT8",VL%0,"C.RAW.INT","NT")
1640 RUNTIME = ELAPSED:RUNTIME$ = STR$(RUNTIME)
1650 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
1660 LOCATE 2,1:PRINT TAB(40-LEN(TITLE$)/2)TITLE$
1670 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
1680 ELAPSED
=TIME-REMAIN:MIN = INT(ELAPSED/60):SEC = CINT(ELAPSED)-MIN*60
1690 LOCATE 7,1 :PRINT THE ELAPSED SAMPLING TIME WAS ";MIN;"MINUTES
";SEC;"SECONDS"
1700 ’ CHECK THAT SAMPLING TIME WAS AT LEAST 5 MINUTES. IF NOT
ABORT THE RUN
1710 GOTO 1770
1720 IF ELAPSED<300 THEN LOCATE 10,1 :PRINT "THIS SAMPLING TIME WAS
INSUFFICIENT FOR ACCURATE TEST RESULTS"
1730 LOCATE 12,1:PRINT "NO LEAD ANALYSIS OF THE COLLECTED SAMPLE
WILL BE PERFORMED."
1740 IF ELAPSED <300 THEN LOCATE 20,5:PRINT "PLEASE WAIT FOR
INSTRUMENT TO RINSE "
1750 IF ELAPSED <300 THEN GOTO 420
1760 ’ TURN OFF AIR PUMP AND COOLING FAN
1770 ELAPSED = SAMPLETIME:TIMER OFF:VL%(0)=0
1780 CALL FGWRITE’("DIGOUT8",VL%0,"C.RAW.INT","NT")
1790 CALL INTOFF
1800 CALL BGCLEAR
1810 LP! =0
1820 ’ FIND NUMBER OF POINTS STORED IN FLOW ARRAY
1830 CALL ARLASTP’("QARRAY",LP!)
1840 LP = LP!:QAVG=0:SUM = O
1850 ’ TRANSFER CONTENTS OF KDAC ARRAY TO GWBASIC ARRAY
1860 FOR N = 1 TO LP
1870 CALL ARGET’("QARRAY",N!,N!,"ANINO“,1,QARRAY!0,"C.VOLTS")
1880 QARRAY(N) = QARRAY! (0)

171
1890 NEXT N
1900 ’ DISCARD FLOW MEASUREMENT VALUE AT TIME ZERO. CALCULATE
AVERAGE FLOWRATE USING REMAINING VALUES.
1910 FOR N = 2 TO LP
1920 SUM = SUM + 10*QARRAY(N)
1930 NEXT N
1940 QAVG = SUM/(LP-1)
1950 ' CALCULATE FLOWRATE BASED ON OCCUPATIONAL STANDARD
TEMPERATURE OF 77 F
1960 QSTD = QAVG * (77 + 460) / (32 + 460)
1970 AVGFLOWRATE = QSTD
1980 ’ CALCULATE THE PERCENT ISOKINETIC FOR THIS RUN
1990 ISO = QAVG/QMFC*100
2000 ’ DISPLAY ERROR MESSAGE IF NOT WITHIN 10% ISOKINETIC
2010 IF ISO<90 THEN CLS:LOCATE 10,1:PRINT "THE FLOWRATE FOR THIS
TEST WAS INSUFFICIENT FOR ISOKINETIC SAMPLING. ROTATE THE AIR
PUMP RECIRCULATION VALVE CLOCKWISE APPROXIMATELY 1 TURN
AND REPEAT TEST'
2020 IF ISO> 110 THEN CLS:LOCATE 10,1:PRINT THE FLOWRATE FOR THIS
RUN WAS TOO HIGH FOR ACCURATE TEST RESULTS. IF THIS
CONDITION PERSISTS ON SUBSEQUENT RUNS, CHECK THE
OPERATION OF THE MASS FLOW CONTROLLER."
2030 IF ISO>89 AND ISO<111 THEN GOTO 2060
2040 LOCATE 20,18:PRINT "PRESS ANY KEY TO CONTINUE "
2050 IF INKEYS = "" THEN GOTO 2050
2060 KEY(5) OFF
2070 ON KEY(5) GOSUB 420
2080 KEY (5) ON
2090 RUNTIME = ELAPSED:RUNTIME$ = STR$(RUNTIME)
2100 CLS:LOCATE 10,10:PRINT "TRANSFERRING SOLUTION TO CELL
FOR ANALYSIS. PLEASE WAIT "
2110 ’ TRANSFER SOLUTION FROM IMPACTOR TO POLAROGRAPHIC CELL
2120 GOSUB 5930
2130 IF CHOICE=3 THEN QMFC = 1:TIME = 1
2140 IF CHOICE =3 THEN CLS:PRINT:PRINT:INPUT "ENTER DESCRIPTION FOR
THIS TEST “¡DESCRIPTIONS
2150 ’ ANALYZE COLLECTED SAMPLE
2160 ' SET THE INITIAL CURRENT RANGE TO 20K RESISTOR (10 MICROAMP
SCALE)
2170 RANGE=6
2180 REMAIN = PURGETIME
2190 ’ BEGIN NITROGEN PURGE OF POLAROGRAPHIC CELL
2200 VL%(0) = 1
2210 ’ OPEN NITROGEN SOLENOID

172
2220 CALL FGWRITE’("DIGOUT1")VL%0,"C.RAW.INT")"NT")
2230 VL%(0)=0
2240 ’ INITIATE PURGE ON MODEL 303A
2250 CALL FGWRITE’("DIGOUT5">VL%0,"C.RAW.INT"I"NT")
2260 ’ INITIATE STIR ON MODEL 303A
2270 CALL FGWRITE’("DIGOUT6",VL%0,"C.RAW.INT","NT")
2280 TIMER OFF:TIMER ON
2290 CLS:TITLE$ = "LEAD ANALYSIS"
2300 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
2310 LOCATE 2,1 :PRINT TAB(40-LEN(TITLE$)/2)TITLE$
2320 LOCATE 3,1:FOR J = 1 TO 10:PRINT ,,********";:NEXT J
2330 LOCATE 20,17:PRINT "VERIFY ROTAMETER SETTING IS BETWEEN
0.03 AND 0.05 LPM"
2340 LOCATE 10,20:PRINT "PURGE TIME REMAINING =
2350 ’ ROUTINE FOR RESETTING AND DISPLAYING ELAPSED TIME EVERY 1
SECOND
2360 ON TIMER (1) GOSUB 2380
2370 IF REMAIN >0 THEN GOTO 2370 ELSE 2430
2380 REMAIN = REMAIN-1
2390 MIN = INT(REMAIN/60):SEC = CINT(REMAIN)-MIN*60
2400 LOCATE 10,44:PRINT MIN;"MINUTES ";SEC;"SECONDS "
2410 RETURN
2420 ’ CLOSE NITROGEN SOLENOID AND DISCONTINUE PURGE AND STIR
FUNCTIONS ON MODEL 303A
2430 TIMER OFF
2440 VL%(0) = 0
2450 CALL FGWRITE’("DIGOUT1",VL%0,"C.RAW.INT","NT")
2460 VL%(0) = 1
2470 CALL FGWRITE’("DIGOUT5",VL%0,"C.RAW.INT","NT')
2480 CALL FGWRITE’(,,DIGOUT6",VL%0,"C.RAW.INT","NT')
2490 ’
2500 ’ INITIALIZE ARRAYS FOR STORING DATA FROM ANALYSIS OF
COLLECTED LEAD
2510 ON KEY(5) GOSUB 3920
2520 KEY (5) ON
2530 ’ RESET DECADE BOARD RELAYS TO "OPEN" POSITION
2540 FOR J=4 TO 8
2550 VL%(0) = 1:J$ = STR$(J)
2560 BOARDS = "PCM" + RIGHT$(J$, 1)
2570 CALL FGWRITE’(BOARD$,VL%0,"C.RAW.INT","NT")
2580 NEXT J
2590 ’ SET RANGE OF CURRENT SCAN
2600 VL%(0)=0
2610 RANGES = STR$(RANGE)

173
2620 RANGES = "PCM" + RIGHT$(RANGE$, 1)
2630 ’ PLACE DECADE RESISTANCE BOARD IN-LINE
2640 CALL FGWRITE’("PCM9",VL%0,"C.RAW.INT","NT')
2650 CALL FGWRITE’(RANGE$,VL%0,"C.RAW.INT\"NT")
2660 VL%(0)=0
2670 ’ INITIATE "SCAN" ON MODEL 264
2680 CALL FGWRITE’("PCM1",VL%0,"C.RAW.INT")"NT")
2690 VL%(0) = 1
2700 CALL FGWRITE’("PCM1")VL%0,"C.RAW.INT,,"NT")
2710 ’ INITIALIZE VARIABLE ARRAYS
2720 STAT1% = 1
2730 RR=0:LP! =0!
2740 LOCATE 10,20:PRINT "DEPOSITING LEAD ON ELECTRODE
2750 LOCATE 20,17:PRINT " PLEASE WAIT
2760 ’ ROUTINE FOR DETECTING WHEN MODEL 264 HAS BEGUN THE
SCAN. USE THE AVERAGE OF 10 READINGS
2770 FOR J = 1 TO 10
2780 CALL FGREAD’("ANIN4">"NONE"1VL!(),"C.VOLTS","NT")
2790 SUM = SUM + VL!(0):NEXT J
2800 AVG = SUM/10:IF AVG>2 THEN SUM=0:AVG = 0:GOTO 2770
2810 SUM=0:AVG=0
2820 CLS:TITLE$ = "LEAD ANALYSIS"
2830 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
2840 LOCATE 2,1:PRINTTAB(40-LEN(TITLES)/2)TITLE$
2850 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
2860 LOCATE 10,20:PRINT " SCAN DETECTED
2870 SCAN = 1
2880 ’
2890 ’ READ OUTPUTS FROM MODEL 264 (CURRENT VS SCAN VOLTAGE)
AND STORE IN KDAC ARRAYS
2900 CALL BGREAD,("XARRAY",800.,"ANIN3",1,"NONE",1,"NT","TASK1")
2910 CALL BGREAD’("YARRAY",800.,"ANIN1",1,"NONE", 1,"NT","TASK2")
2920 CALL INTON'(200,"MIL")
2930 CALL BGGO’fNT","")
2940 START=TIMER
2950 CALL BGSTATUS’("TASK1",STAT1%)
2960 ’ ROUTINE FOR DETECTING WHEN MODEL 264 HAS COMPLETED THE
SCAN. USE THE AVERAGE OF 10 READINGS
2970 FOR J = 1 TO 10
2980 CALL FGREAD’("ANIN4")"NONE",VL!0,"C.VOLTS","NT")
2990 SUM = SUM + VL!(0):NEXT J
3000 AVG = SUM/10:IF AVG > 3 THEN LOCATE 10,20:PRINT "SCAN COMPLETED.
PERFORMING CALCULATIONS ":GOTO 3030
3010 AVG = 0:SUM=0:GOTO 2970

