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Properties of petroleum oils in relation to performance as citrus tree sprays in Florida

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Title:
Properties of petroleum oils in relation to performance as citrus tree sprays in Florida
Creator:
Trammel, Kenneth, 1937-
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Language:
English
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x, 131 leaves : ill. ; 28 cm.

Subjects

Subjects / Keywords:
Distillation ( jstor )
Eggs ( jstor )
Fruits ( jstor )
Leaves ( jstor )
Mites ( jstor )
Molecular weight ( jstor )
Orange fruits ( jstor )
Petroleum ( jstor )
Transpiration ( jstor )
Viscosity ( jstor )
Citrus -- Diseases and pests ( lcsh )
Dissertations, Academic -- Entomology and Nematology -- UF
Entomology and Nematology thesis Ph. D
Petroleum products ( lcsh )
Spraying ( lcsh )
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bibliography ( marcgt )
non-fiction ( marcgt )

Notes

Thesis:
Thesis (Ph. D.)--University of Florida, 1965.
Bibliography:
Includes bibliographical references (leaves 121-129).
General Note:
Typescript.
General Note:
Vita.
Statement of Responsibility:
by Kenneth Trammel.

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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.
Resource Identifier:
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37463456 ( OCLC )

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PROPERTIES OF PETROLEUM OILS

IN RELATION TO PERFORMANCE AS

CITRUS TREE SPRAYS IN FLORIDA
















By

KENNETH TRAMMEL


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











UNIVERSITY OF FLORIDA


April, 1965
















ACKNOWLEDGMENTS


The author expresses sincere appreciation to Dr. J. T. Creighton

for serving as chairman of his supervisory committee and for financial

aid obtained through a National Defense Education Act fellowship. He

is deeply indebted to Dr. W. A. Simanton, co-chairman, for supervision

and assistance during the course of the investigations, for obtaining

grant funds to support the investigations, and for his invaluable

guidance in preparation of the manuscript. Appreciation is extended

to Dr. A. H. Krezdorn, Dr. Milledge Murphey, and Dr. V. G. Perry for

serving on the supervisory committee and for critically reviewing the

manuscript.

He is grateful to Dr. H. J. Reitz for financial aid and for use of

the facilities at the Citrus Experiment Station, and to numerous staff

members of the Citrus Experiment Station for consultation, advice, and

use of their laboratory facilities. Appreciation is expressed to Mrs.

Harriet Long of the Citrus Experiment Station for taking the photo-

graphs. The assistance of Mr. B. G. Shively in conducting the experi-

ments, especially his willingness to work long hours at night and on

week ends, is greatly appreciated.

Gratitude is expressed to the personnel of Humble Oil and Refining

Company, especially Mr. R. C. Halter, for the grant which supported the

investigations and for numerous oil samples used in this work. Contri-

bution of samples by the following oil companies is acknowledged: Gulf

Oil Corporation; Sun Oil Company; Shell Oil Company; Texaco, Incorpo-

rated; and American Oil Company. Contribution of emulsifiers by the









Rohm and Haas Company is appreciated.

The author expresses special appreciation to his wife for her

understanding, encouragement, and support during the years of study

prior to the preparation of the manuscript, and for her cooperation

and assistance in preparation of the manuscript.

He wishes to thank Mrs. Cynthia Boyd Evans for performing the

final typing and assisting in the Multilith duplication of the

manuscript.
















TABLE OF CONTENTS

Page

ACKNOWLEDGMENTS ..................................................... ii

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

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

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

LITERATURE REVIEW .................................................. 3

Source and Properties of Petroleum Spray Oil................... 3
Historical Use of Spray Oil ..................................... 5
Insecticidal and Ovicidal Action of Petroleum Oil............... 7
Phytotoxicity of Petroleum Oil................................... 12

Penetration of oil into plants................................ 12
Effects of oil on the physiological processes of plants...... 14
Injurious effects of oil sprays on citrus..................... 17

Specifications for Plant Spray Oils.............................. 19

MATERIALS AND METHODS .............................................. 23

Oil Specifications .............................................. 23
Preparation of Oils ............................................. 27
Application of Oils in Laboratory Studies........................ 27
Oil Deposit Determination........................................ 32
Insecticidal and Ovicidal Efficiency Studies.................... 34

Florida red scale studies .................................... 34

Infestation............................................... 34
Holding infested fruit .................................... 36
Scale development, treatment, and mortality counts........ 38
Testing the oils .......................................... 40

Citrus red mite studies ....................................... 41

Phytotoxicity Studies ............................................ 43

Laboratory experiments........................................ 43

Respiration studies ....................................... 43
Transpiration study ........................................ 45

Field experiments ......... .. ................................. 46









Page

Field Experiment No. 1: oil blotch, leaf drop, and
fruit drop ............................................. 47
Field Experiment No. 2: fruit color and internal fruit
quality ............................... .. ............ 47
Color measurement and ethylene degreening................. 48
Fruit quality............................................ 49

RESULTS AND DISCUSSION............................................ 50

Relation of Composition and Heaviness of Oils to Insecticidal
and Ovicidal Efficiency...................................... 50

Results ...................................................... 50

Florida red scale studies................................. 50
Citrus red mite studies................................... 61

Discussion ................................................... 71

Relation of Composition, Heaviness, and Refinement of Oil to
Phytotoxicity ................................................ 77

Respiration and transpiration............................... 77

Results .............................................. .. ... 77
Discussion ........................................... . .. 84

Oil blotch, leaf drop, and fruit drop........................ 88

Results.................................. ............... 88
Discussion ............................................. .. 92

Fruit color and ethylene degreening.......................... 96

Results............... ............................... .... 96
Discussion................ ...... ... ........... ...... 99

Internal fruit quality................ ...................... 106

Results ..... .................. ...... ... ............. 106
Discussion .............................. 0.. ......... ... .. 109

General Discussion ............... .................... ........... 112

SUMMARY AND CONCLUSIONS................... ...... ................ 115

LITERATURE CITED.................................................. 121

ADDITIONAL REFERENCES............................................... 130

BIOGRAPHICAL SKETCH............................................... 131















LIST OF TABLES


Table Page

1 Specifications for California spray oils................... 20

2 Specifications for oils applied to fruit and shade trees
in New York ................................................ 22

3 Specifications for various properties of petroleum oils
used in these studies ...................................... 24

4 Oil deposit, number of scales, and per cent kill with 3
series of petroleum oils in dosage-mortality tests against
Florida red scale ......................................... 51

5 Effectiveness of 3 series of petroleum oils against adult
female Florida red scale............................... .... 53

6 Effectiveness of commercial oils at 2 levels of appli-
cation against adult female Florida red scale............ 59

7 Oil deposit, number of eggs, and per cent kill with 3
series of petroleum oils in dosage-mortality tests
against citrus red mite eggs............................... 62

8 Effectiveness of 3 series of petroleum oils against
citrus red mite eggs ................ ....... ..... ..... . 65

9 Spider mite counts at 1, 4, and 7 weeks after application
of spray oils on 6 May 1964 in Block 23.................... 72

10 Respiratory rates of oil-sprayed 'Pineapple' seedlings
expressed as per cent of the check. Each value is the
mean of 6 determinations. Oils were applied at 70 to 80
pg/cm ................... ..... .. .... ... ........... ..... 78

11 Effect of 365-mol wt paraffinic oil on respiration of
adjacent treated and untreated leaves of 'Pineapple'
seedlings, measured as 02 uptake in pg/cm2 leaf surface
in a 2-hour period. The oil deposit was high
(154.4 pg/cm2) ........... *.. ***.. ............. .... 79

12 Transpiration rate of 'Pineapple' seedlings sprayed with
1.5% concentration of low, medium, and high molecular
weight fractions of paraffinic and naphthenic oils......... 80











13 Leaf drop by young 'Hamlin' trees following application
of oil sprays on 6 May 1964 in Block 23.................... 89

14 Fruit drop by young 'Hamlin' trees following application
of oil sprays on 6 May 1964 in Block 23.................... 93

15 Color of oil-sprayed 'Hamlin' oranges before and after
different intervals of ethylene degreening and per cent
pack-out at 4 and 8 weeks after spraying................... 97

16 Regression equations for the degreening rate of oil-
sprayed 'Hamlin' oranges and hours required to degree
to 30% absorbance level................................... 100

17 Analysis of oil-sprayed 'Hamlin' oranges at 4 dates of
harvest. Each mean is the average of determinations on
four 40-fruit samples. Sprayed 18 September 1964.......... 107


vii


Table


Page
















LIST OF FIGURES


Figure Page

1 Laboratory air-blast sprayer. A, high velocity blower;
B, motor; C, pump; D, spray tank; E, pressure regulator;
F, nozzle; G, deflector vanes; H, operating lever; I,
turntable .................................................. 29

2 Spray coverage obtained on fruit with the laboratory air-
blast sprayer. A, fruit sprayed with oil at 1.0% concen-
tration containing fluorescent dye to show the distribu-
tion of the oil; B, unsprayed fruit. Photographed under
ultra-violet light. The rectangular area on fruit "A"
was left unsprayed to show the contrast between sprayed
and unsprayed surface ...................................... 31

3 Method of infesting grapefruit with Florida red scale for
laboratory studies. A, ivy leaves with natural infesta-
tion of crawler-producing female scales; B, cheesecloth
strip with infested leaf sections; C, strip of leaf
sections wrapped firmly in position around the equator
of a grapefruit to allow crawlers to transfer; D, typical
infestation obtained by this method, at time of treatment
application (4.5 weeks after infestation).................. 35

4 Scale-infested grapefruit on moist vermiculite in holding
tray ... ................................................... .37

5 Holding facilities for infested fruit in laboratory
studies. A, chamber for holding trays of scale-infested
grapefruit; B, racks supporting immature oranges in-
fested with citrus red mite eggs........................... 39

6 Regression of per cent kill on deposit level for 3 series
of narrow-boiling petroleum fractions tested against adult
female Florida red scale. The number on each line indi-
cates the average molecular weight of the fraction......... 54

7 Efficiency in relation to molecular weight for 3 series of
narrow-boiling petroleum fractions against adult female
Florida red scale ......................................... 55

8 Efficiency in relation to viscosity for 3 series of narrow-
boiling petroleum fractions against adult female Florida
red scale ................. ............ ...... ....... ... 56


viii











9 Efficiency in relation to 50% distillation point for 3
series of narrow-boiling petroleum fractions against
adult female Florida red scale............................. 57

10 Regression of per cent kill on deposit level for 3 series
of narrow-boiling petroleum fractions tested against citrus
red mite eggs. The number on each line indicates the
average molecular weight of the fraction. The solid por-
tion of each line indicates the range of data collected;
the broken extension is extrapolation to the 50 or 95%
kill level ................................................. 67

11 Efficiency in relation to molecular weight for 3 series of
narrow-boiling petroleum fractions and 2 commercial oils
against citrus red mite eggs............................... 68

12 Efficiency in relation to viscosity for 3 series of narrow-
boiling petroleum fractions and 2 commercial oils against
citrus red mite eggs....................................... 69

13 Efficiency in relation to 50% distillation point for 3
series of narrow-boiling petroleum fractions and 2
commercial oils against citrus red mite eggs............... 70

14 Effect of light, medium, and heavy paraffinic fractions
on the transpiration rate of treated 'Pineapple' orange
seedlings in relation to time after treatment. Shaded
symbols indicate significance from check................... 82

15 Effect of light, medium, and heavy naphthenic fractions
on the transpiration rate of treated 'Pineapple' orange
seedlings in relation to time after treatment. Shaded
symbols indicate significance from the check............... 83

16 Accumulated leaf drop from 'Hamlin' orange trees in the
5-week period following application of 4 oils on 6 May
1964 ....................................................... 91

17 Degreening rate of oil-sprayed 'Hamlin' oranges 4 weeks
after spraying as indicated by decrease in per cent
absorbance with time in ethylene degreening chamber.
Sprays applied 18 September 1964; fruit harvested 16
October 1964 ............................................... 101

18 Degreening rate of oil-sprayed 'Hamlin' oranges 8 weeks
after spraying, as indicated by decrease in per cent
absorbance with time in ethylene degreening chamber.
Sprays applied 18 September 1964; fruit harvested 12
November 1964 .............................................. 102


Figure


Page









Figure


Page


19 'Hamlin' oranges from plots receiving late-season appli-
cation of 4 oils and degreened for 0, 24, 48, and 72
hours; sampled 4 and 8 weeks after treatment. Sprays
applied 18 September 1964.................................. 105

20 Effect of 4 oils on soluble solids development in 'Hamlin'
oranges. Sprays applied 18 September 1964................. 108
















INTRODUCTION


Petroleum oil is one of the most important pesticides used on

Florida citrus. It will control most species of scale insects, spider

mites, and the fungus disease greasy spot, caused by Cercospora citri-

grisea Fisher. Compared to most chemical pesticides, oil is economical

and safe for the user, has little adverse effect on biological control

agents, and its use creates no pesticidal residue problem. Because of

the physical mode of action of oil, development of resistance by the

above pests is unlikely. However, the use of oil is limited to a

short application period in June and July because of its adverse ef-

fects on the citrus plant. Improper application of oil sprays may re-

sult in fruit blemishes, excessive leaf and fruit drop, reduced fruit

set, poor fruit color and quality, and increased susceptibility of the

tree to cold weather injury.

Foliage-type spray oils are characterized by the physical proper-

ties of viscosity, distillation range, and molecular weight, and the

chemical properties of unsulfonated residue, or refinement, and hydro-

carbon composition. There are no recommended specifications for these

properties for oils used in Florida at present and a wide range of

materials are currently in use. Specifications for oils used on citrus

in California and on deciduous fruits in New York are well defined. In

recent years, some major oil companies have used specifications from

these states as guides in producing base oils for use on Florida cit-

rus, mainly because no information was available to indicate different









requirements. Although the available oils are quite diverse in their

properties, their use by Florida citrus growers over the past few years

has not generally resulted in excessive damage. However, damage from

oil sprays is not uncommon even though it is not always striking.

Where problems do occur, information about oil properties, formulation,

and application, sufficient to establish a probable cause, is seldom

available. Information pertaining to the relationship between chemical

and physical properties of spray oils and performance on Florida citrus

is needed.

The objective of the work reported herein was to establish the re-

lationship of physical and chemical properties of petroleum oil to in-

secticidal and ovicidal efficiency, and to phytotoxicity to citrus,

under Florida conditions. Three series of narrow-distillation range,

experimental fractions and numerous commercial oils provided wide

ranges of the various properties for study. The oils were tested in

the laboratory against adult female Florida red scale, Chrysomphalus

aonidum (L.), and against eggs of the citrus red mite, Panonychus citri

(McGregor), to establish the effective ranges of the various properties

for insecticidal and ovicidal efficiency. Phytotoxicity studies were

conducted under both laboratory and field conditions to relate oil

heaviness, refinement, and chemical composition to various adverse

effects on citrus. The results obtained may serve as a guide for ad-

ditional field studies, leading eventually to more rigid specifications

for petroleum oils used on citrus in Florida.















LITERATURE REVIEW


Source and Properties of Petroleum Spray Oil

Petroleum or "rock oil" (Greek petros = rock, and oleum = oil) is

mainly an oily liquid mixture of numerous hydrocarbons believed to have

been formed from the remains of animal and vegetable marine organisms.

It is comprised chiefly of paraffins aliphaticc chains), naphthenes or

asphaltics (saturated ring hydrocarbons), aromatics (ring hydrocarbons

with conjugated double bonds), and unsaturates aliphaticc or cyclic

hydrocarbons with one or more active double or triple bonds). The oil-

producing areas or fields in the United States are regionally referred

to as Eastern, Mid-continent, and Western or Californian. The Eastern

fields produce predominantly paraffin-base crudes, the Californian

fields produce predominantly asphaltic- or naphthenic-base crudes, and

the Mid-continent fields produce crudes of a mixed-base type. However,

any one of these types may be produced by individual wells in any area

(24).

In the distillation of a crude, the various petroleum fractions

come off in the order of liquified gas, petroleum ether, gasoline,

naphtha, kerosene, fuel oil, mineral seal oil, transformer oil, summer

spray oil, dormant spray oil, and lubricating oil. The summer and

dormant spray oils are in the light lubricating range. The heavier

materials withdrawn from the bottom of the fractionating tower, called

the residuum, may be used as fuel or, if from a suitable crude, re-

worked into asphalt. Distillation of the fractions from transformer









oil on up is conducted under vacuum to avoid heating above 750 F, at

which temperature decomposition, or cracking, occurs (24).

After distillation, the various cuts must be refined to remove un-

desirable substances. Kerosene, spray oils, and lubricating oils are

refined by essentially the same methods. The once common sulfuric acid

treatment has given way in recent years to a process employing sulfur

dioxide, known as the Edeleanu process. The oil and sulfur dioxide gas

are mixed in a pressure system and cooled to obtain 2 layers: 1) the

extract (lower layer), containing aromatic and other unsaturated hydro-

carbons dissolved in the liquid sulfur dioxide; and 2) the raffinate

(upper layer), consisting of sulfur dioxide dissolved in the remaining

hydrocarbons. The raffinate yields the refined oil and the extract

becomes a source of industrial solvents. The sulfuric acid process

functions chemically while the sulfur dioxide method is a physical

process, its action being that of solvent extraction. Other solvent

extraction processes are now in use: nitrobenzene, Chlorax, phenol,

furfural, and Duosol. Spray oils require further refinement with sul-

furic acid after the usual treatment given the lubricating oils. The

oil is treated with hot sulfuric acid which has the combined properties

of strong acid, drying agent, and oxidizing agent. Hence, the sul-

fonation process removes all but the most inert substances. The com-

pounds removed are: 1) unsaturated hydrocarbons (both straight chain

and aromatic); 2) oxygen compounds (e.g., phenols and naphthenic acids);

3) sulfur compounds (e.g., mercaptans, pentamethylene sulfides, and

thiophene); and 4) nitrogen compounds (e.g., quinoline). That part of

the oil not reacting with the sulfuric acid, the saturated hydrocarbons,

is known as the unsulfonated residue, or UR. Hence the UR of an oil is









in direct relationship to its degree of refinement (25).

The most important properties used for defining spray oils are

those which indicate "heaviness" or volatility, refinement, and hydro-

carbon composition. Viscosity (seconds Saybolt Universal = SSU) and

molecular weight are measures of the heaviness of oils but are valid

only for comparing oils of the same composition. Distillation temper-

atures are most directly related to volatility and may be used to com-

pare oils of varying hydrocarbon composition. Oil refinement is indi-

cated by the per cent unsulfonated residue as explained above and is

especially important in relation to plant safety. Hydrocarbon compo-

sition refers to the relative content of paraffinic and naphthenic com-

pounds, since both types are present in spray oils (9, 24, 25). Gener-

ally speaking, paraffinic oils contain approximately 65 to 75% paraf-

finic carbons and naphthenic oils contain about 45 to 55% naphthenic

carbons.


Historical Use of Spray Oil

The insecticidal efficiency of petroleum oil was recognized nearly

a century ago, as undiluted kerosene was applied directly to insect-

infested trees around 1870 (72). Kerosene, soap, and water mixtures

were recommended during the 1870's and the Riley-Hubbard formula for a

kerosene, whale-oil soap, and water emulsion was published in 1883 (72).

Hubbard (35) recognized kerosene as the most effective insecticide for

combating scale insects on citrus in Florida in 1885. The kerosene-

soap emulsion remained a standard insecticide for use on citrus both in

Florida and California for many years. In addition to kerosene, crudes

and distillates were also tried with varying degrees of success (72).









Others (103) introduced lubricating oils about 1911 and these

gradually came into wide use in controlling scale insects and white-

flies on citrus in Florida.

The interest in oil sprays declined somewhat during the years 1910

to 1920, especially in California, in favor of lime-sulfur spray and

HCN gas. However, after a few years, interest in oil sprays was

revived, but this time to lubricating-oil emulsions instead of the

older kerosenes, crudes, and distillates. This renewed interest was

due mainly to the alarming increase in damage caused by the San Jose

scale, Aspidiotus perniciosus Comstock, to deciduous fruit trees and

the development of resistance to HCN gas by the California red scale,

Aonidiella aurantii (Maskell), and the black scale, Saissetia oleae

(Bernard), (72).

The interest in oil emulsion sprays was greatly stimulated about

1925 by the publicity given to the formulae of Yothers (106) and

Burroughs (3) for boiled lubricating oil emulsions and cold engine oil

emulsions. These formulae, and the method of emulsification, were

essentially the same as those suggested by Hubbard (35) in the early

1880's, except that lubricating oil was specified instead of kerosene,

crude oil, and distillates.

Renewed interest in oil sprays stimulated research in all phases

of the subject--insecticidal, miticidal, and phytocidal. The main

problem with petroleum oil was that of phytotoxicity. Hence the bulk

of the research since the early 1920's has been concerned with the

phytotoxic properties of oils, and with the development, through re-

finement and other means, of oils less detrimental to plants. Con-

current with this, the insecticidal properties were studied in order to









maintain high insecticidal efficiency of oil while reducing its degree

of phytotoxicity.

Since the early work of Hubbard and Yothers in Florida, research

workers in many areas of the country, particularly in Florida

(Thompson), California (DeOng, Smith, Knight, Chamberlin, Ebeling,

Wedding, Riehl, and others), and New York (Pearce, Chapman, and Smith),

have expended considerable time and effort in spray oil research.


Insecticidal and Ovicidal Action of Petroleum Oil

DeOng et al. (19) attributed the insecticidal action of unrefined

petroleum oil to suffocation and toxic action, the latter due chiefly

to the action of unsaturated hydrocarbons and the former due to non-

volatility or film-permanence. They stated that the wax solubility of

oil determined to a great extent the insecticidal effectiveness of

lubricating oils against the California red scale. The oils dissolve

the waxy coating of the insect and penetrate to the spiracles, thus

halting the respiratory process. DeOng (18) had earlier found that

scales could expell the highly refined volatile oils, e.g., kerosene,

from the tracheal system, thus rendering these materials ineffective.

But any volatile oil containing a large amount of unsaturated hydro-

carbons seemed to pass throughout the body cavity, dissolving first the

fat bodies and finally even the entire cellular structure of the in-

terior part of the body. Non-volatile oils could not be expelled from

the spiracles by the insects.

Swingle and Snapp (81) cited reports that oil did not affect

respiration of insects, and also that it was not suffocation which

killed the insect but rather the gases given off by the oil after

entering the tracheal system. These views are in conflict with the









results obtained by other authors reporting on the subject.

Nelson (40) reported that kerosene penetrated throughout the tra-

cheal system and eventually into muscles and nerve ganglia. Woglum

(101) and Woglum and LaFollette (102) found that the residual oil film

killed scale crawlers through inhibition of settling and concluded that

this was an important means by which oil controlled California red

scale.

Smith (73) pointed out that in many instances the oil does not

reach the tracheal system of scale insects, in which case, "...if the

insect succumbs, death is apparently caused by a prolonged impairment

of physiological processes such as might be induced by the presence of

the oil film in the scale covering or in contact with the derm of the

insect's body."

Ebeling (22) corroborated the reports of Woglum (101) and Woglum

and LaFollette (102) concerning inhibition of settling of scale

crawlers and of Smith (73) as to the effect of oil in the scale cover-

ing. Ebeling (22) established that crawler settling is inhibited,

whitecap mortality is high where settling does occur, young stages are

more easily killed than adults, and tracheal penetration is the chief

cause of adult mortality but death can occur without it. In addition,

he found adult scales were much more vulnerable to oil treatments where

the margins of their armors were loosened from the substratum. The

scales that survived the treatment gave birth to a high percentage of

dead embryos and dead crawlers. Scales on the branches of the tree

were harder to control because of the absorptive nature of the rough

bark.









Oil is also an important ovicide. It has proved effective against

eggs of various insects and mites. Smith and Pearce (70) suggested

that the mode of ovicidal action of oil may be the prevention of ready

elimination of toxic metabolites, causing their accumulation in lethal

amounts. The respiratory rate of eggs of the oriental fruit moth,

Grapholitha molesta (Busck), was immediately reduced following oil

application. They demonstrated that oil must remain on the chorion for

at least 24 hours to be completely effective. Older eggs were less

susceptible than younger ones. Smith (71) summarized various theories

on the mode of ovicidal action of oils:

"The oil may prevent the normal exchange of gases through the
outer covering of the egg.

"The oil may harden the outer covering so as to prevent
hatching.

"The oil may interfere with the water balance.

"The oil may soften or dissolve the outer covering of the
egg, through interfering with the normal development of
the embryo.

"The oil may penetrate the egg and cause coagulation of
the protoplasm.

"The oil may penetrate the egg and interfere with enzyme
or hormone activity.

"The oil may come in contact with the emerging insect and
exert its toxic effect upon the delicate integument."

But he stated that the precise mechanism might vary with different

species or that several modes of action might operate simultaneously or

at different stages in the development of the embryo.

Ebeling (21) showed that the effectiveness of an oil spray against

citrus pests was related to the heaviness of the oil and the amount of

oil applied. Chapman et al. (5) also found that control of apple pests

was in proportion to the amount of oil applied. Pearce et al. (43)









concluded that structural composition and molecular weight of the oil

were the basic factors involved in efficiency in insect control.

The composition and heaviness of petroleum oil in relation to in-

secticidal and ovicidal efficiency has been studied by several investi-

gators (6, 15, 23, 42, 43, 44, 47, 48, 49, 55). Pearce et al. (43)

found that high paraffinicity and low content of aromatic structures

were related to kill of eggs of the fruit-tree leaf roller, Archips

argyrospilus (Walker). Chapman et al. (6) obtained similar results

with eggs of oriental fruit moth, codling moth, Carpocapsa pomonella

(L.), and eye-spotted bud moth, Spilonota ocellana (Denis and

SchiffermUller). Pearce and Chapman (44) further demonstrated the re-

lationship between paraffinicity and efficiency against eggs of

oriental fruit moth and European red mite, Panonychus ulmi (Koch), and

against cottony peach scale, Pulvinaria amygdali Cockerell. Efficiency

also increased with viscosity and molecular weight up to a point. The

critical value in molecular weight was 320. The maximum efficiency in

relation to viscosity was obtained at about 50 SSU, 70 SSU, and 90 SSU

for isoparaffinic, paraffinic, and naphthenic types, respectively.

Riehl and LaDue (47) found definite correlation of oil viscosity

and molecular weight to efficiency in control of California red scale

adults and citrus red mite eggs. They found paraffinic oils superior

to naphthenic oils and concluded that efficiency of spray oils against

citrus pests may be considerably improved by proper selection with

respect to structural character and molecular size. These conclusions

were strengthened by the work of Riehl and Carmen (48) and Riehl and

Jeppson (49). Insecticidal efficiency increased with molecular weight

in the range 220 to 360. Maximum efficiency for highly paraffinic









petroleum oils occurred at approximately 340 mol wt (49).

Fiori et al. (27) found an inverse relationship between volatility

of petroleum oils and ovicidal efficiency. Generally, oils fell into

three distinct groups: 1) ineffective oils, those volatilizing within

12 hours; 2) moderately effective oils, those volatilizing in 12 to 24

hours; and 3) highly effective oils, those with little or no volatili-

zation in 24 hours. Chapman et al. (9) considered volatility, as de-

termined by distillation, to be the most definitive and useful desig-

nation for a spray oil.

Thompson (84, 88), Thompson and Griffiths (86), and Thompson

et al. (89, 90) have reported on the effectiveness of oil in controll-

ing citrus insects in Florida. When timed properly to avoid injury to

the trees, oil generally has given satisfactory control of purple scale,

Lepidosaphes beckii (Newman), Florida red scale, and related forms, and

citrus red mite. The recommended rate for scale control was 1.3%.

Thompson (84) reported no difference between paraffinic and

naphthenic oils in controlling purple scale and Florida red scale when

applied at concentrations of 1.3 to 1.4% oil. However, at a concen-

tration of 1.0%, paraffinic oil was superior to naphthenic oil. He

found no correlation between scale control and increase in viscosity in

the range 72 to 110 SSU. Dean and Bailey (15) reported superiority of

paraffinic oils and correlation of oil heaviness to efficiency in con-

trolling Texas citrus mites, Eutetranychus banks (McGregor).

Cressman and Dawsey (11) found no relationship between kill of

camphor scale, Pseudaonidia duplex (Cockerell), and oil refinement in

a UR range of 67 to 94%.









Phytotoxicity of Petroleum Oil

Hubbard (35) reported serious defoliation of citrus plants sprayed

with kerosene emulsion. Almost every author reporting on oil sprays

since then has pointed out the phytotoxic hazards of spraying plants

with petroleum oils. Others (104) concluded that all oils apparently

interfered with the physiological processes of the citrus tree. He

concluded the oil film interfered with chlorophyll production and noted

adverse effects of low temperatures following application of oil sprays

and blotchingg" of fruit after an early-season application.

Gray and DeOng (29) showed a relationship between degree of re-

finement and phytotoxic effects of petroleum oils. They suggested the

sulfonation test as a useful guide in judging the safety of an oil.

DeOng et al. (19) described 2 distinct types of injury to citrus

foliage by petroleum oils. These were acute and chronic, the former

being related to light oils and the latter to heavy oils. They ob-

served defoliation, fruit spotting and dropping, and killing of twigs

and branches, and noted the apparent interference with transpiration

and respiration of the plant. Burroughs (4) reported severe leaf burn

and heavy leaf drop following summer application of oil sprays to apple

trees.

Penetration of oil into plants

DeOng et al. (19) cited Volck (97) as showing that penetration of

oil into the citrus leaf was most rapid on the abaxial surface, the

site of the stomatal openings. Knight et al. (36) reported both stoma-

tal and cuticular absorption of oil by citrus leaves, but penetration

was not uniform over the entire leaf. Certain focal points were pene-

trated and the oil spread peripherally from these. Extensive









translocation of the oil in the citrus plant was reported. However,

Rohrbaugh (60) studied the fate of the oil film on citrus leaves,

twigs, and fruit, and found no evidence of translocation or other move-

ment of oils from leaves into twigs or from small twigs into larger

twigs, except that oil may migrate short distances between the cells by

capillarity, and only in cases of heavy applications did it penetrate

to a depth of more than a few cells beneath the epidermis.

Oil-soaked areas appear on citrus leaves after spraying with oil.

This oil eventually migrates internally to an area along the midrib and

margins of the leaf, resulting in dark discoloration of leaf tissue in

that area (24).

Ginsburg (28) concluded oil penetration into leaves of apple,

peach, and tomato plants was related inversely to viscosity. McMillan

and Riedhart (37) reported pure hydrocarbons, having a distillation

range of 419 to 487 F, penetrated citrus leaves more rapidly than did

those of a higher boiling range. They concluded that little or no

cuticular penetration occurred. Young (108) concluded that petroleum

oil penetration was aided by external forces such as those caused by

gravitation, capillarity, and bending of tissues by wind. Tucker (94)

found oil penetration into apricot leaves related to the opening and

closing of stomata.

Dallyn and Sweet (12) stated that highly toxic herbicidal oils

entered the plant indiscriminately from the point of contact and in-

ternal spread was negligible, while relatively nontoxic oils entered

largely through the stomata and spread throughout the plant to a con-

siderable extent. Van Overbeek and Blondeau (96) stated that phyto-

toxic oils could penetrate only after cells were injured; this was









accomplished by breaking down of the plasma membrane of the cell by the

process of solubilization. However, they pointed out that solubiliza-

tion would not occur with molecules as large as those of foliage spray

oils. Other workers (10, 13, 39) have studied the penetration and

phytotoxic action of herbicidal oils. In general, the herbicidal

activity is related inversely to the heaviness of oil and directly to

the aromatic hydrocarbon content. However, the petroleum spray oils

are considerably higher-boiling and more highly-refined than the

herbicidal oils. The light herbicidal oils are considerably more pene-

trating than the foliage spray oils.

Effects of oil on the physiological processes of plants

Application of oil sprays has resulted in reduced transpiration

rates of citrus trees (36, 38, 56, 58) and of deciduous fruit trees

(109). Merrin (38) reported a 25 to 30% decrease on citrus in Florida,

with very little difference between first, second, or third-flush

growth. Knight et al. (36) reported reduction of transpiration of

citrus by 50-SSU and 106-SSU oils but recovery was faster with the

light oil.

Riehl et al. (56) determined the effect of a medium-grade

California oil on transpiration of several varieties of citrus in the

laboratory. On the first day after the application of 1.75% oil in

aqueous mixture, transpiration of the oil-sprayed plants was reduced to

one-third that of untreated plants. The reduction seemed to be due to

physical interference by the oil on or in the leaf tissue and recovery

was apparently related to dissipation of the oil from the leaves.

Transpiration was restored to original levels in the treated plants in

3 to 5 weeks after treatment. Riehl and Wedding (58) studied the









relation of molecular structure of oil to effect on transpiration of

lemon and lime plants. A 306-mol wt naphthenic oil and a 308-mol wt

paraffinic oil both reduced transpiration more than 50%, but recovery

was faster in plants sprayed with the naphthenic oil than in those re-

ceiving the paraffinic oil.

The effect of petroleum oils on photosynthesis and respiration of

various plants has been studied. Knight et al. (36) reported inhi-

bition of photosynthesis in citrus leaves by light (50 SSU) and heavy

(106 SSU) oils, but recovery was faster in the plants treated with the

light oil. The same workers observed a significant stimulation of

respiration by the same oils. Other workers have reported increases in

respiration of plants treated with oil sprays. According to Green and

Johnson (30) respiration of bean leaves increased following application

of low refined oils of less than 84 UR, but a reduction in respiration

followed applications of oils of more than 84% unsulfonated residue.

Green (31), working with oils of both high and low refinement on bean

plants, apple leaves and twigs, and barley seedlings, found a general

increase in respiration, but the effect of the low UR oils was more

than triple that of the highly refined oils. McMillan and Riedhart

(37) observed an increase in oxygen uptake by leaves of 'Valencia'

sweet orange, Citrus sinensis, following application of pure hydro-

carbons of a distillation range of 419 to 487 F, while those treated

with pure hydrocarbons and spray oil of a distillation range of 552 F

and higher showed a definite decrease in respiration.

Schroeder (62) reported that inhibition of photosynthesis in apple

foliage was directly related to viscosity and rate of application of

the oil. Oberle et al. (41) obtained similar results with heavier









dormant-type oils. Riedhart (46) reported inhibition of photosynthesis

of banana leaves by a 75-SSU paraffinic oil.

Wedding et al. (98) reported a depression of both photosynthesis

and respiration in sweet orange and lemon plants sprayed with petroleum

oil emulsions in amounts approximating the deposit level obtained in

field applications in California. Recovery of photosynthesis occurred

sooner in lemon plants than in orange plants. In no case did they get

an increase in respiration as reported by Knight et al. (36), Green and

Johnson (30), and Green (31). They attributed at least part of the re-

duction in soluble solids of citrus fruits accompanying oil spray

applications to inhibition of photosynthesis.

Riehl and Wedding (57) compared naphthenic and paraffinic oils of

different molecular weights as to their effect on photosynthesis in

citrus leaves. No consistent inhibition was observed with insecti-

cidally efficient deposits of 150 Lg/cm2, but deposits of 300 to 600

Lg/cm2 greatly inhibited photosynthesis. The principal effect occurred

in oil-soaked tissue. During the first week following application, 50

to 60% reduction was detected. A tetrazolium test showed that cells in

the oil-soaked tissue were not killed. They concluded that inhibition

of photosynthesis was the result of interference with gaseous exchange

caused by the presence of the oil, and that dissipation of the oil was

accompanied by recovery of photosynthesis. Recovery by plants sprayed

with naphthenic oils was faster than by plants treated with paraffinic

oils. Results of a similar experiment by the same authors (59) showed

that the difference in rate of recovery associated with difference in

paraffinicity was greater for oils of comparable viscosity than for

those of comparable molecular weight.









Injurious effects of oil sprays on citrus

Various types of injury resulting from oil applications to citrus

have been reported (2, 16, 19, 22, 34, 35, 45, 51, 52, 53, 61, 66, 67,

83, 84, 89, 91, 92, 93, 99, 104, 105, 107, 110). Types of adverse

effects reported were leaf and fruit drop, fruit burn, fruit blemishes,

rough textured fruit, reduced soluble solids and acid, increased granu-

lation, delayed degreening, crop reduction, upset of normal blossoming,

increased water rot and decay of fruit in wet weather, dead wood, and

increased susceptibility to freeze damage. According to Rohrbaugh (61),

some writers have claimed various beneficial effects such as larger

fruit, larger leaves, and better color, but most of these claims, he

felt, were without foundation.