174
3020 IF (STAT1%)=0! THEN 2950
3030 CALL INTOFF
3040 ’ FIND LOCATION OF LAST POINT STORED IN ARRAY
3050 CALL ARLASTP’("YARRAY",LP!)
3060 TIMER OFF:VL%(0)=0
3070 CALL FGWRITE’("DIGOUT1",VL%0,"C.RAW.INT","NT")
3080 LP = LP!
3090 ’ TRANSFER CONTENTS FROM KDAC ARRAY TO BASIC ARRAY
3100 FOR N = 1 TO LP
3110 CALL ARGET("XARRAY",N!,N!,"ANIN3", 1 ,XARRAY! 0,"C.VOLTS")
3120 XARRAY(N) = XARRAY! (0): IF XARRAY(N) <0 THEN
XARRAY(N) =ABS(XARRAY(N)) ELSE XARRAY(N) = -XARRAY(N)
3130 CALL ARGET’("YARRAY",N!,N! ,"ANIN1", 1,YARRAY! 0,"C.VOLTS")
3140 YARRAY(N)= YARRAY!(0):IF ABS(YARRAY(N))<.01 THEN YARRAY(N)=0
3150 NEXT N
3160 ’ ROUTINE FOR CHECKING AND DISCARDING SPURIOUS VALUES AND
FOR DETERMINING PEAKS VALUES OF LEAD AND COPPER. FIRST, SET
PREVIOUS VALUE = 0
3170 PB=0:CU=0
3180 FOR N = 1 TO LP
3190 IF ABS(YARRAY(N))>7 THEN YARRAY(N)=0
3200 IF ABS(YARRAY(N)-YARRAY(N-1)) > 1 THEN YARRAY(N) =YARRAY(N-1)
3210 IF N<100 OR N>160 THEN 3240
3220 IF ABS(YARRAY(N)) < ABS(YARRAY(N-1)) THEN GOTO 3240
3230 IF ABS(YARRAY(N)) > ABS(PB) THEN PB=YARRAY(N):XX = N
3240 IF N<250 OR N>400 THEN 3260
3250 IF ABS(YARRAY(N))>ABS(CU) THEN CU = YARRAY(N):YY = N
3260 NEXT N
3270 ’ CHECK TO SEE IF CURRENT RANGE WAS EXCEEDED DURING THE
SCAN. IF SO, INCREASE RANGE AND REPEAT THE SCAN
3280 IF ABS(PB)>4.5 OR ABS(CU)>4.5 THEN RANGE = RANGE+1
3290 IF ABS(PB)>4.5 OR ABS(CU)>4.5 THEN CALL ARDEL’("XARRAY")
3300 IF ABS(PB)>4.5 OR ABS(CU)>4.5 THEN CALL ARDEL’("YARRAY")
3310 IF ABS(PB)>4.5 OR ABS(CU)>4.5 THEN GOTO 2180
3320 IF RANGE = 6 AND ABS(CU)<.3 THEN GOTO 6480
3330 ’ CALCULATE LEAD CONCENTRATION (PPB) IN SOLUTION
3340 LIQUIDPB = PB/CU*COPPERSTD*2.33
3350 ’ CALC LEAD-IN-AIR CONCENTRATION (MICROGRAMS PER CUBIC
METER)
3360 IF CHOICE=3 THEN AIRPB=0:QSTD=0:ISO=0:GOTO 3380
3370 AIRPB = LIQUIDPB*50/(QSTD*SAMPLETIME)*60
3380 ’ DELETE CONTENTS OF BASIC ARRAYS AND REDIMENSION
3390 PRINT "xx = ";XX:PRINT
3400 ERASE XARRAY:ERASE YARRAY:DIM XARRAY(800):DIM YARRAY(800)

175
3410 ’
3420 ’ LISTING OF ANALYSIS RESULTS
3430 CLS
3440 TITLES = "SUMMARY OF RESULTS"
3450 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
3460 LOCATE 2,1 :PRINT TAB(40-LEN(TITLE$)/2)TITLE$
3470 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
3480 LOCATE 10,10:PRINT "CALCULATED LIQUID LEAD CONC =
";CINT(LIQUIDPB);" PARTS/BILLION
3490 LOCATE 11,10:PRINT "CALCULATED AIR LEAD CONC= ";CINT(AIRPB);H
MICROGRAMS PER CUBIC METER-
3500 LOCATE 13,10:PRINT "COPPER PEAK= ";CU;" VOLTS"
3510 LOCATE 14,10:PRINT "LEAD PEAK= ";PB;" VOLTS"
3520 LOCATE 16,10:PRINT "VOLUME SAMPLED (STANDARD LITERS)
" ;CI NT(QSTD*SAM PLETIM E/60)
3530 LOCATE 15,10:PRINT "% ISOKINETIC= ";CINT(ISO)
3540 ' IF SCAN HAS TAKEN PLACE, DELETE CONTENTS OF KDAC ARRAYS
3550 IF SCAN = 1 THEN CALL ARDEL’("XARRAY")
3560 IF SCAN = 1 THEN CALL ARDEL'("YARRAY")
3570 IF CHOICE=3 THEN GOTO 3590
3580 IF SCAN = 1 THEN CALL ARDEL’("QARRAY")
3590 ’ IF OPERATING IN UNATTENDED MODE, DISPLAY THE TEST RESULTS
FOR 30 SECONDS THEN CONTINUE OPERATION
3600 IF CHOICE = 2 THEN GOTO 6910
3610 LOCATE 23,20:PRINT "PRESS ANY KEY TO CONTINUE "
3620 IF INKEYS = "" THEN GOTO 3620
3630 ’ ROUTINE TO SAVE TEST RESULTS TO HARD DRIVE
3640 ’ USE CURRENT DATE AS FILENAME
3650 FILENAMES = LEFT$(DATE$,6) + RIGHTS (DATES, 2)
3660 OPEN "R",#1,FILENAMES,120
3670 FIELD#1, 2 AS N$, 5 AS STARTS, 4 AS ELAPSEDS, 4 AS AVGFLOWRATES,
4 AS LIQUIDPBS, 4 AS AIRS, 30 AS DESCS
3680 ’ FIND LOCATION OF LAST RECORD STORED ON THIS DAY
3690 N% = 1
3700 GET#1,N%
3710 IF CVI(N$)< >0 THEN N% = N%+1:GOTO 3700
3720 LSET N$ = MKI$(N%)
3730 LSET STARTS = STARTTIME$
3740 IF CHOICE = 3 THEN LSET STARTS = "0"
3750 IF CHOICE=3 THEN ELAPSED=0:AVGFLOWRATE = 0:AIRPB=0
3760 LSET ELAPSEDS = MKI$(ELAPSED)
3770 LSET AVGFLOWRATES = MKI$(AVGFLOWRATE)
3780 LSET LIQUIDPBS = MKI$(LIQUIDPB)
3790 LSET AIR$ = MKI$(AIRPB)

176
3800 LSET DESC$ = DESCRIPTIONS
3810 PUT#1, N%
3820 CLOSE
3830 TIMER OFF
3840 IF CHOICE=3 THEN GOTO 410
3850 ’ IF OPERATING IN UNATTENDED MODE, REPEAT MAIN CYCLE
3860 ’ EXECUTE MAIN RINSE ROUTINE
3870 GOSUB 5290
3880 IF QQ = 1 AND CHOICE=2 THEN 3910
3890 IF CHOICE = 2 THEN GOSUB 5800
3900 IF CHOICE = 2 THEN GOTO 1300
3910 QQ=0:CLS:GOTO 420
3920 ’ ROUTINE FOLLOWING MANUAL ABORT OF SCAN
3930 ’ IF SCAN HAS TAKEN PLACE, DELETE CONTENTS OF KDAC ARRAY
3940 IF SCAN = 1 THEN CALL ARDEL’fXARRAY")
3950 IF SCAN = 1 THEN CALL ARDEL’fYARRAY")
3960 TIMER OFF
3970 CALL INTOFF
3980 ’ ACTIVATE "STOP" OF 264A
3990 VL!(0)=0:CALL FGWRITE’("PCM2",VL!0,"C.VOLTS","NT")
4000 VL!(0) = 1:CALL FGWRITE,("PCM2",VL!0,"C.VOLTS",,,NT")
4010 GOTO 420
4020 ’
4030 ' ROUTINE FOR VIEWING RESULTS OF PREVIOUS TESTS
4040 CLS:TITLE$ = "VIEW PREVIOUS TEST RESULTS"
4050 ON KEY(5) GOSUB 4050:KEY(5) ON
4060 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
4070 LOCATE 2,1:PRINT TAB(40-LEN(TITLES)/2)TITLE$
4080 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
4090 LOCATE 7,4:PRINT "TEST RESULTS ARE SAVED UNDER FILES NAMES
SPECIFIED BY THE SAMPLING DATE"
4100 TITLES = "MENU OF TEST RESULTS"
4110 LOCATE 12,1: PRINT TAB(40-LEN(TITLES)/2)TITLE$
4120 TITLES = " "
4130 LOCATE 13,1:PRINT TAB(40-LEN(TITLES)/2)TITLE$
4140 LOCATE 15,1
4150 PRINT TAB(25) "(1) LIST EXISTING FILE NAMES"
4160 PRINT TAB(25) "(2) VIEW ARCHIVED TEST RESULTS"
4170 PRINT TAB(25) "(3) PRINT ARCHIVED TEST RESULTS"
4180 PRINT TAB(25) "(4) EXIT TO MAIN MENU"
4190 LOCATE 20,15:INPUT "ENTER YOUR CHOICE
";CHOICE:CHOICE = CINT(CHOICE)
4200 IF CHOICE< 1 OR CHOICE>4 THEN LOCATE 20,15:PRINT "
":GOTO 4190