Others and McBride (107) first reported a decrease in solids in

fruit from oil-sprayed trees in Florida in 1929. Thompson and Sites

(83), using oils of 72 and 100 SSU, concluded that oil sprays applied

after 1 August either delayed or prevented the formation of maximum

soluble solids, especially during the early part of the season.

Thompson and Deszyck (91) observed a greater effect on fruit quality

with 1.3% oil than with 0.7% oil in combination with parathion.

Sinclair et al. (66) reported that applications of light-medium grade

oils to citrus in California, at concentrations of 0.25 to 1.75%, caused

reduction in the total soluble solids and that timing of application

was relatively unimportant. However, Riehl et al. (54) found a defi-

nite correlation between timing of oil sprays and fruit quality in

California. Applications during the period November to June had the

most adverse effect on solids.









Numerous workers (66, 68, 80, 82, 89, 100) reported retardation of

the degreening rate of oil-sprayed citrus fruit. But the author found

no report of studies having been made of the relation of oil properties

to effect on fruit color, except that an 80-SSU oil retarded color

development less than did a 95-SSU oil (100).

A grade-lowering fruit blemish, referred to as "oil blotch," is

associated with oil sprays applied in Florida when the fruit is between

0.75 and 1.50 inches in diameter. Thompson (85) described the con-

dition as being round in shape, varying from light to dark brown in

color, and of a superficial nature; but it was a definite grade-lower-

ing blemish.

Thompson et al. (87) reported more than twice the amount of dead

wood in oil-sprayed sweet orange trees than in either parathion-sprayed

or unsprayed trees. Oil-sprayed tangerine trees dropped 10 times as

many leaves following a February application as did those receiving

parathion sprays. Thompson (92) found the greatest leaf drop to occur

when oil applications were made just prior to, or during, the time of

normal shedding of old or weak leaves and concluded that while oil

sprays are the most common cause of leaf drop, tree condition apparent-

ly is a factor where excessive drop occurs. Thompson (84) reported no

difference in leaf drop or shock to the tree with oils of 72 to 100 SSU

viscosity or oils of low and high refinement. However, Ebeling (24)

reported heavy leaf drop following application of 2.0% heavy oil of 86

UR, and decreasing drop with oils of 95 and 100 UR, respectively. He

stated that leaf drop constitutes a rather accurate index of the phy-

totoxicity of an oil.









Ziegler (110) noted 3 definite physiological responses of

'Valencia' sweet orange trees in Florida following applications on 12

May of an oil of 70 SSU viscosity and 83 UR at 1.66% concentration.

These were: 1) size of immature fruit was retarded, except where the

reduction of the crop was approximately proportional to reduction in

leaf area; 2) the number of fruit borne in the succeeding crop was re-

duced, and 3) the subsequent flush of growth was accelerated. He con-

cluded that the insecticidal and phytocidal properties of mineral oils

were closely correlated and applications of these must be timed to

allow maximum deposit without detrimental plant reaction and minimum

deposit for thorough pest control.

California workers (76, 77, 78, 79) reported successful use of

2,4-dichlorophenoxyacetic acid and 2,4,5-trichlorophenoxyacetic acid as

spray oil amendments to counteract some of the adverse effect of oil.

Addition of 4 or 8 ppm 2,4-D to the oil spray mixture increased yield,

reduced both leaf and fruit drop, and had less effect on soluble solids

in grapefruit than oil alone; the 2,4-D had no apparent adverse effect

on trees other than some curling and distortion of young leaves.


Specifications for Plant Spray Oils

Five classes or grades of foliage spray oils are recommended for

citrus in California (24). These are based on the work of Gray and

DeOng (29), DeOng (18), DeOng et al. (19), and of Smith (72). Accord-

ing to Ebeling (25), distillation range and per cent unsulfonated

residue are the most valuable criteria by which summer oils can be

standardized. The 5 recognized grades and identifying properties are

given in Table 1. Ebeling (25) pointed out that these standards do

not necessarily hold for oils applied to citrus in other states. He















Table 1. Specifications for California spray oilsa


Temperature, F, for Per cent
Grade distillation of: distilled Minimum unsul-
5% 50% 90% at 636 F fonated residue


Light 555 617 675 66.2 90

Light-medium 571 628 703 55.4 92

Medium 582 643 715 43.2 92

Heavy-medium 585 656 728 39.1 92

Heavy 612 671 727 18.0 94

aAfter Ebeling (25), p. 58, in part.









stated, "It is known, for example, that oils as low as 80 UR, which

would be excessively injurious to citrus trees in California, can be

safely used in Texas, Florida, and Mexico. It appears that in more

humid regions a citrus tree is not so adversely affected by oil as in

California, and that oils of a lower degree of refinement can be safely

used."

Chapman and Pearce (7) first published standardized specifications

for dormant spray oils for New York in 1947. They recognized 2 types,

"regular" and "superior"; both were 100-SSU oils but of different re-

finement. In 1959, Chapman (8) presented specifications for a "70-

second superior oil" in addition to the 1947 "100-second superior oil."

Chapman et al. (9) added to these a "60-second superior oil," dropping

the 100-second oil from the recommendations. Specifications for these

are presented in Table 2. Some oils currently used in Florida on cit-

rus are patterned after Chapman's "70-second superior oil."

Dean and Bailey (14) published tentative specifications for oils

for use on Texas grapefruit in 1961. They specified unsulfonated

residue, 92% minimum; distillation (760 mm Hg), 50% at 716 F with a 10

to 90% range of 85 F; and a neutralization number of 0.03 minimum.

No grade standards have been established for oils used on citrus

in Florida. The oils currently in use vary as follows: viscosity, 60

to 110 SSU; 50% distillation point, 651 to 788 F; 10 to 90% distil-

lation range, 52 to 261 F; average molecular weight, 300 to 350; and

refinement, 80 to 96 UR (compiled from specification data for various

commercial oils).








Table 2. Specifications for oils applied to fruit and shade trees in New Yorka


100-second 70-second 60-second
superior oil superior oil superior oil


Saybolt Universal 90-120 66-74 56-62
viscosity at 100 F

Gravity, API 31 33 34
(minimum)

Unsulfonated residue 90 92 92
(minimum), %

Pour point, F 30 20 20
(maximum)

Distillation temperature, F, (a relatively narrow
at 760 mm Hg distillate portion of
petroleum)

50% point 670 + 10 645 + 8

10%-90% range 90 75
(maximum)


aCompiled from Chapman and Pearce (7), Chapman (8), and Chapman et al. (9).














MATERIALS AND METHODS


Oil Specifications

The oils used in these studies were obtained from the following

major oil companies: Humble Oil and Refining Company; Gulf Oil Corpora-

tion; Sun Oil Company; Shell Oil Company; Texaco, Incorporated; and the

American Oil Company. Of these, Humble was by far the largest con-

tributor, providing 23 narrow-distilling, experimental fractions and 10

commercial oils. The other companies contributed both experimental and

commercial products. Specifications on important properties of these

oils appear in Table 3. The 3 narrow-boiling series provided by
2
Humble were comprised of paraffinic, naphthenic, and "reformed"2 frac-

tions. These oils provided wide ranges of molecular weight, viscosity,

and distillation temperature in which to study insecticidal, ovicidal,

and phytocidal properties. The commercial-type oils included most of

the oils presently used on Florida citrus plus several experimental

materials. Specification data were provided by the oil companies; the

methods by which the data were obtained are indicated by footnotes to

Table 3.



1"Boiling" is used synonomously with "distilling" throughout this
paper and refers to the 10 to 90% distillation range, unless otherwise
specified. "Narrow-boiling" is a relative term applying to the first
23 oils listed in Table 3; the remaining oils are commercial products
of wider distillation ranges.

2The word "reformed" in this paper refers to spray oils which have
received special treatment to alter the component hydrocarbons; the
reformed oils are predominantly paraffinic.









Table 3. Specifications for various properties of petroleum oils used in these studies


d Temperature, F,
Oil Chemical composition for distillation
_________ Avg Viscosity, (760 mm Hg) of: 10-90%
mol SSU at UR, API distillation
No.a Name wt 100 Fc % 7A N P gravitye 10% 50% 90% range, F
Name Awt gaiy 107.c 507% 907. range, *F


P-250
P-265
P-285
P-305
P-320

P-365
P-435
P-520
R-250
R-265

R-285
R-295
R-305
R-320
R-365

N-250
N-265
N-285
N-305
N-320


252
265
285
305
322

365
433
520
250
265

285
295
305
320
365

250
265
285
305
320


41.0
45.0
50.0
59.8
71.0

99.0
199.1
396.0
42.8
46.6

52.8
55.9
59.3
66.5
100.2

47.6
51.4
57.7
68.3
79.7


95.6
95.8
95.8
91.8
93.4

94.6
94.0
93.0
86.4
91.4

94.0
94.4
91.0
94.0
95.0

96.4
96.2
96.6
96.6
97.2


2.1
0.0
2.8
4.5
4.6

3.1
5.1
4.4
2.3
4.0

0.4
0.3
2.3
2.4
2.7

1.6
1.0
0.0
1.0
1.0


23.9
29.0
25.2
18.0
22.4

25.4
29.9
26.1
39.2
41.0

34.6
31.7
28.7
27.6
31.3

52.9
51.4
47.5
49.0
48.0


74.0
71.0
72.0
77.5
73.0

71.5
65.0
69.5
58.5
55.0

65.0
68.0
69.0
70.0
66.0

45.5
47.5
52.5
50.0
51.0


40.9
39.8
37.9
36.3
35.0

42.2
31.6
30.8
34.4
35.6

36.0
36.1
36.4
35.9
33.6

32.8
32.6
33.1
31.7
31.3


579
609
639
674
698

743
812
887
572
608

649
666
673
701
751

585
607
629
661
675


581
614
646
696
715

752
831
911
597
615

656
675
700
716
766

593
611
635
665
689


591
622
652
701
734

779
856
944
614
624

661
680
706
721
784

602
620
656
678
703








Table 3--Continued


composition Temperature, F,
Oil Chemical composition for distillation
_________ Avg Viscosity, API (760 mm Hg) of: 10-907%
mol SSU at UR, distillation
No. a Name wt 100 F % OWA *N X P gravity 10% 50% 90% range, F


N-365
N-395
N-440
P-74
P-87

P-96
N-80
N-84
N-95
BR- 1

BR-2
BR-3
R-60
T- I
T-2

T-3
G-1
G-2
G-3
G-4


365
395
440
317
317

330
294
294
305
348

297
330
300



342
320
347
310
280


131.6
202.0
402.0
84.7
79.6

74.3
84.5
83.9
74.2
92.5

71.7
112.1
57.6
70.5
100.0

72.0
75.0
105.0
76.6
76.9


95.2
93.8
91.8
74.0
87.0

95.6
79.4
84.0
95.2
94.0

85.0
85.0
96.1
87.0
78.0

92.0
93.0
95.0
88.0
93.5


0.5
1.7
0.5
13.0
10.0

3.0
14.0
12.6
2.0
2.4

13.6
15.1
3.6



5.0
4.0
4.0
12.0
4.0


50.0
47.8
51.5
25.0
30.0

27.0
47.0
47.4
51.0
27.6

26.4
26.9
23.9



36.8
24.0
24.0
24.0
46.0


49.5
50.5
48.0
62.0
60.0

70.0
39.0
40.0
47.0
70.0

60.0
58.0
72.5



58.2
72.0
72.0
64.0
50.0


29.8
28.1
25.9
30.2
31.4

35.0
25.4
25.9
30.5
33.4

29.6
27.5
36.3
30.0
29.2

30.0
33.9
33.3
31.0
29.0


734
764
801
687
676

681
622
632
623
701

637
693
652
639
684


656
733
670
602


738
767
808
721
720

732
678
681
680
751

688
737
681
666
788


684
763
717
646


750
777
816
763
761

779
732
732
732
826

774
792
707
718
945


726
813
750
724


16
13
15
76
85

98
110
100
109
125

137
94
55
79
261


71
80
80
122








Table 3--Continued


d Temperature, F,
Oil Chemical composition for distillation
Avg Viscosity, AI(760 mm Hg) of: 10-90%
N mol SSU at UR, API 7 distillation
No.a Nameb wt 100 Fc % %CA 7CN 'CP gravity 10% 50% 90% range, 0F


46 G-5 384 103.0 93.0 4.0 44.0 52.0 28.5 643 700 756 113
47 S-1 61.8 91.0 16.2 37.5 613 671 711 98
48 S-2 310 69.6 95.0 4.0 32.0 64.0 33.9 644 688 696 52
49 S-3 86.5 94.0 32.6 666 695 723 57
50 A-1 85-98 89.0 30.0 -

51 NG-1 310 76.5 88+ 12.0 24.0 64.0 671 717 750 79
52 NG-2 312 56.0 92+ 12.0 22.0 66.0 628 651 690 62
53 SL-1 275 58.8 94.8 31.1 582 640 692 110
54 SL-2 275 57.6 93.6 30.7 582 630 688 106
55 P-60 60.0 -

a
Oil numbers were drawn from a larger table of specifications.
P = paraffinic; R = reformed; N = naphthenic; all other letters are code numbers for convenient reference.

Converted from Kinematic to Saybolt Universal, in accordance with ASTM D-446, or similar methods.

dCA = aromatic carbons; CN = naphthenic carbons; Cp = paraffinic carbons.

eBy ASTM D-287, or similar methods.

fConverted from 10 mm Hg in accordance with Note 2 of ASTM D-1160, or similar methods.









Preparation of Oils

Measurement of oil deposits on sprayed fruit and plant surfaces

required the addition of an indicator dye to the base oils. An oil-

soluble, water-insoluble red dye, DuPont Oil Red A (17), was added to

each oil at approximately 2.5 g/liter. Mixtures of oil and dye were

heated in a water bath to about 140 F and then were shaken continuously

for several hours to obtain maximum dye concentration in the oil.

Finally, the solutions were drawn through a medium-porosity fritted-

glass filter to remove any undissolved dye particles. These stock

solutions of dyed oils were used in all toxicity and phytotoxicity

studies.

The oils were formulated as emulsifiable oils in the laboratory as

needed. An oil-soluble, non-ionic emulsifier, Experimental emulsifier

9D-207 (Rohm and Haas Co., Philadelphia, Pa.), consisting of alkyl aryl

polyether alcohol plus a non-ionic solubilizer, was used. Extensive

tests under the conditions of this work showed that 0.4% (v/v) 9D-207

gave adequate and similar emulsification for all the oils tested except

the 2 heaviest fractions of the narrow-boiling paraffinic and naphthenic

series. P-435 and P-520 required 0.6% and 0.8% respectively, and N-395

and N-440 required 0.5% and 0.6%, respectively. The emulsifier was

measured volumetrically with a calibrated dropping-pipette and added to

each oil. The 2 materials were thoroughly and uniformly mixed by

stirring vigorously for 3 to 5 min, depending on the volume of oil.


Application of Oils in Laboratory Studies

The oils were applied as dilute aqueous sprays with a laboratory

air-blast sprayer (65) similar in performance to the commercial air-

blast sprayers widely used by Florida citrus growers. The idea behind









this method of application was to duplicate the type of deposits ob-

tained in field spraying. The spray unit, shown in Figure 1, consisted

of the following main components:

A. Blower, high velocity centrifugal; manufactured by Ideal
Industries, Inc., Sycamore, Ill.; 1.33-hp universal motor,
11,350 rpm; "egg-crate" air straightener vanes attached
at outlet; discharge velocity 6,000 fpm.

B. Electric motor for pump; 0.75-hp; 1,725 rpm.

C. Pump, manufactured by Hypro Engineering, Inc., Minneapolis,
Minn., Model 6500; nylon roller impeller, positive displace-
ment; operated at 500 rpm.

D. Spray tank, stainless steel; tapered botton, center drain;
4,000-ml capacity.

E. Pressure regulator and gauge with by-pass to the tank.

F. Sprayer nozzle of "whirljet" type as used on "Speed
Sprayer," but with 3/64-inch orifice; stainless steel;
centered 3.25 inches in front of blower outlet; mounted
on 1/8-inch pipe to minimize volume of stagnant liquid
in the line beyond the shut-off valve.

G. Deflector vanes for shaping the air blast to a vertical
column of uniform velocity and spray impingement above
the turntable.

H. Operating lever with air baffle that extends over blower
outlet. Lever is linked to the quick shut-off valve to
start and stop air and liquid simultaneously.

I. Turntable centered 7 feet 9 inches from the sprayer nozzle;
operated at 15 rpm.

Emulsification of the oils was obtained by circulating the desired

amounts of emulsifiable oil and water through the spray unit 4 times,

or 32 sec for each 1,000 ml emulsion. The shearing action of the pump

and pressure regulator and the high velocity stream of liquid returning

to the tank produced a uniform emulsion.

The liquid was atomized through the nozzle at 70 psi and dis-

charged into a 6,000 fpm-air blast. At the start of each spraying in-

terval, the quick shut-off valve was opened for about 3 sec to clear












































Figure 1. Laboratory air-blast sprayer. A, high velocity blower; B,
motor; C, pump; D, spray tank; E, pressure regulator; F, nozzle; G,
deflector vanes; H, operating lever; I, turntable.


w r -
G't -A A









the line of stagnant liquid. A stop watch was used for timing the

spraying interval. As the timer-hand approached the starting time, the

blower was turned on to build up speed. When the timer-hand reached

the starting point, the operating lever was raised, thereby opening the

valve and injecting the spray into the air blast released simultaneous-

ly by a baffle plate on the end of the lever. At the end of the spray-

ing interval, both liquid and air were stopped instantly by reverse

action of the lever.

Uniform coverage was obtained and the spray was applied just to

the point of runoff by spraying fruit for 3 revolutions, or 12.3 sec,

and potted plants for 4 revolutions, or 16.4 sec. Plants were sprayed

individually by placing the container directly in the center of the

turntable. Individual fruit were placed stem-end up on a tripod at the

center of the turntable, in which position the sides of the fruit re-

ceived a uniform coverage of spray droplets (Figure 2). No attempt was

made to spray the ends of the fruit because both mortality counts and

oil deposit determinations were made only on the equatorial area of the

fruit. Generally, 8 fruit were sprayed from each 4,000-ml tank of

spray. Five infested fruit served as replicates for each treatment,

and 3 fruit, occupying positions 1, 4, and 7 in the spraying sequence,

were used for deposit determinations. Two shallow grooves were cut

around each deposit fruit before spraying to define the equatorial area

on which the deposit was to be measured.

Oil deposits obtained on fruit surfaces with the laboratory

sprayer were in direct linear relationship to the oil concentration in

the spray. The coefficient for regression of deposit (|Ig/cm2) on con-

centration (as per cent oil in the spray) was 0.6732 x 100 with a 95%























































Figure 2. Spray coverage obtained on fruit with the laboratory air-
blast sprayer. A, fruit sprayed with oil at 1.0% concentration
containing fluorescent dye to show the distribution of the oil; B,
unsprayed fruit. Photographed under ultra-violet light. The
rectangular area on fruit "A" was left unsprayed to show the con-
trast between sprayed and unsprayed surface.









confidence interval for slope of 0.6237 to 0.7227. This was computed

from data for 8 oils of 3 types applied on 4 different days. Regres-

sions for the individual oils were very close to the 8-oil average,

with slopes within the range 0.64 to 0.72. One per cent oil emulsion

usually deposited 66 to 76 pg/cm2 on the equatorial area of fruit.

Similar deposit levels were obtained on plants.


Oil Deposit Determination

Oil deposits obtained on sprayed fruit and leaf surfaces were

measured spectrophotometrically by the method of Riehl et al. (50),

with modifications. The dyed oil was removed from the sprayed surface

by solvent-stripping with dioxane (1,4-diethylene dioxide). The dye

content of the strip solution was determined and used to calculate the

total amount of oil recovered.

A Beckman Model DB spectrophotometer, with a 40-mm rectangular cell,

was used. Readings were taken at 524 mL, the wavelength of maximum

absorbance for Oil Red A in dioxane. A series of standards of known

concentrations of the dye in dioxane was prepared and used to determine

the regression of dye concentration on per cent absorbance. The re-

gression coefficient (0.3093) was subsequently used to calculate the

dye content of solutions of unknown dye concentration.

The dye content of each oil was determined by weighing triplicate

samples (about 15 to 20 mg) to the nearest 0.1 mg on an analytical

balance, diluting each sample with dioxane to 25 or 50 ml (depending on

the weight and relative dye concentration of the sample), and reading

the per cent absorbance in the spectrophotometer. The per cent dye in

each oil sample was calculated by the following equation:










per cent dye = Total 4g dye x 100 = (A)(b)(vol) x 100
Total Lg oil Total ig oil

where A = spectrophotometer reading in per cent absorbance x 10
b = regression coefficient, 0.3093
vol = volume in ml to which weighed oil sample was diluted
Total |ig oil = mg oil x 1,000.

The oil deposit on fruit was measured only on an equatorial band

of 1.0 to 1.5 inches on immature oranges and 2.0 to 2.5 inches on im-

mature grapefruit. This area was defined by the shallow grooves near

and around each end of the fruit, as described earlier. The sprayed

fruit was held with its polar axis horizontal over a 6-inch glass fun-

nel for stripping. The fruit was slowly rotated on axis and a jet of

dioxane from a 250-ml polyethylene squeeze-bottle was directed at the

equatorial area. The flow of solvent followed the curvature of the

fruit and did not run into the grooves along the margins. The strip

solution was collected in a graduated cylinder for measurement. From

10 to 15 ml of solvent were sufficient for removal of the oil deposit

from immature Valencia oranges and 20 to 30 ml were adequate for near-

ly-mature grapefruit. The oil deposit was measured on 3 fruit for each

tank of spray or treatment. The rind was removed from the equatorial

bank of each fruit and traced on paper; the area was measured with a

planimeter. The oil deposit was calculated as follows:


Pg oil/cm2 = (A)(b)(vol)
(cm2)(D)

where A = spectrophotometer reading of the strip solution in
per cent absorbance x 10
b = regression coefficient, 0.3093
vol = volume in ml of strip solution
cm2 = surface area in cm2 from which the deposit was
stripped
D = per cent dye in the oil.









Oil deposits on leaves of sprayed potted plants were determined in

the same manner as described above for fruit. Either 2 leaves selected

at random from each of 5 treated plants or 10 leaves from a single

plant constituted a deposit sample. Each leaf was carefully removed

from the plant with forceps and scissors, and held over the funnel for

stripping. Approximately 5 ml of solvent were sufficient for washing

the oil from both sides of the leaf. The leaves were traced on paper

and measured with a planimeter. The area was doubled to account for

both leaf surfaces.


Insecticidal and Ovicidal Efficiency Studies

Florida red scale studies

The insecticidal efficiency of the oils was studied using adult

female Florida red scale as the test insect. A natural infestation of

this species on English ivy, Hedera sp., was the source of test materi-

al. Crawlers from these scales were used to infest nearly-mature

grapefruit in the laboratory. These scales were allowed to grow to the

early third stage at which time treatments were applied to the infested

grapefruit.

Infestation.--Laboratory infestations were obtained as follows

(Figure 3): ivy leaves heavily infested with crawler-producing red

scale were picked, brought into the laboratory, and cut into small sec-

tions, each section bearing several female scales. Five to eight of

these leaf sections were stapled.between 2 strips of cheesecloth

measuring 1.5 x 14 inches. Nearly-mature grapefruit were harvested,

brought to the laboratory, washed, and then placed stem-end down on

2.5-inch diameter juice cans filled with wet vermiculite, where they

remained throughout the infestation period. The prepared strips were






















































Figure 3. Method of infesting grapefruit with Florida red scale for
laboratory studies. A, ivy leaves with natural infestation of
crawler-producing female scales; B, cheesecloth strip with infested
leaf sections; C, strip of leaf sections wrapped firmly in position
around the equator of a grapefruit to allow crawlers to transfer; D,
typical infestation obtained by this method, at time of treatment
application (4.5 weeks after infestation).








wrapped firmly around the equatorial bands of the grapefruit with the

infested side of the leaf sections adjacent to the fruit surface. As

the leaf sections began to dry out, the scale crawlers migrated to the

surface of the grapefruit and settled in the equatorial area. The

fruit were checked periodically and when 200 to 300 crawlers had

transferred to the fruit, the strip of leaf sections was removed and

placed on another fruit. This period of infestation varied from under

24 hours up to 48 hours. The 48-hour limit was imposed to maintain a

maximum 2-day spread in age of the insects, since age has been found to

affect the response of scale insects to insecticidal treatments (22).

This level of infestation resulted in an average of about 100 third-

stage females per fruit at the time of treatment.

As the fruit became infested, they were transferred to a 24 x 24 x

2-inch wooden tray in an enclosed chamber for holding. The tray con-

tained a 1.5-inch layer of wet vermiculite overlain with double-thick-

ness cheesecloth (Figure 4).

Holding infested fruit.--It was necessary to hold large numbers of

detached grapefruit for 51 days in the laboratory. Attempts to hold

fruit in the absence of a water supply failed due to dehydration and

shriveling of the rind. This was alleviated by holding the fruit stem-

end down in moist vermiculite. By this method,dehydration was prevented

and approximately 90% of the fruit remained turgid throughout the hold-

ing period. Another serious problem was that of a stem-end rot of the

fruit. This condition was alleviated by dipping the stem-end of each

fruit in a 5% thiourea solution immediately after harvesting and weekly

thereafter up to about 4 weeks. The number of fruit lost due to the

rot was reduced to less than 10%. These fruit were discarded as
























































Figure 4. Scale-infested grapefruit on moist vermiculite in holding
tray.








detected and were never included. in the treatments. Where the rot set

in after treatment, its advancement was observed and if the affected

area extended into the scale-infested equatorial area before the sched-

uled time for mortality counts, the scales were counted early to avoid

loss of a treatment replication. These early counts were within 4 to 7

days of the scheduled mortality counts and the results did not differ

markedly from the other replicates of the same treatment.

The infested grapefruit were held in a chamber made of 2 x 4-inch

wood framing, enclosed on the sides with translucent polyethylene

sheeting, but open at the top and bottom for ventilation (Figure 5).

The size of the chamber measured 8.5 x 2 x 7 feet in width, depth, and

height, respectively. Six shelves, spaced 12 inches apart, vertically,

starting 18 inches above floor-level, accommodated 24 trays. Each tray

held a maximum of 36 medium-size grapefruit, with adequate clearance

between fruit. Conditions inside the chamber were maintained at 78 +

4 F and 70% + 5% relative humidity. Lighting, in alternating 12-hour

light and dark periods, in phase with the diurnal cycle, was provided by

six 48-inch, 40-watt "daylight' fluorescent bulbs hanging vertically on a

wall immediately behind the chamber, and overhead room lights of the

same type in front of the chamber. Diffusion of the light by the

translucent polyethylene sheeting resulted in fairly uniform distribu-

tion of the light inside the chamber.

Scale development, treatment, and mortality counts.--Treatments

were applied when the female scales reached the early third stage of

development. Under the conditions of this work, the insects required

approximately 4.5 weeks to reach this stage. Treatments were scheduled

32 to 33 days from the date of infestation and mortality counts were





















































Figure 5. Holding facilities for infested fruit in laboratory studies.
A, chamber for holding trays of scale-infested grapefruit; B, racks
supporting immature oranges infested with citrus red mite eggs.









made 18 days after treatment. The scales killed by the oil were easily

identified by the brown discoloration of the body in contrast to the

bright lemon-yellow color of live, healthy scales. Mortality was de-

termined by turning the scale armor and inspecting the condition of the

insect's body under 3X magnification. Only the scales in an equatorial

band of 2.0 to 2.5 inches were considered.

Testing the oils.--The testing of the oils against Florida red

scale included dosage-mortality tests for selected oils of the 3 nar-

row-boiling series and screening of the commercial-type oils at 2

levels of application.

Dosage-mortality tests were run on 6 selected oils of the

naphthenic and paraffinic series and 5 of the reformed series. Each

oil was applied at 8 concentrations, each replicated on 3 scale-infested

fruit. Therefore each point on the dosage-mortality curves represents

the response of approximately 300 individuals. In these tests, all

dosage levels for the oils in a given series were applied on the same

day.

The dosage-mortality data were submitted to the University of

Florida Computing Center for analysis. Probit regression lines were

fitted according to the methods of Finney (26), giving the maximum like-

lihood solution with adjustment for natural mortality. The input data

were oil deposit (4g/cm2), total scales, and the number killed for each

deposit level. The computer print-out provided regression coefficients

and both LD50 and LD95 values with their 95% confidence intervals.

The commercial oils were compared at 0.5% and 1.25% oil concentra-

tion in randomized block experiments with 5 replicates for each treat-

ment. Due to the large number of oils tested and differences in age of









the insects from group to group, it was necessary to apply the treat-

ments over a period of 5 days. The data were corrected for natural

mortality by use of Abbott's (1) formula to equate for difference in

time of application. Natural mortality among the check groups varied

only from 2.3 to 6.5%. The results were expressed as corrected per

cent kill since the number of scales varied from fruit to fruit. Since

percentage data tend to be binomial in distribution (74), the corrected

per cent kill data were transformed by the arcsin transformation in

order that the assumptions of normality, additivity, and homogeneous

variance in the analysis of variance could be met. Analysis of vari-

ance was run on the data and the significant differences between means

were determined by the Duncan Multiple Range Test (20).

Citrus red mite studies

The ovicidal properties of the oils were studied using eggs of

citrus red mite. Infestations of eggs were obtained on immature

'Valencia' oranges in the following manner. One day prior to use,

the fruit were harvested and washed, and the ends of each were coated

with paraffin to confine the oviposition activity of the mites to an

equatorial band of 1.0 to 1.5 inches, and to provide mite-free areas

for handling the fruit. Thirty to forty adult female mites were hand-

transferred to each fruit from plants growing in a greenhouse. After a

2-day oviposition period, the fruit were inspected under 15X magnifica-

tion and approximately 100 eggs were marked for post-treatment identi-

fication by encircling each with India ink. The infested fruit were

held before and after treatment under controlled conditions of 78 + 4 F,

65% + 10% relative humidity, and a 12-hour light period in phase with

the diurnal cycle. Lighting consisted of a mixture of natural and








fluorescent light. The fruit were supported on racks made of 0.5-inch

plywood and No. 8 finishing nails, as shown in Figure 5. Treatments

were applied on the third day after infestation and mortality rates

were determined 8 days later by counting the numbers hatched and not

hatched. The controls were sprayed with water in the same manner as

the treatment applications.

Representative oils from the 3 series of narrow-boiling fractions,

selected to cover the ranges of molecular weight, viscosity, and 50%

distillation point, were tested. Dosage-mortality relationships were

established by applying 7 to 10 concentrations of each oil. Each con-

centration was applied to 5 egg-infested fruit in a randomized block

design. Thus each point on the dosage-mortality curves represents the

response of 400 to 500 eggs. Due to the problem of infesting a large

number of fruit with enough mite eggs of known age, it was not possible

to apply all concentrations of an oil on the same date. However,

dosages sufficient to establish the effective ranges were applied in

initial tests and subsequent tests were conducted under the same

environmental conditions to add supplementary points to the dosage-

mortality curves. The data were analyzed by probit analysis in the

same manner as were the Florida red scale data.

In Field Experiment No. 1, described below, residual control of

spider mites by 4 oils was determined. Spider mite counts were made 1,

4, and 7 weeks after spraying as follows: 25 leaves were picked from

each of 4 trees in a plot; eggs and active stages of mites on the 100

leaves were collected by brushing onto a rotating circular glass plate

(6 inches in diameter) covered with moistened glue; counts were made of

the eggs, immature stages, and adult females of both citrus red mite









and Texas citrus mite on one-fourth the surface of the plate. These

counts were multiplied by 4 to obtain an estimate of the total numbers

on the 100 leaves. This is the standard technique used by entomolo-

gists at the Citrus Experiment Station in making spider mite counts in

miticide experiments.


Phytotoxicity Studies

Laboratory experiments

Studies were made to compare the effects of oils of different

molecular weight and base-type on the rates of respiration and transpi-

ration of potted 'Pineapple' sweet orange seedlings. Simultaneously,

observations were made of any abnormal reactions by the plants to the

various treatments, such as leaf drop, leaf burn, and oil-soaking. The

plants used in these studies were grown from seed in the greenhouse.

Seedlings were transplanted from seed flats to 46-ounce juice cans 4 to

6 months after planting. The potting medium was a 3:1:1 mixture of

soil, peat, and vermiculite. The plants were approximately 1 year old

when used.

Respiration studies.--The rates of oxygen uptake by leaves of

'Pineapple' sweet orange seedlings, sprayed with light (305 mol wt) and

heavy (365 mol wt) fractions of both paraffinic and naphthenic oils,

were determined. The oils were applied at 1.5% concentration.

The plants were held both before and after treatment under green-

house conditions with temperature fluctuation in the range of 60 to 90F.

Six plants, selected for uniformity in size and appearance, were as-

signed to each treatment. Five pairs of adjacent leaves were selected

on each plant and 1 of each pair was protected from the spray by

shielding with aluminum foil during the spraying operation. The









unsprayed leaf served as the check on the adjacent sprayed leaf. One

pair of leaves per plant was harvested each sampling date, starting

with the basal-most pair and working up the plant on successive sam-

pling dates. Thirty 0.25-inch discs were taken from each leaf with an

ordinary hand-grip paper punch. Hence, 12 samples of 30 punches each,

6 sprayed and 6 unsprayed, were run for each oil. The 30 discs from a

single leaf constituted a sample.

Oxygen uptake was measured by standard manometric techniques using

a 14-flask Warburg respirometer. The flasks were of 16-ml capacity

with 2 side arms. The ambient CO2 level was maintained by placing 0.2

ml 10% KOH in the center well of each flask to absorb the evolved C02.

The flasks were kept dry,but 1 ml distilled water was placed in 1 side

arm of each flask to maintain constant relative humidity. The flasks

were shaken at 100 cycle/min in a water bath maintained at 25 + 0.1 C.

The operation was carried out in a 68 F darkroom.

A manometer-calibration period of 50 min was followed by 02 uptake

determinations for 2 successive 30-min and one 60-min periods. The

total 02 uptake during the last 2 hours was used to calculate the res-

piration rate in I" 02/cm2 per hour. Determinations were made 1, 3, 7,

and 14 days after treatment. The rates of the treated leaves were con-

verted to per cent of the rates of the untreated leaves and these

values were used for comparing the different treatments on each sam-

pling date, An analysis of variance was run on the data.

In a follow-up experiment, the heavy paraffinic fraction, P-365,

was applied at 2.0% concentration as a drenching spray to 6 plants.

The same procedures were followed as in the above experiment except

that the sample size was increased to 48 leaf punches. Respiration








rates were measured 1, 3, and 7 days after treatment. The total 02

consumption per sample during the 2-hour period was used to compare the

adjacent sprayed and unsprayed leaves. The differences between treated

and non-treated leaves were tested by the "t" test.

Transpiration study.--The effect of light (285 mol wt), medium

(320 mol wt), and heavy (365 mol wt) fractions of paraffinic and

naphthenic oils on the transpiration rate of treated 'Pineapple' seed-

lings was determined by methods somewhat similar to those of Riehl

et al. (56). The plants were selected for uniformity in stem height

and number of fully expanded leaves. All but fully expanded leaves

were removed from each plant and additional new growth was removed as

it appeared so that the leaf surface area remained constant. Soil

moisture was equalized by bringing each container of soil to field ca-

pacity and allowing 1 day for excess water to leach and drain off. The

weights of the plants and containers were then determined and these

weights were used as the initial weight thereafter. The containers

were placed in polyethylene freezer bags and sealed against evaporation

loss of soil moisture by gathering the top of the bag firmly around the

base of the plant and taping with masking tape. Transpirational water

loss was determined as the difference between successive weights of the

plants at 24-hour intervals, weighing to the nearest 0.1 g. The soil

moisture was replenished after each 50-g loss by transpiration. Pre-

treatment determinations revealed a uniform transpiration rate varying

directly with number of leaves per plant. A randomized block experi-

ment was set up with 7 treatments replicated 5 times. Blocking was

on the basis of leaves per plant and position on the laboratory table.

The oils were applied at 1.5% concentration in the dilute spray and









check plants were sprayed with water in the same manner as the treat-

ment application. The plants were held in the laboratory at 78 + 4 F

and 60% + 10% relative humidity. Alternating 12 hours light and dark

prevailed. Illumination was provided by four 48-inch 40-watt "day-

light" fluorescent bulbs placed 30 inches directly above the tops of

the plants.

Weighing was continued to 70 days after treatment application.

The difference between 2 successive 24-hour weighing was divided by

the total leaf area (considering only 1 side of the leaf since essen-

tially all the stomata of citrus leaves are on the abaxial surface) to

obtain the rate in mg/cm2 per 24 hours. The data were analyzed in this

form.

Field experiments

Two experiments were conducted to obtain phytotoxicity data under

field conditions. Block No. 23 of the Citrus Experiment Station groves

was used for these studies. The trees were 'Hamlin' sweet orange on

rough lemon rootstock, 6 years of age, and 8 to 10 feet in height.

Five treatments, consisting of 4 oils and a check, were applied in a

randomized block design with 4 replicates of 4 trees each. Although

these young trees varied considerably in size and crop, the differences

were somewhat equated between treatments. Oils 31, 35, 36, and 38 of

Table 3 were used in both experiments and the second experiment uti-

lized the same trees as did the first. The oils were applied at 1.5%

concentration at approximately 5 gallons of spray per tree.

The oils were prepared as described earlier and oil deposits were

measured on both fruit and leaves by the same technique except for the

method of sampling and size of the samples. Twenty-four leaves and 24









fruit were picked from each 4-tree plot immediately after spraying.

The oil was removed by dipping each fruit or leaf in 2 successive

dioxane washes. After the sample was collected,the 2 washes were com-

bined for the spectrophotometer reading. Leaf areas were determined as

previously described, but the surface areas of the fruit were measured

by the method of Turrell (95). The major and minor axes of each fruit

were measured and the corresponding surface area was obtained from a

prepared table.

Field Experiment No. 1: oil blotch, leaf drop, and fruit drop.--

The first experiment was applied on 6 May 1964, during the time the

fruit sizes were in the range of 0.75 to 1.50 inches in diameter. The

object was to induce oil blotch and to relate oil type to the incidence

of the condition. Diameter measurements of 15 fruit on each of 40

trees averaged 2.57 cm, or approximately 1 inch. Treatments were ap-

plied with a "Speed Sprayer" Model 705 CP air-blast sprayer traveling

at 1 mph. A large plastic shield was used to protect adjacent trees

from the spray drift.

The fruit were checked periodically on the tree for oil blotch.

For 5 weeks after spraying, the rates of fruit and leaf drop were de-

termined weekly. An area under each tree,extending to about 1 foot be-

yond the drip line, was raked clean after spraying. One week later, and

weekly thereafter up to the fifth week, the dropped leaves and fruit

were collected. The fruit were counted but the leaves were weighed be-

cause of the excessive amount of drop.

Field Experiment No. 2: fruit color and internal fruit quality.--

A late-season application of 4 oils was made on 18 September 1964, with

the objective of relating oil heaviness and refinement to effect on








degreening and fruit quality. Treatments were applied with a high-

pressure sprayer and a double-nozzle hand gun. The plastic shield was

used to protect adjacent trees from spray drift as in the above experi-

ment. Fruit samples were harvested on 16 October, 1 and 12 November,

and 7 December, or approximately 4, 6, 8, and 12 weeks after treatment.

The samples consisted of 40 fruit from each 4-tree plot. Where possi-

ble, the fruit were picked from the outside canopy of the tree at a

height of 3 to 6 feet and both very large and very small fruit were

avoided. However, due to limited quantity of fruit on some trees, some

of the sampling, especially the fourth sample, was done without regard

to fruit size or location on the tree, both of which are recognized

sources of error, especially for fruit quality (69). Both the degreen-

ing and fruit quality studies utilized the same fruit samples.

Color measurement and ethylene degreening.--The first and third

40-fruit samples were degreened for 72 hours with ethylene gas after

harvesting. A 4 x 4 x 4-foot degreening chamber was used and commer-

cial recommendations on temperature, humidity and ethylene gas concen-

tration were followed (32). Degreening rates were determined instru-

mentally, using the reflectance attachment of a Bausch and Lomb

"Spectronic 20" spectrophotometer (33). The amount of green color in

the peel was measured as per cent absorbance at 675 mi. A 1-inch-

diameter circular area was randomly selected and marked on the equator

of each fruit and a color reading was taken in this circle after 0, 24,

48, and 72 hours degreening time. The degreening rate was indicated by

the decrease in absorbance from 1 reading to the next. Color measure-

ments were taken 4 and 8 weeks after treatment. The coefficient of re-

gression of per cent absorbance on degreening time was calculated for









each treatment, and these were used for comparing the effects of the

various treatments on degreening rate.

To supplement the instrumental measurements of the degreening rate,

20-fruit samples from each treatment were degreened for the same time

intervals and photographed together to illustrate the color changes

visually. Twenty extra fruit were harvested from each plot at the

same time as were the 40-fruit samples. The 4 samples from each treat-

ment were mixed and then divided randomly into four 20-fruit lots. One

lot of 20 fruit for each treatment was placed in the degreening chamber

at the start of the 72-hour period, a second lot was added at 24 hours,

and a third at 48 hours; the fourth lot received no ethylene degreening.

Therefore, the 4 lots of fruit were degreened 72, 48, 24, and 0 hours,

respectively. At the end of the 72-hour period, the 4 lots of fruit for

all 5 treatments were photographed together in color. These photo-

graphs are presented with the numerical data.

Fruit quality.--After the degreening treatments described above,

the 40-fruit samples were analyzed for internal quality by standard

methods (75). The analyses included the following determinations:

per cent soluble solids (0 Brix); per cent acid; Brix/acid ratio; fruit

weight; juice weight; and per cent juice (by weight). Solids determi-

nations were made with a Brix hydrometer and acid was determined titri-

metrically with standard sodium hydroxide solution and phenolphthalein

indicator. The treatments were compared mainly on the basis of per

cent soluble solids.















RESULTS AND DISCUSSION


Relation of Composition and Heaviness of Oils
to Insecticidal and Ovicidal Efficiency

Dosage-mortality tests were conducted for selected fractions of

the narrow-boiling paraffinic, reformed, and naphthenic series against

citrus red mite eggs and adult female Florida red scale, and 30 com-

mercial-type oils were screened against Florida red scale, in the

laboratory. The properties of molecular weight, viscosity, 50% distil-

lation point, and chemical composition or base-type (paraffinic, re-

formed, or naphthenic) were studied with respect to control efficiency.

A field application of 4 commercial-type oils gave some information on

residual control of spider mites.

Results

Florida red scale studies.--Oil deposit, total number of scales,

and per cent kill for each dosage level of the oils used in the dosage-

mortality tests against Florida red scale adults are listed in Table 4.

The LD50 and LD95 values, their 95% confidence intervals, and slopes of

the regression lines as obtained by probit analysis are presented in

Table 5. The probit regression lines in Figure 6 show the dosage-

mortality relationships of the various fractions in each series. The

relationship of oil heaviness to efficiency in kill is depicted in

Figures 7, 8, and 9, where LD95 values are plotted, according to chemi-

cal composition, against molecular weight, viscosity, and 50% distilla-

tion point, respectively. Efficiency varies inversely with the LD95





Table 4. Oil deposit, number of scales,
dosage-mortality tests against


and per cent kill
Florida red scale


with 3 series of petroleum oils in


Dosage levels, high to low deposit

Oil 1 2 3 4 5 6 7 8 9


P-265



P-285



P-305



P-320


P-365


P-435



R-265



R-285


Lg/cm2
Scales
% kill

pg/cm2
Scales
% kill
pg/cm2
Scales
% kill
pg/cm2
Scales
% kill
ig/cm2
Scales
% kill
pg/cm2
Scales
% kill

pg/cm2
Scales
% kill

pg/cm2
Scales
% kill


108
220
85

115
278
96
119
309
100

105
390
100
122
315
100
121
376
99

108
182
91

118
256
100


94
180
98

107
368
98
94
357
100

101
233
100
89
338
100
95
277
99

94
336
93

102
235
99


81
214
92

95
262
98
87
226
99

83
256
99
79
286
98
94
381
95

81
207
92

101
285
99


67
221
86

88
265
100
63
468
96

69
297
99
70
420
78
71
189
96

67
253
94

87
297
99


54
159
84

71
307
94
50
328
94

54
300
98
62
237
92
59
234
91

54
176
95

62
364
93


40
361
77

53
389
91
39
307
82
41
353
98
46
362
65
46
392
55

40
261
17

49
242
88


27
151
90

36
267
20
26
311
27
27
310
49
32
303
31
30
343
11

27
226
12

37
231
64


0
209
2.8


26
319
2
15
468
8
14
387
10
17
448
12
18
312
12


0
318
5.6
0
318
5.6

0
318
5.6
0
318
5.6
0
318
5.6


0
209
2.8


26
291
10


0
336
1.4





Table 4--Continued


Dosage levels, high to low deposit

Oil 1 2 3 4 5 6 7 8 9


R-305


R-320


R-365


N-265



N-285


N-305


N-320


N-365


N-395


pg/cm2
Scales
% kill
ig/cm2
Scales
% kill
Pg/cm2
Scales
% kill
jg/cm2
Scales
% kill
pg/cm2
Scales
% kill
Pg/cm2
Scales
% kill
pg/cm2
Scales
% kill
pg/cm2
Scales
% kill
pg/cm2
Scales
% kill


95
255
100
102
201
98
130
314
99
108
253
89
122
257
100
110
348
100
111
171
100
113
281
98
120
214
100


94
230
99
100
308
99
106
219
98
94
117
96
102
233
99
96
288
99
92
225
100
111
195
98
109
232
100


92
244
100
92
349
99
98
356
99
81
146
89
88
246
92
87
223
97
90
239
99
96
210
95
100
271
97


78
238
99
70
258
99
79
269
98
67
130
73
70
257
93
69
313
96
71
257
98
80
213
96
70
189
97


70
318
98
62
300
98
67
236
92
54
205
40
63
314
93
57
171
95
64
218
95
62
226
80
50
258
81


48
256
95
50
248
92
50
185
94
40
229
7
52
222
78
41
264
66
42
326
76
55
335
82
38
211
72


31
370
49
31
281
62
33
236
56
27
246
2
39
293
26
27
255
7
29
205
21
32
267
53
26
256
34


15
353
5
16
300
17
16
339
8
0
209
2.8
28
267
20
15
238
6
14
227
4
18
300
9
16
295
12


0
336
1.4
0
336
1.4
0
336
1.4


0
246
4.4
0
246
4.4
0
246
4.4
0
246
4.4
0
246
4.4
















Table 5. Effectiveness of 3 series of petroleum oils against adult
female Florida red scale



Slope of LD50, [ig/cm2 LD95, jig/cm2
Slope of ) J
regression
Oil line Dose 95% CL Dose 95% CL


P-265 3.389 30.0 .. .. 91.1 .. ..
P-285 6.932 43.9 15.7 60.1 75.8 56.1 385.2
P-305 6.420 31.4 26.8 35.2 56.7 50.2 68.4
P-320 5.944 31.3 25.6 35.5 59.2 51.7 74.2
P-365 5.420 41.9 27.8 50.7 84.2 69.1 130.8
P-435 6.758 45.5 35.8 52.9 79.7 67.1 112.8

R-265 5.189 43.9 .. .. 91.0 .. ..
R-285 7.030 35.9 30.6 40.6 61.5 52.8 80.8
R-305 6.635 30.5 25.7 34.3 54.0 47.1 67.8
R-320 4.703 26.2 22.3 29.8 58.6 50.6 71.3
R-365 4.649 30.6 25.6 35.3 69.0 58.6 86.3

N-265 6.818 58.0 .. -.. 100.1 .. ..
N-285 6.409 43.5 34.0 50.6 78.6 66.3 109.6
N-305 7.117 39.2 32.4 44.8 66.8 57.4 87.2
N-320 7.174 36.1 31.9 39.5 61.1 54.6 72.9
N-365 4.300 35.6 30.4 40.2 85.9 74.9 103.4
N-395 4.542 31.8 27.8 35.5 73.1 63.5 88.5


aValues for slopes of dosage-mortality regression lines and 95%
confidence limits (CL) for lethal doses (LD) for 50% and 95% kill
were obtained by probit analysis. Confidence limits were not cal-
culated for the lightest fraction in each series.












7- 395 98
S 195
85

70

5 50
30
S- 20
10


REFORMED 1





H
7 98

985





32-i
PARFFI ,, 85
914 70 giL4

5 J50
H 30
20
4 10
H

z
PARAFFINIC
7 98 o
95

6 2585
70

5 -50
36 30
4 eX; -20
I p 10
30 40 60 80

OIL DEPOSIT, 4g/cm2
Figure 6. Regression of per cent kill on deposit level for 3 series of
narrow-boiling petroleum fractions tested against adult female
Florida red scale. The number on each line indicates the average
molecular weight of the fraction.






' I I I


I I I


I


K> /


I I


i I


260


280


300


Figure 7. Efficiency in relation
fractions against adult female


320 340 360 380
AVERAGE MOLECULAR WEIGHT

to molecular weight for 3 series of
Florida red scale.


400


420


440


narrow-boiling petroleum


I I


A I


I I


i I


I I


I I


B B


' I


j I* I I I'

-* PARAFFINIC

REFORMED

*.- -- NAPHTHENIC







' I I I I I I I I


.PARAFFINIC

REFORMED

..- NAPTHTENIC


100





90





80


- I





'*1


a I I


I I a I


100


140


a I a I


160


VISCOSITY, SSU AT 100 F


Figure 8. Efficiency in relation to viscosity for 3 series of
tions against adult female Florida red scale.


narrow-boiling petroleum frac-


_- _____-___


Ce'
U
bo
ZL
:0
m
0r>


I I


I I


200


220


' I I


I I I


i I






I I I I I


100




90




80




70




60


I I


. i l i i


/
/ /


I I I I


620 640 660 680 700 720

50% DISTILLATION POINT, -F

Figure 9. Efficiency in relation to 50% distillation point for
petroleum fractions against adult female Florida red scale.


740


760


3 series of narrow-boiling


I I


',\\.



\
\


c','


a I


I I


o I


I I


1 I


a __ I


U I f I I I

GPARAFFINIC

- REFORMED
NAPHTHENIC


I I


/N









values. The relative efficiency of the 3 series, in decreasing order,

was reformed, paraffinic, and naphthenic. Efficiency increased with

heaviness up to a point, after which the trend reversed. The points of

maximum efficiency of the 3 physical properties considered for the dif-

ferent types of oil were:

1) Molecular weight--paraffinic, 305; reformed, 305; and
naphthenic, 320.

2) Viscosity, SSU at 100 F--paraffinic, 59.8; reformed,
59.3; and naphthenic, 79.7.

3) Fifty per cent distillation point--paraffinic, 696 F;
reformed, 700 F; and naphthenic, 689 F.

A practical deposit level of 70 |jg/cm2 was selected as the maximum

deposit for efficient kill of scale insects. The following minimum

physical property values were derived by this criterion from the curves

in Figures 7, 8, and 9:

1) Molecular weight--reformed, 279; paraffinic, 291; and
naphthenic, 300.

2) Viscosity, SSU at 100 F--reformed, 51; paraffinic, 53;
and naphthenic, 66.

3) Fifty per cent distillation point--reformed, 644 F;
naphthenic, 657 F; and paraffinic, 661 F.

Thirty commercial distillation range oils were compared at 0.5%

and 1.25% concentration. These oils represented 5 viscosity classes:

60, 70, 80, 90, and 100 SSU at 100 F. Oil deposit, corrected per cent

kill for each replicate, and mean per cent kill for the oils at each of

the 2 dosage levels appear in Table 6. Although arranged from high to

low kill in each viscosity class at the low dosage level, the data were

analyzed together. Therefore, the letters denoting significance apply

across all viscosity classes under a given dosage level. Levels of

kill were quite variable within each viscosity class at the 0.5% dosage





Table 6. Effectiveness of commercial oils at 2 levels of application against adult female Florida red
scale

0.507. oil 1.25% oil
Replications, % kill Replications, % kill
Oil Viscosity Deposi- Deposi-
No. SSU at 100 F pg/cmi 1 2 3 4 5 Meanc pg/cml 1 2 3 4 5 Meanc


55
38
47
52a*
52
54
53

44
42
51 a*
31
34
41
39
36
48
45
51

29
30
32
33
49
35
50a*
50


60.0
57.6
61.8
57.0
57.0
57.6
58.8

76.6
75.0
76.5
74.3
74.2
72.0
70.5
71.7
69.6
76.9
76.5

84.7
79.6
84.5
83.9
86.5
92.5
92.0
92.0


85 64 83 88 74 78.9 abcd
80 66 88 69 70 74.7 abcd
45 77 47 56 52 55.8 cdefg
54 27 30 28 26 33.1 ghi
7 54 32 24 11 25.6 hi
2 45 20 7 42 23.1 i
56 6 29 18 6 22.6 i

80 65 87 81 86 79.5 abc
71 66 58 92 85 74.2 abed
68 66 82 83 59 71.5 abcde
61 39 63 89 76 65.6 abcde
63 53 71 58 82 65.5 abcdef
66 83 65 42 61 63.3 abcdef
65 45 88 36 70 60.7 bcdef
55 59 78 49 59 59.9 cdef
81 78 55 42 35 58.5 cdef
42 79 45 62 62 57.8 cdefg
53 51 62 62 56 56.9 cdefg

74 64 80 72 64 70.7 abcde
61 56 70 45 97 65.8 abcde
76 64 57 50 64 62.3 bcdef
59 60 63 52 52 57.1 cdefg
42 54 47 70 62 54.8 defg
67 64 94 95 90 81,9 ab
69 68 52 60 35 56.9 cdefg
52 36 44 18 56 41.1 fgh


92 98 94 100 100
98 92 98 100 98
98 100 100 100 100
100 97 99 100 100
100 100 100 100 100
94 97 95 98 97
99 91 97 97 97

96 100 99 98 100
96 99 100 100 98
97 99 98 99 93
99 97 96 100 100
99 99 100 99 100
97 100 88 100 98
93 100 97 93 100
99 99 99 100 100
100 100 99 100 96
91 92 100 100 100
99 98 97 100 100

99 100 100 100 100
92 99 98 100 100
93 100 98 94 100
99 92 98 98 100
100 100 100 98 92
96 100 99 100 100
96 88 99 100 64
100 98 97 100 100


96.9 abc
97.4 abc
99.6 a
99.1 ab
100.0 a
96.3 bc
96.2 bc

98.5 ab
98.5 ab
97.1 abc
98.3 ab
99.3 ab
96.5 abc
96.5 abc
99.5 ab
99.0 ab
96.6 abc
98.7 ab

99.8 a
97.7 abc
97.0 abc
97.4 abc
97.9 ab
98.9 ab
89.3 c
98.8 ab





Table 6--Continued


0.50% oil 1.25% oil

Replications, % killb Replications, % kill
Oil Viscosity Deposit Deposit
No. SSU at 100 F ig/cm2 1 2 3 4 5 Meanc jig/cm2 1 2 3 4 5 Meanc


43 105.0 38 80 93 79 82 90 84.7 a 89 100 100 98 100 100 99.6 a
40 100.0 38 59 78 80 68 64 70.1 abcde 87 100 100 100 100 100 100.0 a
37 112.1 40 66 68 48 73 60 62.9 abcdef 107 100 100 99 97 100 99.1 ab
46 103.0 37 50 53 40 72 26 48.1 fg 96 94 93 97 92 100 95.3 bc


aOils grouped in 5 viscosity classes: 60, 70, 80, 90 and 100 SSU.
bper cent kill corrected for natural mortality, according to Abbott's formula. Replicate values rounded
to whole numbers for presentation.
cTreatment means at a given dosage level followed by the same letter are not significantly different at
the 5% level according to Duncan's New Multiple Range Test.
*Oils denoted by "a" are commercial formulations of the oils denoted by the corresponding numbers without
the a."









level. None of the oils attained 95% kill at this dosage; however, the

deposits were considerably less than the lowest LD95 values obtained

in the dosage-mortality tests. On the other hand, only 1 oil, No. 50a,

failed to give above 95% kill at the 1.25% dosage level and this fail-

ure can be attributed to the low level of kill obtained on replicate

No. 5. The deposits obtained were all as high or higher than the

70 tg/cm2 level discussed above. Correlation between oil viscosity and

scale kill is not apparent from the data in Table 6. However, the

viscosity range covered by these commercial oils lies well within the

effective range for viscosity as indicated in Figure 8.

Citrus red mite studies.--Oil deposit, total number of eggs, and

per cent kill for each dosage level of the oils used in the dosage-

mortality tests on citrus red mite eggs are listed in Table 7. The

oils are identified by name in the table. The results of the computer

analyses are presented in Table 8. Certain of the LD95 values had

rather broad 95% confidence intervals but this was due in part to an

excessive number of points occurring above this level of kill and per-

haps to the fact that the various points were run over a period of

several weeks. Although the confidence limits were wide in certain in-

stances, LD95 values were found to be quite reproducible. In subse-

quent tests in which 10 concentrations were applied on the same day,

LD95 values obtained for the P-320 and P-365 fractions were 16.4 and

17.0 g/cm2, respectively, with confidence intervals of 13.4 to 26.1

and 10.5 to 46.6, respectively. The confidence limits varied somewhat

from test to test for the same oil but the LD95 values were quite close

in terms of actual oil deposit.






Table 7. Oil deposit, number of eggs, and per cent kill with 3 series of petroleum oils in dosage-
mortality tests against citrus red mite eggs


Dosage levels, high to low deposit

Oil 1 2 3 4 5 6 7 8 9 10 11


pg/cm2
P-250 Eggs
% kill
Lg/cm2
P-265 Eggs
% kill
pg/cm2
P-285 Eggs
% kill
Pg/cm2
P-305 Eggs
% kill
pg/cm2
P-320 Eggs
% kill
pg/cm2
P-365 Eggs
% kill

pg/cm2
P-435 Eggs
% kill

pg/cm2
P-520 Eggs
% kill


135 124 111 69 42 16 0
421 372 408 417 431 405 430
45 38 32 19 9 10 2.0
108 90 74 43 32 18 0
397 487 410 443 404 405 430
71 57 71 41 34 9 2.0
121 78 45 36 25 20 0
427 550 412 392 384 419 430
99 95 85 80 34 20 2.0
88 48 42 20 20 17 14
414 443 547 453 484 491 472
98 100 99 98 90 89 69
84 45 36 18 15 13 9
410 419 464 471 481 502 449
99 98 100 97 96 87 68
78 48 47 31 18 16 8
449 434 497 515 473 443 464
97 99 99 98 98 96 95

82 58 48 38 26 23 19
444 432 497 487 502 452 431
100 95 97 96 95 97 96

85 50 42 32 26 21 18
485 483 474 464 429 456 439
99 95 86 87 86 87 83


6
448
62
8
433
86
5
413
86
16
447
92

13
440
76


3
404
35
4
117
59
3
472
83

14
467
89

10
395
77


0
442
1.3
3
451
62
2
428
70

5
424
82

10
406
66


0
442
1.3
0
442
1.3
0
442
1.3

0
442
1.3





Table 7--Continued


Dosage levels, high to low deposit

Oil 1 2 3 4 5 6 7 8 9 10 11


pig/cm2 147 143 120 108 90 53 19
R-250 Eggs 464 448 477 477 404 438 490
% kill 64 63 51 42 36 18 14
1ig/cm2 135 133 121 86 43 40 19
R-265 Eggs 485 444 460 396 459 424 476
% kill 84 85 83 78 62 62 4


Ig/cm2
R-285 Eggs
% kill
jg/cm2
R-295 Eggs
% kill

ig/cm2
R-305 Eggs
% kill


90 54 33 20 16 11 9
394 385 475 461 352 464 488
99 97 98 89 74 28 6
89 44 38 28 15 14 9
514 437 448 488 508 460 458
98 99 97 96 90 76 28
94 64 42 22 17 16 14
463 474 479 555 460 462 472
96 100 99 96 95 82 85


Pg/cm2 74 46 37 17 16 15 14
R-320 Eggs 408 544 474 602 435 467 474
% kill 100 100 100 98 98 98 85


ig/cm2
R-365 Eggs
% kill


74 40 33 19 16 14 11
470 457 460 422 547 474 487
99 100 100 96 92 92 76


Pg/cm2 107 99 93 87 54 21 0
N-250 Eggs 427 486 380 500 442 445 427
% kill 40 23 49 34 40 17 2.5


0
463
3.2
0
463
3.2
0
463
3.2
0
463
3.2

6
470
45
9
467
77


7
460
80


2
476
24
6
488
64
4
500
74


0
459
2.1


5
440
60


0
461
2.6


0
459
2.1





Table 7--Continued


Dosage levels, high to low deposit

Oil 1 2 3 4 5 6 7 8 9 10 11


pg/cm2 111 100 94 87 50 42 25
N-265 Eggs 398 500 416 496 339 470 384
% kill 65 65 76 36 51 19 13
Ig/cm2 114 98 96 52 52 39 22
N-285 Eggs 500 471 496 423 470 500 402
% kill 87 89 94 94 60 27 27


pg/cm2
N-305 Eggs
% kill


88 49 42 39 29 19 15
573 472 506 500 469 468 500
99 98 99 91 86 82 73


Pg/cm2 86 54 28 18 17 16 15
N-320 Eggs 405 439 560 470 445 486 500
% kill 100 96 99 96 94 97 91
pg/cm2 80 58 45 36 31 21 12
N-365 Eggs 437 510 415 453 398 500 493
% kill 100 100 99 97 97 91 89
pg/cm2 90 55 46 30 28 22 17
N-395 Eggs 421 434 451 487 515 454 457
% kill 100 99 98 97 97 93 92
Ig/cm2 93 58 43 23 22 20 16
N-440 Eggs 468 401 447 566 500 407 500
% kill 99 98 96 93 97 88 89
pg/cm2 82 76 48 40 19 15 14
P-96 Eggs 444 437 442 421 469 445 490
% kill 99 98 97 97 100 97 89
pg/cm2 74 38 32 16 12 3 3
R-60 Eggs 541 517 470 497 457 458 464
% kill 99 98 99 90 85 28 15


0
434
2.5
14
500
6
15
460
62
13
500
72
11
500
87
11
500
76
14
504
86
7
448
89
0
463
2.1


0
440
2.5
0
436
1.8
8
488
50
9
500
58
9
487
65
10
453
73
4
223
85


6
500
43
0
436
1.8
0
436
1.8
9
410
93
2
400
46


0
442
1.8


0
442
1.8
0
441
1.3














Table 8. Effectiveness of 3 series of petroleum oils against citrus
red mite eggsa


Slope of LD50, Pg/cm2 LD95, ig/cm2
Oil regression
line Dose 95% CL Dose 95% CL


N-250 2.438 138.0 .. .. 1,950.0 .. -
N-265 2.528 77.5 .. .. 346.8 .. -
N-285 3.338 40.9 21.6 57.4 127.3 83.8 457.9
N-305 2.775 10.3 6.2 13.4 40.3 32.4 60.1
N-320 3.584 7.4 0.2 10.9 21.2 16.2 50.1
N-365 2.574 5.6 2.4 8.0 24.5 18.8 42.7
N-395 2.557 5.8 4.0 7.4 25.6 21.8 32.3
N-440 1.386 2.1 0.03- 5.2 32.2 24.0 63.9

R-250 3.565 126.1 .. .. 364.8 .. -
R-265 2.457 45.3 .. .. 211.4 .. -
R-285 5.233 14.4 11.1 17.8 28.8 21.8 53.7
R-295 3.610 9.9 3.2 14.3 28.3 19.0 137.7
R-305 2.320 5.4 2.1 8.5 27.6 16.7 88.0
R-320 3.104 4.7 2.9 6.0 15.9 12.7 23.9
R-365 1.693 2.3 0.5 4.1 21.5 14.9 47.6

P-250 2.806 167.9 .. .. 647.3 .. -
P-265 2.198 58.4 .. .. 327.2 .. -
P-285 4.631 29.2 22.2 35.7 66.2 54.5 93.3
P-305 2.080 4.7 3.1 6.3 28.8 20.3 48.4
P-320 1.784 2.6 1.0 4.1 21.8 14.4 51.2
P-365 1.202 0.6 0.1 1.4 14.9 9.9 29.9
P-435 1.061 0.7 0.1 2.0 25.7 18.4 41.8
P-520 1.334 3.9 1.3 6.5 66.1 44.9 147.4

P-96 1.531 1.6 0.5 2.8 18.6 12.1 38.8
R-60 2.778 5.6 4.2 7.2 22.1 16.2 34.8


aValues for slopes of dosage-mortality regression lines and 95% confi-
dence limits (CL) for lethal doses (LD) for 50% and 95% kill were ob-
tained by probit analysis. Confidence limits were not calculated for
the oils exhibiting very low toxicity.









The dosage-mortality relationships for the various fractions in

the 3 series are shown by the probit regression lines in Figure 10.

These regression lines show a direct relationship between efficiency

and weight of the oil, up to a point. The trend reverses with the

heavier fractions in each series. The relationship is shown more

vividly in Figures 11, 12, and 13, in which LD95 values are plotted

against molecular weight, viscosity, and 50% distillation point, re-

spectively. The LD95 values for the 2 commercial oils, P-96 and R-60,

are plotted for comparison. These wide-boiling oils were slightly more

efficient than the narrow-distilling fractions of corresponding proper-

ty values in their respective series. The reformed oils appeared rela-

tively more efficient than the paraffinic or naphthenic types. Only

with respect to distillation temperature did the naphthenic base frac-

tions show superiority to those of paraffinic base; this occurred in

the range of 660 to 700 F. The 3 series of oil were most efficient at

the following physical property values:

1) Molecular weight--paraffinic, 365; reformed, 320; and
naphthenic, 320.

2) Viscosity, SSU at 100 F--paraffinic, 99; reformed, 66;
and naphthenic, 80.

3) Fifty per cent distillation point--paraffinic, 752 F;
reformed, 716 F; and naphthenic, 689 F.

Beyond this point of maximum efficiency for each of the series,

the trend was toward decreasing efficiency with increase in heaviness

of the oil.

At a deposit of 30 pg/cm2, selected as the maximum deposit for

efficient kill, the curves of Figures 11, 12, and 13 show that the 3

series of oils were ovicidally efficient down to the following minimum

physical property values:






67





NAPHTHENIC /99
77 98

90


5 - L-50



6 99
1. 7 REFORMED / ^ ~9




P7AF I 01- 98L
E- 7-7'95





zI d 90
6 / 80
70






1 5 50-- 0'-----/... 50


E 30
a 4 15~







4 PARAFFINIC 97,^ /I I ,
REORE 98

6 3(01 do 80~






70^80 7
p.'.^ V ^ y^-7










2 5 10 20 50 100 200

OIL DEPOSIT, Lg/cm2

Figure 10. Regression of per cent kill on deposit level for 3 series
of narrow-boiling petroleum fractions tested against citrus red mite
eggs. The number on each line indicates the average molecular
weight of the fraction. The solid portion of each line indicates
the range of data collected; the broken extension is extrapolation
to the 50 or 95% kill level.






1,000 I 1 1 1 1 I, 11, 1 11

\

500 \ PARAFFINIC,0 P-96 _
400 REFORMED, A R-60 -
300 \ "-- NAPHTHENIC

200 \

C\\

i 100- \ \



50


30 t___*- -
20 -

50 1 \

10 __ I i I I I I I I i I I II I I
260 280 300 320 340 360 380 400 420 440 460 480 500 520 540

AVERAGE MOLECULAR WEIGHT

Figure 11. Efficiency in relation to molecular weight for 3 series of narrow-boiling petroleum fractions
and 2 commercial oils against citrus red mite eggs.








I ( I I I I I I I I I I I I I I I


1,000




500

400

300


200 I-


2-


- ** -


ilil I I i~I ilililil ilil I--a Ii 111111


40 60 80 100 120 140 160 180 200 220 340 360 380 400

VISCOSITY, SSU AT 100 F

Figure 12. Efficiency in relation to viscosity for 3 series of narrow-boiling petroleum fractions and 2
commercial oils against citrus red mite eggs.


- 'PARAFFINIC, 0 P-96

.- -------. REFORMED, & R-60

*-NAPHTHENIC


ei
C.





i-o


100


50

40

30


20


I" I I I I I I [ --r


m
B







1,000


500
400

300

200


Ul


100


600 650 700 750 800 850 900

50% DISTILLATION POINT, 'F

Figure 13. Efficiency in relation to 50% distillation point for 3 series of narrow-boiling petroleum
fractions and 2 commercial oils against citrus red mite eggs.









1) Molecular weight--reformed, 285; paraffinic, 304; and
naphthenic, 313.

2) Viscosity, SSU at 100 F--reformed, 52; paraffinic, 61;
and naphthenic, 75.

3) Fifty per cent distillation point--reformed, 660 F;
naphthenic, 677 F; and paraffinic, 694 F.

The property values for maximum efficiency and the minimum proper-

ty values for efficient kill were slightly higher for citrus red mite

eggs than for red scale. However, LD95 values for red scale were more

than double those for the mite eggs, except with the 265-mol wt frac-

tions. These lighter fractions attained 95% kill of red scale at 90 to

100 pg/cm2, but required over 200 pg/cm2 for citrus red mite eggs.

The 4 oils applied in Field Experiment No. I covered a viscosity

range of 60 to 90 SSU. Detailed spider mite counts were made 1, 4, and

7 weeks after application. The data presented in Table 9 show the

relative abundance of citrus red mite and Texas citrus mite,

Eutetranychus banks (McGregor), at these times. All 4 oils signifi-

cantly reduced the spider mite population throughout the 7-week period,

except for Texas citrus mite in the seventh week. Although differences

between oils were not significant, residual control by the heavy and

medium oils appeared better than by the light oil.

Discussion

These studies were primarily concerned with the relationship of

chemical composition and heaviness of petroleum oil to insecticidal and

ovicidal efficiency. The main comparisons for composition were between

the paraffinic and naphthenic series. The reformed oils were paraffinic

fractions obtained by a special refining technique which resulted in

products of slightly lower paraffinic hydrocarbon content than the

paraffinic series. This was probably due to the retention in the










Table 9.


Spider mite counts at 1, 4, and 7 weeks after application of spray
oils on 6 May 1964 in Block 23


Plot Live adult female and young mites per 100 leaves per 4-
Treatment (4 trees) tree plot


Citrus red mite


4th
week
260
236
288
168


Texas citrus mite


7th
week
272
532
456
708


1st
week
284
172
140
80


4th
week
2,656
2,204
3,828
1,044


7th
week
28
48
36
28


17.0 a 238.0 a


32
48
36
92


2.0 b 52.0 b


4
16
12
4


492.0 a 169.0 a 2,433.0 a


76
136
184
212


112
116
116
100


1,180
500
124
728


152.0 b 111.0 ab 633.0 b


36
52
116
68


80
0
108
112


188
340
36
24


0.0 b 9.0 b 68.0 b 75.0 b 147.0 b 50.0 b


8
4
32
8


28
28
48
124


160
168
88
76


32
16
12
56


5.0 b 13.0 b 45.0 b 57.0 b 123.0 b 29.0 b


12
8
16
8


12
8
8
100


308
268
260
120


52
88
124
124


2.0 b 11.0 b 149.0 b 32.0 b 239.0 b 97.0 a


Total mites for
each week


104 1,292


3,624


1,776


14,300 1,180


Check


1st
week
24
20
24
0


Mean


R-60


Mean


P-96


35.0 b

84
88
88
76

84.0 a

20
52
64
64


Me an


BR- 1


Mean


BR-2


Mean


aTreatment means for a given week followed by the same letter are not sig-
nificantly different at the 5% level according to Duncan's New Multiple
Range Test.









refining process of certain ring compounds (e.g., naphthenic acids and

partially saturated aromatics) which are removed in the normal acid

treating process of refining. The 3 physical properties discussed,

molecular weight, viscosity, and distillation temperatures, are all

measures of oil heaviness.

The most striking features of the results as depicted in Figures

7 to 9 and 11 to 13 are: the relative efficiency of the 3 series of

oil fractions; the abrupt change from increasing efficiency with in-

crease in oil heaviness to a more gradual rate of increase--especially

with citrus red mite eggs; the trend of decreasing efficiency beyond a

point of maximum efficiency--especially with Florida red scale; and

the difference in the minimum effective dosage for the 2 pest species.