177
4210 ON CHOICE GOTO 4220,4260,4700, 420
4220 CLS:FILES
4230 LOCATE 22,20:PRINT "PRESS ANY KEY TO CONTINUE "
4240 IF INKEY$< >CHR$(32) THEN 4240
4250 GOTO 4040
4260 CLS:TITLE$ = "VIEW TEST RESULTS"
4270 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
4280 LOCATE 2,1 :PRINT TAB(40-LEN(TITLE$)/2)TITLE$
4290 LOCATE 22,20:PRINT "PRESS KEY TO RETURN TO THE
MENU "
4300 ’ DELETE PREVIOUS FILE NAMES FROM MEMORY
4310 FILES = ""¡FILENAMES = ""
4320 LOCATE 12,1 ¡INPUT "ENTER THE FILE NAME YOU WISH TO VIEW";FILE$
4330 IF LEN(FILE$)<6 THEN 4040
4340 ’ CONVERT IMPROPER MM/DD/YY FORMAT TO MM-DD-YY FORMAT
4350 FOR J = 1 TO LEN(FILES)
4360 IF ASC(MID$(FILE$, J, 1)) = 47 THEN FILE$(J) = "-" ELSE
FILE$(J) = MID$(FILE$, J,1)
4370 FILENAMES = FI LENAMES+ FILES (J)
4380 NEXT J
4390 ’ CONVERT IMPROPER M-DD-YY FORMAT TO MM-DD-YY FORMAT
4400 FOR J = 1 TO LEN (FILENAMES)
4410 IF J>1 THEN GOTO 4420 ELSE IF ASC(MID$(FILENAME$,J + 1,1))=45
THEN FILENAME$ = "0" + FILENAME$
4420 IF J< >4 THEN GOTO 4430 ELSE IF ASC(MID$(FILENAME$,J+1,1))=45
THEN FILENAMES = LEFT$(FILENAME$,3)+ "0"+ RIGHT$(FILEÑAMES,4)
4430 NEXT J
4440 OPEN "R",#1,FILENAMES,120
4450 FIELD#1, 2 AS N$, 5 AS STARTS, 4 AS ELAPSEDS, 4 AS AVGFLOWRATES,
4 AS LIQUIDPBS, 4 AS AIRS, 30 AS DESCS
4460 N% = 1:GET#1, N%
4470 ’ CHECK THAT SPECIFIED FILENAME EXISTS
4480 IF CVI(N$) =0 THEN PRINT:PRINT "FILENAME DOES NOT EXIST. HIT ANY
KEY "
4490 IF CVI(N$) =0 THEN CLOSE:KILL FILENAMES
4500 IF CVI(N$) =0 THEN FILENAMES = "": IF INKEYS = "" THEN 4500
4510 IF CVI(N$)=0 THEN GOTO 4040
4520 ’
4530 ’ LOAD AND DISPLAY CONTENTS OF SPECIFIED FILENAME
4540 CLS:COUNTER=0:TITLE$ = "FILENAME= " + FILENAME$:PRINT
TAB(40-LEN(TITLE$)/2)TITLE$
4550 LOCATE 5,1
4560 PRINT TAB(15)"RUN";TAB(21 )"FLOW";TAB(29)"LIQUID";TAB(39)"AIR"
4570 PRINT TAB( 7)"START";TAB(14)"TIME";TAB(21)"RATE";TAB(28)"PB

178
CONC";TAB(38)"PB CONC"
4580 PRINT TAB(2)"RUN#";TAB(8)"TIME";TAB(14)"(SEC)";TAB(21)"(LPM)"
;TAB(29)"(PPB)";TAB(37)"(UG/M/'3),,;TAB(49)"DESCRIPTION"
4590 FOR J = 1 TO 80:PRINT"-";:NEXT J:PRINT
4600 PRINT TAB(1) USING "###";CVI(N$);:PRINT TAB(7)START$;: PRINT
TAB(14) USING "###";CVI(ELAPSED$);: PRINT TAB(22) USING
H##“;CVI (AVGFLOWRATES)PRINT TAB(29) USING
"####";CVI(LIQUIDPB$);:PRINT TAB( 38) USING "####";CVI(AIR$);:
PRINT TAB(48)DESC$
4610 N% = N%+1
4620 ’ LIMIT DISPLAY TO 10 RECORDS
4630 COUNTER = COUNTER + 1:IF COUNTER> 9 THEN GOTO 4650
4640 GET#1,N%:IF CVI(N$)< >0 THEN 4600
4650 LOCATE 23.20.PRINT "PRESS ANY KEY TO CONTINUE "
4660 IF INKEY$ = "" THEN GOTO 4660
4670 ’ LIMIT DISPLAY TO 10 RECORDS
4680 GET#1,N%
4690 IF COUNTER > 9 THEN GOTO 4540 ELSE CLOSE:GOTO 4040
4700 ' ROUTINE FOR PRINTING
4710 CLS:TITLE$ = "PRINT PREVIOUS TEST RESULTS"
4720 LOCATE 1,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
4730 LOCATE 2,1 :PRINT TAB(40-LEN(TITLE$)/2)TITLE$
4740 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
4750 LOCATE 7,17:PRINT "A PARALLEL PRINTER MUST BE CONNECTED TO
PORT#1"
4760 ’ DELETE PREVIOUS FILE NAMES FROM MEMORY
4770 FILES = ""¡FILENAMES =
4780 LOCATE 12,1:INPUT "ENTER THE FILE NAME YOU WISH TO PRINT";FILE$
4790 IF LEN(FILE$)<6 THEN 4040
4800 ’ CONVERT IMPROPER DD/MM/YY FORMAT TO DD-MM-YY FORMAT
4810 FOR J = 1 TO LEN(FILES)
4820 IF ASC(MID$(FILE$, J,1)) =47 THEN FILE$(J) ="-" ELSE
FILE$(J) = MID$(FILE$, J, 1)
4830 FILENAMES = FILENAMES + FILE$(J)
4840 NEXT J
4850 ’ CONVERT IMPROPER D-M-YY FORMAT TO DD-MM-YY FORMAT
4860 FOR J = 1 TO LEN(FILENAMES)
4870 IF J = 1 AND ASC(MID$(FILENAME$, J + 1,1)) =45 THEN
FI LEN AM E$ = "0" + FI LEN AM E$
4880 IF J = 4 AND ASC(MID$(FILENAME$, J + 1,1)) = 45 THEN
FILENAMES = LEFT$(FILENAME$,3) + "0" + RIGHT$(FILENAME$,4)
4890 NEXT J
4900 CLOSE
4910 OPEN "R",#1,FILENAMES, 120

179
4920 FIELD#1, 2 AS N$, 5 AS STARTS, 4 AS ELAPSEDS, 4 AS AVGFLOWRATE$,
4 AS LIQUIDPBS, 4 AS AIR$, 30 AS DESC$
4930 N% = 1:GET#1, N%
4940 ’ CHECK THAT SPECIFIED FILENAME EXISTS
4950 IF CVI(N$) =0 THEN PRINT:PRINT "FILENAME DOES NOT EXIST. HIT ANY
KEY "
4960 IF CVI(N$)=0 THEN CLOSE:KILL FILENAMES
4970 IF CVI(N$) =0 THEN FILENAMES IF INKEYS = "" THEN 4500
4980 IF CVI(N$)=0 THEN CLOSE: GOTO 4040
4990 LOCATE 20,20:PRINT "PRESS ANY KEY TO BEGIN PRINTING "
5000 IF INKEY$ = "" THEN GOTO 5000
5010 ’
5020 ’ LOAD AND PRINT CONTENTS OF SPECIFIED FILENAME
5030 TITLE$ = "FILENAME= " + FILENAME$:LPRINT
TAB(40-LEN(TITLE$)/2)TITLE$:LPRINT:LPRINT
5040 LPRINT TAB(15)"RUN";TAB(21)"FLOW";TAB(29)"LIQUID";TAB(39)"AIR"
5050 LPRINT TAB( 7)"START";TAB(14)"TIME";TAB(21)"RATE";TAB(28)"PB
CONC";TAB(38)"PB CONC"
5060 LPRINTTAB(2)"RUN#";TAB(8)"TIME";TAB(14)"(SEC)";TAB(21)"(LPM)"
;TAB(29)"(PPB)“ ;TAB(37)"(UG/M/N3)";TAB(49)"DESCRIPTION"
5070 FOR J = 1 TO 80:LPRINT'-";:NEXT J:LPRINT
5080 LPRINT TAB(1) USING "###";CVI(N$);:LPRINT TAB(7)STARTS;: LPRINT
TAB(14) USING "###";CVI(EU\PSED$);: LPRINT TAB(22) USING
"##";CVI(AVGFLOWRATES);:LPRINT TAB(29) USING
"####";CVI(LIQUIDPB$);:LPRINT TAB( 38) USING "####";CVI(AIR$);:
LPRINT TAB(48)DESC$
5090 N% = N%+1
5100 GET#1,N%:IF CVI(N$)< >0 THEN 5080
5110 CLOSE.GOTO 4040
5120 ’ TERMINATE PROGRAM EXECUTION
5130 CHDIR "\":CHDIR "\K500":CLOSE:END
5140 ’ CHECK ELECTROLYTE LEVEL SWITCH POSITION. USE AVERAGE OF
10 READINGS
5150 VL%(0) = 1
5160 CALL FGWRITE’("DIGOUT0",VL%(),"C.RAW.INT","NT")
5170 SUM=0:AVG=0
5180 VL!(0)=0
5190 FOR J = 1 TO 10
5200 CALL FGREAD’("ANIN2","NONE",VL!0,"C.VOLTS","NT")
5210 SUM = SUM + VL!(0):NEXT J
5220 AVG = SUM/10:IF AVG>3 THEN RETURN
5230 CLS:LOCATE 7, 9:PRINT "NOTICE: ELECTROLYTE SUPPLY IS
INSUFFICIENT FOR CONTINUED OPERATION"
5240 LOCATE 10,24: PRINT "REFILL RESERVOIR BEFORE CONTINUING"

180
5250 FOR J = 1 TO 5:BEEP:FOR K = 1 TO 4000:NEXT K:NEXT J
5260 LOCATE 20,26: PRINT "PRESS ANY KEY TO CONTINUE "
5270 IF INKEY$ = "" THEN GOTO 5270
5280 GOTO 420
5290 ’ MAIN RINSE ROUTINE
5300 CLS:LOCATE 10,20:PRINT "CLEANING POU\ROGRAPHIC CELL PLEASE
WAIT "
5310 STAT% = 10
5320 ’ LP1 PUMP 50 ML (66 CYCLES)
5330 CALL BGWRITE’(,,LPARRAY","DIGOUT2")1,66,"NT","TASK2")
5340 ’ TURN ON STIRRING OF POLAROGRAPHIC CELL DURING RINSE
5350 VL%(0)=0
5360 CALL FGWRITE’("DIGOUT6",VL%0,"C.RAW.INT","NT")
5370 ’ LP3 EMPTY FLOW-THROUGH CELL
5380 CALL BGWRITE’("LPARRAY","DIGOUT4",1,55,"NT","TASK4")
5390 ’ SET PUMP STROKE INTERVAL
5400 CALL INTON’(250,"MIL")
5410 CALL BGGO’C'NT',"")
5420 STAT% = 10
5430 CALL BGSTATUS’("TASK2",STAT%)
5440 IF STAT%< >0 THEN GOTO 5430
5450 ’ DEACTIVATE PUMP LP1
5460 VL%(0)=0
5470 CALL FGWRITE’("DIGOUT2",VL%0,"C.RAW.INT","NT")
5480 ’ TURN ON AIR FLOW FOR 10 SECONDS DURING RINSE
5490 GOSUB 6340
5500 ’ FILL FLOW-THROUGH CELL WITH 18 ML USING PUMP LP2
5510 CALL BGWRITE,(“LPARRAY","DIGOUT3",1,33,"NT","TASK3")
5520 CALL INTON’(250,"MIL")
5530 CALL BGGO’C'NT',"")
5540 STAT% = 10
5550 CALL BGSTATUS’("TASK3",STAT%)
5560 IF STAT%< >0 THEN GOTO 5550
5570 ’ ACTIVATE BOTH LP2 AND LP3 TO PUMP EQUAL VOLUMES
5580 CALL BGWRITE’("LPARRAY","DIGOUT3",1,80,"NT',"TASK5")
5590 CALL BGWRITE’("LPARRAY","DIGOUT4",1,70,"NT","TASK6")
5600 CALL INTON’(250,"MIL")
5610 CALL BGGO’C'NT","")
5620 STAT% = 10
5630 CALL BGSTATUS'("TASK6",STAT%)
5640 IF STAT%< >0 THEN GOTO 5630
5650 ’ TURN OFF STIR FUNCTION
5660 VL%(0) = 1
5670 CALL FGWRITE’("DIGOUT6",VL%0,"C.RAW.INT","NT”)

181
5680 ’ DEACTIVATE PUMP LP3
5690 VL%(0) = 0
5700 CALL FGWRITE’("DIGOUT4",VL%0,"C.RAW.INT","NT")
5710 STAT% = 10
5720 CALL BGSTATUS’("TASK5",STAT%)
5730 IF STAT%< >0 THEN GOTO 5720
5740 ’ DEACTIVATE PUMP LP2
5750 VL%(0)=0
5760 CALL FGWRITE'("DIGOUT3",VL%0,"C.RAW.INT,,"NT")
5770 CALL BGCLEAR
5780 CALL INTOFF
5790 STAT% = 10:RETURN
5800 ’ SUBROUTINE TO TRANSFER 50 ML FROM RESERVOIR TO IMPACTOR
5810 GOSUB 5140
5820 CALL BGWRITE’("LPARRAY","DIGOUT2',,1)66)"NT,,"TASK11")
5830 CALL INTON’(250,"MIL")
5840 CALL BGGO’C'NT',"")
5850 STAT% = 10
5860 CALL BGSTATUS’("TASK11",STAT%)
5870 IF STAT%< >0 THEN GOTO 5860
5880 ’ DEACTIVATE LP1
5890 CALL INTOFF
5900 VL%(0)=0
5910 CALL FGWRITE’("DIGOUT2",VL%0,"C.RAW.INT","NT")
5920 RETURN
5930 ’ LP3 EMPTY FLOW-THROUGH CELL
5940 CALL BGWRITE’("LPARRAY","DIGOUT4",1,50,"NT","TASK4")
5950 ’ TURN ON STIRRING OF POLAROGRAPHIC CELL DURING RINSE
5960 VL%(0)=0
5970 CALL FGWRITE’("DIGOUT6",VL%0,,,C.RAW.INT,,"NT")
5980 ’ SET PUMP STROKE INTERVAL
5990 CALL INTON’(250,"MIL")
6000 CALL BGGO’C'NT',"")
6010 STAT% = 10
6020 CALL BGSTATUS ’ ("TASK4", STAT%)
6030 IF STAT%< >0 THEN GOTO 6020
6040 ’ FILL FLOW-THROUGH CELL WITH 18 ML USING PUMP LP2
6050 CALL BGWRITE’("LPARRAY',,"DIGOUT3",1,33,"NT","TASK3")
6060 CALL INTON’(250,"MIL")
6070 CALL BGGO’C'NT',"")
6080 STAT% = 10
6090 CALL BGSTATUS’("TASK3",STAT%)
6100 IF STAT%< >0 THEN GOTO 6090
6110 ’ ACTIVATE BOTH LP2 AND LP3 TO PUMP EQUAL VOLUMES

182
6120 CALL BGWRITE’("LPARRAY","DIGOUT3", 1,75,"NT","TASK5")
6130 CALL BGWRITE,("LPARRAY","DIGOUT4",1,60,"NT',"TASK6")
6140 CALL INTON’(250,"MIL")
6150 CALL BGGO’("NT","")
6160 STAT% = 10
6170 CALL BGSTATUS’ ("TAS K6", STAT%)
6180 IF STAT%< >0 THEN GOTO 6170
6190 ’ TURN OFF STIR FUNCTION
6200 VL%(0) = 1
6210 CALL FGWRITE,("DIGOUT6",VL%0,"C.RAW.INT","NT")
6220 ’ DEACTIVATE PUMP LP3
6230 VL%(0)=0
6240 CALL FGWRITE’("DIGOUT4",VL%0,"C.RAW.INT","NT")
6250 STAT% = 10
6260 CALL BGSTATUS’(TASK5",STAT%)
6270 IF STAT%< >0 THEN GOTO 6260
6280 ’ DEACTIVATE PUMP LP2
6290 VL%(0) =0
6300 CALL FGWRITE’ ("DIGOUT3", VL%0, "C. RAW. I NT', "NT")
6310 CALL BGCLEAR
6320 CALL INTOFF
6330 STAT% = 10:RETURN
6340 ’ TURN ON AIR FLOW FOR 10 SECONDS DURING RINSE
6350 VL!(0) = 1.5
6360 CALL FGWRITETANOUTr.VUO/C.VOLTSV'NT")
6370 VL%(0) = 1
6380 CALL FGWRITE’("DIGOUT8">VL%0,"C.RAW.INT","NT")
6390 TIMER ON:RINSETIME = 10
6400 ON TIMER (1) GOSUB 6420
6410 IF RINSETIME>0 THEN GOTO 6410 ELSE 6440
6420 RINSETIME = RINSETIME-1
6430 RETURN
6440 VL%(0)=0
6450 CALL FGWRITE’("DIGOUT8",VL%0,"C.RAW.INT","NT")
6460 TIMER OFF
6470 RETURN
6480 CLS:LOCATE 10,1:PRINT "THE RESPONSE TO THE COPPER INTERNAL
STANDARD WAS MUCH LOWER THAN EXPECTED. THE PREVIOUS TEST
RESULTS ARE INVALID. IF THE PROBLEM PERSISTS DURING
SUBSEQUENT TESTS, PLEASE CHECK THE OPERATING MANUAL FOR
POSSIBLE CAUSES"
6490 ’ ROUTINE TO INITIATE 15 MERCURY DROP DISPENSE/DISLODGE
CYCLES TO ENSURE COLUMN CONTINUITY
6500 FOR J = 1 TO 15

183
6510 VL%(0) = 0
6520 CALL FGWRITE’("DIGOUT7")VL%0,"C.RAW.INT","NT")
6530 VL%(0) = 1
6540 CALL FGWRITE’("DIGOUT7",VL%0,"C.RAW.INT","NT")
6550 FOR K = 1 TO 2000:NEXT K
6560 NEXT J
6570 LOCATE 20,20:PRINT "PRESS ANY KEY TO CONTINUE "
6580 IF INKEY$ = '"' THEN GOTO 6580
6590 CALL KDINIT
6600 CLEAR
6610 GOTO 10
6620 CLS:LOCATE 1,1:FOR J = 1 TO 10:PRINT "********,,;:NEXT J
6630 TITLES = "LEAD-IN-AIR MONITOR"
6640 LOCATE 2,1 :PRINT TAB(40-LEN(TITLE$)/2)TITLE$
6650 LOCATE 3,1:FOR J = 1 TO 10:PRINT "********";:NEXT J
6660 TITLES = "FLUID HANDLING OPTIONS"
6670 LOCATE 9,1:PRINT TAB(40-LEN(TITLE$)/2)TITLE$
6680 TITLES = " "
6690 LOCATE 10,1:PRINT TAB(40-LEN(TITLES)/2)TITLE$
6700 LOCATE 12,1
6710 PRINT TAB(25) "(1) MAIN RINSE-
6720 PRINT TAB(25) "(2) FILL IMPACTOR"
6730 PRINT TAB(25) "(3) EMPTY IMPACTOR"
6740 PRINT TAB(25) "(4) EMPTY POLAROGRAPHIC CELL"
6750 PRINT TAB(25) "(5) EXIT TO MAIN MENU"
6760 PRINT:PRINT:INPUT "ENTER YOUR CHOICE";CHOICE
6770 ON CHOICE GOSUB 5290, 5800, 5930, 6790, 410
6780 GOTO 410
6790 CALL BGWRITE’(”LPARRAY","DIGOUT4",1,50,"NT","TASK6")
6800 CALL INTON’(250,"MIL")
6810 CALL BGGO’("NT',"")
6820 STAT% = 10
6830 CALL BGSTATUS’("TASK6",STAT%)
6840 IF STAT%< >0 THEN GOTO 6830
6850 ’ DEACTIVATE PUMP LP3
6860 VL%(0)=0
6870 CALL FGWRITE’("DIGOUT4",VL%0,"C.RAW.INT","NT")
6880 CALL INTOFF
6890 CALL BGCLEAR
6900 GOTO 6620
6910 BEEP:BEEP:BEEP
6920 ON KEY (5) GOSUB 7000
6930 KEY (5) ON
6940 LOCATE 20,18:PRINT "PRESS F5 TO ABORT UNATTENDED OPERATION"

184
6950 TIMER ON:WT=30
6960 ON TIMER (1) GOSUB 6980
6970 IF WT>0 THEN GOTO 6970 ELSE 3650
6980 WT=WT-1
6990 RETURN
7000 KEY (5) OFF
7010 LOCATE 20,15:PRINT "UNATTENDED OPERATION HAS BEEN MANUALLY
ABORTED"
7020 QQ = 1
7030 RETURN

APPENDIX E
OPERATING MANUAL FOR THE LEAD-IN-AIR MONITOR

E.1 SETTING UP THE LEAD-IN-AIR MONITOR
Unpacking Instructions
Parts List
The lead-in-air monitor consists of the following major components:
Qtv Description
1 Module 1. Contains liquid pumps, electrolyte
reservoir, impactor, nitrogen handling components,
digital logic board, and compression fittings.
1 Module 2. Contains air pump, cartridge filter,
mass flow controller, recirculation valve, and
compression fittings.
1 EG&G Model 303A static mercury drop electrode
system with Model 305 stirrer.
1 EG&G Model 264A polarograph control unit.
1 PC Brand Model 286/25 computer with
monochrome monitor and keyboard.
1 10 liter capacity polypropylene wide mouth waste
container (Fisher 02-961-65A) with attached teflon
bulkhead 1 /4 inch pipe connectors.
1 Stainless steel utility cart (McMaster-Carr 2544T4).
1 22 inch long, 1/4 inch O.D. teflon tube for
connecting Module 1 waste outlet to waste
container.
5 6 ft. 120 VAC power cords.
The Model 303A, Model 264A, Keithley 575, and computer each have their
own instruction manuals and set of accessories. Refer to these manuals for
specific operating requirements and maintenance.
186

187
The following accessories are also included with the system:
Qtv Description
2 10 liter capacity polypropylene wide mouth
containers (Fisher 02-961-65A) for preparation and
storage of electrolyte.
1 3 lbs. triple-distilled mercury.
1 34 liter cylinder of ultra-high purity nitrogen.
1 1/4 inch tubing grooving tool.
1 1 liter capacity polypropylene volumetric flask
(Fisher 10-198-50F) for preparing and storage of
calibration check standard.
1 15 ml and 25 ml pipettes and squeeze bulb.
1 Spare cartridge filter.
1 39 inch teflon-lined sampling probe and fittings.
1 EG&G Model 9103 Ag/AgCI filling solution for
reference electrode.
1 Replacement teflon fittings and tubing.
1 Thermocouple readout (Omega HH-25KF Type K),
flexible connector, and probe (CASS-14G-24).
1 Parallel printer cable.
1 1 ml positive displacement precision pipette with
disposable tips.
3 Spare 25A solid state relays.