The relative efficiency of the 3 series of oils tested, in de-

creasing order, was reformed, paraffinic, and naphthenic. These re-

sults are in general agreement with the findings of other workers (9,

42, 43, 44, 47, 48, 49). Chapman et al. (9) summarized years of exten-

sive research and cited other workers in correlating basic structural

composition of petroleum oils to insecticidal efficiency. Paraffin

content was found to be the key variable among saturated compositions

and a direct relationship between efficiency and the proportion of car-

bon atoms present in the form of chains was established. Riehl and

LaDue (47) found paraffinic oils superior to naphthenic oils against

adult female California red scale and citrus red mite eggs in labora-

tory studies similar to those reported herein. Riehl and Carmen (48)

and Riehl and Jeppson (49) reported the same relationship under field

conditions in California. Thompson (84) reported no difference between

paraffinic and naphthenic oils in scale control on citrus in Florida at









1.3 to 1.4% oil concentration, but at 1.0% there was a slight trend in

favor of the paraffinic type.

While the results obtained in the present work support the above

conclusions, the correlation between paraffin content and efficiency

was not as pronounced. The reformed series, which is indicated by the

data in Table 3 as being intermediate in paraffin content, appeared

more efficient, up to 340 mol wt and 85 viscosity, than either of the

other 2 series. With respect to 50% distillation temperature, the

naphthenic series tended to be more efficient against both pest species

than the paraffinic series, at least in the low portion of the efficient

range of distillation temperature.

The change in increase in efficiency with increase in oil heavi-

ness was more abrupt where heaviness was measured by molecular weight

(Figures 7 and 11) and viscosity (Figures 8 and 12) than where measured

by distillation temperature (Figures 9 and 13). The curves showing the

relationship of LD95 values to molecular weight and viscosity are strik-

ingly similar to those presented by Riehl and LaDue (47) for California

red scale and citrus red mite. The pattern of the curves was quite

similar in both instances. The main differences were that generally

lower LD95 values were obtained in the present work and the importance

of chemical composition was not as apparent as was shown by the above

authors. Riehl and Carmen (48) concluded that insecticidal efficiency

for California red scale increased with increase in molecular weight up

to 360, and Riehl and Jeppson (49) reported a critical value of 340 mol

wt for citrus red mite control in the field.

Pearce and Chapman (44) obtained maximum efficiency at 320 mol wt

for European red mite eggs, cottony peach scale nymphs, and oriental









fruit moth eggs. The minimum molecular weight values for efficient

kill established in the present work were considerably lower than the

above values, but the points for maximum efficiency obtained here were

quite similar.

Beyond a point of maximum efficiency for each of the 3 series

studied, the trend was toward decreasing efficiency with increase in

oil heaviness. This reversal was much more drastic with Florida red

scale than with citrus red mite eggs. Riehl and LaDue (47) observed

the same phenomenon with California red scale but not with citrus red

mite eggs. They reasoned that the spreading characteristics of the

larger hydrocarbon molecules was the limiting factor and were able to

show some proof of this by diluting the heavier fractions with a non-

toxic amount of kerosene to reduce the viscosity of the oils. Pearce

and Chapman (44) obtained similar results with oriental fruit moth eggs

and greatly increased the efficiency of a 479-mol wt isoparaffin by

diluting with deodorized kerosene. Thompson (84) reported no differ-

ence in scale control on Florida citrus with oils in the viscosity

range of 72 to 100 SSU. The screening data for the commercial oils

presented in Table 6 tended to bear this out. Although differences

occurred at the low deposit level, these were not correlated with

viscosity, which ranged from 57 to 112 SSU. At the high deposit level,

all the oils were effective. The field data for spider mites presented

in Tables 9 and 10 failed to show significant correlation of control to

viscosity in the range of 60 to 90 SSU.

Although the minimum LD95 values obtained for Florida red scale

were 2 to 3 times as great as those for citrus red mite eggs, it is

interesting to note that the very light fractions in each series









attained 95% kill of red scale at a much lower deposit level than for

citrus red mite eggs. Pearce and Chapman (44) observed this same dif-

ference between cottony peach scale nymphs and eggs of both European

red mite and oriental fruit moth. They suggested that this difference

may be due to the differences between the respiratory systems of the

active insect and the mite egg,

Correlations between efficiency and 50% distillation temperature

for both test species are depicted in Figures 9 and 13. Very little

difference was shown between the paraffinic and naphthenic types.

Chapman et al. (9) stated that distillation range is the single most

useful physical property for specifying a spray oil since this is most

directly related to the volatility of the material. The results ob-

tained here suggest that naphthenic oils may be equally as efficient as

paraffinic oils if compared on the basis of distillation temperature

rather than viscosity or molecular weight.

Comparison of the 3 series of oils tested in these laboratory

studies at the LD95 values of 30 and 70 |jg/cm2 for citrus red mite eggs

and Florida red scale, respectively, has much practical significance.

The recommended rates of oil applied for spider mites and scale insects

on Florida citrus are 0.7% and 1.3%, respectively. With standard field

application procedures, sprays containing these oil concentrations de-

2
posit in the neighborhood of 30 and 70 fg/cm respectively. Therefore,

the correlations made between these maximum efficient deposits and the

physical property values may indicate that the use of oils lighter than

those presently used on Florida citrus is feasible, in which case some

of the phytotoxicity problems discussed in the following section may be

alleviated. However, it is often difficult to obtain uniform









distribution of oil deposits over the entire citrus tree. In such

cases, the inhibition of crawler settling by the residual oil film be-

comes the important aspect of scale control. The increased dissipation

rate of the lighter, more volatile oils,and consequent reduction in

residual effectiveness, may be the limiting factor in the use of oils

lighter than the 60 to 70 viscosity range.


Relation of Composition, Heaviness, and
Refinement of Oil to Phytotoxicity

Respiration and transpiration

Results.--Determinations of the respiratory rates of treated and

untreated leaves of 'Pineapple' seedlings were made 1, 3, 7, and 14

days after treatment with 305- and 365-mol wt fractions of paraffinic

and naphthenic oils. The mean of 6 determinations for each oil are

presented in Table 10. Analysis of variance of the data detected no

significant difference between treatments at the 5% level. In a

2
follow-up experiment, P-365, at 154 4g/cm effected reduction in 02

uptake of 4.3%, 11.8%, and 16.0% on the first, third, and seventh days

after treatment, respectively (Table 11). The reduction on the third

and seventh days was highly significant.

The relationship of oil heaviness and composition to effect on the

transpiration rate of 'Pineapple' seedlings is shown by the data in

Table 12 and by Figures 14 and 15. The transpiration rate for the

2
check is given as mean water loss in mg/cm leaf surface per day; the

rates for the treated groups of plants are presented as per cent of the

check. Analysis of variance was run on the data in mg/cm2 per day, and

the means were converted to per cent of the check for presentation.



























Table 10.


Respiratory rates of oil-sprayed 'Pineapple'
seedlings expressed as per cent of the check.
Each value is the mean of 6 determinations.
Oils were applied at 70 to 80 pg/cm2


Days after treatment

Oil 1 3 7 14


P-305 105.1 100.5 98.6 87.4

P-365 112.4 94.4 88.2 97.6

N-305 92.7 98.8 96.2 102.4

N-365 85.2 101.8 96.5 103.4







Table 11. Effect of 365-mol wt paraffinic oil on respiration of adjacent treated
and untreated leaves of 'Pineapple' seedlings, measured as 02 uptake in
Lg/cm2 leaf surface in a 2-hour period. The oil deposit was high
(154.4 ig/cm2)


Days after treatment

1 3 7

Untreated Treated Untreated Treated Untreated Treated


141.0 131.3 150.3 136.9 167.3 137.0

163.3 136.5 150.8 116.0 160.5 136.5

133.6 138.4 147.2 132.5 170.0 136.2

142.1 147.4 149.5 135.9 157.0 141.6

135.6 125.3 137.6 132.7 165.6 134.6

141.0 140.9 150.5 127.4 160.1 137.0

Mean 142.8 136.6 147.6 130.2 163.4 137.2

Significance -** **

Per cent
reduction 4.3 11.8 16.0


**Double asterisk indicates significance at the 1% level.






Table 12.


Transpiration rate of 'Pineapple' seedlings sprayed with 1.5% concentration of low, medium,
and high molecular weight fractions of paraffinic and naphthenic oils


Transpiration rate of oil sprayed plants as per cent of checka
Days from Water loss Paraffinic oils Naphthenic oils
treatment from check arfic olNateici
in mg/cm2 P-285 P-320 P-365 N-285 N-320 N-365


-14 9.8 a
-13 17.2 a
-12 14.0 a
8 17.1 a
Sprayed
28 October 1964
1 15.3 a
2 24.3 a
3 17.2 a
4 24.3 a

5 16.8 a
6 15.6 a
7 24.0 a
8 8.4.a


8.2
25.5
26.4
15.7

22.2
22.8
22.1
22.9


115.8
109.2
110.3
98.0


91.4
61.8
63.8
78.6

74.7
73.3
70.6
74.0

87.0
82.6
75.4
79.5

79.0
78.8
76.4
77.5


89.6
97.5
103.5
100.1


68.0
37.2
33.3
34.4

52.1
46.9
37.1
64.7

89.4
43.3
45.9
54.5

47.4
54.2
61.5
57.6


85.3
116.8
102.3
105.6


98.0
60.2
51.5
56.2

68.0
59.6
52.5
71.3

79.0
63.6
54.1
61.5

56.5
62.6
66.4
61.1


a
bc
bc
bcd

bc
bc
bcd
b

a
bc
bc
cd

cd
bc
cd
cd


86.3
104.5
111.7
104.1


76.4
68.9
65.1
73.6

81.8
73.5
68.0
77.7

78.1
86.0
98.8
81.1

80.6
85.4
89.6
85.1


91.0
83.3
115.5
97.3


67.7
46.1
40.6
50.1

54.9
62.4
51.1
70.3

81.4
63.4
61.6
69.2

70.7
68.5
70.7
72.2


c
bc
cd
b

a
be
bc
bcd

b
bc
bcd
bcd


92.0
101.6
92.5
94.3


76.4
53.7
43.4
44.5

56.5
54.5
50.6
76.6

90.6
55.7
40.2
51.0

47.0
53.6
52.5
54.4






Table 12--Continued


Transpiration rate of oil sprayed plants as per cent of check
Days from Water loss Paraffinic oils Naphthenic oils
treatment from check aa -fncol-ahh-col
in mg/cm2 P-285 P-320 P-365 N-285 N-320 N-365


17 35.1 ab 94.5 ab 60.8 b 73.1 b 120.3 a 100.6 ab 70.2 b
18 29.4 ab 91.7 abc 51.0 d 70.9 cd 115.0 a 85.8 bc 59.1 d
19 18.2 a 87.3 a 61.5 b 62.6 b 95.7 a 84.0 a 56.6 b
20 22.9 a 84.0 ab 64.6 b 66.7 b 95.6 a 87.6 ab 66.2 b

21 18.9 a 87.2 a 60.8 c 63.9 c 95.6 a 82.3 ab 69.0 bc
25 18.2 ab 92.3 ab 55.3 c 68.3 bc 112.8 a 84.0 abc 58.4 c
26 11.5 abc 130.9 a 67.0 c 81.0 bc 134.5 a 104.6 ab 68.0 c
32 29.2 b 101.9 ab 64.9 c 56.0 c 126.2 a 104.6 ab 58.4 c

33 18.8 a 79.6 b 60.3 c 59.6 c 100.9 a 82.7 a 63.0 bc
34 10.5 a 80.4 bc 66.8 c 74.1 c 95.7 ab 79.0 c 70.6 c
35 15.5 a 80.3 bc 68.4 cd 68.4 cd 90.6 ab 81.0 bc 62.2 d
53 16.7 ab 96.2 ab 71.8 b 75.8 b 124.0 a 83.7 b 75.8 b

54 20.3 b 106.9 b 73.0 b 73.1 b 154.5 a 100.7 b 76.6 b
60 11.9 bc 96.0 bc 69.8 c 69.6 c 149.3 a 110.7 b 69.8 c
61 19.9 ab 84.2 bc 74.2 bc 59.0 c 122.0 a 91.5 abc 62.6 c
62 16.4 ab 87.5 ab 69.4 b 69.7 b 109.5 a 104.3 a 69.3 b

67 17.3 bc 98.7 bc 73.8 cd 71.1 d 127.9 a 106.7 ab 70.1 d
68 18.1 ab 79.9 bc 55.7 cd 49.1 d 112.9 a 97.2 ab 43.1 d
69 17.6 b 88.7 bc 75.7 cd 66.9 cd 123.2 a 107.3 ab 59.1 d
70 17.5 a 87.7 ab 63.0 bc 50.8 c 109.4 a 96.5 a 51.6 c
aFigures in the table are means of 5 replications. Treatment means for a given day which are followed by
the same letter are not significantly different at the 5% level according to Duncan's New Multiple Range
Test. (Analyses of variance were run on daily water loss in mg/cmz; means converted to per cent of
check for presentation.)








140


0 285 mol wt
4 320 mol wt
0 365 mol wt


== \
S120 \
z
9: Check j
4P 100
M \
%C- \



S60
i3^lP O -"\ \'\-






40

-8 0 2 4 6 8 10 12 14 16 18 20 26 32 34 54 60 62 67 69
DAYS AFTER TREATMENT
Figure 14. Effect of light, medium, and heavy paraffinic fractions on the transpiration rate of treated
'Pineapple' orange seedlings in relation to time after treatment. Shaded symbols indicate significance 0
from check.






0 285 mol wt
A 320 mol wt
0 365 mol wt


120-
I, \
S Check /
\ ~ / -\/^\ -^ ^
R 100-


80 --, /%'7 p
E-.4
8 0--



40-


11~~~~lm p I IM 1 14 1 1 I.I I L AI IA
-8 0 2 4 6 8 10 12 14 16 18 20 26 32 34 54 60 62 67 69
DAYS AFTER TREATMENT
Figure 15. Effect of light, medium, and heavy naphthenic fractions on the transpiration rate of treated
'Pineapple' orange seedlings in relation to time after treatment. Shaded symbols indicate significance
from the check.









The response of the plants to the various treatments is readily

apparent from the graphs in Figures 14 and 15. The 320-mol-wt

paraffinic oil and all 3 naphthenic oils effected significant reduc-

tion in transpiration the first day after treatment. Further reduction

occurred with all 6 oils on the second and third days, after which some

recovery was evident. A strong recovery period began after the seventh

day for all the oil-treated plants and none were significantly differ-

ent from the check on the ninth day. After this time, the P-320, P-365,

and N-365 fractions significantly depressed transpiration throughout

the remainder of the 70-day period of measurement with only a few days

excepted. The transpiration rates of the plants treated with the P-285,

N-285, and N-320 fractions were not significantly different from that

of the check after the ninth day except on occasional days. The plants

treated with the N-285 oil transpired at a level significantly higher

than the check on several days. In Figures 14 and 15, the shaded

symbols indicate significant difference from the check. The pretreat-

ment transpiration rates shown in Table 13 indicate only minor differ-

ences between the groups of plants in their normal transpiration rates.

Discussion.--The data presented in Table 10 fail to show signifi-

cant inhibition of respiration in citrus seedlings sprayed with light

and heavy oils at a deposit level normally applied for scale control in

Florida. Although an initial increase followed by a gradual reduction

in 02 uptake by the plants sprayed with the paraffinic oils and the

opposite response to the naphthenic oils were indicated, these trends

were inconsistent and probably could occur by chance. At a deposit

level twice that of normal field applications (approximately 150 pgkmn2),

the 365-mol wt paraffinic oil significantly reduced the rate of 02









uptake (Table 11) 3 and 7 days after treatment. Although conditions at

the time did not permit further determinations, a trend toward in-

creased inhibition was indicated. These data are quite limited, but

they lead to the conclusion that effects on the respiratory process are

associated with increasing oil deposit and increasing oil heaviness.

These factors would tend to place more oil on and in the leaf and hold

it there for a longer period of time.

The results presented in Table 12 and Figures 14 and 15 show that

the transpirational process of citrus may be more markedly affected by

normal rates of oil application than the respiratory process. Also, a

direct correlation is indicated between oil heaviness, particularly as

measured by distillation range, and inhibition of transpiration. A

significant reduction in transpiration was associated with all 6 oils

the first several days after treatment. The plants sprayed with the 2

lightest fractions, i.e., 285 mol wt, showed the least initial reduc-

tion and also the fastest recovery rate. Of these two oils, the

fastest recovery was associated with the naphthenic fraction. The data

in Table 3 show that the paraffinic fraction had a higher distillation

range than the naphthenic fraction. The difference in the recovery

rates associated with the two 320-mol wt fractions were even greater.

The recovery pattern for the 320-mol wt naphthenic fraction was nearly

the same as that for the 285-mol wt paraffinic fraction. The 320-mol

wt paraffinic fraction depressed transpiration throughout the 70-day

period to about the same extent as did both 365-mol wt fractions. The

most peculiar aspects of these curves are that the P-365 oil had less

effect on transpiration the first few days following treatment than did

the P-320 or N-365 oils, and that the plants sprayed with N-285 showed









significant increase in transpiration on certain days beyond the twenty-

fifth.

The results discussed above are in general agreement with reports

of other workers. Wedding et al. (98) reported significant reduction

in both respiration and photosynthesis in 'Washington' navel orange

leaves with a California medium-grade naphthenic oil at 150 Pg/cm2.

Photosynthesis was affected to a greater extent than was respiration.

However, Riehl and Wedding (57) reported no consistent inhibition of

photosynthesis in lemon or lime leaves by California light-medium or

medium-grade spray oils at the same deposit level. But a definite re-

lationship between inhibition of photosynthesis and increasing oil de-

posit was established (57, 59). Recovery was faster in plants sprayed

with naphthenic oils than in those treated with paraffinic oils, but

the paraffinic oils used were of a higher boiling range and the de-

posits were probably more persistent.

Riehl et al. (56) obtained a two-thirds reduction of transpiration

in citrus by a California medium-grade naphthenic oil. They concluded

that the effect on transpiration was due to physical interference by

the spray oil on or in the leaf tissue and that recovery of transpi-

ration occurred with dissipation of the oil from the leaves. Full re-

covery occurred in 3 to 5 weeks after application (56). Recovery was

faster in plants sprayed with a naphthenic oil than in plants sprayed

with a paraffinic oil of comparable molecular weight (58). However,

the paraffinic oil had a 50% distillation temperature of 663 F while

that of the naphthenic oil was only 642 F. Table 3 shows that the 50%

distillation points of the 285, 320, and 365 molecular weight fractions

used in the present study were 1) naphthenic: 635 F, 689 F, and 738 F;









and 2) paraffinic: 646 F, 715 F, and 752 F, respectively.

Distillation range should be stressed because of its relation to

the volatility of an oil. Because of this relationship, the dissipation

rate of oil deposits from citrus leaves and fruit should be inversely

related to the distillation temperatures of the oil. The importance of

oil evaporation rate with respect to insect control was discussed ear-

lier. Apparently, the adverse effect of oils on the physiological

processes of citrus trees is closely associated with endurance of the

oil deposit. Thus, insecticidal and phytotoxic properties of oils are

closely related.

The transpiration measurements made in this study are probably

most important as indicators of the endurance of oil deposits and of the

depressive effect on the other processes discussed--respiration and

photosynthesis. Riehl and Wedding (57) showed that the reduction of

these processes was due to physical interference with gaseous exchange

caused by the presence of the spray oil in the tissue and not to death

of the cells. The principal effects occurred in the tissue of the leaf

marked by the dark discoloration known as oil-soaking. Tests with

tetrazolium showed the cells of the discolored tissue were not killed.

Recovery of physiological processes accompanied dissipation of the oil

deposit. Inspection of the response curves for the 285-mol wt paraf-

finic and the 320-mol wt naphthenic fractions in Figures 14 and 15,

reveals striking similarity in the recovery patterns after the tenth

day. Assuming that this pattern of response is intermediate between

temporary and prolonged physiological effects on the citrus plant, the

distillation temperatures of these 2 oils offer a reasonable approach

to the selection of an optimum distillation range with respect to plant









safety. As mentioned above,the 50% distillation points for these 2

oils are 646 F and 689 F, respectively. However, these are laboratory

determinations; if field conditions are considered, the effects of

weathering factors might increase the dissipation rates to the extent

that the above distillation temperatures could be increased considerably

without drastically increasing the effects of oil on the physiology of

the citrus tree. Comparison of the resulting temperatures with the

minimum distillation temperatures for efficiency against citrus pests

derived from Figures 9 and 13, reveals some interesting possible corre-

lations between insecticidal efficiency and plant safety.

Oil blotch, leaf drop, and fruit drop

Results.--Treatments were applied when the fruit were in the stage

of highest susceptibility to oil blotch. Inspections of the fruit were

made on the tree throughout the season and at harvest time. Although a

variety of oils were applied at a heavy dosage, no fruit were found to

exhibit this condition.

Weekly leaf drop in grams per 4-tree plot for each treatment is

presented in Table 13. The accumulated leaf drop for the 5-week period

is shown in Figure 16. It is readily apparent that a higher rate of

drop occurred in the treated plots than in the check plots. The great-

est portion of the leaves dropped during the first 2 weeks in the

treated plots, with the rate gradually diminishing up to the fifth

week. At this time a reversal in the relative rates of leaf drop oc-

curred. Whereas the check plots and the plots sprayed with the 60-SSU,

high-UR oil, R-60, had the lowest rate of drop during the first 4 weeks,

they now showed an increased rate, and the plots treated with the 74-

and 92-SSU, high-UR oils, P-96 and BR-1, showed a relatively low rate








Leaf drop by young 'Hamlin' trees following application of oil sprays on 6 May 1964 in Block 23


Leaf drop, grams per 4-tree plot

Total Total for
Plot, 1st 2nd 3rd 4th 5th for 5 first
Treatment 4 trees week week week week week weeks 4 weeks


Check


38
55
47
42


81
90
82
91


64
126
165
95


110
108
53
163


286
313
194
319


579
692
541
710


293
379
347
391


45.5 a

617
370
865
219

517.8 b

769
946
1,334
1,201

1,062.5 c


86.0 a 112.5 a


407
90
531
385


181
177
172
205


353.2 ab 183.8 ab


819
814
983
727


212
313
526
210


108.5 a 278.0 b


140
100
95
49


256
273
236
311


96.0 a 269.0 b


224
96
168
68


72
84
136
68


835.8 c 315.2 bc 139.0 ab 90.0 a


630.5 a

1,601
1,010
1,899
1,169

1,419.8 ab

2,096
2,253
3,147
2,274

2,442.5 b


352.5 a

1,345
737
1,663
858

1,150.7 ab

2,024
2,169
3,011
2,206

2,352.5 c


Mean


R-60


Mean


P-96


Mean


Table 13.








Table 13--Continued


Leaf drop, grams per 4-tree plot

Total Total for
Plot, 1st 2nd 3rd 4th 5th for 5 first
Treatment 4 trees week week week week week weeks 4 weeks


BR-I 1 385 682 185 249 293 1,794 1,501
2 440 452 83 142 219 1,336 1,117
3 618 666 229 242 87 1,842 1,755
4 894 774 337 291 151 2,447 2,296

Mean 584.2 b 643.5 bc 208.5 abc 231.0 b 187.5 ab 1,854.8 b 1,667.2 bc

BR-2 1 1,439 1,363 432 318 299 3,851 3,552
2 275 340 236 44 83 978 895
3 952 591 427 132 220 2,322 2,102
4 869 408 273 50 67 1,667 1,600

Mean 883.8 bc 675.5 bc 342.0 c 136.0 ab 167.2 ab 2,204.5 b 2,037.2 bc

Total for
all treatments 12,375 10,376 4,648 2,842 3,967


Treatment means for a given week followed by the same letter are
level according to Duncan's New Multiple Range Test.


not significantly different at the 5%




Full Text
28
this method of application was to duplicate the type of deposits ob
tained in field spraying. The spray unit, shown in Figure 1, consisted
of the following main components:
A. Blower, high velocity centrifugal; manufactured by Ideal
Industries, Inc., Sycamore, Ill.; 1.33-hp universal motor,
11,350 rpm; "egg-crate" air straightener vanes attached
at outlet; discharge velocity 6,000 fpm.
B. Electric motor for pump; 0.75-hp; 1,725 rpm.
C. Pump, manufactured by Hypro Engineering, Inc., Minneapolis,
Minn., Model 6500; nylon roller impeller, positive displace
ment; operated at 500 rpm.
D. Spray tank, stainless steel; tapered botton, center drain;
4,000-ml capacity.
E. Pressure regulator and gauge with by-pass to the tank.
F. Sprayer nozzle of "whirljet" type as used on "Speed
Sprayer," but with 3/64-inch orifice; stainless steel;
centered 3.25 inches in front of blower outlet; mounted
on 1/8-inch pipe to minimize volume of stagnant liquid
in the line beyond the shut-off valve.
G. Deflector vanes for shaping the air blast to a vertical
column of uniform velocity and spray impingement above
the turntable.
H. Operating lever with air baffle that extends over blower
outlet. Lever is linked to the quick shut-off valve to
start and stop air and liquid simultaneously.
I. Turntable centered 7 feet 9 inches from the sprayer nozzle;
operated at 15 rpm.
Emulsification of the oils was obtained by circulating the desired
amounts of emulsifiable oil and water through the spray unit 4 times,
or 32 sec for each 1,000 ml emulsion. The shearing action of the pump
and pressure regulator and the high velocity stream of liquid returning
to the tank produced a uniform emulsion.
The liquid was atomized through the nozzle at 70 psi and dis
charged into a 6,000 fpm-air blast. At the start of each spraying in
terval, the quick shut-off valve was opened for about 3 sec to clear


Table 6. Effectiveness of commercial oils at 2 levels of application against adult female Florida red
scale3
0.507 oil
1.257 oil
Oil
No.
Viscosity
SSU at 100 F
Deposit
pg/cm2
Replications, 7 kill'3
Deposit
pg/cm2
Replications, 7 kill'3
1 2 3 4 5 Mean0
1 2 3 4 5
Mean0
55
60.0
34
85
64
83
88
74
78.9
abed
87
92
98
94
100
100
96.9
abc
38
57.6
42
80
66
88
69
70
74.7
abed
76
98
92
98
100
98
97.4
abc
47
61.8
31
45
77
47
56
52
55.8
edef g
101
98
100
100
100
100
99.6
a
52 a*
57.0
30
54
27
30
28
26
33.1
ghi
68
100
97
99
100
100
99.1
ab
52
57.0
32
7
54
32
24
11
25.6
hi
74
100
100
100
100
100
100.0
a
54
57.6
40
2
45
20
7
42
23.1
i
93
94
97
95
98
97
96.3
be
53
58.8
34
56
6
29
18
6
22.6
i
87
99
91
97
97
97
96.2
be
44
76.6
37
80
65
87
81
86
79.5
abc
88
96
100
99
98
100
98.5
ab
42
75.0
34
71
66
58
92
85
74.2
abed
83
96
99
100
100
98
98.5
ab
51a*
76.5
-
68
66
82
83
59
71.5
abede
-
97
99
98
99
93
97.1
abc
31
74.3
29
61
39
63
89
76
65.6
abede
83
99
97
96
100
100
98.3
ab
34
74.2
34
63
53
71
58
82
65.5
abedef
84
99
99
100
99
100
99.3
ab
41
72.0
38
66
83
65
42
61
63.3
abedef
95
97
100
88
100
98
96.5
abc
39
70.5
33
65
45
88
36
70
60.7
bedef
84
93
100
97
93
100
96.5
abc
36
71.7
41
55
59
78
49
59
59.9
edef
94
99
99
99
100
100
99.5
ab
48
69.6
39
81
78
55
42
35
58.5
edef
87
100
100
99
100
96
99.0
ab
45
76.9
40
42
79
45
62
62
57.8
edefg
83
91
92
100
100
100
96.6
abc
51
76.5
28
53
51
62
62
56
56.9
edefg
70
99
98
97
100
100
98.7
ab
29
84.7
31
74
64
80
72
64
70.7
abede
103
99
100
100
100
100
99.8
a
30
79.6
30
61
56
70
45
97
65.8
abede
82
92
99
98
100
100
97.7
abc
32
84.5
35
76
64
57
50
64
62.3
bedef
98
93
100
98
94
100
97.0
abc
33
83.9
41
59
60
63
52
52
57.1
edefg
92
99
92
98
98
100
97.4
abc
49
86.5
36
42
54
47
70
62
54.8
defg
98
100
100
100
98
92
97.9
ab
35
92.5
46
67
64
94
95
90
81.9
ab
81
96
100
99
100
100
98.9
ab
50a*
92.0
27
69
68
52
60
35
56.9
edefg
73
96
88
99
100
64
89.3
c
50
92.0
30
52
36
44
18
56
41.1
fgh
73
100
98
97
100
100
98.8
ab
t/1
VO


53
Table 5. Effectiveness of 3 series of petroleum oils against adult
female Florida red scale3
Slope of
regression
line
O
LD50, |ig/cm
r\
ld95> pg/cnr
Oil
Dose 95% CL
Dose 95% CL
P-265
3.389
30.0

-

91.1

-

P-285
6.932
43.9
15.7
-
60.1
75.8
56.1
-
385.2
P-305
6.420
31.4
26.8
-
35.2
56.7
50.2
-
68.4
P-320
5.944
31.3
25.6
-
35.5
59.2
51.7
-
74.2
P-365
5.420
41.9
27.8
-
50.7
84.2
69.1
-
130.8
P-435
6.758
45.5
35.8
-
52.9
79.7
67.1
-
112.8
R-265
5.189
43.9

-

91.0
-

R-285
7.030
35.9
30.6
-
40.6
61.5
52.8
-
80.8
R-305
6.635
30.5
25.7
-
34.3
54.0
47.1
-
67.8
R-320
4.703
26.2
22.3
-
29.8
58.6
50.6
-
71.3
R-365
4.649
30.6
25.6
-
35.3
69.0
58.6
-
86.3
N-265
6.818
58.0

.

100.1
..

N-285
6.409
43.5
34.0
-
50.6
78.6
66.3
-
109.6
N-305
7.117
39.2
32.4
-
44.8
66.8
57.4
-
87.2
N-320
7.174
36.1
31.9
-
39.5
61.1
54.6
-
72.9
N-365
4.300
35.6
30.4
-
40.2
85.9
74.9
-
103.4
N-395
4.542
31.8
27.8

35.5
73.1
63.5

88.5
aValues for slopes of dosage-mortality regression lines and 95%
confidence limits (CL) for lethal doses (LD) for 50% and 95% kill
were obtained by probit analysis. Confidence limits were not cal
culated for the lightest fraction in each series.


17
Injurious effects of oil sprays on citrus
Various types of injury resulting from oil applications to citrus
have been reported (2, 16, 19, 22, 34, 35, 45, 51, 52, 53, 61, 66, 67,
83, 84, 89, 91, 92, 93, 99, 104, 105, 107, 110). Types of adverse
effects reported were leaf and fruit drop, fruit burn, fruit blemishes,
rough textured fruit, reduced soluble solids and acid, increased granu
lation, delayed degreening, crop reduction, upset of normal blossoming,
increased water rot and decay of fruit in wet weather, dead wood, and
increased susceptibility to freeze damage. According to Rohrbaugh (61),
some writers have claimed various beneficial effects such as larger
fruit, larger leaves, and better color, but most of these claims, he
felt, were without foundation.
Yothers and McBride (107) first reported a decrease in solids in
fruit from oil-sprayed trees in Florida in 1929. Thompson and Sites
(83), using oils of 72 and 100 SSU, concluded that oil sprays applied
after 1 August either delayed or prevented the formation of maximum
soluble solids, especially during the early part of the season.
Thompson and Deszyck (91) observed a greater effect on fruit quality
with 1.3% oil than with 0.7% oil in combination with parathion.
Sinclair et al. (66) reported that applications of light-medium grade
oils to citrus in California, at concentrations of 0.25 to 1.75%, caused
reduction in the total soluble solids and that timing of application
was relatively unimportant. However, Riehl et al. (54) found a defi
nite correlation between timing of oil sprays and fruit quality in
California. Applications during the period November to June had the
most adverse effect on solids.


128
94. Tucker, R. P. 1936. Oil sprays: chemical properties of petro
leum oil unsaturates causing injury to foliage. Ind. Eng.
Chem. 28:458-464.
95. Turrell, F. M. 1946. Tables of surfaces and volumes of spheres
and of prolate and oblate spheroids, and spheroidal coef
ficients. First edition. Univ. California Press, Berkeley
and Los Angeles. 153 p.
96. Van Overbeek, J., and R. Blondeau. Mode of action of phytotoxic
oils. Weeds 3(1):55-65.
97. Volck, W. H. 1903. Spraying with distillates. California Agr.
Exp. Sta. Bull. 153. 31 p.
98. Wedding, R. T., L. A. Riehl, and W. A. Rhoads. 1952. Effect of
petroleum oil spray on photosynthesis and respiration in citrus
leaves. Plant Physiol. 27(2):269-278 .
99. Wedding, R. T., and L. A. Riehl. 1958. Influence of petroleum
oil on the translocation of phosphorus in small lemon plants.
Amer. J. Bot. 45(2):138-142.
100. Winston, J. R. 1942. Degreening of oranges affected by oil
sprays. Proc. Florida State Hort. Soc. 55:42-45.
101. Woglum, R. S. 1926. The use of oil spray on citrus trees.
(abstract) J. Econ. Entomol. 19(5):732-733.
102. Woglum, R. S., and J. R. LaFollette. 1934. The double treat
ment for scale pests in California citrus orchards. J. Econ.
Entomol. 27(5):978-980.
103. Yothers, W. W. 1911. Recent results of spraying experiments for
the control of the whitefly on citrus. Proc. Florida State
Hort. Soc. 24:53-59.
104. Yothers, W. W. 1913. The effects of oil insecticides on citrus
trees and fruits. J. Econ. Entomol. 6(2):161-164.
105. Yothers, W. W. 1918. Spraying for control of insects and mites
attacking citrus trees in Florida. U. S. Dep. Agr. Farmers'
Bull. 933. 38 p.
106. Yothers, W. W. 1925. Cold process oil emulsions. J. Econ.
Entomol. 18(3):545-546.
107. Yothers, W. W. and 0. C. McBride. 1929. The effects of oil
sprays on the maturity of citrus fruits. Proc. Florida State
Hort. Soc. 42:193-218.
108. Young, P. A. 1935. Oil-mass theory of petroleum oil penetration
into protoplasm. Amer. J. Bot. 22(1):1-8.


104
adverse effect on degreening rate. The fact that the fruit from the
plots sprayed with the heavy oil and the low-UR oil overcame the
initial on-tree color differences after 24 hours degreening indicates
differences in rates of degreening with ethylene gas. The regression
coefficients in the equations in Table 16 for the 8-week samples indi
cate that the oil-sprayed fruit degreened at a faster rate than the un
sprayed fruit. However, the differences in on-tree color, i.e. the "a"
values in the regression equations, were so great that this increased
degreening rate was insufficient to overcome the color differences in
72 hours.
The faster degreening rate of the oil-sprayed fruit is illustrated
in still another way by the data in Table 16, perhaps having some
economic importance. The time required for the fruit to degreen to a
desirable color level was calculated by the regression equations. The
spread between the check and the heavy oil was 18 hours for the 4-week
sample; this was reduced to 13 hours for the 8-week sample. The dif
ference is amplified even more if the difference in the "a" values, or
on-tree color, are considered. The fruit from the heavy-oil treatment
were only 57o greener than the check fruit at 4 weeks but were almost
20% greener at 8 weeks. This brings out still another interesting ob
servation. Comparison of the "a" values for the fruit treated with the
heavy oil at 4 and 8 weeks after spraying indicates no on-tree color
break during this time interval. Since this statement is contradictory
to the appearance of the fruit in the photographs in Figure 19, it
should be pointed out that the photographs were taken 4 days after the
fruit were harvested and apparently some degreening had occurred with
out the aid of ethylene gas, although the fruit were stored at a


16
dormant-type oils. Riedhart (46) reported inhibition of photosynthesis
of banana leaves by a 75-SSU paraffinic oil.
Wedding et al. (98) reported a depression of both photosynthesis
and respiration in sweet orange and lemon plants sprayed with petroleum
oil emulsions in amounts approximating the deposit level obtained in
field applications in California. Recovery of photosynthesis occurred
sooner in lemon plants than in orange plants. In no case did they get
an increase in respiration as reported by Knight et al. (36), Green and
Johnson (30), and Green (31). They attributed at least part of the re
duction in soluble solids of citrus fruits accompanying oil spray
applications to inhibition of photosynthesis.
Riehl and Wedding (57) compared naphthenic and paraffinic oils of
different molecular weights as to their effect on photosynthesis in
citrus leaves. No consistent inhibition was observed with insecti-
cidally efficient deposits of 150 pg/cm^, but deposits of 300 to 600
pg/cnr greatly inhibited photosynthesis. The principal effect occurred
in oil-soaked tissue. During the first week following application, 50
to 607o reduction was detected. A tetrazolium test showed that cells in
the oil-soaked tissue were not killed. They concluded that inhibition
of photosynthesis was the result of interference with gaseous exchange
caused by the presence of the oil, and that dissipation of the oil was
accompanied by recovery of photosynthesis. Recovery by plants sprayed
with naphthenic oils was faster than by plants treated with paraffinic
oils. Results of a similar experiment by the same authors (59) showed
that the difference in rate of recovery associated with difference in
paraffinicity was greater for oils of comparable viscosity than for
those of comparable molecular weight.