188
Polaroaraph Setup
Most of the lead-in-air monitor’s components can be handled and
transported without special precautions. The Model 303A polarograph,
however, is a sensitive piece of equipment and requires special attention with
regard to its handling and use.
During its use, the polarograph is housed within Module 1 and is
connected to the various Module components. As long as the system remains
fairly level, the unit may be safely moved from one location to another. If the
equipment must be shipped, however, the polarograph should be removed
from the module and prepared for shipping. Instructions for preparing the
polarograph for shipping are detailed in Section E-5.
Following its shipping, the polarograph can be setup for operation by the
following procedures:
1) Unpack the Model 303A from its shipping container and place it on a
stable, level surface. If available, use of a ventilated fume hood is
recommended.
2) Unpack the Model 264A control unit and place it next to the Model
303A. Using the 25 pin D-sub ribbon cable (coded AA-JJ), connect
the Model 264A to the Model 303A. Connecting ports are located at
the rear of each unit. Connect the Model 264A to a 120 VAC power
source.
3) Unpack and install the glass capillary in the Model 303A electrode
support block according to the procedures outlined in the Model 303A
manual.
4) Carefully following the procedure described in the Model 303A manual,
fill the Model 303A reservoir with approximately 2 kg mercury. To
ensure accurate test results, use only high-purity, triply-distilled or
better analytical grade mercury. The mercury supplied by Bethlehem
Apparatus Corp. has been found suitable for this purpose and is
recommended.
Should you encounter any difficulty in filling the mercury reservoir or
attaining continuity in the glass capillary, contact the manufacturer for
assistance.

189
5) Unpack the polarograph reference electrode. Using the technique
outlined in the Model 303A manual, fill the glass sleeve of the
reference electrode to within 1 cm of capacity using the supplied
Ag/AgCI solution. Make sure the sleeve is free of air bubbles before
its installation. If necessary, a very small quantity of petroleum jelly
can be applied to the sleeve’s external o-ring to ease its insertion into
the electrode support block.
6) Add approximately 10 to 15 ml of D.I. water to a teflon static cell and
install it within the Model 303A. This immerses the electrodes in the
water and prevents the reference electrode from drying out. The static
cell will later be replaced by the flow-through cell.
7) Unpack Module 1 and place it on the utility cart’s top shelf in the
location shown in Figure E-1. Make sure its door can open and close
freely without hitting the upraised edge of the cart.
8) Disconnect the ribbon cable from the Model 303A. Carefully place the
Model 303A inside Module 1 in the location shown in Figure E-2.
Connect the 25 pin D-sub cable (attached to the digital logic board)
to the rear of the Model 303A. Also attach the 1 /4 inch flexible tube
(which supplies nitrogen purge gas) to the hose-barb fitting at the rear
of the Model 303A.
Setup of Remaining Components
1) Place the Model 264A on the cart’s second shelf in the position
indicated in Figure E-1. Connect the Model 264A ribbon cable to the
rear of Module 1 as coded.
2) Unpack Module 2 and place it on the cart’s lower shelf in the position
shown in Figure E-1.
3) Unpack the computer and place it next to the Model 264A on the
second shelf. Place the monochrome monitor on the cart’s top shelf
next to Module 1 and connect the monitor cable to the computer’s
labeled port. Attach the keyboard cable to the computer port (marked
K.B.).
4) Unpack the Keithley 575 data acquisition and control system and
place it on top of the Model 264A.

190
Figure E-1. Photograph of lead-in-air monitor showing arrangement of
components on utility cart.

191
Figure E-2. Photograph of Module 1 interior showing location of components.

192
5) Connect all remaining ribbon cables into the appropriate component
ports using the connectors codes as guides. Descriptions of external
cable connections are provided in Table E-1.
6) Attach power cords to the computer, Module 1, Module 2, and
Model 264A. Plug these cords (plus the monitor’s power cord) into
the power strip installed on the cart’s lower shelf.
7) Unpack the 10 liter polypropylene waste container and place it on the
the cart’s bottom shelf next to the power strip. Connect the waste
container to the Module 1 waste outlet using the supplied 22 inch long
1/4 inch O.D. teflon tube.
Note: To prevent fluid leakages, all teflon tubes in the lead-in-air
monitor have been scored using the supplied tubing grooving
tool. Should tubing ever need to be replaced, refer to the
grooving tool’s manual for instructions concerning its use.
Use the following procedures to ensure that tubing connectors
are properly installed.
1) Slide the ferrule nut past the groove on the teflon tube.
2) Insert the end of the tube into the fitting until it bottoms out.
3) Slide the ferrule nut to the fitting and hand tighten.
4) Pull on the tube slowly until it catches on the grooved edge.
5) Hand tighten the ferrule an additional 1 /2 to 3/4 of a turn.
Should a leak in the fitting occur during its use, repeat the
above steps. If the leak persists, replace the fitting and the
teflon tubing.
8) Connect the Module 1 air outlet to the Module 2 air inlet using the
supplied 1/2 inch O.D. polypropylene tube.
9) Install a nitrogen cylinder (with attached regulator) within its support
block inside Module 1. Connect the 1/4 inch flexible tube to the
regulator outlet. Open the regulator valve by turning it fully
counterclockwise.
10) Unpack the 5 liter teflon reservoir and place it within its Module 1
support block. As shown in Figure E-2, make sure the fluid level

193
Table E-1
Description of External Cable Connections
Cable Code
AA (Module 1)
BB (Module 1)
CC (Model 575)
DD (Model 575)
EE (Model 575)
FF (Model 575)
GG (Model 575)
HH (Model 264A)
II (Model 264A)
JJ (Model 264A)
KK (Module 2)
LL (Computer)
Connection
JJ (Model 264A)
DD (Model 575)
II (Model 264A)
BB (Module 1)
KK (Module 2)
LL (Computer)
HH (Model 264A)
GG (Model 575)
CC (Model 575)
AA (Module 1)
EE (Model 575)
FF (Model 575)

194
switch is positioned within the cutout of the support block. Plug in the
level switch quick-disconnect wires. Attach the 1/4 inch O.D. flexible
tygon tube to the hose barb connector of the glass-wool packed
drying tube. Lastly, attach the 1 /4 inch teflon tube to the inlet fitting
of liquid pump LP1.
11) To fill the electrolyte reservoir, first remove the container’s outer and
inner caps and place them on a clean surface. Using the supplied
polypropylene funnel to prevent spillage, fill the reservoir with the
0.5M HNOg/200 ppb copper electrolyte. Procedures for preparing the
electrolyte are outlined in section E . Remove the funnel and replace
the two teflon caps.
12) Remove the static cell from the polarograph. To do this, support the
cell with one hand and swing the spring-loaded support plate out of
position. Then lower the teflon cup straight down until the electrodes
are free from the cup. Discard the cup’s contents and store the cup
for later use.
13) Unpack the teflon flow-through cell and place the supplied magnetic
stirring bar inside it. Rinse the cell twice with D.l. water. Install the
cup under the electrode support block and hold in place. While
holding the cell in position, slide the Model 305 stirrer under the cell
until the cell is centered over the stirrer. The stirrer supports the cell
in place. Connect the cell’s outlet tube to the inlet of liquid pump LP3.
Note that the polarographic will have to shifted back and forth slightly
to properly attach the tube fittings.
14) Using the supplied 15 ml pipette and squeeze bulb, introduce 15 ml
of D.l. water into the flow-through cell through the open connector of
the electrode support block. If the liquid is observed to flow down to
liquid pump LP2, it indicates a leak in the tubing connectors.
15) Attach the teflon tube from liquid pump LP2 to the inlet tube on the
electrode support block. See Figure E-3 for a view of the flow-through
cell and the support block connector.
16) Set the Model 303A front panel controls as indicated in Table E-2.
Once these switches are set, they need not be changed during use
of the lead-in-air monitor.
17) Set the Model 264A front panel controls as outlined in Table E-2.
Make sure that values are set properly. Once the values are set, they
need not be changed during normal use of the instrument.

195
Figure E-3. Photograph of flow-through polarographic cell showing location of
inlet and outlet fittings.

Table E-2
Standard Settings for Polaroaraph and Analyzer
Model 303A Polaroaraph
Drop Enable = On
Mode = HMDE
Drop Size = M
Purge Time (min) = 2
Model 264A Analyzer
Initial Potential (Volts) = - 0.60
Final Potential (Volts) = +0.20
Scan Rate (mV/sec) = 10
Meter = Current
Current Range = 20 /jA
Filter (DC Only) = Off
Output Offset = Straight Up
Purge Time (minutes) = 0
Deposition Time (seconds) = 180
Equil Time = 15 sec
Drop Time = 0.5 sec
Pulse Height = 50 mV
Replication = 1
Analysis Mode = Diff Pulse Stripping

197
18) With the power strip off, plug in all power cords. Then with the power
still off, turn on the Model 264A (rear panel), Kiethley 575 (front panel),
monitor (front panel), and computer (front panel). These components
will thus power up when the power strip is turned on.
This completes the initial setup of the lead-in-air monitor. Procede to the
following section to perform initial checks of the system.