66
The dosage-mortality relationships for the various fractions in
the 3 series are shown by the probit regression lines in Figure 10.
These regression lines show a direct relationship between efficiency
and weight of the oil, up to a point. The trend reverses with the
heavier fractions in each series. The relationship is shown more
vividly in Figures 11, 12, and 13, in which LD^ values are plotted
against molecular weight, viscosity, and 507o distillation point, re
spectively. The LDg[j values for the 2 commercial oils, P-96 and R-60,
are plotted for comparison. These wide-boiling oils were slightly more
efficient than the narrow-distilling fractions of corresponding proper
ty values in their respective series. The reformed oils appeared rela
tively more efficient than the paraffinic or naphthenic types. Only
with respect to distillation temperature did the naphthenic base frac
tions show superiority to those of paraffinic base; this occurred in
the range of 660 to 700 F. The 3 series of oil were most efficient at
the following physical property values:
1) Molecular weight--paraffinic, 365; reformed, 320; and
naphthenic, 320.
2) Viscosity, SSU at 100 F--paraffinic, 99; reformed, 66;
and naphthenic, 80.
3) Fifty per cent distillation point--paraffinic, 752 F;
reformed, 716 F; and naphthenic, 689 F.
Beyond this point of maximum efficiency for each of the series,
the trend was toward decreasing efficiency with increase in heaviness
of the oil.
At a deposit of 30 |j.g/cm selected as the maximum deposit for
efficient kill, the curves of Figures 11, 12, and 13 show that the 3
series of oils were ovicidally efficient down to the following minimum
physical property values:


95
indicates that over a longer period of time the total leaf drop would
be about equal for both sprayed and unsprayed trees. Perhaps the oil
merely hastens an inevitable process. It is interesting to note that
no leaf drop followed the second application of the oils to the same
trees in September.
The data in Table 14 show that fruit drop resulted from the oil
application. From the data presented,it is difficult to relate this
drop to any particular property of the oils. The plots treated with
the 74-SSU oil and the low-UR oil were consistently high in fruit drop
and the rate was significantly higher than that of the check, except in
the first and fifth weeks. The light and heavy oils were not signifi
cant from the check for the total 5-week period. However, after the
first week, the rate of drop associated with the light, highly refined
oil was lower than that caused by the other oils.
The time of application of these oils was about 5 weeks prior to
the normal "June drop" of fruit in Florida citrus, during which the
trees shed about 20% of the crop. However, the checks did not indicate
that the fruit drop following these treatments was associated with the
June drop. Ebeling (24) discussed the problem in California. Oil
sprays are normally applied to citrus in that state beginning in late
July, after termination of the normal "June drop" period. Beginning 1
or 2 weeks after spraying and continuing for a month or more, a heavy
fruit drop amounting to as much as 50% or more was caused or accentu
ated by the oil spray. The effect was unpredictable and was not found
to be related to any particular predisposing factor. He quoted the
following statement from Smith (72): "Drop has occurred when the soil
moisture was high, when it was moderate, and when it was low. In many


61
level. None of the oils attained 95% kill at this dosage; however, the
deposits were considerably less than the lowest LD95 values obtained
in the dosage-mortality tests. On the other hand, only 1 oil, No. 50a,
failed to give above 95% kill at the 1.25% dosage level and this fail
ure can be attributed to the low level of kill obtained on replicate
No. 5. The deposits obtained were all as high or higher than the
r\
70 |_ig/cnr level discussed above. Correlation between oil viscosity and
scale kill is not apparent from the data in Table 6. However, the
viscosity range covered by these commercial oils lies well within the
effective range for viscosity as indicated in Figure 8.
Citrus red mite studies.--Oil deposit, total number of eggs, and
per cent kill for each dosage level of the oils used in the dosage-
mortality tests on citrus red mite eggs are listed in Table 7. The
oils are identified by name in the table. The results of the computer
analyses are presented in Table 8. Certain of the LD?5 values had
rather broad 957 confidence intervals but this was due in part to an
excessive number of points occurring above this level of kill and per
haps to the fact that the various points were run over a period of
several weeks. Although the confidence limits were wide in certain in
stances, LD quent tests in which 10 concentrations were applied on the same day,
LD95 values obtained for the P-320 and P-365 fractions were 16.4 and
r\
17.0 |j.g/cm respectively, with confidence intervals of 13.4 to 26.1
and 10.5 to 46.6, respectively. The confidence limits varied somewhat
from test to test for the same oil but the LD95 values were quite close
in terms of actual oil deposit.


31
Figure 2. Spray coverage obtained on fruit with the laboratory air-
blast sprayer. A, fruit sprayed with oil at 1.0% concentration
containing fluorescent dye to show the distribution of the oil; B,
unsprayed fruit. Photographed under ultra-violet light. The
rectangular area on fruit "A" was left unsprayed to show the con
trast between sprayed and unsprayed surface.


Table 6--Continued
Oil
No.
Viscosity
SSU at 100 F
0.
,50%
oil
1
.25%
oil
Deposit
pg/cm2
Replications
, /o
kill
b
mc
Deposit
pg/cm2
Replications,
% killb
Meanc
1
2
3
4
5
Me.
1
2
3
4
5
43
105.0
38
80
93
79
82
90
84.7
a
89
100
100
98
100
100
99.6
a
40
100.0
38
59
78
80
68
64
70.1
abcde
87
100
100
100
100
100
100.0
a
37
112.1
40
66
68
48
73
60
62.9
abcdef
107
100
100
99
97
100
99.1
ab
46
103.0
37
50
53
40
72
26
48.1
fg
96
94
93
97
92
100
95.3
be
^ils grouped in 5 viscosity classes: 60, 70, 80, 90 and 100 SSU.
bper cent kill corrected for natural mortality, according to Abbott's formula. Replicate values rounded
to whole numbers for presentation.
cTreatment means at a given dosage level followed by the same letter are not significantly different at
the 5% level according to Duncan's New Multiple Range Test.
by "a"
*0ils denoted
the "a."
are commercial formulations of the oils denoted by the corresponding numbers without


Table 16. Regression equations for the degreening rate of oil-sprayed
'Hamlin' oranges and hours required to degreen to 30%
absorbance level3
Treatment
4 weeks after spraying
Hours
to
degreen
Y= a + bx
95%
CL
for ba
Check
83.6-.8543x
- .8870
to
-.8216
ab
62.74
R-60
89.2-.8200x
- .8424
to
- .7976
b
72.19
BR-2
89.9-.8033x
-.8265
to
- .7801
b
74.56
P-96
87.6- .8681x
-.8935
to
-.8427
a
66.35
BR-1
87.8- .7168x
-.7413
to
- .6923
c
80.63
8 weeks after spraying
Y= a + bx
95%
CL
for ba
Check
74.5-.7770x
-.7994
to
-.7546
c
57.27
R-60
84.2-.8422x
-.8629
to
- .8215
ab
64.35
BR-2
86.3-,8522x
-.8741
to
-.8303
a
66.06
P-96
82.5-.7954x
-.8260
to
-.7648
be
66.00
BR-1
89.2-.8412x
-.8576
to
- .8258
ab
70.33
degression coefficients not followed by the same letter are con
sidered significantly different since their 957o confidence intervals
do not overlap.


126
66. Sinclair, W. B., E. T. Bartholomew, and W. Ebeling. 1941. Com
parative effects of oil spray and hydrocyanic acid fumigation
on the composition of orange fruits. J. Econ. Entomol. 34(6):
821-829.
67. Sites, J. W. 1947. Internal fruit quality as related to pro
duction practices. Proc. Florida State Hort. Soc. 60:55-62.
68. Sites, J. W., and W. L. Thompson. 1948. Timing of oil sprays
as related to fruit quality, scale control, coloring, and tree
condition. The Citrus Ind. 29(4):5-9, 26.
69. Sites, J. W. 1953. Some factors affecting the quality of citrus
fruits. Univ. Florida Citrus Exp. Sta. Mimeo Rep. 54-7.
70. Smith, E. H., and G. W. Pearce. 1948. The mode of action of
petroleum oils as ovicides. J. Econ. Entomol. 41(2):173-180.
71. Smith, E. H. 1952. Tree spray oils. In Agricultural application
of petroleum products. Amer. Chem. Soc., Washington, D. C.
Advances in Chem. Ser. 7:3-11.
72. Smith, R. H. 1932. The tank-mixture method of using oil spray.
Univ. California Agr. Exp. Sta. Bull. 527. 86 p.
73. Smith, R. H. 1932. Experiments with toxic substances in highly
refined spray oils. J. Econ. Entomol. 25(5):988-990.
74. Snedecor, G. D. 1956. Statistical methods. Fifth edition. The
Iowa State Univ. Press, Ames. 534 p.
75. Soule, M. J., Jr., and F. P. Lawrence. 1959. What every citrus
grower should know--maturity tests for fresh fruit. Univ.
Florida Agr. Ext. Serv. Cir. 191. 18 p.
76. Stewart, W. S., and W. Ebeling. 1946. Preliminary results with
the use of 2,4-dichlorophenoxyacetic acid as a spray-oil
amendment. Bot. Gaz. 108:286-294.
77. Stewart, W. S., and L. A. Riehl. 1948. Addition of 2,4-D to oil
sprays. California Citrograph 33(10):456-458 .
78. Stewart, W. S., and H. Z. Hield. 1950. Effects of 2,4-dichloro-
phenoxyacetic acid and 2,4,5-trichlorophenoxyacetic acid on
fruit drop, fruit production, and leaf drop of lemon trees.
Proc. Amer. Soc. Hort. Sci. 55:163-171.
79. Stewart, W. S., L. A. Riehl, and L. C. Erickson. 1952. Effects
on citrus of 2,4-D used as an amendment to oil sprays. J. Econ.
Entomol. 45(4):658-668.


27
Preparation of Oils
Measurement of oil deposits on sprayed fruit and plant surfaces
required the addition of an indicator dye to the base oils. An oil-
soluble, water-insoluble red dye, DuPont Oil Red A (17), was added to
each oil at approximately 2.5 g/liter. Mixtures of oil and dye were
heated in a water bath to about 140 F and then were shaken continuously
for several hours to obtain maximum dye concentration in the oil.
Finally, the solutions were drawn through a medium-porosity fritted-
glass filter to remove any undissolved dye particles. These stock
solutions of dyed oils were used in all toxicity and phytotoxicity
studies.
The oils were formulated as emulsifiable oils in the laboratory as
needed. An oil-soluble, non-ionic emulsifier, Experimental emulsifier
9D-207 (Rohm and Haas Co., Philadelphia, Pa.), consisting of alkyl aryl
polyether alcohol plus a non-ionic solubilizer, was used. Extensive
tests under the conditions of this work showed that 0.4% (v/v) 9D-207
gave adequate and similar emulsification for all the oils tested except
the 2 heaviest fractions of the narrow-boiling paraffinic and naphthenic
series. P-435 and P-520 required 0.6% and 0.87 respectively, and N-395
and N-440 required 0.5% and 0.6%, respectively. The emulsifier was
measured volumetrically with a calibrated dropping-pipette and added to
each oil. The 2 materials were thoroughly and uniformly mixed by
stirring vigorously for 3 to 5 min, depending on the volume of oil.
Application of Oils in Laboratory Studies
The oils were applied as dilute aqueous sprays with a laboratory
air-blast sprayer (65) similar in performance to the commercial air-
blast sprayers widely used by Florida citrus growers. The idea behind


Table 11. Effect of 365-mol wt paraffinic oil on respiration of adjacent treated
and untreated leaves of 'Pineapple' seedlings, measured as O2 uptake in
o
pg/cm^ leaf surface in a 2-hour period. The oil deposit was high
(154.4 pg/cm^)
Days after
treatment
1
3
7
Untreated
Treated
Untreated
Treated
Untreated
Treated
141.0
131.3
150.3
136.9
167.3
137.0
163.3
136.5
150.8
116.0
160.5
136.5
133.6
138.4
147.2
132.5
170.0
136.2
142.1
147.4
149.5
135.9
157.0
141.6
135.6
125.3
137.6
132.7
165.6
134.6
141.0
140.9
150.5
127.4
160.1
137.0
Mean 142.8
136.6
147.6
130.2
163.4
137.2
Significance
-
**
**
Per cent
reduction
4.3
11.8
16.0
**Double asterisk indicates significance at the 17 level.


PROPERTIES OF PETROLEUM OILS
IN RELATION TO PERFORMANCE AS
CITRUS TREE SPRAYS IN FLORIDA
By
KENNETH TRAMMEL
A DISSERTATION PRESENTED TO THE GRADUATE COUNCIL OF
THE UNIVERSITY OF FLORIDA
IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE
DEGREE OF DOCTOR OF PHILOSOPHY
UNIVERSITY OF FLORIDA
April, 1965


This dissertation was prepared under the direction of the chairman
of the candidate's supervisory committee and has been approved by all
members of that committee. It was submitted to the Dean of the College
of Agriculture and to the Graduate Council, and was approved as partial
fulfillment of the requirements for the degree of Doctor of Philosophy.
24 April 1965
^j^Dean, College of Agriculture
Dean, Graduate School
Supervisory Committee:


LITERATURE CITED
1. Abbott, W. S. 1925. A method of computing the effectiveness of an
insecticide. J. Econ. Entomol. 18(2):265-267 .
2. Bartholomew, E. T., W. B. Sinclair, and E. C. Raby. 1934. Granu
lation (crystallization) of Valencia oranges. California Citro-
graph 19:88-89, 106, 108.
3. Burroughs, A. M., and W. M. Grube. 1923. A simplified method for
making lubricating oil emulsions. J. Econ. Entomol. 16(6): 534-
539.
4. Burroughs, A. M. 1923. Effects of oil sprays on fruit trees.
Proc. Amer. Soc. Hort. Sci. 20:269-277.
5. Chapman, P. J., G. W. Pearce, and A. W. Avens. 1941. The use of
petroleum oils as insecticides. Ill: Oil deposits and the con
trol of the fruit tree leafroller and other apple pests. J.
Econ. Entomol. 34(5):639-647 .
6. Chapman, P. J., G. W. Pearce, and A. W. Avens. 1943. Relation of
composition to the efficiency of foliage or summer type petrole
um fractions. J. Econ. Entomol. 36(2):241-247.
7.Chapman, P. J. and G. W. Pearce,
2(3):17-20.
1947. Oil sprays. Agr. Chem.
8. Chapman, P. J. 1959. Tree spray oils--their present status. New
York State Agr. Exp. Sta. Farm Research 25(1):7.
9. Chapman, P. J., S. E. Lienk, A. W. Avens, and R. W. White. 1962.
Selection of a plant spray oil combining full pesticidal ef
ficiency with minimum plant injury hazards. J. Econ. Entomol.
55(5):737-744.
10. Crafts, A. S., and H. G. Reiber. 1948. Herbicidal properties of
oils. Hilgardia 18(2):77-156.
11. Cressman, A. W., and L. H. Dawsey. 1936. The comparative insecti
cidal efficiency against the camphor scale of spray oils with
different unsulfonatable residues. J. Agr. Res. 52(11):865-878.
12. Dallyn, E. L., and R. D. Sweet. 1951. Theories on the herbicidal
action of petroleum hydrocarbons. Proc. Amer. Soc. Hort. Sci.
57:347-354.
121


39
Figure 5. Holding facilities for infested fruit in laboratory studies.
A, chamber for holding trays of scale-infested grapefruit; B, racks
supporting immature oranges infested with citrus red mite eggs.


Page
Field Experiment No. 1: oil blotch, leaf drop, and
fruit drop 47
Field Experiment No. 2: fruit color and internal fruit
quality 47
Color measurement and ethylene degreening 48
Fruit quality 49
RESULTS AND DISCUSSION 50
Relation of Composition and Heaviness of Oils to Insecticidal
and Ovicidal Efficiency 50
Results 50
Florida red scale studies 50
Citrus red mite studies 61
Discussion 71
Relation of Composition, Heaviness, and Refinement of Oil to
Phytotoxicity 77
Respiration and transpiration 77
Results 77
Discussion 84
Oil blotch, leaf drop, and fruit drop 88
Results 88
Discussion 92
Fruit color and ethylene degreening 96
Results 96
Discussion 99
Internal fruit quality 106
Results 106
Discussion 109
General Discussion 112
SUMMARY AND CONCLUSIONS 115
LITERATURE CITED 121
ADDITIONAL REFERENCES 130
BIOGRAPHICAL SKETCH 131
v


TABLE OF CONTENTS
Page
ACKNOWLEDGMENTS ii
LIST OF TABLES vi
LIST OF FIGURES viii
INTRODUCTION 1
LITERATURE REVIEW 3
Source and Properties of Petroleum Spray Oil 3
Historical Use of Spray Oil 5
Insecticidal and Ovicidal Action of Petroleum Oil 7
Phytotoxicity of Petroleum Oil.... 12
Penetration of oil into plants 12
Effects of oil on the physiological processes of plants 14
Injurious effects of oil sprays on citrus 17
Specifications for Plant Spray Oils 19
MATERIALS AND METHODS 23
Oil Specifications 23
Preparation of Oils 27
Application of Oils in Laboratory Studies 27
Oil Deposit Determination 32
Insecticidal and Ovicidal Efficiency Studies 34
Florida red scale studies 34
Infestation 34
Holding infested fruit 36
Scale development, treatment, and mortality counts 38
Testing the oils 40
Citrus red mite studies 41
Phytotoxicity Studies 43
Laboratory experiments 43
Respiration studies. 43
Transpiration study.... 45
Field experiments
46


42
fluorescent light. The fruit were supported on racks made of 0.5-inch
plywood and No. 8 finishing nails, as shown in Figure 5. Treatments
were applied on the third day after infestation and mortality rates
were determined 8 days later by counting the numbers hatched and not
hatched. The controls were sprayed with water in the same manner as
the treatment applications.
Representative oils from the 3 series of narrow-boiling fractions,
selected to cover the ranges of molecular weight, viscosity, and 50%
distillation point, were tested. Dosage-mortality relationships were
established by applying 7 to 10 concentrations of each oil. Each con
centration was applied to 5 egg-infested fruit in a randomized block
design. Thus each point on the dosage-mortality curves represents the
response of 400 to 500 eggs. Due to the problem of infesting a large
number of fruit with enough mite eggs of known age, it was not possible
to apply all concentrations of an oil on the same date. However,
dosages sufficient to establish the effective ranges were applied in
initial tests and subsequent tests were conducted under the same
environmental conditions to add supplementary points to the dosage-
mortality curves. The data were analyzed by probit analysis in the
same manner as were the Florida red scale data.
In Field Experiment No. 1, described below, residual control of
spider mites by 4 oils was determined. Spider mite counts were made 1,
4, and 7 weeks after spraying as follows: 25 leaves were picked from
each of 4 trees in a plot; eggs and active stages of mites on the 100
leaves were collected by brushing onto a rotating circular glass plate
(6 inches in diameter) covered with moistened glue; counts were made of
the eggs, immature stages, and adult females of both citrus red mite


36
wrapped firmly around the equatorial bands of the grapefruit with the
infested side of the leaf sections adjacent to the fruit surface. As
the leaf sections began to dry out, the scale crawlers migrated to the
surface of the grapefruit and settled in the equatorial area. The
fruit were checked periodically and when 200 to 300 crawlers had
transferred to the fruit, the strip of leaf sections was removed and
placed on another fruit. This period of infestation varied from under
24 hours up to 48 hours. The 48-hour limit was imposed to maintain a
maximum 2-day spread in age of the insects, since age has been found to
affect the response of scale insects to insecticidal treatments (22).
This level of infestation resulted in an average of about 100 third-
stage females per fruit at the time of treatment.
As the fruit became infested, they were transferred to a 24 x 24 x
2-inch wooden tray in an enclosed chamber for holding. The tray con
tained a 1.5-inch layer of wet vermiculite overlain with double-thick
ness cheesecloth (Figure 4).
Holding infested fruit.--It was necessary to hold large numbers of
detached grapefruit for 51 days in the laboratory. Attempts to hold
fruit in the absence of a water supply failed due to dehydration and
shriveling of the rind. This was alleviated by holding the fruit stem-
end down in moist vermiculite. By this method, dehydration was prevented
and approximately 907. of the fruit remained turgid throughout the hold
ing period. Another serious problem was that of a stem-end rot of the
fruit. This condition was alleviated by dipping the stem-end of each
fruit in a 57o thiourea solution immediately after harvesting and weekly
thereafter up to about 4 weeks. The number of fruit lost due to the
rot was reduced to less than 10%. These fruit were discarded as


Table 7--Continued
Dosage levels, high to low deposit
Oil
1
2
3
4
5
6
7
8
9
10
11
Hg/cm2
147
143
120
108
90
53
19
0
R-250
Eggs
464
448
477
477
404
438
490
463
-
-
-
% kill
64
63
51
42
36
18
14
3.2
-
-
-
l_ig/cm2
135
133
121
86
43
40
19
0
-
_
-
R-265
Eggs
485
444
460
396
459
424
476
463
- .
-
-
% kill
84
85
83
78
62
62
4
3.2
-
-
-
|ig/cm2
90
54
33
20
16
11
9
0
-
-
-
R-285
Eggs
394
385
475
461
352
464
488
463
-
-
-
% kill
99
97
98
89
74
28
6
3.2
-
-
-
M-g/cm
89
44
38
28
15
14
9
0
-
_
_
R-295
Eggs
514
437
448
488
508
460
458
463
-
-
-
% kill
98
99
97
96
90
76
28
3.2
-
-
-
(ig/cm2
94
64
42
22
17
16
14
6
2
0
_
R-305
Eggs
463
474
479
555
460
462
472
470
476
459
-
7o kill
96
100
99
96
95
82
85
45
24
2.1
-
M-g/ cm2
74
46
37
17
16
15
14
9
6
5
0
R-320
Eggs
408
544
474
602
435
467
474
467
488
440
461
% kill
100
100
100
98
98
98
85
77
64
60
2.6
p.g/cm2
74
40
33
19
16
14
11
7
4
0
_
R-365
Eggs
470
457
460
422
547
474
487
460
500
459
-
% kill
99
100
100
96
92
92
76
80
74
2.1
-
fig/cm2
107
99
93
87
54
21
0
-
-
-
-
N-250
Eggs
427
486
380
500
442
445
427
-
*
-
% kill
40
23
49
34
40
17
2.5
-
-
-
-
u>


Figure 11. Efficiency in relation to molecular weight for 3 series of narrow-boiling petroleum fractions
and 2 commercial oils against citrus red mite eggs.
00


INTRODUCTION
Petroleum oil is one of the most important pesticides used on
Florida citrus. It will control most species of scale insects, spider
mites, and the fungus disease greasy spot, caused by Cercospora citri-
grisea Fisher. Compared to most chemical pesticides, oil is economical
and safe for the user, has little adverse effect on biological control
agents, and its use creates no pesticidal residue problem. Because of
the physical mode of action of oil, development of resistance by the
above pests is unlikely. However, the use of oil is limited to a
short application period in June and July because of its adverse ef
fects on the citrus plant. Improper application of oil sprays may re
sult in fruit blemishes, excessive leaf and fruit drop, reduced fruit
set, poor fruit color and quality, and increased susceptibility of the
tree to cold weather injury.
Foliage-type spray oils are characterized by the physical proper
ties of viscosity, distillation range, and molecular weight, and the
chemical properties of unsulfonated residue, or refinement, and hydro
carbon composition. There are no recommended specifications for these
properties for oils used in Florida at present and a wide range of
materials are currently in use. Specifications for oils used on citrus
in California and on deciduous fruits in New York are well defined. In
recent years, some major oil companies have used specifications from
these states as guides in producing base oils for use on Florida cit
rus, mainly because no information was available to indicate different
1


19
Ziegler (110) noted 3 definite physiological responses of
'Valencia' sweet orange trees in Florida following applications on 12
May of an oil of 70 SSU viscosity and 83 UR at 1.66% concentration.
These were: 1) size of immature fruit was retarded, except where the
reduction of the crop was approximately proportional to reduction in
leaf area; 2) the number of fruit borne in the succeeding crop was re
duced, and 3) the subsequent flush of growth was accelerated. He con
cluded that the insecticidal and phytocidal properties of mineral oils
were closely correlated and applications of these must be timed to
allow maximum deposit without detrimental plant reaction and minimum
deposit for thorough pest control.
California workers (76, 77, 78, 79) reported successful use of
2,4-dichlorophenoxyacetic acid and 2,4,5-trichlorophenoxyacetic acid as
spray oil ammendments to counteract some of the adverse effect of oil.
Addition of 4 or 8 ppm 2,4-D to the oil spray mixture increased yield,
reduced both leaf and fruit drop, and had less effect on soluble solids
in grapefruit than oil alone; the 2,4-D had no apparent adverse effect
on trees other than some curling and distortion of young leaves.
Specifications for Plant Spray Oils
Five classes or grades of foliage spray oils are recommended for
citrus in California (24). These are based on the work of Gray and
DeOng (29), DeOng (18), DeOng et al. (19), and of Smith (72). Accord
ing to Ebeling (25), distillation range and per cent unsulfonated
residue are the most valuable criteria by which summer oils can be
standardized. The 5 recognized grades and identifying properties are
given in Table 1. Ebeling (25) pointed out that these standards do
not necessarily hold for oils applied to citrus in other states. He


34
Oil deposits on leaves of sprayed potted plants were determined in
the same manner as described above for fruit. Either 2 leaves selected
at random from each of 5 treated plants or 10 leaves from a single
plant constituted a deposit sample. Each leaf was carefully removed
from the plant with forceps and scissors, and held over the funnel for
stripping. Approximately 5 ml of solvent were sufficient for washing
the oil from both sides of the leaf. The leaves were traced on paper
and measured with a planimeter. The area was doubled to account for
both leaf surfaces.
Insecticidal and Ovicidal Efficiency Studies
Florida red scale studies
The insecticidal efficiency of the oils was studied using adult
female Florida red scale as the test insect. A natural infestation of
this species on English ivy, Heder sp., was the source of test materi
al. Crawlers from these scales were used to infest nearly-mature
grapefruit in the laboratory. These scales were allowed to grow to the
early third stage at which time treatments were applied to the infested
grapefruit.
Infestation.--Laboratory infestations were obtained as follows
(Figure 3): ivy leaves heavily infested with crawler-producing red
scale were picked, brought into the laboratory, and cut into small sec
tions, each section bearing several female scales. Five to eight of
these leaf sections were stapled.between 2 strips of cheesecloth
measuring 1.5 x 14 inches. Nearly-mature grapefruit were harvested,
brought to the laboratory, washed, and then placed stem-end down on
2.5-inch diameter juice cans filled with wet vermiculite, where they
remained throughout the infestation period. The prepared strips were


48
degreening and fruit quality. Treatments were applied with a high-
pressure sprayer and a double-nozzle hand gun. The plastic shield was
used to protect adjacent trees from spray drift as in the above experi
ment. Fruit samples were harvested on 16 October, 1 and 12 November,
and 7 December, or approximately 4, 6, 8, and 12 weeks after treatment.
The samples consisted of 40 fruit from each 4-tree plot. Where possi
ble, the fruit were picked from the outside canopy of the tree at a
height of 3 to 6 feet and both very large and very small fruit were
avoided. However, due to limited quantity of fruit on some trees, some
of the sampling, especially the fourth sample, was done without regard
to fruit size or location on the tree, both of which are recognized
sources of error, especially for fruit quality (69). Both the degreen
ing and fruit quality studies utilized the same fruit samples.
Color measurement and ethylene degreening.--The first and third
40-fruit samples were degreened for 72 hours with ethylene gas after
harvesting. A 4 x 4 x 4-foot degreening chamber was used and commer
cial recommendations on temperature, humidity and ethylene gas concen
tration were followed (32). Degreening rates were determined instru-
mentally, using the reflectance attachment of a Bausch and Lomb
"Spectronic 20" spectrophotometer (33) The amount of green color in
the peel was measured as per cent absorbance at 675 m|i. A 1-inch-
diameter circular area was randomly selected and marked on the equator
of each fruit and a color reading was taken in this circle after 0, 24,
48, and 72 hours degreening time. The degreening rate was indicated by
the decrease in absorbance from 1 reading to the next. Color measure
ments were taken 4 and 8 weeks after treatment. The coefficient of re
gression of per cent absorbance on degreening time was calculated for


Table 13. Leaf drop by young 'Hamlin' trees following application of oil sprays on 6 May 1964 in Block 23
£
Leaf drop, grams per 4-tree plot
Treatment
Plot,
4 trees
1st
week
2nd
week
3rd
week
4 th
week
5 th
week
Total
for 5
weeks
Total for
first
4 weeks
Check
1
38
81
64
110
286
579
293
2
55
90
126
108
313
692
379
3
47
82
165
53
194
541
347
4
42
91
95
163
319
710
391
Mean
45.5
a
86.0
a
112.5
a
108.5
a
278.0
b
630.5
a
352.5 a
R-60
1
617
407
181
140
256
1,601
1,345
2
370
90
177
100
273
1,010
737
3
865
531
172
95
236
1,899
1,663
4
219
385
205
49
311
1,169
858
Mean
517.8
b
353.2
ab
183.8
ab
96.0
a
269.0
b
1,419.8
ab
1,150.7 ab
P-96
1
769
819
212
224
72
2,096
2,024
2
946
814
313
96
84
2,253
2,169
3
1,334
983
526
168
136
3,147
3,011
4
1,201
727
210
68
68
2,274
2,206
Mean
1,062.5
c
835.8
c
315.2
be
139.0
ab
90.0
a
2,442.5
b
2,352.5 c


LIST OF FIGURES
Figure Page
1 Laboratory air-blast sprayer. A, high velocity blower;
B, motor; C, pump; D, spray tank; E, pressure regulator;
F, nozzle; G, deflector vanes; H, operating lever; I,
turntable 29
2 Spray coverage obtained on fruit with the laboratory air-
blast sprayer. A, fruit sprayed with oil at 1.0% concen
tration containing fluorescent dye to show the distribu
tion of the oil; B, unsprayed fruit. Photographed under
ultra-violet light. The rectangular area on fruit "A"
was left unsprayed to show the contrast between sprayed
and unsprayed surface 31
3 Method of infesting grapefruit with Florida red scale for
laboratory studies. A, ivy leaves with natural infesta
tion of crawler-producing female scales; B, cheesecloth
strip with infested leaf sections; C, strip of leaf
sections wrapped firmly in position around the equator
of a grapefruit to allow crawlers to transfer; D, typical
infestation obtained by this method, at time of treatment
application (4.5 weeks after infestation).. 35
4 Scale-infested grapefruit on moist vermiculite in holding
tray 37
5 Holding facilities for infested fruit in laboratory
studies. A, chamber for holding trays of scale-infested
grapefruit; B, racks supporting immature oranges in
fested with citrus red mite eggs 39
6 Regression of per cent kill on deposit level for 3 series
of narrow-boiling petroleum fractions tested against adult
female Florida red scale. The number on each line indi
cates the average molecular weight of the fraction 54
7 Efficiency in relation to molecular weight for 3 series of
narrow-boiling petroleum fractions against adult female
Florida red scale 55
8 Efficiency in relation to viscosity for 3 series of narrow
boiling petroleum fractions against adult female Florida
red scale 56
viii


PER CENT TOTAL SOLUBLE SOLIDS
108
16 1 12 7
October November December
DATE OF HARVEST
Figure 20. Effect of 4 oils on soluble solids development in 'Hamlin'
oranges. Sprays applied 18 September 1964.


38
detected and were never included.in the treatments. Where the rot set
in after treatment, its advancement was observed and if the affected
area extended into the scale-infested equatorial area before the sched
uled time for mortality counts, the scales were counted early to avoid
loss of a treatment replication. These early counts were within 4 to 7
days of the scheduled mortality counts and the results did not differ
markedly from the other replicates of the same treatment.
The infested grapefruit were held in a chamber made of 2 x 4-inch
wood framing, enclosed on the sides with translucent polyethylene
sheeting, but open at the top and bottom for ventilation (Figure 5).
The size of the chamber measured 8.5 x 2 x 7 feet in width, depth, and
height, respectively. Six shelves, spaced 12 inches apart, vertically,
starting 18 inches above floor-level, accommodated 24 trays. Each tray
held a maximum of 36 medium-size grapefruit, with adequate clearance
between fruit. Conditions inside the chamber were maintained at 78 +
4 F and 70% + 5% relative humidity. Lighting, in alternating 12-hour
light and dark periods, in phase with the diurnal cycle, was provided by
six 48-inch, 40-watt "daylight!1 fluorescent bulbs hanging vertically on a
wall immediately behind the chamber, and overhead room lights of the
same type in front of the chamber. Diffusion of the light by the
translucent polyethylene sheeting resulted in fairly uniform distribu
tion of the light inside the chamber.
Scale development, treatment, and mortality counts.--Treatments
were applied when the female scales reached the early third stage of
development. Under the conditions of this work, the insects required
approximately 4.5 weeks to reach this stage. Treatments were scheduled
32 to 33 days from the date of infestation and mortality counts were


30
the line of stagnant liquid. A stop watch was used for timing the
spraying interval. As the timer-hand approached the starting time, the
blower was turned on to build up speed. When the timer-hand reached
the starting point, the operating lever was raised, thereby opening the
valve and injecting the spray into the air blast released simultaneous
ly by a baffle plate on the end of the lever. At the end of the spray
ing interval, both liquid and air were stopped instantly by reverse
action of the lever.
Uniform coverage was obtained and the spray was applied just to
the point of runoff by spraying fruit for 3 revolutions, or 12.3 sec,
and potted plants for 4 revolutions, or 16.4 sec. Plants were sprayed
individually by placing the container directly in the center of the
turntable. Individual fruit were placed stem-end up on a tripod at the
center of the turntable, in which position the sides of the fruit re
ceived a uniform coverage of spray droplets (Figure 2). No attempt was
made to spray the ends of the fruit because both mortality counts and
oil deposit determinations were made only on the equatorial area of the
fruit. Generally, 8 fruit were sprayed from each 4,000-ml tank of
spray. Five infested fruit served as replicates for each treatment,
and 3 fruit, occupying positions 1, 4, and 7 in the spraying sequence,
were used for deposit determinations. Two shallow grooves were cut
around each deposit fruit before spraying to define the equatorial area
on which the deposit was to be measured.
Oil deposits obtained on fruit surfaces with the laboratory
sprayer were in direct linear relationship to the oil concentration in
the spray. The coefficient for regression of deposit (pg/cm^) on con
centration (as per cent oil in the spray) was 0.6732 x 100 with a 95%


Table 12--Continued
Transpiration rate of oil sprayed plants as per cent of check3
Days from Water loss Paraffinic oils Naphthenic oils
treatment from check3
in mg/cm2 P-285 P-320 P-365 N-285 N-320 N-365
17
35.1
ab
94.5
ab
60.8
b
73.1
b
120.3
a
100.6
ab
70.2
b
18
29.4
ab
91.7
abc
51.0
d
70.9
cd
115.0
a
85.8
be
59.1
d
19
18.2
a
87.3
a
61.5
b
62.6
b
95.7
a
84.0
a
56.6
b
20
22.9
a
84.0
ab
64.6
b
66.7
b
95.6
a
87.6
ab
66.2
b
21
18.9
a
87.2
a
60.8
c
63.9
c
95.6
a
82.3
ab
69.0
be
25
18.2
ab
92.3
ab
55.3
c
68.3
be
112.8
a
84.0
abc
58.4
c
26
11.5
abc
130.9
a
67.0
c
81.0
be
134.5
a
104.6
ab
68.0
c
32
29.2
b
101.9
ab
64.9
c
56.0
c
126.2
a
104.6
ab
58.4
c
33
18.8
a
79.6
b
60.3
c
59.6
c
100.9
a
82.7
a
63.0
be
34
10.5
a
80.4
be
66.8
c
74.1
c
95.7
ab
79.0
c
70.6
c
35
15.5
a
80.3
be
68.4
cd
68.4
cd
90.6
ab
81.0
be
62.2
d
53
16.7
ab
96.2
ab
71.8
b
75.8
b
124.0
a
83.7
b
75.8
b
54
20.3
b
106.9
b
73.0
b
73.1
b
154.5
a
100.7
b
76.6
b
60
11.9
be
96.0
be
69.8
c
69.6
c
149.3
a
110.7
b
69.8
c
61
19.9
ab
84.2
be
74.2
be
59.0
c
122.0
a
91.5
abc
62.6
c
62
16.4
ab
87.5
ab
69.4
b
69.7
b
109.5
a
104.3
a
69.3
b
67
17.3
be
98.7
be
73.8
cd
71.1
d
127.9
a
106 .7
ab
70.1
d
68
18.1
ab
79.9
be
55.7
cd
49.1
d
112.9
a
97.2
ab
43.1
d
69
17.6
b
88.7
be
75.7
cd
66.9
cd
123.2
a
107.3
ab
59.1
d
70
17.5
a
87.7
ab
63.0
be
50.8
c
109.4
a
96.5
a
51.6
c
aFigures in the table are means of 5 replications. Treatment means for a given day which are followed by
the same letter are not significantly different at the 57 level according to Duncan's New Multiple Range
Test. (Analyses of variance were run on daily water loss in mg/cm2; means converted to per cent of
check for presentation.)