198
E.2 PREPARATION OF STANDARD SOLUTIONS
Electrolyte Preparation
The electrolyte used in the lead-in-air monitor consists of 0.5M HN03
with a 200 ppb internal copper standard. The accuracy and detection limit
of the monitor depends on the quality of the prepared electrolyte.
Preparation of the electrolyte should be performed in a clean work area
and the following steps performed as carefully as possible.
1) To a clean, acid-washed 10 liter polypropylene container, add
approximately 5 liters of D.l. water. The exact volume added is
not critical.
Note: Use the best quality water available. Distilled water
manufactured by Zephyrhills Spring Water Co. has been
found satisfactory for this purpose and is available from
most supermarkets. Other brands may also be used as
long the water passes the "Solution Background Check"
outlined in Section E.3.
2) To the container, add 300 ml of concentrated nitric acid. The use
of trace metal grade (Fisher A509-212) is recommended for this
purpose. Do not use reagent grade nitric acid as its impurity
content may be unacceptably high.
3) Add 2 ml of 1000 ppm copper standard (Fisher SC194-500) to the
container. The use of the supplied positive displacement pipette
with disposable tips is recommended to ensure accurate results.
Refer to the pipette’s accompanying manual to ensure its proper
use.
4) Add distilled water to the container until the 10 liter fluid level is
reached. Cap the container tightly and mix the contents
thoroughly. Label and date the container. This solution may be
stored up to one month in this container. After one month, the
contents should be disposed of properly and a new solution
prepared.
5) To fill the Module 1 reservoir, remove the reservoir’s outer and
inner caps and place them on a clean surface. Using the
supplied polypropylene funnel to minimize spillage, fill the

199
reservoir with the electrolyte. Immediately wipe up any spills
which may occur. Remove the funnel and replace the two teflon
caps.
100 ppb Lead Standard Preparation
The 100 ppb lead standard is used to verify the accuracy of the lead-
in-air monitor’s analysis section. Prepare the lead standard in a clean
work area free from possible lead contamination. To ensure accurate test
results, perform the following steps carefully:
1) To an acid-washed, 1000 ml volumetric polypropylene flask
(Fisher 10-198-50F), add approximately 500 ml of distilled water.
The exact volume of water added is not critical. Use the same
quality water used for preparation of the electrolyte.
2) To the container, add 30 ml of trace metal grade nitric acid.
3) Using a clean 25 ml pipette and squeeze bulb, add to the
container 25 ml of certified 1000 ppb lead standard (Fisher SL21-
500).
4) Add distilled water to the container until the 1000 ml level is
reached. Cap the container tightly and mix the contents
thoroughly.
The resulting solution is a 25 ppm lead standard solution which
will later be diluted to prepare the 100 ppb lead standard. Label
and date the container. If this 25 ppm container is refrigerated,
it may be stored for several months before a fresh solution need
be prepared.
5) To an separate acid-washed, 1000 ml volumetric polypropylene
flask, add approximately 500 ml of the 0.5M HN03/200 ppb
copper electrolyte prepared earlier. The exact volume of
electrolyte added is not critical.
6) Using the 1 ml positive displacement pipette with a fresh tip, add
4 ml of the 25 ppm lead standard solution to the container.

200
7) Add 0.5M HNO3/2OO ppb copper electrolyte to the container until
the 1000 ml fluid level is achieved. Cap the container and mix the
contents thoroughly.
The resulting concentration of this solution is 100 ppb lead
standard in 0.5M HN03 with a 200 ppb copper standard. Label
and date the container. The solution can then be used to
perform the calibration check which will be outlined in Section 3.3.
The shelf life of this solution is approximately two weeks. After
that time period, its contents should be disposed of properly and
a fresh solution prepared.

201
E.3 INITIAL SYSTEM CHECKS
The following system checks should be performed whenever the system
has been setup following its shipping. These system checks can also be
performed at any time to verify the working condition of the lead-in-air monitor.
Instrument Status
Turn on the power strip. Following the autoload of the main computer
program, verify the following instrument conditions:
Kiethley 575: Red power light is on
Model 303A: Green "drop dispenser" light is on
Red "cell on" light is on
Model 264A: Digital panel meter reads 0.000 ± 0.010 volts
The meter typically displays a +0.004 V value
Red "standby" light is on. All other lights on the
Model 264A should be off.
Computer: Yellow "turbo" light is on
Green "power" light is on
Monitor: Lead-in-air monitor’s Main Menu appears
If the system passes these initial checks, procede to the next section.
Otherwise consult the troubleshooting guide in Section E-6 for possible
explanations.
Solution Background Check
The following procedure is useful for verifying the overall operation of
instrument.
1) Turn on the power strip to power the system components.
On the monitor, the following menu will appear:

202
Main Menu
1) Perform Single Sampling and Analysis
2) Unattended Sampling and Analysis
3) Analyze Solution Only
4) View or Print Previous Test Results
5) Fluid Handling Options
6) Exit Program
2) From this main menu, select option 5 - Fluid Handling
Option.
3) A menu of fluid handling options will appear:
Fluid Handling Options
1) Main Rinse
2) Fill Impactor
3) Empty Impactor
4) Empty Polarographic Cell
5) Exit to Main Menu
From this menu, select option 1 - Main Rinse.
Caution: Make sure the inlet plug is removed from the
Module 1 air inlet section.
4)With the Module 1 door open, observe the sequence of the
main rinse routine. Liquid pumps LP1 and LP3 should
simultaneously fill the impactor and empty the polarographic
cell, respectively. Check the liquid fittings for possible leaks.
Once the impactor is filled, the air pump should activate for
10 seconds to thoroughly rinse the containers walls. Liquid
pump LP2 will then activate to fill the flow-through cell.
Once filled, LP3 and LP2 will operate concurrently until the
impactor is empty. The flow-through cell should now
contain approximately 15-18 ml of electrolyte. The exact
volume present is not critical.
You will then be returned to the Main Menu.

203
5) If the system is being checked following its shipment or
transport, repeat steps 2 through 4. Otherwise procede to
step 6.
6) From the main menu, select option 3 - Analyze Solution.
At the prompt, enter an appropriate description for this test.
Analysis will first begin with a 3 minute nitrogen purge.
Adjust the rotameter until the flowrate reads 0.03 to 0.05
Ipm. Following the purge cycle, the 3 minute deposition
phase will begin as indicated by the monitor and the
deposit light on the Model 264A front panel. A 15 second
equilibrium time will then take place indicated by the
equilibrate light. An 80 second analysis time will then occur
indicated by the scan light and the computer monitor.
During the analysis phase, the 264A panel meter displays
the measured scan currents.
7) Following a brief calculation phase, the test results will be
displayed on the monitor. Record the value of the liquid
lead concentration (ppb) and the magnitude of the lead and
copper peak heights (volts). Repeat steps 6 and 7 at least
two more times.
The average of the reported liquid lead concentrations
during three analysis should be less than 20 ppb. As
explained in Chapter 5 of the text, this response is normally
due to the presence of hydronium ions rather than
background lead content of the solution itself. If the
average calculated lead concentration is higher than 20 ppb,
consult the troubleshooting guide for assistance.
The average voltage corresponding to the 200 ppb copper
content of the electrolyte should be approximately
-1.600 V ±50%.
This completes the instrument background check. Procede to the
following section to verify the instrument’s lead detection capabilities.

204
Lead Calibration Check
To verify the instrument’s ability to accurately quantify a known liquid
lead concentration, perform the following steps:
1) Turn on the power strip to power the system components.
At the Main Menu, select option 5 - Fluid Handling Options.
2) Select option 1 to perform a Main Rinse.
3) At the completion of the rinse routine, you will be returned
to the Main Menu. Select option 5 - Fluid Handling Options.
4) Select option 4 - Empty Polarographic Cell.
5) Loosen the ferrule nut at the electrode support inlet fitting
(Figure E-3) and remove the teflon tube.
6) Using the supplied 15 ml pipette and squeeze bulb,
dispense 15 ml of the prepared 100 ppb lead standard
solution through the inlet fitting into the flow-through cell.
Reattach the inlet tube.
7) Select option 5 - Exit to Main Menu.
8) From the Main Menu, select option 3 - Analyze Solution
Only. At the prompt, enter an appropriate description for
this test.
9) Following the analysis, the test results will be displayed on
the monitor. Record the values of the liquid lead
concentration (ppb) and the magnitude of the lead and
copper peak heights (volts). Steps 8 and 9 should be
repeated at least two additional times.
The average of the reported liquid lead concentrations
during three analyses should be equal to 100 ppb ± 5%.
If the reported concentration is outside this range, consult
the troubleshooting section for possible causes.

205
The average voltage corresponding to the 200 ppb copper
content of the electrolyte should be approximately
-1.600 V ±50%.
10) From the Main Menu, select option 5 - Fluid Handling
Option. From the fluid handling menu, select option 1 -
Main Rinse.

206
E.4 OPERATING INSTRUCTIONS
Presampling Checklist
Once the lead-in-air monitor has been setup and the initial system checks
completed, air sampling can be performed. Prior to the sampling, it is
recommended that the following steps be performed.
1) Inspect the electrolyte reservoir and verify that the available supply is
sufficient for the intended tests. If necessary, fill the reservoir before
use. Also make sure that the nitrogen tank pressure is at least 50
psig. If not, replace the tank using the procedures outlined in
section E.5.
2) Make sure that the 10 liter waste container is not more than half full.
As a conservative guideline, the waste container should be emptied
each time the electrolyte reservoir is filled.
Note: The waste fluid consists of nitric acid with significant quantities
of lead and copper. Handle and dispose of this solution
properly.
The waste container will also contain small amounts of
mercury. Rather than pouring this mercury out each time the
container is emptied, it is recommended that the mercury be
allowed to accumulate at the bottom of the waste container.
When a significant quantity of mercury accumulates (over
several hundred test runs), it may be collected and shipped
to Bethlehem Apparatus Corp. to be refined and reused.
3) If static sampling is to be performed, make sure the following
components are available:
a. Temperature gauge, flexible connector, and temperature probe.
b. 6 inch long, 1 inch O.D. stainless steel inlet nozzle.
c. Extension cord of sufficient length, rated for 20A service.
d. Tools for attaching inlet nozzle to Module 1 bulkhead inlet fitting.
e. Notebook

207
4)If duct sampling is to be performed, the following components are
required:
a. Temperature gauge, flexible connector, and temperature probe.
b. Stainless steel inlet nozzles of 3/16, 1/4, and 1/2 inch diameter
with accompanying 1 inch female connector.
c. Flexible teflon-lined probe.
d. Stainless steel standard pitot tube (Dwyer 160-24) with two six foot
section of 3/16 inch I.D. tygon tubes.
e. 0-3 inch H20 manometer gauge (Dwyer Mark II Model 25) or
equivalent pressure gauge.
f. Extension cord of sufficient length, rated for 20A service.
g. Tools for attaching nozzles and probe.
h. Notebook
Sampling and Analysis Procedures
Still Air Sampling
1) Attach the stainless steel nozzle to the bulkhead fitting at the top of
Module 1 and tighten the compression fitting. It is recommended that
this inlet be covered with a plastic bag until just prior to air sampling.
2) Move the monitor to the desired point of sampling.
3) Using the extension cord, connect the power strip to an available
120 VAC, 20A power supply.
4) With the temperature gauge, measure and record the air temperature
(°F) at the intended point of sampling.
5) Turn on the power strip to power the system components.
6) At power up, the computer program loads and executes automatically
to present the main menu:

208
Main Menu
1) Perform Single Sampling and Analysis
2) Unattended Sampling and Analysis
3) Analyze Solution Only
4) View or Print Previous Test Results
5) Fluid Handling Options
6) Exit Program
Select either option 1 or 2 as desired. Single point sampling is
chosen if the user wants to perform single point analysis at various
sampling locations within the plant. After each test, the user is
returned to the Main Menu for the next selection. The unattended
sampling and analysis option allows the user to perform repeated
sampling and analysis tests at a single sampling without input from
the operator.
7) At the prompt, enter the gas temperature measured earlier.
8) The user is then prompted for the measured gas velocity pressure.
For the still (static) air sampling, enter a 0 value.
9) At the prompt, enter an appropriate description for this test. This
description may contain up to 30 characters and will be saved on the
computer’s hard drive along with the test results.
10) Press the spacebar to begin air sampling. Sampling will be
performed for 15 minutes at a flowrate of 15 alpm. During the test,
the sampling time remaining will be displayed on the monitor.
11) When the air sampling is completed, the collected lead is quantified
and the test results displayed on the monitor. These results are
automatically saved to the computer’s hard drive for later inspection.
If operating in Single Sampling and Analysis mode, press any key to
return to the Main Menu.
If operating in Unattended Sampling and Analysis mode, the test
results will be displayed for 30 seconds before beginning another
sampling and analysis cycle. During this display period, the user is
prompted to press function key F5 if he desires to abort the

209
unattended operation. Pressing F5 returns the user to the main
menu for the next selection.
12) Upon completing the desired tests, the lead-in-air monitor can be
shutdown. To do this, simply exit the program and turn off the
system’s power strip.
Note: Should a power interruption occur during the sampling or analysis
cycle, the computer will automatically reboot the program and the
current test information will be lost. If the interruption occurred during
air sampling, 50 ml of the electrolyte will remain in the impactor. This
volume must be removed prior to the next test or the flow-through
cell will overflow. To empty the impactor following a power outage,
perform the following steps:
1) At the Main Menu, select option 5 - Fluid Handling Options.
2) At the Fluid Handling Menu, select option 3 - Empty Impactor.
Liquid pumps LP2 and LP3 will be sequenced to transfer the
impactor’s contents to the waste container.
The user can then return to the Main Menu and repeat the test
series.
Ducted Air Sampling
As discussed in Chapter 4, accurate collection and transport of
particulates from ducted airstreams requires that special sampling
considerations be observed. Alternatives to the supplied sampling nozzles
and probe have been presented and can be investigated. This section will
outline procedures necessary for use of the supplied duct sampling
equipment.
1) Position the lead-in-air monitor as close to the intended point of
sampling as possible. Access to ducted airstreams may require that
special support platforms be designed and constructed to
accommodate the monitor.
2) Using the extension cord, connect the power strip to an available
120 VAC, 20A power supply.

210
3) Select the point of sampling based on the duct configuration and
access availability. Consider port locations at 90° duct bends where
the sampling probe can be directed into the oncoming airstream. For
single point sampling, it is better to sample at the centroid rather than
the midpoint of the duct’s cross-section.
4) With the temperature gauge, measure and record the air temperature
(°F) at the intended point of sampling.
5) Prepare the standard pitot tube for velocity measurements. Connect
the total pressure port of the pitot tube to the high side of the
manometer using one section of the 3/16 inch I.D. flexible tubing.
Using the other piece of tubing, connect the static port of the pitot
tube to the low side of the manometer. Zero and level the
manometer at this time.
6) At the desired point of sampling, direct the pitot tube into the
oncoming flowstream and record the resulting velocity pressure
(inches of water) indicated on the manometer.
7) Turn on the power strip to provide power to the lead-in-air monitor’s
components.
8) At power up, the computer program loads and executes automatically
to present the main menu:
Main Menu
1) Perform Single Sampling and Analysis
2) Unattended Sampling and Analysis
3) Analyze Solution Only
4) View or Print Previous Test Results
5) Fluid Handling Options
6) Exit Program
Select either option 1 or 2 as desired. Single point sampling is
chosen if the user wants to perform single point analysis at various
sampling locations within the plant. After each test, the user is
returned to the Main Menu for the next selection. The unattended
sampling and analysis option allows the user to perform repeated
sampling and analysis tests at a single sampling without input from
the operator.

211
9) At the prompt, enter the gas temperature measured earlier.
10) As requested, enter the measured velocity pressure recorded earlier.
11) A calculation is then made of the gas’ velocity and the user is notified
of the recommended nozzle size required to achieve isokinetic
sampling under these conditions. Select an available nozzle diameter
nearest to this size and enter the diameter into the program. The
program will later adjust the sampling flowrate to provide isokinetic
sampling through the selected nozzle.
12) At the prompt, enter an appropriate description for this test. This
description may contain up to 30 characters and will be saved on the
computer’s hard drive along with the test results.
13) As indicated in Figure 4-1, attach the selected nozzle to the sampling
probe then connect the probe to the Module 1 bulkhead inlet. Make
sure that all fittings are tight.
14) Insert the nozzle and probe through the sampling port. Position the
probe so it is directed into the oncoming airstream. Support the
probe as needed.
15) Press the spacebar to begin the air sampling cycle. Air sampling will
be performed for 15 minutes.
16) When the air sampling is completed, carefully remove the probe from
the duct and support it as needed. When the collected lead is
quantified, the test results will be displayed on the monitor. These
results are automatically saved to the computer’s hard drive for later
inspection.
If operating in Single Sampling and Analysis mode, press any key to
return to the Main Menu.
If operating in Unattended Sampling and Analysis mode, the test
results will be displayed for 30 seconds before beginning another
sampling and analysis cycle. During this display period, the user is
prompted to press function key F5 if he desires to abort the
unattended operation. Pressing F5 returns the user to the main
menu for the next selection.

212
17) Upon completing the desired tests, the lead-in-air monitor can be
shutdown. To do this, simply exit the program and turn off the
system’s power strip.
Note: Should a power interruption occur during the sampling or analysis
cycle, the computer will automatically reboot the program and the
current test information will be lost. If the interruption occurred during
air sampling, 50 ml of the electrolyte will remain in the impactor. This
volume must be removed prior to the next test or the flow-through
cell will overflow. To empty the impactor following a power outage,
perform the following steps:
1) At the Main Menu, select option 5 - Fluid Handling Options.
2) At the Fluid Handling Menu, select option 3 - Empty Impactor.
Liquid pumps LP2 and LP3 will be sequenced to transfer the
impactor’s contents to the waste container.
The user can then return to the Main Menu and repeat the test
series.
Viewing or Printing Previous Test Results
Following each sampling and analysis test, the test results are displayed
on the computer monitor for the user’s inspection. These results are also
automatically saved on the computer’s hard drive for later inspection. All test
results are stored in the directory C:\K500\RESULTS created for this purpose.
To view previously saved test results, perform the following steps:
1) From the Main Menu, select option 4 - View or Print Previous Test
Results. The following menu will appear:
Menu of Test Results
1) List Existing File Names
2) View Archived Test Results
3) Print Archived Test Results
4) Exit to Main Menu
2) If desired, select option 1 to display the directory of existing file names.

213
Test results are stored under filenames equivalent to the date the test
was performed. Multiple test results performed on the same day are
saved in the same file. After viewing the file directory, press any key to
return to the menu.
3) To view a specific saved file, select option 2 - View Archived Test
Results. At the prompt, enter the filename you wish to view. Either the
mm/dd/yy or mm-dd-yy format is acceptable.
Information displayed for each test includes the test’s starting time, test
duration, average sampling flowrate, liquid and air lead concentration,
and a test description. The monitor will display ten test results at a time.
Press the spacebar to view the next screen of test results. When the
last test results have been viewed, press any key to return to the view
menu.
4) Printing previous test results first requires that the user connect the
computer to a parallel letter-quality or dot-matrix printer using the
supplied parallel printer cable. Once the printer is connected and turned
on, select option 3 - Print Archived Test Results.
At the prompt, enter the filename you wish to view. Either the
mm/dd/yy or mm-dd-yy format is acceptable.
Information printed for each test includes the test’s starting time, test
duration, average sampling flowrate, liquid and air lead concentration,
and a test description. When the test results have been printed, press
any key to return to the view menu.

214
E.4 MAINTENANCE OF THE LEAD-IN-AIR MONITOR
If normal care is observed during its handling and use, the lead-in-air
monitor is expected to require little periodic maintenance. Unless a
malfunction occurs, the computer, data acquisition and control system, and
the Model 264A control unit should provide extended service without the need
for periodic maintenance. At regular intervals, however, it is recommended
that the following maintenance be performed to ensure that the monitor
functions accurately.
Maintenance of the Reference Electrode
The Model 303A polarograph’s reference electrode contains a Ag/AgCI
reference solution which provides a stable potential upon which the voltametric
measurements are based. Because the reference electrode is immersed in the
nitric acid electrolyte, the reference solution will eventually become diluted with
time. This may result in a shift in the peak potentials measured during the lead
analysis. To ensure accurate test results, it is recommended that the
reference solution be replaced at monthly intervals. Procedures for replacing
the solution are as follows:
1) Turn on the power strip to provide power to the system components.
2) At the Main Menu, select option 5 - Fluid Handling Options.
3) At the Fluid Handling Menu, select option 4 - Empty Polarographic
Cell. When the cell is empty, turn off the power strip.
4) Remove the flow-through cell from Module 1. First, loosen the teflon
ferrule at the liquid pump LP3 inlet. Rotate the inlet connector slightly
to remove the teflon tube from the fitting. While supporting the flow¬
through cell with one hand, slide the Model 305 stirrer forward until it
is free from the cell. Set the stirrer aside. Lower the cell straight down
until the electrodes are free from the cup.
Caution: The cell may contain a small quantity of mercury from
previous test runs. Collect this mercury for later recycle.
The cup can also be cleaned at this time by rinsing it with
0.1 M nitric acid, wiping it with a KimWipe, and rinsing it with
distilled water.

215
5) Using firm downward pressure, remove the glass electrode from the
plastic support block and discard its contents. Inspect the Vycor frit
at the end of the glass sleeve. If it appears cracked or damaged,
replace it according to the procedures outlined in the Model 303A
manual.
Rinse out the electrode with the supplied Ag/AgCI filling solution then
fill it to within 1 cm of capacity. Make sure the sleeve is free of air
bubbles before proceeding.
6) Reinstall the reference electrode within the support block. In
necessary, a very small quantity of petroleum jelly may be applied to
the sleeve’s external o-ring to ease its insertion into the support block.
7) Reinstall the flow-through cell, replace the stirrer, and reconnect the
teflon tube to the liquid pump LP3 inlet.
8) Turn on the power strip to provide power to the system components.
At the Main Menu, select option 5 - Fluid Handling Options.
9) At the Fluid Handling Menu, select option 1 - Main Rinse. Perform the
main rinse routine two times. Return to the Main Menu and exit the
program.
This completes the required maintenance of the reference electrode.
Impactor Maintenance
Repeated use of the impactor to collect particulates may result in the
accumulation of deposits within the impactor’s inner surfaces. It is
recommended that these deposits be removed at regular intervals. Experience
will dictate the frequency at which this maintenance occurs. For static or
recirculation air sampling, it is expected that many tests can be performed
before cleaning is necessary. A greater cleaning frequency can be expected
if higher aerosol concentrations are routinely sampled.
Cleaning of the impactor requires its removal from Module 1. Refer to
Figure 4-1 and perform the following steps:
1) Loosen the ferrules of the 3/8 inch union elbow (component 9) and
remove the elbow. Loosen and remove the 3 7/8 inch tube
(component 8) attached to the elbow.

216
2) Loosen the retaining nut of the 1 inch bulkhead connector
(component 4) until the nut has traveled approximately 1 inch on the
threads.
3) Loosen the teflon ferrule of the impactor liquid inlet and remove the
teflon tube.
4) Rotate the impactor counter-clockwise to unscrew it from liquid pump
LP2. When detached, lift the impactor straight up and tilt it until its
bottom fitting is clear of the pump. Lower the impactor until the
stainless steel inlet tube is clear of the bulkhead fitting. Remove the
impactor from Module 1.
5) Begin disassembly of the impactor by unscrewing and removing its
teflon housing inlet from the main body. Rinse the interior surfaces of
the housing with 0.1 M nitric acid and wipe its surfaces with a KimWipe.
Rinse the housing with distilled water and set aside to dry. When dry,
remove any teflon tape from the bottom pipe fitting and rewrap with
two turns of 1 /2 wide teflon tape.
Unscrew the impactor stage from the central tube and rinse these
components with 0.1M nitric acid. Wipe all surfaces with KimWipes,
rinse with distilled water, and set aside to dry.
When all the impactor components are dry, reassemble the impactor
and install it within Module 1 by reversing the disassembly procedures.
Make sure all fittings are tight to ensure proper seals.
Nitrogen Cylinder Replacement
The supplied nitrogen cylinders have a rated capacity of 34 liters of
nitrogen at standard conditions. This supply is sufficient for approximately 200
separate analyses before the cylinder need be replaced. Periodically check
the pressure gauge to ensure that the supply pressure has not dropped below
50 psig. To replace the cylinder, perform the following steps:
1) Close the regulator valve by turning the valve fully clockwise.
2) Remove the flexible tubing from the regulator’s hose barb outlet
connector. Remove the cylinder from its Module 1 support block.

217
3) Unscrew the regulator and remove it from the empty cylinder. Dispose
of the cylinder properly. These cylinders are not rechargeable.
4) Screw the regulator Into a fresh cylinder and Install the cylinder inside
Module 1. Attach the flexible tubing and fully open the regulator valve.

218
E.5 SHIPPING THE LEAD-IN-AIR MONITOR
With the exception of the Model 303A polarograph, most of the lead-in-air
monitor’s components can be packed and shipped successfully simply by
taking normal packing precautions. The procedures necessary to prepare the
polarograph for shipping will be outlined in this section. Preparation of other
system components will also be discussed.
1) Turn on the power strip to power the system components. At the Main
Menu, select option 5 - Fluid Handling Option. At the Fluid Handling
Menu, select option 4 - Empty Polarograph Cell. When the cell is
empty, turn off the power strip.
2) Remove the flow-through cell from Module 1. First, loosen the teflon
ferrule at the liquid pump LP3 inlet. Rotate the inlet connector slightly
to remove the teflon tube from the fitting. While supporting the flow¬
through cell with one hand, slide the Model 305 stirrer forward until it
is free from the cell. Set the stirrer aside. Lower the cell straight
down until the electrodes are free from the cup.
Caution: The cell may contain a small quantity of mercury from
previous test runs. Collect this mercury for later recycle.
The cup can also be cleaned at this time by rinsing it with
0.1 M nitric acid, wiping it with a KimWipe, and rinsing it with
distilled water.
3) To a static teflon polarographic cell, add 10 to 15 ml of distilled water.
Mount the cell in the polarograph using the spring-loaded arm to
support the cell.
4) Disconnect the ribbon cable and flexible nitrogen supply tube from the
rear of the Model 303A. Carefully remove the Model 303A from
Module 1 and place it on a stable, level surface. If available, use of a
ventilated fume hood is recommended.
5) Remove the ribbon cable (coded AA-JJ) connecting the Model 264A
to Module 1. After unplugging its power cord, place the 264A next to
the polarograph. Connect the two instruments using the coded AA-JJ
ribbon cable. Connect the Model 264A to a 120 VAC power source.
6) Using the procedures outlined in the Model 303A manual, remove the
glass capillary and pack for shipping. To prevent mercury leakage

219
during shipping, carefully drain the mercury from the polarograph (as
described in the manual) and store in a leak-free container.
Using firm downward pressure, remove the glass reference electrode
from the plastic support block and discard its liquid contents. To
prevent the frit from drying out, place the electrode in a sealed plastic
container filled with distilled water.
To minimize contamination during shipping and handling, it is
recommended that sensitive components (such as the glass capillary,
flow-through cell, and reference electrode) be placed in separate
press-lock style plastic bags prior to their packing.
7) To remove the electrolyte reservoir from Module 1, first disconnect the
flexible tygon tube from the filter column. Next loosen the teflon ferrule
at the inlet of liquid pump LP1 and remove the teflon tube. Disconnect
the level switch’s electrical connector. Remove the reservoir from
Module 1 and discard its contents in an appropriate manner.
8) Close the nitrogen regulator valve by turning it fully clockwise.
Disconnect the flexible tubing at the top of the regulator and remove
the nitrogen tank from Module 1.
9) Disconnect and remove the 1/4 inch tube which connects the
Module 1 waste outlet to the polypropylene waste container. Dispose
of the waste container’s contents in an appropriate manner.
10) Disconnect all power cords and ribbon cables from the lead-in-air
monitor’s various components.
11) Remove the remaining components from the utility cart. Pack the
components in a manner which will minimize the chance of their
damage during shipping.

220
E.6 TROUBLESHOOTING GUIDE
SvmDtom
Possible Cause and Solution
Instrument fails "status check"
Power cables or ribbon cables not
plugged in or improperly connected.
Check cables and connections.
Component power switches not on.
Check each instrument.
Model 303A and Model 264A panel
switches incorrectly set. Check
Table E-2.
Problem with electrical connectors.
Checks all connections.
Computer program does not
load.
Disk in drive A. Make sure drive A is
empty.
Problem with main program. Load
backup program from floppy drive.
Instrument fails solution
background check.
Background lead content of water too
high. Replace with better quality water.
Electrolyte improperly prepared.
Prepare fresh solution.
Liquid leaks at fittings.
Fitting improperly connected. Reattach
tubing using outlined procedures. If
problem continues, replace fitting and
tubing.

221
Polarographic cell overflows.
Liquid pump inoperative or out of
calibration. Check behavior of pumps
during main rinse cycle. Recalibrate or
replace as necessary.
Insufficient nitrogen flowrate.
Nitrogen cylinder is empty. Check
pressure and replace cylinder is below
50 psig.
Nitrogen solenoid inoperative. Check
condition of solenoid and controlling
electromechanical relay.
Rotameter improperly adjusted. Rotate
valve clockwise to increase flowrate.
Regulator valve closed. Turn counter¬
clockwise to open valve.
Leak in tubing or connector. Inspect
flow system for cause.
Copper peak not within 1.6V ±
50% during calibration check.
Electrolyte improperly prepared.
Prepare fresh solution and repeat test.
Reference electrode solution has been
diluted. Replace solution and repeat
test.
Model 264A controls improperly set.
Refer to Table E-2 for correct settings.
Response to 100 ppb lead
standard not within 5%.
Lead standard improperly prepared.
Prepare fresh standard and repeat test.
Reference electrode solution has been
diluted. Replace solution and repeat
test.
Model 264A controls improperly set.
Refer to Table E-2 for correct settings.

222
"Low Electrolyte" message when
reservoir is full.
Level switch connector not plugged in.
Check connection.
Float switch stuck in open position.
Inspect switch and replace if necessary.
Problem with electrical connection.
Trace connection and check for
continuity.
Air pump does not activate.
Ribbon cable not connected to Module
2. Check cable and connections.
Module 2 power cord not plugged in.
Check cable.
Sampling less than 90%
Isokinetic.
Flow pressure drop too high. Close
pump recirculation valve one turn and
repeat test. If problem persists, replace
cartridge filter.
Mass flow controller inoperative. Check
flow controller and power supply.
Air pump malfunction. Check pump
condition.
Sampling greater than 110%
isokinetic.
Mass flow controller inoperative. Check
flow controller and power supply.
Power surge occurs during test.
Load to power source is too high.
Locate alternative outlet.

REFERENCE LIST
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(1989).

BIOGRAPHICAL SKETCH
Robert William Vanderpool was born on November 13, 1955,
in Evanston, Illinois. He attended primary and secondary
school in Ocala, Florida. In 1988, he received a Bachelors of
Engineering degree from the University of Florida. He was
awarded a Masters of Engineering (with thesis option) from the
University of Florida in 1983. Following a six year period as
an engineering consultant, he began a doctorate program at the
University of Florida with a specialty in aerosol science and
air pollution control.
224

I certify that I have read this study and that in my opinion it conforms to
acceptable standards of scholarly presentation and is fully adequate, in scope and
quality, as a dissertation for the degree of Doctor of Philosophy.
Dale A. Lundgren, Chairman
Professor of Environmental
Engineering Sciences
I certify that I have read this study and that in my opinion it conforms to
acceptable standards of scholarly presentation and is fully adequate, in scope and
quality, as a dissertation for the degree of Doctor of Philosophy.
Eric R. Allen
Professor of Environmental
Engineering Sciences
I certify that I have read this study and that in my opinion it conforms to
acceptable standards of scholarly presentation and is fully adequate, in scope and
quality, as a dissertation for the degree of Doctor of Philosophy.
Professor of Materials Science
and Engineering
I certify that I have read this study and that in my opinion it conforms to
acceptable standards of scholarly presentation and is fully adequate, in scope and
quality, as a dissertation for the degree of Doctor of Philosophy.
Paul A. Chadik
Assistant Professor of
Environmental Engineering Sciences
I certify that I have read this study and that in my opinion it conforms to
acceptable standards of scholarly presentation and is fully adequate, in scope and
quality, as a dissertation for the degree of Doctor of Philosophy.
Roger ArGater
Associate Professor of
Mechanical Engineering

This dissertation was submitted to the Graduate Faculty of the College of
Engineering and to the Graduate School and was accepted as partial fulfillment of
the requirements for the degree of Doctor of Philosophy.
December 1991
J Cl - /Q>
Winfred M. Phillips
Dean, College of
Engineering
Madelyn M. Lockhart
Dean, Graduate School

UNIVERSITY OF FLORIDA
3 1262 08285 426 5




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