Figure 13. Efficiency in relation to 50% distillation point for 3 series of narrow-boiling petroleum
fractions and 2 commercial oils against citrus red mite eggs.


87
and 2) paraffinic: 646 F, 715 F, and 752 F, respectively.
Distillation range should be stressed because of its relation to
the volatility of an oil. Because of this relationship, the dissipation
rate of oil deposits from citrus leaves and fruit should be inversely
related to the distillation temperatures of the oil. The importance of
oil evaporation rate with respect to insect control was discussed ear
lier. Apparently, the adverse effect of oils on the physiological
processes of citrus trees is closely associated with endurance of the
oil deposit. Thus, insecticidal and phytotoxic properties of oils are
closely related.
The transpiration measurements made in this study are probably
most important as indicators of the endurance of oil deposits and of the
depressive effect on the other processes discussed--respiration and
photosynthesis. Riehl and Wedding (57) showed that the reduction of
these processes was due to physical interference with gaseous exchange
caused by the presence of the spray oil in the tissue and not to death
of the cells. The principal effects occurred in the tissue of the leaf
marked by the dark discoloration known as oil-soaking. Tests with
tetrazolium showed the cells of the discolored tissue were not killed.
Recovery of physiological processes accompanied dissipation of the oil
deposit. Inspection of the response curves for the 285-mol wt paraf
finic and the 320-mol wt naphthenic fractions in Figures 14 and 15,
reveals striking similarity in the recovery patterns after the tenth
day. Assuming that this pattern of response is intermediate between
temporary and prolonged physiological effects on the citrus plant, the
distillation temperatures of these 2 oils offer a reasonable approach
to the selection of an optimum distillation range with respect to plant


18
Numerous workers (66, 68, 80, 82, 89, 100) reported retardation of
the degreening rate of oil-sprayed citrus fruit. But the author found
no report of studies having been made of the relation of oil properties
to effect on fruit color, except that an 80-SSU oil retarded color
development less than did a 95-SSU oil (100).
A grade-lowering fruit blemish, referred to as "oil blotch," is
associated with oil sprays applied in Florida when the fruit is between
0.75 and 1.50 inches in diameter. Thompson (85) described the con
dition as being round in shape, varying from light to dark brown in
color, and of a superficial nature; but it was a definite grade-lower
ing blemish.
Thompson et al. (87) reported more than twice the amount of dead
wood in oil-sprayed sweet orange trees than in either parathion-sprayed
or unsprayed trees. Oil-sprayed tangerine trees dropped 10 times as
many leaves following a February application as did those receiving
parathion sprays. Thompson (92) found the greatest leaf drop to occur
when oil applications were made just prior to, or during, the time of
normal shedding of old or weak leaves and concluded that while oil
sprays are the most common cause of leaf drop, tree condition apparent
ly is a factor where excessive drop occurs. Thompson (84) reported no
difference in leaf drop or shock to the tree with oils of 72 to 100 SSU
viscosity or oils of low and high refinement. However, Ebeling (24)
reported heavy leaf drop following application of 2.07 heavy oil of 86
UR, and decreasing drop with oils of 95 and 100 UR, respectively. He
stated that leaf drop constitutes a rather accurate index of the phy
totoxicity of an oil.


Table 1. Specifications for California spray oils3
Grade
Temperature, F, for
distillation of:
5% 507o 907o
Per cent
distilled
at 636 F
Minimum unsul-
fonated residue
Light
555
617
675
66.2
90
Light-medium
571
628
703
55.4
92
Medium
582
643
715
43.2
92
Heavy-medium
585
656
728
39.1
92
Heavy
612
671
727
18.0
94
aAfter Ebeling (25), p. 58, in part.


IZJ
T77/p
AGRI
CULTURAL
LIBRARY
UNIVERSITY OF FLORIDA
3 1262 08554 8500


Ill
The increase in soluble solids in the fruit during the maturation
period of citrus is directly dependent on the synthesis of the materi
als, mainly carbohydrates, by the leaves and subsequent translocation
to the fruit. Any limitations imposed on either the synthesis or
translocation of these products probably are reflected in the mature
fruit in the form of reduced solids content. It seems likely that re
duction in total functional leaf surface, resulting from excessive leaf
drop, and inhibition of photosynthesis in oil-sprayed leaves would both
be limiting factors in solids development in the fruit. Wedding et al.
(98) stated that the reduction of the soluble solids caused by oil
sprays is probably due to an interference with the net production of
photosynthate by the tree, or to a decrease in the translocation of
elaborated foods from the leaves to the fruit, or to a combination of
these factors. Wedding and Riehl (99) reported inhibition of phos
phorus translocation into leaves of oil-treated citrus plants and, on
the basis of reduced ash content of the leaves, concluded that inhibi
tion of translocation was general and non-specific. Knight et al.
(36) attributed starch build-up in oil-sprayed leaves to inhibition of
outward translocation of carbohydrates from the treated leaves.
Wedding and Riehl (99) stated the probability of physical interference
with the transport system, especially since the highly refined oils are
quite unreactive. They wrote:
"...it is probable that the effect on translocation comes
about through a physical interference with the transport
mechanism. This might be due to actual obstruction of the
vessels with oil but it seems more reasonable to assume
that the presence of oil partially disables translocation
by altering interfacial tensions within the protoplasm or
by changing the structure and molecular orientation of
transport pathways within the protoplasm by 'solubiliza
tion' in its lipid phases."


76
attained 957 kill of red scale at a much lower deposit level than for
citrus red mite eggs. Pearce and Chapman (44) observed this same dif
ference between cottony peach scale nymphs and eggs of both European
red mite and oriental fruit moth. They suggested that this difference
may be due to the differences between the respiratory systems of the
active insect and the mite egg.
Correlations between efficiency and 507 distillation temperature
for both test species are depicted in Figures 9 and 13. Very little
difference was shown between the paraffinic and naphthenic types.
Chapman et al. (9) stated that distillation range is the single most
useful physical property for specifying a spray oil since this is most
directly related to the volatility of the material. The results ob
tained here suggest that naphthenic oils may be equally as efficient as
paraffinic oils if compared on the basis of distillation temperature
rather than viscosity or molecular weight.
Comparison of the 3 series of oils tested in these laboratory
o
studies at the LD^ values of 30 and 70 pg/cnr for citrus red mite eggs
and Florida red scale, respectively, has much practical significance.
The recommended rates of oil applied for spider mites and scale insects
on Florida citrus are 0.77o and 1.370, respectively. With standard field
application procedures, sprays containing these oil concentrations de-
2
posit in the neighborhood of 30 and 70 pg/cm respectively. Therefore,
the correlations made between these maximum efficient deposits and the
physical property values may indicate that the use of oils lighter than
those presently used on Florida citrus is feasible, in which case some
of the phytotoxicity problems discussed in the following section may be
alleviated. However, it is often difficult to obtain uniform


110
relatively small trees at the time of the third sampling prevented
selection of the fruit with regard to fruit size and location on the
tree, both of which are recognized (69) sources of error in sampling
for fruit quality. However, this fruit supply limitation existed in
the plots treated with the other oils as well.
The adverse effect of oil sprays on citrus fruit quality has re
ceived much attention in both Florida (34, 67, 83, 89, 91) and
California (51, 52, 53, 54, 66). The work in Florida has dealt mainly
with timing of application without particular attention to the heavi
ness of the oil. Thompson and Sites (83) used both 72-SSU and 100-SSU
oils in their experiments dealing with the timing of oil sprays. It
is unlikely that beyond 70-SSU viscosity differences would occur with
increase in oil heaviness. But the results discussed above indicate
that oils lighter than 70 SSU might well have less adverse effect on
fruit quality than the heavier oils. However, Riehl et al. (51) found
no relationship between the molecular weight gradient of petroleum
fractions in the range 200 to 350 and the effect of the oil on solids
and acid in juice of 'Valencia' oranges in California, almost 1 year
after spraying. Apparently the adverse effect of oil on solids is
more prolonged under California conditions than under Florida condi
tions, because Thompson and Sites (83) reported very little adverse
effect on solids of early, midseason, and late varieties of sweet
oranges by oil sprays applied in June or July in Florida. The timing
experiments of Thompson and Sites (83) and the results obtained in the
present work suggest that the lighter, more volatile oils would have
less adverse effect on fruit quality in Florida than the heavier oils
which dissipate more slowly.


67
iJ
M
H
¡S
PJ
U
Pi
w
PM
fn
O
PQ
§
PM
Cfl
O
O
w
w
H
S
Q
3
C/3
§
H
M
U
Pm
O
J
tJ
w
>£
99
98
95
90
80
70
50
30
15
P3
o
Pi
w
PM
Figure 10. Regression of per cent kill on deposit level for 3 series
of narrow-boiling petroleum fractions tested against citrus red mite
eggs. The number on each line indicates the average molecular
weight of the fraction. The solid portion of each line indicates
the range of data collected; the broken extension is extrapolation
to the 50 or 95% kill level.


37
Figure 4. Scale-infested grapefruit on moist vermiculite in holding
tray.


113
light oils have been highly successful in controlling insect and mite
pests very similar to those affecting citrus in this state. The light-
medium and medium grades (Table 1) of naphthenic oils widely used in
California are approximately equivalent to 50- to 57-SSU paraffinic
oils in distillation and volatility. If oils in this viscosity range
can be used effectively in the pest control program on Florida citrus,
the results obtained in these studies indicate that some of the phyto
toxic effects of oil would be alleviated. However, the residual pesti-
cidal effectiveness of these lighter oils might not be as good as that
of the 70- to 80-SSU oils currently used. This brings up the question
of seasonal timing of applications with respect to oil heaviness to ob
tain the most effective pest control with minimum adverse effect to the
tree. In early-season application, up to 15 July, when residual control
is of greatest importance, oils of approximately 70 viscosity might
exert sufficient residual control to carry over to the fall miticide
spray. Thompson and Sites (83) showed that applications of oils of 72
to 100 SSU had little adverse effect on fruit quality when applied be
fore 1 August. After 15 July, the lighter, more volatile oils probably
would give effective pest control up to the time of the fall spray
applications, with minimum phytotoxic effects, especially on early
varieties. Applications of the lightest effective oils after 1 August
might be feasible.
Current recommendations caution growers against applying oil
sprays after 1 August. The results of the fruit quality study dis
cussed above showed that the reduction of solids by the 60-SSU oil was
overcome in 8 weeks after spraying. This indicates the possibility of
applying these lighter oils up to 15 August or later without appreciable


124
41. Oberle, G. D., G. W. Pearce, P. J. Chapman, and A. W. Avens.
1944. Some physiological responses of deciduous fruit trees
to petroleum oil sprays. Proc. Amer. Soc. Hort. Sci. 45:
119-130.
42. Pearce, G. W., P. J. Chapman, and A. W. Avens. 1942. Efficiency
of dormant type oils in relation to their composition. J.
Econ. Entomol. 35(2):211-220.
43. Pearce, G. W., P. J. Chapman, and D. E. H. Frear. 1948. In
secticidal efficiency of saturated petroleum fractions. Ind.
Eng. Chem. 40(2):284-293 .
44. Pearce, G. W., and P. J. Chapman. 1952. Insecticidal efficiency
of petroleum fractions and synthetic isoparaffins. J[n Agri
cultural applications of petroleum products. Amer. Chem. Soc.,
Washington, D. C. Advances in Chem. Ser. 7:12-14.
45. Rhoads, W. A., and R. T. Wedding. 1953. Leaf drop in citrus.
California Agr. 7(10):9.
46. Riedhart, J. M. 1961. Influence of petroleum oils on photo
synthesis of banana leaves. Trop. Agr. Trinidad. 38(1):23-27.
47. Riehl, L. A., and J. P. LaDue. 1952. Evaluation of petroleum
fractions against California red scale and citrus red mite.
In Agricultural application of petroleum products. Amer. Chem.
Soc., Washington, D. C. Advances in Chem. Ser. 7:25-36.
48. Riehl, L. A., and G. E. Carman. 1953. Narrow-cut petroleum
fractions of naphthenic and paraffinic composition for control
of California red scale. J. Econ. Entomol. 46(6):1007-1013.
49. Riehl, L. A., and L. R. Jeppson. 1953. Narrow-cut petroleum
fractions of naphthenic and paraffinic composition for control
of citrus red mite and citrus bud mite. J. Econ. Entomol. 46
(6):1014-1020.
50. Riehl, L. A., F. A. Gunther and R. L. Beier. 1953. Application
of precision photoelectric colorimeter to determination of oil
deposit on laboratory-sprayed grapefruit. J. Econ. Entomol.
46(5):743-750.
51. Riehl, L. A., E. T. Bartholomew, and J. P. LaDue. 1954. Effects
of narrow-cut petroleum fractions of naphthenic and paraffinic
composition on leaf drop and fruit juice quality of citrus. J.
Econ. Entomol. 47(1): 107-113.
52. Riehl, L. A., R. T. Wedding, and J. R. Rodriguez. 1956. Effect
of oil spray application timing on juice quality, yield, and
size of Valencia oranges in a southern California orchard. J.
Econ. Entomol. 49(3):376-382.


103
early oranges. They also indicate that the extent of the effect might
be related to oil heaviness. That all 4 oils delayed degreening on
the tree is evident from the significance tests of the color readings
taken before ethylene degreening (zero hours), both 4 and 8 weeks after
spraying. The data for the 8-week sampling indicates that color de
velopment was retarded more by the low-UR oil and the high-viscosity
oil than by the other treatments. The effect of the oils on the rate
of degreening with ethylene is shown by the data for 24, 48, and 72
hours degreening time. Considering the 4-week sample, differences
between oils were detected after 24 hours; these differences were
accentuated at the 48- and 72-hour readings. Inspection of the re
gression coefficients in Table 16 for the 4-week samples reveals that
the fruit sprayed with 3 of the oils degreened at a slower rate
than did the check; the rate for the fruit sprayed with the heavy oil
was significantly lower than that of the check. It is noticed that the
regression coefficient for the medium oil, P-96, is slightly, but not
significantly, higher than that of the check. However, it should be
pointed out again that due to faulty application of this treatment, it
is not known what the actual oil deposit was relative to the other
treatments.
The data in Table 15 for the 8-week sample show that the initial
on-tree differences in color of the oil-treated fruit were rapidly
overcome by ethylene degreening. Although color differences between
check and treated fruit remained significant through 72 hours degreen
ing, except the light-oil samples which were not significant from the
check after 72 hours, no differences were detected between oils. How
ever, the mean color readings favor the light oil, R-60, for least


58
values. The relative efficiency of the 3 series, in decreasing order,
was reformed, paraffinic, and naphthenic. Efficiency increased with
heaviness up to a point, after which the trend reversed. The points of
maximum efficiency of the 3 physical properties considered for the dif
ferent types of oil were:
1) Molecular weight--paraffinic, 305; reformed, 305; and
naphthenic, 320.
2) Viscosity, SSU at 100 F--paraffinic, 59.8; reformed,
59.3; and naphthenic, 79.7.
3) Fifty per cent distillation point--paraffinic, 696 F;
reformed, 700 F; and naphthenic, 689 F.
o
A practical deposit level of 70 p,g/cnr was selected as the maximum
deposit for efficient kill of scale insects. The following minimum
physical property values were derived by this criterion from the curves
in Figures 7, 8, and 9:
1) Molecular weight--reformed, 279; paraffinic, 291; and
naphthenic, 300.
2) Viscosity, SSU at 100 F--reformed, 51; paraffinic, 53;
and naphthenic, 66.
3) Fifty per cent distillation point--reformed, 644 F;
naphthenic, 657 F; and paraffinic, 661 F.
Thirty commercial distillation range oils were compared at 0.5%
and 1.25% concentration. These oils represented 5 viscosity classes:
60, 70, 80, 90, and 100 SSU at 100 F. Oil deposit, corrected per cent
kill for each replicate, and mean per cent kill for the oils at each of
the 2 dosage levels appear in Table 6. Although arranged from high to
low kill in each viscosity class at the low dosage level, the data were
analyzed together. Therefore, the letters denoting significance apply
across all viscosity classes under a given dosage level. Levels of
kill were quite variable within each viscosity class at the 0.5% dosage


45
rates were measured 1, 3, and 7 days after treatment. The total C>2
consumption per sample during the 2-hour period was used to compare the
adjacent sprayed and unsprayed leaves. The differences between treated
and non-treated leaves were tested by the "t" test.
Transpiration study.--The effect of light (285 mol wt), medium
(320 mol wt) and heavy (365 mol wt) fractions of paraffinic and
naphthenic oils on the transpiration rate of treated 'Pineapple' seed
lings was determined by methods somewhat similar to those of Riehl
et al. (56). The plants were selected for uniformity in stem height
and number of fully expanded leaves. All but fully expanded leaves
were removed from each plant and additional new growth was removed as
it appeared so that the leaf surface area remained constant. Soil
moisture was equalized by bringing each container of soil to field ca
pacity and allowing 1 day for excess water to leach and drain off. The
weights of the plants and containers were then determined and these
weights were used as the initial weight thereafter. The containers
were placed in polyethylene freezer bags and sealed against evaporation
loss of soil moisture by gathering the top of the bag firmly around the
base of the plant and taping with masking tape. Transpirational water
loss was determined as the difference between successive weights of the
plants at 24-hour intervals, weighing to the nearest 0.1 g. The soil
moisture was replenished after each 50-g loss by transpiration. Pre
treatment determinations revealed a uniform transpiration rate varying
directly with number of leaves per plant. A randomized block experi
ment was set up with 7 treatments replicated 5 times. Blocking was
on the basis of leaves per plant and position on the laboratory table.
The oils were applied at 1.5% concentration in the dilute spray and


RESULTS AND DISCUSSION
Relation of Composition and Heaviness of Oils
to Insecticidal and Ovicidal Efficiency
Dosage-mortality tests were conducted for selected fractions of
the narrow-boiling paraffinic, reformed, and naphthenic series against
citrus red mite eggs and adult female Florida red scale, and 30 com
mercial-type oils were screened against Florida red scale, in the
laboratory. The properties of molecular weight, viscosity, 50% distil
lation point, and chemical composition or base-type (paraffinic, re
formed, or naphthenic) were studied with respect to control efficiency.
A field application of 4 commercial-type oils gave some information on
residual control of spider mites.
Results
Florida red scale studies.--Oil deposit, total number of scales,
and per cent kill for each dosage level of the oils used in the dosage-
mortality tests against Florida red scale adults are listed in Table 4.
The LD50 and LDg^ values, their 95% confidence intervals, and slopes of
the regression lines as obtained by probit analysis are presented in
Table 5. The probit regression lines in Figure 6 show the dosage-
mortality relationships of the various fractions in each series. The
relationship of oil heaviness to efficiency in kill is depicted in
Figures 7, 8, and 9, where LDg^ values are plotted, according to chemi
cal composition, against molecular weight, viscosity, and 50% distilla
tion point, respectively. Efficiency varies inversely with the LD95
50


47
fruit were picked from each 4-tree plot immediately after spraying.
The oil was removed by dipping each fruit or leaf in 2 successive
dioxane washes. After the sample was collected,the 2 washes were com
bined for the spectrophotometer reading. Leaf areas were determined as
previously described, but the surface areas of the fruit were measured
by the method of Turrell (95) The major and minor axes of each fruit
were measured and the corresponding surface area was obtained from a
prepared table.
Field Experiment No. 1; oil blotch, leaf drop, and fruit drop.--
The first experiment was applied on 6 May 1964, during the time the
fruit sizes were in the range of 0.75 to 1.50 inches in diameter. The
object was to induce oil blotch and to relate oil type to the incidence
of the condition. Diameter measurements of 15 fruit on each of 40
trees averaged 2.57 cm, or approximately 1 inch. Treatments were ap
plied with a "Speed Sprayer" Model 705 CP air-blast sprayer traveling
at 1 mph. A large plastic shield was used to protect adjacent trees
from the spray drift.
The fruit were checked periodically on the tree for oil blotch.
For 5 weeks after spraying, the rates of fruit and leaf drop were de
termined weekly. An area under each tree, extending to about 1 foot be
yond the drip line, was raked clean after spraying. One week later, and
weekly thereafter up to the fifth week, the dropped leaves and fruit
were collected. The fruit were counted but the leaves were weighed be
cause of the excessive amount of drop.
Field Experiment No. 2: fruit color and internal fruit quality.--
A late-season application of 4 oils was made on 18 September 1964, with
the objective of relating oil heaviness and refinement to effect on


43
and Texas citrus mite on one-fourth the surface of the plate. These
counts were multiplied by 4 to obtain an estimate of the total numbers
on the 100 leaves. This is the standard technique used by entomolo
gists at the Citrus Experiment Station in making spider mite counts in
miticide experiments.
Phytotoxicity Studies
Laboratory experiments
Studies were made to compare the effects of oils of different
molecular weight and base-type on the rates of respiration and transpi
ration of potted 'Pineapple' sweet orange seedlings. Simultaneously,
observations were made of any abnormal reactions by the plants to the
various treatments, such as leaf drop, leaf burn, and oil-soaking. The
plants used in these studies were grown from seed in the greenhouse.
Seedlings were transplanted from seed flats to 46-ounce juice cans 4 to
6 months after planting. The potting medium was a 3:1:1 mixture of
soil, peat, and vermiculite. The plants were approximately 1 year old
when used.
Respiration studies.--The rates of oxygen uptake by leaves of
'Pineapple' sweet orange seedlings, sprayed with light (305 mol wt) and
heavy (365 mol wt) fractions of both paraffinic and naphthenic oils,
were determined. The oils were applied at 1.5% concentration.
The plants were held both before and after treatment under green
house conditions with temperature fluctuation in the range of 60 to 90 F.
Six plants, selected for uniformity in size and appearance, were as
signed to each treatment. Five pairs of adjacent leaves were selected
on each plant and 1 of each pair was protected from the spray by
shielding with aluminum foil during the spraying operation. The


Table 15--Continued
Relative green color at 4 weeks
Per cent
Relative green color at 8 weeks
Per cent
Hours in
degreening
chamber
Treat
ment
Replicate^
pack-
out at
4 weeks
Replicate^
pack-
out at
8 weeks
1 2 3 4 Meane
1
2 3 4 Meane
Check
26.5
29.2
26.6
21.8
26.02
a
99.4
24.9
24.6
17.8
19.4
21.68
a
100.0
R- 60
36.2
37.6
30.5
30.1
33.60
b
95.0
22.7
26.2
29.2
24.6
25.64
ab
99.4
72
BR-2
41.3
35.4
36.4
28.8
35.47
be
89.4
29.4
29.1
23.6
26.5
27.16
b
99.4
P-96
35.9
29.9
23.4
25.5
28.67
a
98.1
30.0
26.2
29.2
24.6
27.46
b
100.0
BR-1
40.5
44.1
34.4
39.4
39.60
c
87.5
28.9
38.4
27.0
27.0
30.34
b
98.8
aPer cent absorbance at 675 m(j.; absorbance decreases as green color decreases.
^Sprays applied 18 September 1964; Block 23, Citrus Experiment Station,
c
Readings were made on the same fruit at 24-hour intervals.
^Each value is the average of readings from 40 fruit.
eTreatment means for a given degreening period followed by the same letter are not significantly differ
ent at the 57o level, according to Duncan's New Multiple Range Test.


41
the insects from group to group, it was necessary to apply the treat
ments over a period of 5 days. The data were corrected for natural
mortality by use of Abbott's (1) formula to equate for difference in
time of application. Natural mortality among the check groups varied
only from 2.3 to 6.5%. The results were expressed as corrected per
cent kill since the number of scales varied from fruit to fruit. Since
percentage data tend to be binomial in distribution (74), the corrected
per cent kill data were transformed by the arcsin transformation in
order that the assumptions of normality, additivity, and homogeneous
variance in the analysis of variance could be met. Analysis of vari
ance was run on the data and the significant differences between means
were determined by the Duncan Multiple Range Test (20).
Citrus red mite studies
The ovicidal properties of the oils were studied using eggs of
citrus red mite. Infestations of eggs were obtained on immature
'Valencia' oranges in the following manner. One day prior to use,
the fruit were harvested and washed, and the ends of each were coated
with paraffin to confine the oviposition activity of the mites to an
equatorial band of 1.0 to 1.5 inches, and to provide mite-free areas
for handling the fruit. Thirty to forty adult female mites were hand-
transferred to each fruit from plants growing in a greenhouse. After a
2-day oviposition period, the fruit were inspected under 15X magnifica
tion and approximately 100 eggs were marked for post-treatment identi
fication by encircling each with India ink. The infested fruit were
held before and after treatment under controlled conditions of 78 + 4 F,
65% + 10% relative humidity, and a 12-hour light period in phase with
the diurnal cycle. Lighting consisted of a mixture of natural and


72
Table 9. Spider mite counts at 1,4, and 7 weeks after application of spray
oils on 6 May 1964 in Block 23
Plot
Live
adult female
and young
mites
per 100 leaves per 4-
Treatment
(4 trees)
tree
plot3
Citrus red mite
Texas citrus
; mite
1st
4 th
7 th
1st
4 th
7 th
week
week
week
week
week
week
Check
1
24
260
272
284
2,656
28
2
20
236
532
172
2,204
48
3
24
288
456
140
3,828
36
4
0
168
708
80
1,044
28
Mean
17.0
a
238.0 a
492.0
a
169.0
a
2,433.0
a
35.0 b
R-60
1
4
32
76
112
1,180
84
2
4
48
136
116
500
88
3
0
36
184
116
124
88
4
0
92
212
100
728
76
Mean
2.0
b
52.0 b
152.0
b
111.0
ab
633.0
b
84.0 a
P-96
1
0
4
36
80
188
20
2
0
16
52
0
340
52
3
0
12
116
108
36
64
4
0
4
68
112
24
64
Mean
0.0
b
9.0 b
68.0
b
75.0
b
147.0
b
50.0 b
BR-1
1
12
8
36
28
160
32
2
4
4
44
28
168
16
3
0
32
32
48
88
12
4
4
8
68
124
76
56
Mean
5.0
b
13.0 b
45.0
b
57.0
b
123.0
b
29.0 b
BR-2
1
0
12
136
12
308
52
2
0
8
136
8
268
88
3
0
16
148
8
260
124
4
8
8
176
100
120
124
Mean
2.0
b
11.0 b
149.0
b
32.0
b
239.0
b
97.0 a
Total mites
for
each week
104
1
,292 3
,624
1
,776
14,300
1
,180
treatment means for a given week followed by the same letter are not sig
nificantly different at the 570 level according to Duncan's New Multiple
Range Test.


Figure 14. Effect of light, medium, and heavy paraffinic fractions on the transpiration rate of treated
'Pineapple' orange seedlings in relation to time after treatment. Shaded symbols indicate significance
from check.


101
HOURS DEGREENED
Figure 17. Degreening rate of oil-sprayed 'Hamlin' oranges 4 weeks
after spraying as indicated by decrease in per cent absorbance with
time in ethylene degreening chamber. Sprays applied 18 September
1964; fruit harvested 16 October 1964.


77
distribution of oil deposits over the entire citrus tree. In such
cases, the inhibition of crawler settling by the residual oil film be
comes the important aspect of scale control. The increased dissipation
rate of the lighter, more volatile oils, and consequent reduction in
residual effectiveness, may be the limiting factor in the use of oils
lighter than the 60 to 70 viscosity range.
Relation of Composition, Heaviness, and
Refinement of Oil to Phytotoxicity
Respiration and transpiration
Results.--Determinations of the respiratory rates of treated and
untreated leaves of 'Pineapple' seedlings were made 1, 3, 7, and 14
days after treatment with 305- and 365-mol wt fractions of paraffinic
and naphthenic oils. The mean of 6 determinations for each oil are
presented in Table 10. Analysis of variance of the data detected no
significant difference between treatments at the 5% level. In a
2
follow-up experiment, P-365, at 154 (ig/cm effected reduction in
uptake of 4.3%, 11.8%, and 16.0% on the first, third, and seventh days
after treatment, respectively (Table 11). The reduction on the third
and seventh days was highly significant.
The relationship of oil heaviness and composition to effect on the
transpiration rate of 'Pineapple' seedlings is shown by the data in
Table 12 and by Figures 14 and 15. The transpiration rate for the
check is given as mean water loss in mg/cm leaf surface per day; the
rates for the treated groups of plants are presented as per cent of the
check. Analysis of variance was run on the data in mg/cm^ per day, and
the means were converted to per cent of the check for presentation.


46
check plants were sprayed with water in the same manner as the treat
ment application. The plants were held in the laboratory at 78 + 4 F
and 60% + 107 relative humidity. Alternating 12 hours light and dark
prevailed. Illumination was provided by four 48-inch 40-watt "day
light" fluorescent bulbs placed 30 inches directly above the tops of
the plants.
Weighing was continued to 70 days after treatment application.
The difference between 2 successive 24-hour weighings was divided by
the total leaf area (considering only 1 side of the leaf since essen
tially all the stomata of citrus leaves are on the abaxial surface) to
obtain the rate in mg/cm^ per 24 hours. The data were analyzed in this
form.
Field experiments
Two experiments were conducted to obtain phytotoxicity data under
field conditions. Block No. 23 of the Citrus Experiment Station groves
was used for these studies. The trees were 'Hamlin' sweet orange on
rough lemon rootstock, 6 years of age, and 8 to 10 feet in height.
Five treatments, consisting of 4 oils and a check, were applied in a
randomized block design with 4 replicates of 4 trees each. Although
these young trees varied considerably in size and crop, the differences
were somewhat equated between treatments. Oils 31, 35, 36, and 38 of
Table 3 were used in both experiments and the second experiment uti
lized the same trees as did the first. The oils were applied at 1.57
concentration at approximately 5 gallons of spray per tree.
The oils were prepared as described earlier and oil deposits were
measured on both fruit and leaves by the same technique except for the
method of sampling and size of the samples. Twenty-four leaves and 24


10
concluded that structural composition and molecular weight of the oil
were the basic factors involved in efficiency in insect control.
The composition and heaviness of petroleum oil in relation to in
secticidal and ovicidal efficiency has been studied by several investi
gators (6, 15, 23, 42, 43, 44, 47, 48, 49, 55). Pearce et al. (43)
found that high paraffinicity and low content of aromatic structures
were related to kill of eggs of the fruit-tree leaf roller, Archips
argyrospilus (Walker). Chapman et al. (6) obtained similar results
with eggs of oriental fruit moth, codling moth, Carpocapsa pomonella
(L.), and eye-spotted bud moth, Spilonota ocellana (Denis and
SchiffermUller). Pearce and Chapman (44) further demonstrated the re
lationship between paraffinicity and efficiency against eggs of
oriental fruit moth and European red mite, Panonychus ulmi (Koch), and
against cottony peach scale, Pulvinaria amygdali Cockerell. Efficiency
also increased with viscosity and molecular weight up to a point. The
critical value in molecular weight was 320. The maximum efficiency in
relation to viscosity was obtained at about 50 SSU, 70 SSU, and 90 SSU
for isoparaffinic, paraffinic, and naphthenic types, respectively.
Riehl and LaDue (47) found definite correlation of oil viscosity
and molecular weight to efficiency in control of California red scale
adults and citrus red mite eggs. They found paraffinic oils superior
to naphthenic oils and concluded that efficiency of spray oils against
citrus pests may be considerably improved by proper selection with
respect to structural character and molecular size. These conclusions
were strengthened by the work of Riehl and Carmen (48) and Riehl and
Jeppson (49). Insecticidal efficiency increased with molecular weight
in the range 220 to 360. Maximum efficiency for highly paraffinic


32
confidence interval for slope of 0.6237 to 0.7227. This was computed
from data for 8 oils of 3 types applied on 4 different days. Regres
sions for the individual oils were very close to the 8-oil average,
with slopes within the range 0.64 to 0.72. One per cent oil emulsion
usually deposited 66 to 76 pg/cnr on the equatorial area of fruit.
Similar deposit levels were obtained on plants.
Oil Deposit Determination
Oil deposits obtained on sprayed fruit and leaf surfaces were
measured spectrophotometrically by the method of Riehl et al. (50),
with modifications. The dyed oil was removed from the sprayed surface
by solvent-stripping with dioxane (1,4-diethylene dioxide). The dye
content of the strip solution was determined and used to calculate the
total amount of oil recovered.
A Beckman Model DB spectrophotometer, with a 40-mm rectangular cell,
was used. Readings were taken at 524 mp, the wavelength of maximum
absorbance for Oil Red A in dioxane. A series of standards of known
concentrations of the dye in dioxane was prepared and used to determine
the regression of dye concentration on per cent absorbance. The re
gression coefficient (0.3093) was subsequently used to calculate the
dye content of solutions of unknown dye concentration.
The dye content of each oil was determined by weighing triplicate
samples (about 15 to 20 mg) to the nearest 0.1 mg on an analytical
balance, diluting each sample with dioxane to 25 or 50 ml (depending on
the weight and relative dye concentration of the sample), and reading
the per cent absorbance in the spectrophotometer. The per cent dye in
each oil sample was calculated by the following equation:


118
rate and internal quality of fruit. Degreening rates were measured
instrumentally and fruit quality determinations were made by standard
methods. Fruit samples were harvested approximately 4, 6, 8, and 12
weeks after spraying.
Degreening rates were determined for the 4- and 8-week samples by
measuring the color of the fruit after 0, 24, 48, and 72 hours of
ethylene degreening. Fruit from oil-sprayed plots were significantly
greener than the check fruit at the time of harvest and after degreen
ing at both 4 and 8 weeks after treatment. At 4 weeks, the check fruit
degreened at a significantly higher rate than the treated fruit. How
ever, fruit sprayed with the light oils degreened at a significantly
faster rate than those treated with the heavy oils, and these differ
ences were reflected in per cent pack-out of the fruit after 72 hours
degreening.
At 8 weeks after spraying, fruit from the oil-sprayed plots were
still significantly greener than those from the check plots and the
fruit treated with the heavy oil were significantly greener than those
treated with the light oils. Fruit treated with the heavy oil showed
no on-tree color break between the fourth and eighth weeks. However,
the rates of degreening with ethylene gas at 8 weeks were greater for
the oil-sprayed fruit than for the check fruit. Although the degreen
ing rates were faster for the oil-sprayed fruit, the rates were not
sufficiently greater to overcome the on-tree color differences. All
treated fruit, except that from the light-oil plots, was significantly
greener after 72 hours degreening than the check fruit. However, these
differences were not reflected in per cent pack-out. The over-all ad
verse effect of the oils was less with the light oil than with the heavy
oil.


4
oil on up is conducted under vacuum to avoid heating above 750 F, at
which temperature decomposition, or cracking, occurs (24).
After distillation, the various cuts must be refined to remove un
desirable substances. Kerosene, spray oils, and lubricating oils are
refined by essentially the same methods. The once common sulfuric acid
treatment has given way in recent years to a process employing sulfur
dioxide, known as the Edeleanu process. The oil and sulfur dioxide gas
are mixed in a pressure system and cooled to obtain 2 layers: 1) the
extract (lower layer), containing aromatic and other unsaturated hydro
carbons dissolved in the liquid sulfur dioxide; and 2) the raffinate
(upper layer), consisting of sulfur dioxide dissolved in the remaining
hydrocarbons. The raffinate yields the refined oil and the extract
becomes a source of industrial solvents. The sulfuric acid process
functions chemically while the sulfur dioxide method is a physical
process, its action being that of solvent extraction. Other solvent
extraction processes are now in use: nitrobenzene, Chlorax, phenol,
furfural, and Duosol. Spray oils require further refinement with sul
furic acid after the usual treatment given the lubricating oils. The
oil is treated with hot sulfuric acid which has the combined properties
of strong acid, drying agent, and oxidizing agent. Hence, the sul-
fonation process removes all but the most inert substances. The com
pounds removed are: 1) unsaturated hydrocarbons (both straight chain
and aromatic); 2) oxygen compounds (e.g., phenols and naphthenic acids);
3) sulfur compounds (e.g., mercaptans, pentamethylene sulfides, and
thiophene); and 4) nitrogen compounds (e.g., quinoline). That part of
the oil not reacting with the sulfuric acid, the saturated hydrocarbons,
is known as the unsulfonated residue, or UR. Hence the UR of an oil is


Table 15.
Color3 of oil-sprayed 'Hamlin' oranges before and after different intervals of ethylene
degreening and per cent pack-out at 4 and 8 weeks after sprayingb>c
Hours in
degreening
chamber
0
24
48
Relative green color at 4 weeks
Per cent
Relative green color at 8 weeks
Per cent
Replicate^
Tvoaf--
pack-
out at
4 weeks
Replicate^
pack-
out at
8 weeks
ment 1234 Meane
1
2 3 4 Meane
Check
85.0
88.0
84.9
84.9
85.70
a
-
81.6
77.7
72.8
70.1
75.57
a
-
R-60
94.7
94.7
88.4
87.6
91.35
b
-
83.2
88.8
83.3
78.7
83.47
b
-
BR-2
95.5
92.8
89.7
90.4
92.10
b
-
91.8
91.1
79.3
81.0
85.81
be
-
P-96
92.7
91.7
87.6
86.8
89.70
b
-
84.3
87.8
78.8
75.4
81.56
b
-
BR-1
91.4
92.4
89.7
88.2
90.42
b
-
92.7
$8.0
83.0
79.8
88.40
c
-
Check
65.6
63.1
59.3
61.7
62.42
a
_
59.6
56.1
54.5
56.0
56.54
a
_
R-60
70.2
72.0
66.4
65.0
68.40
be
-
64.0
69.4
70.4
65.2
67.25
b
-
BR-2
72.3
69.9
70.1
65.3
69.40
c
-
71.7
70.0
63.9
69.7
68.82
b
-
P-96
69.7
68.7
63.4
61.9
65.92
b
-
69.2
72.9
67.2
59.9
67.30
b
-
BR-1
71.0
72.1
66.0
65.4
68.62
c
-
72.4
77.2
67.7
70.9
72.03
b
-
Check
38.0
40.6
35.2
34.5
37.07
a
_
36.4
35.3
28.1
29.5
32.30
a
_
R-60
47.7
48.2
43.6
42.7
45.55
c
-
35.8
40.9
43.4
37.4
39.40
b
-
BR-2
51.7
46.0
48.0
42.1
46.95
cd
-
44.2
42.8
34.7
41.1
40.69
b
-
P-96
47.8
42.9
36.2
38.0
41.22
b
-
42.1
45.7
38.7
30.6
39.28
b
-
BR-1
49.8
53.1
46.4
48.6
49.47
d
-
43.7
52.5
40.5
43.1
44.94
b
-
vO


119
Internal fruit quality, as measured by per cent soluble solids in
the juice, was determined at all 4 sampling dates. All oils delayed
solids development to about the same extent up to 6 weeks after spray
ing. At 8 weeks, the solids content of the fruit sprayed with the heavy
oil was still significantly lower than that of the check fruit but the
fruit from the light-oil plots were not. By the twelfth week, no sig
nificant differences in solids were detected although the solids con
tent was still slightly lower in the sprayed than in the unsprayed
fruit. The unsprayed fruit and the fruit sprayed with the light,
highly-refined oil passed minimum legal maturity standards at an ear
lier date than did those treated with the heavy oil.
On the basis of the results obtained in the studies discussed
above, the following conclusions are drawn:
1) Relatively little difference exists in insecticidal efficiency
and phytotoxicity of oils of paraffinic and naphthenic composi
tion when compared on the basis of distillation temperatures
rather than viscosity or molecular weight.
2) The oils currently used in Florida fall in the effective and
efficient range of physical property values.
3) However, oils lighter than those currently used, in the vis
cosity range of 55 to 60 SSU, might be just as effective at the
normal rates of application.
4) The phytotoxic properties of highly refined petroleum oils are
closely related to the heaviness of the oil and endurance of
the oil deposit, and the extent and duration of phytotoxic
effects are inversely related to the volatility of the oil.


100
90
80
70
60
50
T
i'r
T
T
T
1 r^^-f
\
\
PARAFFINIC
REFORMED
NAPHTHENIC

620 640 660 680 700 720 740 760 830
50% DISTILLATION POINT, F
Efficiency in relation to 507 distillation point for 3 series of narrow-boiling
im fractions against adult female Florida red scale.
Ln


129
109. Young, P. A. 1941. Physiological and physical effects of spray
oils on deciduous trees. J. Econ. Entorno1. 34(6):838-844.
110. Ziegler, L. W. 1939. The physiological effects of mineral oils
on citrus. The Florida Entomol. 22(2):21-30.


Table 3--Continued
Oil
No
a
Name
Avg
mol
wt
Viscosity,
Chemical
d
composxtron
API
Temper ature, F,
for distillation
(760 mm Hg) of:
10-907,
SSU at UR,
100 FC %
di st"i 1 1 ati on
7oC .
A
%CN 7oCp
gravitye
107. 507, 907,
range, F
25
N-365
365
131.6
95.2
0.5
50.0
49.5
29.8
734
738
750
16
27
N-395
395
202.0
93.8
1.7
47.8
50.5
28.1
764
767
777
13
28
N-440
440
402.0
91.8
0.5
51.5
48.0
25.9
801
808
816
15
29
P-74
317
84.7
74.0
13.0
25.0
62.0
30.2
687
721
763
76
30
P-87
317
79.6
87.0
10.0
30.0
60.0
31.4
676
720
761
85
31
P-96
330
74.3
95.6
3.0
27.0
70.0
35.0
681
732
779
98
32
N-80
294
84.5
79.4
14.0
47.0
39.0
25.4
622
678
732
110
33
N- 84
294
83.9
84.0
12.6
47.4
40.0
25.9
632
681
732
100
34
N-95
305
74.2
95.2
2.0
51.0
47.0
30.5
623
680
732
109
35
BR-1
348
92.5
94.0
2.4
27.6
70.0
33.4
701
751
826
125
36
BR-2
297
71.7
85.0
13.6
26.4
60.0
29.6
637
688
774
137
37
BR-3
330
112.1
85.0
15.1
26.9
58.0
27.5
693
737
792
94
38
R-60
300
57.6
96.1
3.6
23.9
72.5
36.3
652
681
707
55
39
T-l
-
70.5
87.0
-
-
-
30.0
639
666
718
79
40
T-2
-
100.0
78.0
-
-
-
29.2
684
788
945
261
41
T-3
342
72.0
92.0
5.0
36.8
58.2
30.0


-

42
G-l
320
75.0
93.0
4.0
24.0
72.0
33.9
656
684
726
71
43
G-2
347
105.0
95.0
4.0
24.0
72.0
33.3
733
763
813
80
44
G-3
310
76.6
88.0
12.0
24.0
64.0
31.0
670
717
750
80
45
G-4
280
76.9
93.5
4.0
46.0
50.0
29.0
602
646
724
122
K>
Ln


Table 13--Continued
Treatment
Plot,
4 trees
Leaf
drop,
grams per
4-tree plot3
1st
week
2nd
week
3rd
week
4 th
week
5 th
week
Total
for 5
weeks
Total for
first
4 weeks
BR-1
1
385
682
185
249
293
1,794
1,501
2
440
452
83
142
219
1,336
1,117
3
618
666
229
242
87
1,842
1,755
4
894
774
337
291
151
2.447
2,296
Mean
584.2
b
643.5
be
208.5
abe
231.0 b
187.5 ab
1,854.8
b
1,667.2 be
BR-2
1
1,439
1,363
432
318
299
3,851
3,552
2
275
340
236
44
83
978
895
3
952
591
427
132
220
2,322
2,102
4
869
408
273
50
67
1,667
1,600
Mean
883.8
be
675.5
be
342.0
c
136.0 ab
167.2 ab
2,204.5
b
2,037.2 be
Total for
all treatments
12,375
10,376
4,648
2,842
3,967
a
Treatment means for a given week followed by the same letter are not significantly different at the 5%
level according to Duncan*s New Multiple Range Test,
o


Figure Page
9 Efficiency in relation to 50% distillation point for 3
series of narrow-boiling petroleum fractions against
adult female Florida red scale 57
10 Regression of per cent kill on deposit level for 3 series
of narrow-boiling petroleum fractions tested against citrus
red mite eggs. The number on each line indicates the
average molecular weight of the fraction. The solid por
tion of each line indicates the range of data collected;
the broken extension is extrapolation to the 50 or 95%
kill level 67
11 Efficiency in relation to molecular weight for 3 series of
narrow-boiling petroleum fractions and 2 commercial oils
against citrus red mite eggs 68
12 Efficiency in relation to viscosity for 3 series of narrow
boiling petroleum fractions and 2 commercial oils against
citrus red mite eggs 69
13 Efficiency in relation to 50% distillation point for 3
series of narrow-boiling petroleum fractions and 2
commercial oils against citrus red mite eggs 70
14 Effect of light, medium, and heavy paraffinic fractions
on the transpiration rate of treated 'Pineapple' orange
seedlings in relation to time after treatment. Shaded
symbols indicate significance from check 82
15 Effect of light, medium, and heavy naphthenic fractions
on the transpiration rate of treated 'Pineapple' orange
seedlings in relation to time after treatment. Shaded
symbols indicate significance from the check 83
16 Accumulated leaf drop from 'Hamlin' orange trees in the
5-week period following application of 4 oils on 6 May
1964 91
17 Degreening rate of oil-sprayed 'Hamlin' oranges 4 weeks
after spraying as indicated by decrease in per cent
absorbance with time in ethylene degreening chamber.
Sprays applied 18 September 1964; fruit harvested 16
October 1964 101
18 Degreening rate of oil-sprayed 'Hamlin' oranges 8 weeks
after spraying, as indicated by decrease in per cent
absorbance with time in ethylene degreening chamber.
Sprays applied 18 September 1964; fruit harvested 12
November 1964 102
ix


SUMMARY AND CONCLUSIONS
Laboratory and field investigations were conducted to determine
the relationship of certain physical and chemical properties of petro
leum oils to insecticidal and ovicidal efficiency and phytotoxicity to
citrus under Florida conditions. Three series of narrow-boiling petro
leum fractions provided wide ranges of molecular weight (250 to 520),
viscosity (41 to 402 SSU), 507 distillation temperature (581 to 911 F),
and base type or composition (naphthenic, paraffinic, and reformed) for
study. A large number of commercial oils were also available and were
tested to a limited extent.
The oils were formulated in the laboratory with an oil-soluble
emulsifier. Laboratory applications were made with a laboratory air-
blast sprayer similar in performance to commercial air-blast sprayers
used in the field. Standard field application methods were used in
field studies. Quantitative determinations of oil deposits were made
by spectrophotometric methods, utilizing an oil-soluble indicator dye.
Dosage-mortality tests were conducted in the laboratory against
adult female Florida red scale on grapefruit and against citrus red
mite eggs on immature 'Valencia' oranges. These infested fruit were
sprayed with various concentrations of selected oils, sufficient to
establish dosage-mortality relationships. The data were computer-
analyzed by probit analysis to obtain the regression coefficient and
LD50 and LD95 values and their 957o confidence limits for each oil.
The LD95 values for the oils in each series were plotted against
increasing values of molecular weight, viscosity, and 50% distillation
115


12
Phytotoxicity of Petroleum Oil
Hubbard (35) reported serious defoliation of citrus plants sprayed
with kerosene emulsion. Almost every author reporting on oil sprays
since then has pointed out the phytotoxic hazards of spraying plants
with petroleum oils. Yothers (104) concluded that all oils apparently
interfered with the physiological processes of the citrus tree. He
concluded the oil film interfered with chlorophyll production and noted
adverse effects of low temperatures following application of oil sprays
and "blotching" of fruit after an early-season application.
Gray and DeOng (29) showed a relationship between degree of re
finement and phytotoxic effects of petroleum oils. They suggested the
sulfonation test as a useful guide in judging the safety of an oil.
DeOng et al. (19) described 2 distinct types of injury to citrus
foliage by petroleum oils. These were acute and chronic, the former
being related to light oils and the latter to heavy oils. They ob
served defoliation, fruit spotting and dropping, and killing of twigs
and branches, and noted the apparent interference with transpiration
and respiration of the plant. Burroughs (4) reported severe leaf burn
and heavy leaf drop following summer application of oil sprays to apple
trees.
Penetration of oil into plants
DeOng et al. (19) cited Volck (97) as showing that penetration of
oil into the citrus leaf was most rapid on the abaxial surface, the
site of the stomatal openings. Knight et al. (36) reported both stoma-
tal and cuticular absorption of oil by citrus leaves, but penetration
was not uniform over the entire leaf. Certain focal points were pene
trated and the oil spread peripherally from these. Extensive


13
translocation of the oil in the citrus plant was reported. However,
Rohrbaugh (60) studied the fate of the oil film on citrus leaves,
twigs, and fruit, and found no evidence of translocation or other move
ment of oils from leaves into twigs or from small twigs into larger
twigs, except that oil may migrate short distances between the cells by
capillarity, and only in cases of heavy applications did it penetrate
to a depth of more than a few cells beneath the epidermis.
Oil-soaked areas appear on citrus leaves after spraying with oil.
This oil eventually migrates internally to an area along the midrib and
margins of the leaf, resulting in dark discoloration of leaf tissue in
that area (24).
Ginsburg (28) concluded oil penetration into leaves of apple,
peach, and tomato plants was related inversely to viscosity. McMillan
and Riedhart (37) reported pure hydrocarbons, having a distillation
range of 419 to 487 F, penetrated citrus leaves more rapidly than did
those of a higher boiling range. They concluded that little or no
cuticular penetration occurred. Young (108) concluded that petroleum
oil penetration was aided by external forces such as those caused by
gravitation, capillarity, and bending of tissues by wind. Tucker (94)
found oil penetration into apricot leaves related to the opening and
closing of stomata.
Dallyn and Sweet (12) stated that highly toxic herbicidal oils
entered the plant indiscriminately from the point of contact and in
ternal spread was negligible, while relatively nontoxic oils entered
largely through the stomata and spread throughout the plant to a con
siderable extent. Van Overbeek and Blondeau (96) stated that phyto
toxic oils could penetrate only after cells were injured; this was


LIST OF TABLES
Table Page
1 Specifications for California spray oils 20
2 Specifications for oils applied to fruit and shade trees
in New York 22
3 Specifications for various properties of petroleum oils
used in these studies 24
4 Oil deposit, number of scales, and per cent kill with 3
series of petroleum oils in dosage-mortality tests against
Florida red scale 51
5Effectiveness of 3 series of petroleum oils against adult
female Florida red scale 53
6
7
8
9
10
11
12
Effectiveness of commercial oils at 2 levels of appli
cation against adult female Florida red scale 59
Oil deposit, number of eggs, and per cent kill with 3
series of petroleum oils in dosage-mortality tests
against citrus red mite eggs 62
Effectiveness of 3 series of petroleum oils against
citrus red mite eggs 65
Spider mite counts at 1, 4, and 7 weeks after application
of spray oils on 6 May 1964 in Block 23 72
Respiratory rates of oil-sprayed 'Pineapple' seedlings
expressed as per cent of the check. Each value is the
mean of 6 determinations. Oils were applied at 70 to 80
Mg/cm2
Effect of 365-mol wt paraffinic oil on respiration of
adjacent treated and untreated leaves of 'Pineapple'
seedlings, measured as 0£ uptake in |_ig/cm2 leaf surface
in a 2-hour period. The oil deposit was high
(154.4 p.g/cm2)
Transpiration rate of 'Pineapple' seedlings sprayed with
1.5% concentration of low, medium, and high molecular
weight fractions of paraffinic and naphthenic oils
78
79
80
vi


49
each treatment, and these were used for comparing the effects of the
various treatments on degreening rate.
To supplement the instrumental measurements of the degreening rate,
20-fruit samples from each treatment were degreened for the same time
intervals and photographed together to illustrate the color changes
visually. Twenty extra fruit were harvested from each plot at the
same time as were the 40-fruit samples. The 4 samples from each treat
ment were mixed and then divided randomly into four 20-fruit lots. One
lot of 20 fruit for each treatment was placed in the degreening chamber
at the start of the 72-hour period, a second lot was added at 24 hours,
and a third at 48 hours; the fourth lot received no ethylene degreening.
Therefore, the 4 lots of fruit were degreened 72, 48, 24, and 0 hours,
respectively. At the end of the 72-hour period, the 4 lots of fruit for
all 5 treatments were photographed together in color. These photo
graphs are presented with the numerical data.
Fruit quality.--After the degreening treatments described above,
the 40-fruit samples were analyzed for internal quality by standard
methods (75). The analyses included the following determinations:
per cent soluble solids ( Brix); per cent acid; Brix/acid ratio; fruit
weight; juice weight; and per cent juice (by weight). Solids determi
nations were made with a Brix hydrometer and acid was determined titri-
metrically with standard sodium hydroxide solution and phenolphthalein
indicator. The treatments were compared mainly on the basis of per
cent soluble solids.


Table 3. Specifications for various properties of petroleum oils used in these studies
Oil
No.a Name*5
Avg Viscosity,
mol SSU at UR,
wt 100 Fc %
Chemical composition
d
Temperature, F,
for distillation^
(760 mm Hg) of: 10-90%
API distillation
gravitye 10% 50% 90% range, F
2
P-250
252
41.0
95.6
2.1
23.9
74.0
40.9
579
581
591
12
3
P-265
265
45.0
95.8
0.0
29.0
71.0
39.8
609
614
622
13
4
P-285
285
50.0
95.8
2.8
25.2
72.0
37.9
639
646
652
13
6
P-305
305
59.8
91.8
4.5
18.0
77.5
36.3
674
696
701
27
7
P-320
322
71.0
93.4
4.6
22.4
73.0
35.0
698
715
734
36
8
P-365
365
99.0
94.6
3.1
25.4
71.5
42.2
743
752
779
36
9
P-435
433
199.1
94.0
5.1
29.9
65.0
31.6
812
831
856
44
10
P-520
520
396.0
93.0
4.4
26.1
69.5
30.8
887
911
944
57
11
R-250
250
42.8
86.4
2.3
39.2
58.5
34.4
572
597
614
42
12
R-265
265
46.6
91.4
4.0
41.0
55.0
35.6
608
615
624
16
13
R-285
285
52.8
94.0
0.4
34.6
65.0
36.0
649
656
661
12
14
R-295
295
55.9
94.4
0.3
31.7
68.0
36.1
666
675
680
14
15
R-305
305
59.3
91.0
2.3
28.7
69.0
36.4
673
700
706
33
16
R-320
320
66.5
94.0
2.4
27.6
70.0
35.9
701
716
721
20
17
R-365
365
100.2
95.0
2.7
31.3
66.0
33.6
751
766
784
33
19
N-250
250
47.6
96.4
1.6
52.9
45.5
32.8
585
593
602
17
20
N-265
265
51.4
96.2
1.0
51.4
47.5
32.6
607
611
620
13
21
N-285
285
57.7
96.6
0.0
47.5
52.5
33.1
629
635
656
27
23
N-305
305
68.3
96.6
1.0
49.0
50.0
31.7
661
665
678
17
24
N-320
320
79.7
97.2
1.0
48.0
51.0
31.3
675
689
703
28
ro


88
safety. As mentioned above>the 50% distillation points for these 2
oils are 646 F and 689 F, respectively. However, these are laboratory
determinations; if field conditions are considered, the effects of
weathering factors might increase the dissipation rates to the extent
that the above distillation temperatures could be increased considerably
without drastically increasing the effects of oil on the physiology of
the citrus tree. Comparison of the resulting temperatures with the
minimum distillation temperatures for efficiency against citrus pests
derived from Figures 9 and 13, reveals some interesting possible corre
lations between insecticidal efficiency and plant safety.
Oil blotch, leaf drop, and fruit drop
Results.Treatments were applied when the fruit were in the stage
of highest susceptibility to oil blotch. Inspections of the fruit were
made on the tree throughout the season and at harvest time. Although a
variety of oils were applied at a heavy dosage, no fruit were found to
exhibit this condition.
Weekly leaf drop in grams per 4-tree plot for each treatment is
presented in Table 13. The accumulated leaf drop for the 5-week period
is shown in Figure 16. It is readily apparent that a higher rate of
drop occurred in the treated plots than in the check plots. The great
est portion of the leaves dropped during the first 2 weeks in the
treated plots, with the rate gradually diminishing up to the fifth
week. At this time a reversal in the relative rates of leaf drop oc
curred. Whereas the check plots and the plots sprayed with the 60-SSU,
high-UR oil, R-60, had the lowest rate of drop during the first 4 weeks,
they now showed an increased rate, and the plots treated with the 74-
and 92-SSU, high-UR oils, P-96 and BR-1, showed a relatively low rate


85
uptake (Table 11) 3 and 7 days after treatment. Although conditions at
the time did not permit further determinations, a trend toward in
creased inhibition was indicated. These data are quite limited, but
they lead to the conclusion that effects on the respiratory process are
associated with increasing oil deposit and increasing oil heaviness.
These factors would tend to place more oil on and in the leaf and hold
it there for a longer period of time.
The results presented in Table 12 and Figures 14 and 15 show that
the transpirational process of citrus may be more markedly affected by
normal rates of oil application than the respiratory process. Also, a
direct correlation is indicated between oil heaviness, particularly as
measured by distillation range, and inhibition of transpiration. A
significant reduction in transpiration was associated with all 6 oils
the first several days after treatment. The plants sprayed with the 2
lightest fractions, i.e., 285 mol wt, showed the least initial reduc
tion and also the fastest recovery rate. Of these two oils, the
fastest recovery was associated with the naphthenic fraction. The data
in Table 3 show that the paraffinic fraction had a higher distillation
range than the naphthenic fraction. The difference in the recovery
rates associated with the two 320-mol wt fractions were even greater.
The recovery pattern for the 320-mol wt naphthenic fraction was nearly
the same as that for the 285-mol wt paraffinic fraction. The 320-mol
wt paraffinic fraction depressed transpiration throughout the 70-day
period to about the same extent as did both 365-mol wt fractions. The
most peculiar aspects of these curves are that the P-365 oil had less
effect on transpiration the first few days following treatment than did
the P-320 or N-365 oils, and that the plants sprayed with N-285 showed


Figure 7. Efficiency in relation to molecular weight for 3 series of narrow-boiling petroleum
fractions against adult female Florida red scale.
Ui
Ln


Yothers (103) introduced lubricating oils about 1911 and these
gradually came into wide use in controlling scale insects and white-
6
flies on citrus in Florida.
The interest in oil sprays declined somewhat during the years 1910
to 1920, especially in California, in favor of lime-sulfur spray and
HCN gas. However, after a few years, interest in oil sprays was
revived, but this time to lubricating-oil emulsions instead of the
older kerosenes, crudes, and distillates. This renewed interest was
due mainly to the alarming increase in damage caused by the San Jose
scale, Aspidiotus perniciosus Comstock, to deciduous fruit trees and
the development of resistance to HCN gas by the California red scale,
Aonidiella aurantii (Maskell), and the black scale, Saissetia oleae
(Bernard), (72).
The interest in oil emulsion sprays was greatly stimulated about
1925 by the publicity given to the formulae of Yothers (106) and
Burroughs (3) for boiled lubricating oil emulsions and cold engine oil
emulsions. These formulae, and the method of emulsification, were
essentially the same as those suggested by Hubbard (35) in the early
1880's, except that lubricating oil was specified instead of kerosene,
crude oil, and distillates.
Renewed interest in oil sprays stimulated research in all phases
of the subject--insecticidal, miticidal, and phytocidal. The main
problem with petroleum oil was that of phytotoxicity. Hence the bulk
of the research since the early 1920's has been concerned with the
phytotoxic properties of oils, and with the development, through re
finement and other means, of oils less detrimental to plants. Con
current with this, the insecticidal properties were studied in order to


Figure 12. Efficiency in relation to viscosity for 3 series of narrow-boiling petroleum fractions and 2
commercial oils against citrus red mite eggs.
ON
VO


65
Table 8. Effectiveness of 3 series of petroleum oils against citrus
red mite eggsa
Oil
Slope of
regression
line
LD50
, pg/cm
2
LDgtj,
o
pg/cnr
Dose
957,
CL
Dose
95%
CL
N-250
2.438
138.0


1,950.0

_

N-265
2.528
77.5


346.8

-

N-285
3.338
40.9
21.6 -
57.4
127.3
83.8
-
457.9
N-305
2.775
10.3
6.2 -
13.4
40.3
32.4
-
60.1
N-320
3.584
7.4
0.2 -
10.9
21.2
16.2
-
50.1
N-365
2.574
5.6
2.4 -
8.0
24.5
18.8
-
42.7
N-395
2.557
5.8
4.0 -
7.4
25.6
21.8
-
32.3
N-440
1.386
2.1
0.03-
5.2
32.2
24.0
-
63.9
R-250
3.565
126.1


364.8

_

R-265
2.457
45.3


211.4

-

R-285
5.233
14.4
11.1 -
17.8
28.8
21.8
-
53.7
R-295
3.610
9.9
3.2 -
14.3
28.3
19.0
-
137.7
R-305
2.320
5.4
2.1 -
8.5
27.6
16.7
-
88.0
R-320
3.104
4.7
2.9 -
6.0
15.9
12.7
-
23.9
R-365
1.693
2.3
0.5 -
4.1
21.5
14.9
-
47.6
P-250
2.806
167.9

647.3

_

P-265
2.198
58.4

. #
327.2

-

P-285
4.631
29.2
22.2 -
35.7
66.2
54.5
-
93.3
P-305
2.080
4.7
3.1 -
6.3
28.8
20.3
-
48.4
P-320
1.784
2.6
1.0 -
4.1
21.8
14.4
-
51.2
P-365
1.202
0.6
0.1 -
1.4
14.9
9.9
-
29.9
P-435
1.061
0.7
0.1 -
2.0
25.7
18.4
-
41.8
P-520
1.334
3.9
1.3 -
6.5
66.1
44.9
-
147.4
P-96
1.531
1.6
0.5 -
2.8
18.6
12.1
_
38.8
R-60
2.778
5.6
4.2 -
7.2
22.1
16.2
34.8
Values for slopes of dosage-mortality regression lines and 957 confi
dence limits (CL) for lethal doses (LD) for 507. and 957, kill were ob
tained by probit analysis. Confidence limits were not calculated for
the oils exhibiting very low toxicity.


75
fruit moth eggs. The minimum molecular weight values for efficient
kill established in the present work were considerably lower than the
above values, but the points for maximum efficiency obtained here were
quite similar.
Beyond a point of maximum efficiency for each of the 3 series
studied, the trend was toward decreasing efficiency with increase in
oil heaviness. This reversal was much more drastic with Florida red
scale than with citrus red mite eggs. Riehl and LaDue (47) observed
the same phenomenon with California red scale but not with citrus red
mite eggs. They reasoned that the spreading characteristics of the
larger hydrocarbon molecules was the limiting factor and were able to
show some proof of this by diluting the heavier fractions with a non
toxic amount of kerosene to reduce the viscosity of the oils. Pearce
and Chapman (44) obtained similar results with oriental fruit moth eggs
and greatly increased the efficiency of a 479-mol wt isoparaffin by
diluting with deodorized kerosene. Thompson (84) reported no differ
ence in scale control on Florida citrus with oils in the viscosity
range of 72 to 100 SSU. The screening data for the commercial oils
presented in Table 6 tended to bear this out. Although differences
occurred at the low deposit level, these were not correlated with
viscosity, which ranged from 57 to 112 SSU. At the high deposit level,
all the oils were effective. The field data for spider mites presented
in Tables 9 and 10 failed to show significant correlation of control to
viscosity in the range of 60 to 90 SSU.
Although the minimum LDq^ values obtained for Florida red scale
were 2 to 3 times as great as those for citrus red mite eggs, it is
interesting to note that the very light fractions in each series


131
BIOGRAPHICAL SKETCH
Kenneth Trammel was born 30 October 1937, at Skipperville,
Alabama. He obtained his elementary and secondary education at Frost
proof, Florida, and was graduated from Frostproof High School in June
1956. In June 1960, he received the degree of Bachelor of Science in
Agriculture from the University of Florida. In September 1960, he
enrolled in the Graduate School of the University of Florida as a
National Defense Education Act Fellow in the Department of Entomology.
Since that time, he has pursued his work toward the degree of Doctor of
Philosophy. He has been employed as a full-time assistant in entomology
at the University of Florida Citrus Experiment Station, Lake Alfred,
since May 1963.
The author is married to the former Bessie Ellen Robinson. They
have 3 sons, Kenny, Keith, and Kurtis.
He is a member of the Entomological Society of America, the
Florida Entomological Society, the Florida State Horticultural Society,
Gamma Sigma Delta, and Alpha Zeta.


5
in direct relationship to its degree of refinement (25).
The most important properties used for defining spray oils are
those which indicate "heaviness" or volatility, refinement, and hydro
carbon composition. Viscosity (seconds Saybolt Universal = SSU) and
molecular weight are measures of the heaviness of oils but are valid
only for comparing oils of the same composition. Distillation temper
atures are most directly related to volatility and may be used to com
pare oils of varying hydrocarbon composition. Oil refinement is indi
cated by the per cent unsulfonated residue as explained above and is
especially important in relation to plant safety. Hydrocarbon compo
sition refers to the relative content of paraffinic and naphthenic com
pounds, since both types are present in spray oils (9, 24, 25). Gener
ally speaking, paraffinic oils contain approximately 65 to 75% paraf
finic carbons and naphthenic oils contain about 45 to 55% naphthenic
carbons.
Historical Use of Spray Oil
The insecticidal efficiency of petroleum oil was recognized nearly
a century ago, as undiluted kerosene was applied directly to insect-
infested trees around 1870 (72). Kerosene, soap, and water mixtures
were recommended during the 1870's and the Riley-Hubbard formula for a
kerosene, whale-oil soap, and water emulsion was published in 1883 (72).
Hubbard (35) recognized kerosene as the most effective insecticide for
combating scale insects on citrus in Florida in 1885. The kerosene-
soap emulsion remained a standard insecticide for use on citrus both in
Florida and California for many years. In addition to kerosene, crudes
and distillates were also tried with varying degrees of success (72) .


7
maintain high insecticidal efficiency of oil while reducing its degree
of phytotoxicity.
Since the early work of Hubbard and Yothers in Florida, research
workers in many areas of the country, particularly in Florida
(Thompson), California (DeOng, Smith, Knight, Chamberlin, Ebeling,
Wedding, Riehl, and others), and New York (Pearce, Chapman, and Smith),
have expended considerable time and effort in spray oil research.
Insecticidal and Ovicidal Action of Petroleum Oil
DeOng et al. (19) attributed the insecticidal action of unrefined
petroleum oil to suffocation and toxic action, the latter due chiefly
to the action of unsaturated hydrocarbons and the former due to non
volatility or film-permanence. They stated that the wax solubility of
oil determined to a great extent the insecticidal effectiveness of
lubricating oils against the California red scale. The oils dissolve
the waxy coating of the insect and penetrate to the spiracles, thus
halting the respiratory process. DeOng (18) had earlier found that
scales could expel the highly refined volatile oils, e.g., kerosene,
from the tracheal system, thus rendering these materials ineffective.
But any volatile oil containing a large amount of unsaturated hydro
carbons seemed to pass throughout the body cavity, dissolving first the
fat bodies and finally even the entire cellular structure of the in
terior part of the body. Non-volatile oils could not be expelled from
the spiracles by the insects.
Swingle and Snapp (81) cited reports that oil did not affect
respiration of insects, and also that it was not suffocation which
killed the insect but rather the gases given off by the oil after
entering the tracheal system. These views are in conflict with the


9
Oil is also an important ovicide. It has proved effective against
eggs of various insects and mites. Smith and Pearce (70) suggested
that the mode of ovicidal action of oil may be the prevention of ready
elimination of toxic metabolites, causing their accumulation in lethal
amounts. The respiratory rate of eggs of the oriental fruit moth,
Grapholitha molesta (Busck), was immediately reduced following oil
application. They demonstrated that oil must remain on the chorion for
at least 24 hours to be completely effective. Older eggs were less
susceptible than younger ones. Smith (71) summarized various theories
on the mode of ovicidal action of oils:
"The oil may prevent the normal exchange of gases through the
outer covering of the egg.
"The oil may harden the outer covering so as to prevent
hatching.
"The oil may interfere with the water balance.
"The oil may soften or dissolve the outer covering of the
egg, through interfering with the normal development of
the embryo.
"The oil may penetrate the egg and cause coagulation of
the protoplasm.
"The oil may penetrate the egg and interfere with enzyme
or hormone activity.
"The oil may come in contact with the emerging insect and
exert its toxic effect upon the delicate integument."
But he stated that the precise mechanism might vary with different
species or that several modes of action might operate simultaneously or
at different stages in the development of the embryo.
Ebeling (21) showed that the effectiveness of an oil spray against
citrus pests was related to the heaviness of the oil and the amount of
oil applied. Chapman et al. (5) also found that control of apple pests
was in proportion to the amount of oil applied. Pearce et al. (43)


Table 4--Continued
Oil
Dosage levels, high to low deposit
1
2
3
4
5
6
7
8
9
Hg/cnT
95
94
92
78
70
48
31
15
0
R-305
Scales
255
230
244
238
318
256
370
353
336
% kill
100
99
100
99
98
95
49
5
1.4
|ig/ cwr
102
100
92
70
62
50
31
16
0
R-320
Scales
201
308
349
258
300
248
281
300
336
7o kill
98
99
99
99
98
92
62
17
1.4
o
|ig/cnr
130
106
98
79
67
50
33
16
0
R-365
Scales
314
219
356
269
236
185
236
339
336
7o kill
99
98
99
98
92
94
56
8
1.4
M-g/ cm
108
94
81
67
54
40
27
0
-
N-265
Scales
253
117
146
130
205
229
246
209
-
7o kill
89
96
89
73
40
7
2
2.8
-
o
\i&/cnr
122
102
88
70
63
52
39
28
0
N-285
Scales
257
233
246
257
314
222
293
267
246
7o kill
100
99
92
93
93
78
26
20
4.4
M-g/cn*
110
96
87
69
57
41
27
15
0
N-305
Scales
348
288
223
313
171
264
255
238
246
7a kill
100
99
97
96
95
66
7
6
4.4
Hg/cnr
111
92
90
71
64
42
29
14
0
N-320
Scales
171
225
239
257
218
326
205
227
246
% kill
100
100
99
98
95
76
21
4
4.4
pg/cnr
113
111
96
80
62
55
32
18
0
N-365
Scales
281
195
210
213
226
335
267
300
246
7o kill
98
98
95
96
80
82
53
9
4.4
[ig/cm2
120
109
100
70
50
38
26
16
0
N-395
Scales
214
232
271
189
258
211
256
295
246
% kill
100
100
97
97
81
72
34
12
4.4


Table 4.
, Oil deposit, number of scales, and per cent kill with 3
dosage-mortality tests against Florida red scale
series of petroleum oils in
Oil
Dosage levels, high to low deposit
1
2
3
4
5
6
7
8
9
pg/cm
108
94
81
67
54
40
27
0
-
P-265
Scales
220
180
214
221
159
361
151
209
-
% kill
85
98
92
86
84
77
90
2.8
pg/cnT
115
107
95
88
71
53
36
26
0
P-285
Scales
278
368
262
265
307
389
267
319
318
% kill
96
98
98
100
94
91
20
2
5.6
pg/cm
119
94
87
63
50
39
26
15
0
P-305
Scales
309
357
226
468
328
307
311
468
318
% kill
100
100
99
96
94
82
27
8
5.6
o
pg/ cm^
105
101
83
69
54
41
27
14
0
P-320
Scales
390
233
256
297
300
353
310
387
318
% kill
100
100
99
99
98
98
49
10
5.6
pg/cmz
122
89
79
70
62
46
32
17
0
P-365
Scales
315
338
286
420
237
362
303
448
318
% kill
100
100
98
78
92
65
31
12
5.6
pg/ cm
121
95
94
71
59
46
30
18
0
P-435
Scales
376
277
381
189
234
392
343
312
318
% kill
99
99
95
96
91
55
11
12
5.6
n
pg/cmz
108
94
81
67
54
40
27
0
R-265
Scales
182
336
207
253
176
261
226
209
-
% kill
91
93
92
94
95
17
12
2.8
-
o
pg/ cnr
118
102
101
87
62
49
37
26
0
R-285
Scales
256
235
285
297
364
242
231
291
336
% kill
100
99
99
99
93
88
64
10
1.4


21
stated, "It is known, for example, that oils as low as 80 UR, which
would be excessively injurious to citrus trees in California, can be
safely used in Texas, Florida, and Mexico. It appears that in more
humid regions a citrus tree is not so adversely affected by oil as in
California, and that oils of a lower degree of refinement can be safely
used
Chapman and Pearce (7) first published standardized specifications
for dormant spray oils for New York in 1947. They recognized 2 types,
"regular" and "superior"; both were 100-SSU oils but of different re
finement. In 1959, Chapman (8) presented specifications for a "70-
second superior oil" in addition to the 1947 "100-second superior oil."
Chapman et al. (9) added to these a "60-second superior oil," dropping
the 100-second oil from the recommendations. Specifications for these
are presented in Table 2. Some oils currently used in Florida on cit
rus are patterned after Chapman's "70-second superior oil."
Dean and Bailey (14) published tentative specifications for oils
for use on Texas grapefruit in 1961. They specified unsulfonated
residue, 927o minimum; distillation (760 mm Hg), 507, at 716 F with a 10
to 907o range of 85 F; and a neutralization number of 0.03 minimum.
No grade standards have been established for oils used on citrus
in Florida. The oils currently in use vary as follows: viscosity, 60
to 110 SSU; 507 distillation point, 651 to 788 F; 10 to 90% distil
lation range, 52 to 261 F; average molecular weight, 300 to 350; and
refinement, 80 to 96 UR (compiled from specification data for various
commercial oils) .


Figure 15. Effect of light, medium, and heavy naphthenic fractions on the transpiration rate of treated
'Pineapple' orange seedlings in relation to time after treatment. Shaded symbols indicate significance
from the check.


/
120
5) Therefore, the adverse effects of oil to Florida citrus could
be alleviated by the use of the lightest insec.ticidally effi
cient oils.
The combination of properties combining the least adverse effect
to the citrus tree with efficient insect control can be determined only
through extensive field testing. However, the results obtained in
these studies point toward this combination of properties. They can
serve as the basis for selecting candidate materials for field testing
which may lead eventually to the recommendation of more rigid specifi
cations for oils used on citrus in Florida.


LITERATURE REVIEW
Source and Properties of Petroleum Spray Oil
Petroleum or "rock oil" (Greek petros = rock, and oleum = oil) is
mainly an oily liquid mixture of numerous hydrocarbons believed to have
been formed from the remains of animal and vegetable marine organisms.
It is comprised chiefly of paraffins (aliphatic chains), naphthenes or
asphaltics (saturated ring hydrocarbons), aromatics (ring hydrocarbons
with conjugated double bonds), and unsaturates (aliphatic or cyclic
hydrocarbons with one or more active double or triple bonds). The oil-
producing areas or fields in the United States are regionally referred
to as Eastern, Mid-continent, and Western or Californian. The Eastern
fields produce predominantly paraffin-base crudes, the Californian
fields produce predominantly asphaltic- or naphthenic-base crudes, and
the Mid-continent fields produce crudes of a mixed-base type. However,
any one of these types may be produced by individual wells in any area
(24).
In the distillation of a crude, the various petroleum fractions
come off in the order of liquified gas, petroleum ether, gasoline,
naphtha, kerosene, fuel oil, mineral seal oil, transformer oil, summer
spray oil, dormant spray oil, and lubricating oil. The summer and
dormant spray oils are in the light lubricating range. The heavier
materials withdrawn from the bottom of the fractionating tower, called
the residuum, may be used as fuel or, if from a suitable crude, re
worked into asphalt. Distillation of the fractions from transformer
3


130
ADDITIONAL REFERENCES
Calpouzos, L., T. Theis, C. M. Rivera, and C. Colberg. 1959. Studies
on the action of oil in the control of Mycosphaerella musicola on
banana leaves. Phytopathology 49(3):119-122 .
Calpouzos, L., N. E. Delfel, C. Colberg, and T. Theis. 1961. Relation
of petroleum oil composition to phytotoxicity and Sigatoka disease
control on banana leaves. Phytopathology 51 (5):317-321.
Calpouzos, L., N. E. Delfel, C. Colberg, and T. Theis. 1961. Viscosi
ty of naphthenic and paraffinic spray oils in relation to phytotox
icity and Sigatoka disease control on banana leaves. Phytopathology
51(8):528-531.
Calpouzos, L., and C. Colberg. 1964. Importance of source of spray
oils for Sigatoka disease control and phytotoxicity to banana leaves.
Phytopathology 54(2):235-236.
Dean, H. A., E. L. Wilson, J. C. Bailey, and L. A. Riehl. 1961.
Fluorescent dye technique for studying distribution of spray oil
deposit on citrus. J. Econ. Entomol. 54(2):333-340.
Johnson, C. M., and W. M. Hoskins. 1952. Relation of acids and per
oxides in spray oils to the respiration of sprayed bean leaves and
the development of injury. Plant Physiol. 27:507-525.
Thompson, W. L., J. R. King, and E. J. Deszyck. 1956. Progress report
on greasy spot and its control. Proc. Florida State Hort. Soc. 69:
98-104.


33
per cent dye = l2£L-fetS.2.e x 100 = (4Kb2Cl) x 100
Total pg oil Total pg oil
where A = spectrophotometer reading in per cent absorbance x 10
b = regression coefficient, 0.3093
vol = volume in ml to which weighed oil sample was diluted
Total pg oil = mg oil x 1,000.
The oil deposit on fruit was measured only on an equatorial band
of 1.0 to 1.5 inches on immature oranges and 2.0 to 2.5 inches on im
mature grapefruit. This area was defined by the shallow grooves near
and around each end of the fruit, as described earlier. The sprayed
fruit was held with its polar axis horizontal over a 6-inch glass fun
nel for stripping. The fruit was slowly rotated on axis and a jet of
dioxane from a 250-ml polyethylene squeeze-bottle was directed at the
equatorial area. The flow of solvent followed the curvature of the
fruit and did not run into the grooves along the margins. The strip
solution was collected in a graduated cylinder for measurement. From
10 to 15 ml of solvent were sufficient for removal of the oil deposit
from immature Valencia oranges and 20 to 30 ml were adequate for near-
ly-mature grapefruit. The oil deposit was measured on 3 fruit for each
tank of spray or treatment. The rind was removed from the equatorial
bank of each fruit and traced on paper; the area was measured with a
planimeter. The oil deposit was calculated as follows:
pg oil/cm^ = (A) (b) (vo-*-)
(cm2)(D)
where A = spectrophotometer reading of the strip solution in
per cent absorbance x 10
b = regression coefficient, 0.3093
vol = volume in ml of strip solution
2 2
cm = surface area in cm from which the deposit was
stripped
D = per cent dye in the oil.


Table Page
13 Leaf drop by young 'Hamlin' trees following application
of oil sprays on 6 May 1964 in Block 23 89
14 Fruit drop by young 'Hamlin' trees following application
of oil sprays on 6 May 1964 in Block 23 93
15 Color of oil-sprayed 'Hamlin' oranges before and after
different intervals of ethylene degreening and per cent
pack-out at 4 and 8 weeks after spraying 97
16 Regression equations for the degreening rate of oil-
sprayed 'Hamlin' oranges and hours required to degreen
to 30% absorbance level 100
17 Analysis of oil-sprayed 'Hamlin' oranges at 4 dates of
harvest. Each mean is the average of determinations on
four 40-fruit samples. Sprayed 18 September 1964 107
vii


93
Table 14. Fruit drop by young 'Hamlin' trees following application of oil
sprays on 6 May 1964 in Block 23
Plot
Treatment (4 trees
Number <
of fruit
per 4-tree plot3
1st
) week
2nd
week
3rd
week
4 th
week
5 th
week
Total
for 5
weeks
Check
1
45
39
5
1
2
92
2
15
35
3
0
0
53
3
13
19
1
3
0
36
4
24
26
2
4
3
59
Mean
24.2
a
29.8
a
2.8
a
2.0 a
1.2
a
60.0
a
R-60
1
55
150
10
16
3
234
2
30
52
13
5
0
100
3
38
101
10
7
1
157
4
0
1
5
0
2
8






Mean
30.8
a
76.0
a
9.5
a
7.0 ab
1.5
ab
124.8
ab
P-96
1
53
157
58
19
4
291
2
109
237
51
15
0
412
3
24
143
51
44
5
267
4
37
89
41
7
1
175
Mean
55.8
a
156.5
b
50.2
c
21.2 b
2.3
ab
286.2
c
BR-1
1
32
74
24
17
6
153
2
46
87
14
18
7
172
3
23
95
39
15
4
176
4
41
86
19
22
11
179
Mean
35.5
a
85.5
ab
24.0
b
18.0 ab
7.0
ab
170.0
ab
BR-2
1
38
192
52
51
33
366
2
36
53
44
. 7
0
140
3
29
103
46
32
22
232
4
18
77
34
11
0
140





Mean
30.2
a
106.2
b
44.0
c
25.2 b
13.8
b
219.5
be
Weekly total
for all treatments
706
1,816
522
294
104
3,442
Treatment means for a given week followed by the same letter are not sig
nificantly different at the 5% level according to Duncan's New Multiple
Range Test.


84
The response of the plants to the various treatments is readily
apparent from the graphs in Figures 14 and 15. The 320-mol-wt
paraffinic oil and all 3 naphthenic oils effected significant reduc
tion in transpiration the first day after treatment. Further reduction
occurred with all 6 oils on the second and third days, after which some
recovery was evident. A strong recovery period began after the seventh
day for all the oil-treated plants and none were significantly differ
ent from the check on the ninth day. After this time, the P-320, P-365,
and N-365 fractions significantly depressed transpiration throughout
the remainder of the 70-day period of measurement with only a few days
excepted. The transpiration rates of the plants treated with the P-285,
N-285, and N-320 fractions were not significantly different from that
of the check after the ninth day except on occasional days. The plants
treated with the N-285 oil transpired at a level significantly higher
than the check on several days. In Figures 14 and 15, the shaded
symbols indicate significant difference from the check. The pretreat
ment transpiration rates shown in Table 13 indicate only minor differ
ences between the groups of plants in their normal transpiration rates.
Discussion.--The data presented in Table 10 fail to show signifi
cant inhibition of respiration in citrus seedlings sprayed with light
and heavy oils at a deposit level normally applied for scale control in
Florida. Although an initial increase followed by a gradual reduction
in O2 uptake by the plants sprayed with the paraffinic oils and the
opposite response to the naphthenic oils were indicated, these trends
were inconsistent and probably could occur by chance. At a deposit
level twice that of normal field applications (approximately 150 pg/fcm^),
the 365-mol wt paraffinic oil significantly reduced the rate of O2


Table 7--Continued
Dosage levels, high to low deposit
Oil
1
2
3
4
5
6
7
8
9
10
11
o
pg/cmz
111
100
94
87
50
42
25
0
-
-
-
N-265
Eggs
398
500
416
496
339
470
384
434
-
-
-
% kill
65
65
76
36
51
19
13
2.5
-
-
-
pg/cnr
114
98
96
52
52
39
22
14
0
-
-
N-285
Eggs
500
471
496
423
470
500
402
500
440
-
-
% kill
87
89
94
94
60
27
27
6
2.5
-
-
r\
pg/cnr
88
49
42
39
29
19
15
15
0
-
-
N-305
Eggs
573
472
506
500
469
468
500
460
436
-
-
% kill
99
98
99
91
86
82
73
62
1.8
-
-
o
pg/cnr
86
54
28
18
17
16
15
13
8
6
0
N-320
Eggs
405
439
560
470
445
486
500
500
488
500
442
7o kill
100
96
99
96
94
97
91
72
50
43
1.8
pg/cm2
80
58
45
36
31
21
12
11
9
0
-
N-365
Eggs
437
510
415
453
398
500
493
500
500
436
-
7o kill
100
100
99
97
97
91
89
87
58
1.8
-
pg/cmz
90
55
46
30
28
22
17
11
9
0
-
N-395
Eggs
421
434
451
487
515
454
457
500
487
436
-
7o kill
100
99
98
97
97
93
92
76
65
1.8
-
o
pg/cnr
93
58
43
23
22
20
16
14
10
9
0
N-440
Eggs
468
401
447
566
500
407
500
504
453
410
442
% kill
99
98
96
93
97
88
89
86
73
93
1.8
pg/cm111
82
76
48
40
19
15
14
7
4
2
0
P-96
Eggs
444
437
442
421
469
445
490
448
223
400
441
7o kill
99
98
97
97
100
97
89
89
85
46
1.3
pg/cnT
74
38
32
16
12
3
3
0
-
-
-
R-60
Eggs
541
517
470
497
457
458
464
463
-
-
-
7. kill
99
98
99
90
85
28
15
2.1
-
-
-
c^


11
petroleum oils occurred at approximately 340 mol wt (49).
Fiori et al. (27) found an inverse relationship between volatility
of petroleum oils and ovicidal efficiency. Generally, oils fell into
three distinct groups: 1) ineffective oils, those volatilizing within
12 hours; 2) moderately effective oils, those volatilizing in 12 to 24
hours; and 3) highly effective oils, those with little or no volatili
zation in 24 hours. Chapman et al. (9) considered volatility, as de
termined by distillation, to be the most definitive and useful desig
nation for a spray oil.
Thompson (84, 88), Thompson and Griffiths (86), and Thompson
et al. (89> 90) have reported on the effectiveness of oil in controll
ing citrus insects in Florida. When timed properly to avoid injury to
the trees, oil generally has given satisfactory control of purple scale,
Lepidosaphes beckii (Newman), Florida red scale, and related forms, and
citrus red mite. The recommended rate for scale control was 1.3%.
Thompson (84) reported no difference between paraffinic and
naphthenic oils in controlling purple scale and Florida red scale when
applied at concentrations of 1.3 to 1.4% oil. However, at a concen
tration of 1.0%,, paraffinic oil was superior to naphthenic oil. He
found no correlation between scale control and increase in viscosity in
the range 72 to 110 SSU. Dean and Bailey (15) reported superiority of
paraffinic oils and correlation of oil heaviness to efficiency in con
trolling Texas citrus mites, Eutetranychus banksi (McGregor).
Cressman and Dawsey (11) found no relationship between kill of
camphor scale, Pseudaonidia duplex (Cockerell), and oil refinement in
a UR range of 67 to 94%.


ACKNOWLEDGMENTS
The author expresses sincere appreciation to Dr. J. T. Creighton
for serving as chairman of his supervisory committee and for financial
aid obtained through a National Defense Education Act fellowship. He
is deeply indebted to Dr. W. A. Simanton, co-chairman, for supervision
and assistance during the course of the investigations, for obtaining
grant funds to support the investigations, and for his invaluable
guidance in preparation of the manuscript. Appreciation is extended
to Dr. A. H. Krezdorn, Dr. Milledge Murphey, and Dr. V. G. Perry for
serving on the supervisory committee and for critically reviewing the
manuscript.
He is grateful to Dr. H. J. Reitz for financial aid and for use of
the facilities at the Citrus Experiment Station, and to numerous staff
members of the Citrus Experiment Station for consultation, advice, and
use of their laboratory facilities. Appreciation is expressed to Mrs.
Harriet Long of the Citrus Experiment Station for taking the photo
graphs. The assistance of Mr. B. G. Shively in conducting the experi
ments, especially his willingness to work long hours at night and on
week ends, is greatly appreciated.
Gratitude is expressed to the personnel of Humble Oil and Refining
Company, especially Mr. R. C. Halter, for the grant which supported the
investigations and for numerous oil samples used in this work. Contri
bution of samples by the following oil companies is acknowledged: Gulf
Oil Corporation; Sun Oil Company; Shell Oil Company; Texaco, Incorpo
rated; and American Oil Company. Contribution of emulsifiers by the
ii


125
53. Riehl, L. A., and J. P. LaDue. 1957. Effects of oil spray and of
variation in certain spray ingredients on juice quality of
citrus fruits in California orchards, 1950-1953. J. Econ.
Entomol. 50(2):197-204.
54. Riehl, L. A., L. R. Jeppson, and R. T. Wedding. 1957. Effect
of timing of oil spray application during the fall on juice
quality and yield of lemons in two orchards in southern
California. J. Econ. Entomol. 50(l):74-76.
55. Riehl, L. A., J. P. LaDue, and J. L. Rodriguez, Jr. 1958. Evalu
ation of representative California spray oils against citrus
red mite and California red scale. J. Econ. Entomol. 51(2):
193-195.
56. Riehl, L. A., R. T. Wedding, J. P, LaDue, and J. L. Rodriguez, Jr.
1958. Effect of a California spray oil on transpiration of
citrus. J. Econ. Entomol. 51(3):317-320 .
57. Riehl, L. A., and R. T. Wedding. 1959. Relation of oil type,
deposit, and soaking to effects of spray oils on photosynthesis
in citrus leaves. J. Econ. Entomol. 52(l):88-94.
58. Riehl, L. A., and R. T. Wedding. 1959. Effects of naphthenic and
paraffinic petroleum fractions of comparable molecular weight
on transpiration of Eureka lemon and Bearss lime plants. J.
Econ. Entomol. 52(2):334-335.
59. Riehl, L. A., and R. T. Wedding. 1959. Effects of naphthenic
and paraffinic petroleum composition of a comparable molecular
weight or viscosity on photosynthesis of Eureka lemon leaves.
J. Econ. Entomol. 52(5):883-884.
60. Rohrbaugh, P. W. 1934. Penetration and accumulation of petroleum
spray oils in the leaves, twigs, and fruit of citrus trees.
Plant Physiol. 9(4):699-730.
61. Rohrbaugh, P. W. 1941. Physiological effects of petroleum oil
sprays on citrus. J. Econ. Entomol. 34(6):812-815.
62. Schroeder, R. A. 1936. The effect of some summer oil sprays
upon the carbon dioxide absorption of apple leaves. Proc. Amer.
Soc. Hort. Sci. 33:170-172.
63. Simanton, W. A. 1960. The reduced status of purple scale as a
citrus pest. Proc. Florida State Hort. Soc. 73:64-69.
64. Simanton, W. A. 1963. Ecological survey of citrus pests and
disorders. Univ. Florida Agr. Exp. Sta. Annu. Rep. p. 218-219.
65. Simanton, W. A., and Kenneth Trammel. 1965. Design and per
formance of a laboratory air-blast sprayer. In press.


29
Figure 1. Laboratory air-blast sprayer. A, high velocity blower; B,
motor; C, pump; D, spray tank; E, pressure regulator; F, nozzle; G,
deflector vanes; H, operating lever; I, turntable.


74
1.3 to 1.4% oil concentration, but at 1.0% there was a slight trend in
favor of the paraffinic type.
While the results obtained in the present work support the above
conclusions, the correlation between paraffin content and efficiency
was not as pronounced. The reformed series, which is indicated by the
data in Table 3 as being intermediate in paraffin content, appeared
more efficient, up to 340 mol wt and 85 viscosity, than either of the
other 2 series. With respect to 50% distillation temperature, the
naphthenic series tended to be more efficient against both pest species
than the paraffinic series, at least in the low portion of the efficient
range of distillation temperature.
The change in increase in efficiency with increase in oil heavi
ness was more abrupt where heaviness was measured by molecular weight
(Figures 7 and 11) and viscosity (Figures 8 and 12) than where measured
by distillation temperature (Figures 9 and 13). The curves showing the
relationship of LDgg values to molecular weight and viscosity are strik
ingly similar to those presented by Riehl and LaDue (47) for California
red scale and citrus red mite. The pattern of the curves was quite
similar in both instances. The main differences were that generally
lower LD95 values were obtained in the present work and the importance
of chemical composition was not as apparent as was shown by the above
authors. Riehl and Carmen (48) concluded that insecticidal efficiency
for California red scale increased with increase in molecular weight up
to 360, and Riehl and Jeppson (49) reported a critical value of 340 mol
wt for citrus red mite control in the field.
Pearce and Chapman (44) obtained maximum efficiency at 320 mol wt
for European red mite eggs, cottony peach scale nymphs, and oriental


90
80
70
60
50
40
30
20
102
HOURS DEGREENED
ure 18. Degreening rate of oil-sprayed 'Hamlin' oranges 8 weeks
after spraying, as indicated by decrease in per cent absorbance with
time in ethylene degreening chamber. Sprays applied 18 September
1964; fruit harvested 12 November 1964.


112
Since the cells in oil-soaked leaf tissue are not killed, the duration
of the effect of oil on these cellular and systemic functions is
indirectly related to the dissipation rate of the oil deposit (57).
Therefore, the lighter oils should have less over-all adverse effect
on the citrus tree than the heavier, less volatile oils.
General Discussion
It is recognized (25, 48) that citrus trees in the more humid
regions, as in Florida, are not as adversely affected by spray oils as
in drier climates, such as that in California; and that heavier, and
possibly less-refined, oils may be used with relative safety. The
relative safety of the heavier oils is good from an entomological point
of view because of the residual effectiveness of the less volatile oils;
the less refined oils are of economic desirability because of their
comparative low cost. However, the main problem associated with the
use of oils on citrus in Florida is that of phytotoxicity and not in
secticidal efficiency. The screening data presented in Table 6 indi
cate that the majority of the oils currently used in Florida fall in
the physical property range of maximum efficiency. The results of the
other insecticidal and ovicidal efficiency studies reported herein sug
gest that paraffinic oils in the viscosity range of 55 to 60 SSU, or
naphthenic oils of comparable distillation range, would render effi
cient pest control at currently recommended rates of application, es
pecially since biological control agents have effectively reduced the
scale problem over the past few years (63, 64).
The oils used on citrus in California are predominantly naphthenic
and as such are considerably lower boiling, hence more volatile, than
the paraffinic oils of comparable viscosity used in Florida. Yet these


15
relation of molecular structure of oil to effect on transpiration of
lemon and lime plants. A 306-mol wt naphthenic oil and a 308-mol wt
paraffinic oil both reduced transpiration more than 50%, but recovery
was faster in plants sprayed with the naphthenic oil than in those re
ceiving the paraffinic oil.
The effect of petroleum oils on photosynthesis and respiration of
various plants has been studied. Knight et al. (36) reported inhi
bition of photosynthesis in citrus leaves by light (50 SSU) and heavy
(106 SSU) oils, but recovery was faster in the plants treated with the
light oil. The same workers observed a significant stimulation of
respiration by the same oils. Other workers have reported increases in
respiration of plants treated with oil sprays. According to Green and
Johnson (30) respiration of bean leaves increased following application
of low refined oils of less than 84 UR, but a reduction in respiration
followed applications of oils of more than 84% unsulfonated residue.
Green (31), working with oils of both high and low refinement on bean
plants, apple leaves and twigs, and barley seedlings, found a general
increase in respiration, but the effect of the low UR oils was more
than triple that of the highly refined oils. McMillan and Riedhart
(37) observed an increase in oxygen uptake by leaves of 'Valencia'
sweet orange, Citrus sinensis, following application of pure hydro
carbons of a distillation range of 419 to 487 F, while those treated
with pure hydrocarbons and spray oil of a distillation range of 552 F
and higher showed a definite decrease in respiration.
Schroeder (62) reported that inhibition of photosynthesis in apple
foliage was directly related to viscosity and rate of application of
the oil. Oberle et al. (41) obtained similar results with heavier


Figure Page
19 'Hamlin' oranges from plots receiving late-season appli
cation of 4 oils and degreened for 0, 24, 48, and 72
hours; sampled 4 and 8 weeks after treatment. Sprays
applied 18 September 1964 105
20 Effect of 4 oils on soluble solids development in 'Hamlin'
oranges. Sprays applied 18 September 1964 108
x


116
temperatures to illustrate the relation of these physical properties to
insecticidal and ovicidal efficiency. The over-all relative efficiency
of the 3 series of oils, in decreasing order, was reformed, paraffinic,
and naphthenic. The optimum and minimum physical property values^ for
scalicidal and (ovicidal)'*' efficiency for the 3 series were:
1)Molecular weight--reformed, 305 and 279 (320 and 285);
paraffinic, 305 and 291 (365 and 304); and naphthenic,
320 and 300 (320 and 313).
2) Viscosity, SSU at 100 F--reformed, 59 and _51 (66 and 52);
paraffinic, 60 and j>3 (99 and _61); and naphthenic, 80 and
66 (80 and 75).
3) Fifty per cent distillation point--reformed, 700 F and
644 F (716 F and 660 F); naphthenic, 689 F and 657 F
(689 F and 677 F); and paraffinic, 696 F and 661 F
(752 F and 694 F) .
The property values for maximum efficiency and the minimum property
values for efficient kill were slightly lower for red scale than for
citrus red mite eggs. However, oil deposits necessary for 95% kill of
red scale were more than double those for the mite eggs, except with
the lightest oils. These were more efficient against red scale than
against mite eggs. Beyond the physical property values corresponding
to maximum efficiency, efficiency declined with increase in heaviness
of the oil. This reversal in effectiveness was more apparent for
Florida red scale than for citrus red mite eggs. Thirty commercial
oils, screened in the laboratory against Florida red scale, failed to
show correlation between kill and increasing heaviness in the viscosity
range of 57 to 112 SSU. Most of these oils fall within the efficient
ranges for the physical properties considered.
^The minimum property value for efficiency is underlined; the
property values for ovicidal efficiency are in parentheses.


Table 17. Analysis of oil-sprayed 'Hamlin' oranges at 4 dates of harvest. Each mean is the average of
determinations on four 40-fruit samples. Sprayed 18 September 1964a
Sample
No.
Date of
harvest Treatment
Total soluble solids, 7 (
Replicate
= Brix)
Mean*5
Acid
(%),
mean0
Ratio
Brix/
acid,
meanb
Juice by
weigh t
(%)>
rnean^
Fruit
diameter
(inches),
mean*5
1
2
3
4
Check
8.20
8.75
8.65
8.20
8.45 a
0.86 a
9.85
a
53.25
a
2.53 a
R-60
7.90
7.85
7.95
7.95
7.91 be
.84 a
9.41
a
52.32
a
2.55 a
1
16 October
BR-2
7.80
7.70
7.85
7.65
7.75 c
.82 a
9.49
a
52.65
a
2.49 a
1964
P-96
8.00
8.05
8.35
8.15
8.14 b
.84 a
9.73
a
52.67
a
2.50 a
BR-1
7.85
7.70
7.75
7.65
7.74 c
.83 a
9.34
a
52.60
a
2 .46 a
(9.2)*
(0.5)*
Check
9.95
8.55
8.45
8.75
8.92 a
0.81 a
10.99
a
48.48
a
2.56 a
R-60
8.55
8.25
8.55
8.35
8.42 be
.80 a
10.61
a
49.72
a
2.56 a
2
1 964
BR-2
8.35
8.25
8.25
8.15
8.25 c
.78 a
10.55
a
48.42
a
2.53 a
P-96
9.35
8.45
8.75
8.65
8.80 ab
.80 a
11.00
a
49.25
a
2.53 a
BR-1
8.35
8.25
8.15
8.15
8.22 c
.82 a
10.05
b
47.75
a
2.45 a
(9.0)*
(0.5)*
Check
9.20
8.80
8.50
8.80
8.82 a
0.75 a
11.86
a
43.38
a
2.60 a
R-60
8.60
8.50
8.70
8.50
8.58 abc .71 a
12.16
a
44.02
a
2.60 a
3
1
BR-2
8.60
7.80
8.70
8.30
8.35 be
.69 a
12.11
a
42.62
a
2.62 a
P-96
8.90
8.40
9.00
8.40
8.68 ab
.72 a
12.16
a
42.75
a
2.55 a
BR-1
8.40
8.30
8.20
8.10
8.25 c
.72 a
11.55
a
42.90
a
2.53 a
(9.0)*
(0.5)*
Check
9.20
9.10
9.20
9.00
9.12 a
0.70 a
12.91
a
48.65
a
-
7, December
R-60
9.20
8.90
9.10
8.60
8.98 a
. 68 a
13.08
a
47.98
a
-
4
1964
BR-2
9.00
9.10
9.10
8.70
8.98 a
.73 a
12.39
a
47.78
a
-
P-96
9.70
8.90
9.60
9.10
9.32 a
.71 a
13.00
a
48.52
a
-
BR-1
9.40
9.20
8.70
8.80
9.02 a
.71 a
12.70
a
44.38
a
-
(8.7)*
(0.5)*
^The fruit samples were degreened with ethylene gas prior to analysis as follows: No. 1, 72 hours; No. 2,
48 hours; No. 3, 72 hours; No. 4, 0 hour.
^Treatment means, on a given date, followed by the same letter are not significantly different at the 57o
level according to Duncan's New Multiple Range Test.
*Minimum legal standard for the harvest date.
107


73
refining process of certain ring compounds (e.g., naphthenic acids and
partially saturated aromatics) which are removed in the normal acid
treating process of refining. The 3 physical properties discussed,
molecular weight, viscosity, and distillation temperatures, are all
measures of oil heaviness.
The most striking features of the results as depicted in Figures
7 to 9 and 11 to 13 are: the relative efficiency of the 3 series of
oil fractions; the abrupt change from increasing efficiency with in
crease in oil heaviness to a more gradual rate of increase--especially
with citrus red mite eggs; the trend of decreasing efficiency beyond a
point of maximum efficiency--especially with Florida red scale; and
the difference in the minimum effective dosage for the 2 pest species.
The relative efficiency of the 3 series of oils tested, in de
creasing order, was reformed, paraffinic, and naphthenic. These re
sults are in general agreement with the findings of other workers (9,
42, 43, 44, 47, 48, 49). Chapman et al. (9) summarized years of exten
sive research and cited other workers in correlating basic structural
composition of petroleum oils to insecticidal efficiency. Paraffin
content was found to be the key variable among saturated compositions
and a direct relationship between efficiency and the proportion of car
bon atoms present in the form of chains was established. Riehl and
LaDue (47) found paraffinic oils superior to naphthenic oils against
adult female California red scale and citrus red mite eggs in labora
tory studies similar to those reported herein. Riehl and Carmen (48)
and Riehl and Jeppson (49) reported the same relationship under field
conditions in California. Thompson (84) reported no difference between
paraffinic and naphthenic oils in scale control on citrus in Florida at


109
indicates the approximate date by which the fruit in the various treat
ments attained the minimum legal solids requirement for color-added
oranges, the category in which these 'Hamlin' oranges would have been
placed. Again, the data for P-96 should be viewed with skepticism be
cause of faulty application of the oil spray.
Discussion.--The data in Table 17 indicate that oil heaviness and
possibly oil refinement are factors in the adverse effect of oil sprays
on internal quality of citrus fruits. All oils significantly delayed
solids development up through 6 weeks after application of the late-
season spray. By the eighth week, the solids level in the fruit from
the light-oil plots had risen to a level not significant from that of
the check fruit. The solids levels of the fruit from the plots sprayed
with the 70-SSU, low-refined oil and the 92-SSU, high-refined oil were
still significantly below that of the check fruit. Although the dif
ferences between the 3 oils were not significant, the results unques
tionably favor the light oil, since it was associated with the least
reduction in solids throughout the sampling period. By the time of the
fourth sampling, reduction in solids by the oils was apparently overcome.
Although the solids levels in the fruit from the sprayed plots were
lower than that of the check, the differences were non-significant.
The graph in Figure 20 indicates that the fruit sprayed with the light
oil attained the minimum legal solids level approximately 1 week ear
lier than the fruit treated with the heavy oil and the low-refined oil.
The reversal in solids development in the check fruit and those
receiving the faulty application of the medium oil from the second to
the third sampling dates is without explanation other than that it
might be due to sampling error. The supply of fruit remaining on the


71
1) Molecular weight--reformed, 285; paraffinic, 304; and
naphthenic, 313.
2) Viscosity, SSU at 100 F--reformed, 52; paraffinic, 61;
and naphthenic, 75.
3) Fifty per cent distillation point--reformed, 660 F;
naphthenic, 677 F; and paraffinic, 694 F.
The prpperty values for maximum efficiency and the minimum proper
ty values for efficient kill were slightly higher for citrus red mite
eggs than for ted scale. However, LD95 values for red scale were more
than double those for the mite eggs, except with the 265-mol wt frac
tions. These lighter fractions attained 957, kill of red scale at 90 to
100 pg/cm but required over 200 pg/cnr for citrus red mite eggs.
The 4 oils applied in Field Experiment No. 1 covered a viscosity
range of 60 to 90 SSU. Detailed spider mite counts were made 1, 4, and
7 weeks after application. The data presented in Table 9 show the
relative abundance of citrus red mite and Texas citrus mite,
Eutetranychus banksi (McGregor), at these times. All 4 oils signifi
cantly reduced the spider mite population throughout the 7-week period,
except for Texas citrus mite in the seventh week. Although differences
between oils were not significant, residual control by the heavy and
medium oils appeared better than by the light oil.
Discussion
These studies were primarily concerned with the relationship of
chemical composition and heaviness of petroleum oil to insecticidal and
ovicidal efficiency. The main comparisons for composition were between
the paraffinic and naphthenic series. The reformed oils were paraffinic
fractions obtained by a special refining technique which resulted in
products of slightly lower paraffinic hydrocarbon content than the
paraffinic series. This was probably due to the retention in the


44
unsprayed leaf served as the check on the adjacent sprayed leaf. One
pair of leaves per plant was harvested each sampling date, starting
with the basal-most pair and working up the plant on successive sam
pling dates. Thirty 0.25-inch discs were taken from each leaf with an
ordinary hand-grip paper punch. Hence, 12 samples of 30 punches each,
6 sprayed and 6 unsprayed, were run for each oil. The 30 discs from a
single leaf constituted a sample.
Oxygen uptake was measured by standard manometric techniques using
a 14-flask Warburg respirometer. The flasks were of 16-ml capacity
with 2 side arms. The ambient CO2 level was maintained by placing 0.2
ml 107c KOH in the center well of each flask to absorb the evolved C02
The flasks were kept dry, but 1 ml distilled water was placed in 1 side
arm of each flask to maintain constant relative humidity. The flasks
were shaken at 100 cycle/min in a water bath maintained at 25 + 0.1 C.
The operation was carried out in a 68 F darkroom.
A manmeter-calibration period of 50 min was followed by O2 uptake
determinations for 2 successive 30-min and one 60-min periods. The
total O2 uptake during the last 2 hours was used to calculate the res-
piration rate in pi 02/cm per hour. Determinations were made 1, 3, 7,
and 14 days after treatment. The rates of the treated leaves were con
verted to per cent of the rates of the untreated leaves and these
values were used for comparing the different treatments on each sam
pling date. An analysis of variance was run on the data.
In a follow-up experiment, the heavy paraffinic fraction, P-365,
was applied at 2.07o concentration as a drenching spray to 6 plants.
The same procedures were followed as in the above experiment except
that the sample size was increased to 48 leaf punches. Respiration


35
Figure 3. Method of infesting grapefruit with Florida red scale for
laboratory studies. A, ivy leaves with natural infestation of
crawler-producing female scales; B, cheesecloth strip with infested
leaf sections; C, strip of leaf sections wrapped firmly in position
around the equator of a grapefruit to allow crawlers to transfer; D,
typical infestation obtained by this method, at time of treatment
application (4.5 weeks after infestation).


117
The effects of various oils on the respiration and transpiration
rates of potted 'Pineapple' seedlings were determined in the laboratory.
At deposit levels comparable to those obtained in normal field applica
tions, paraffinic and naphthenic oils of 305 and 365 mol wt failed to
affect respiration significantly. However, at twice the normal deposit
level, the heavier paraffinic fraction caused significant reduction.
The effect on transpiration rate was related to oil heaviness. Paraf
finic and naphthenic fractions of 285, 320, and 365 mol wt reduced
transpiration significantly the first few days after treatment but the
reduction was greatest for the 2 heavier fractions in each series.
Rather rapid recovery was associated with the 2 light fractions and the
320-mol wt naphthenic fraction but the 320-mol wt paraffinic and both
365-mol wt fractions significantly inhibited transpiration throughout
a 70-day period of measurement. Inspection of the physical property
data of the oils indicated that the duration of the effect on transpi
ration was related more to distillation temperatures, hence volatility,
than to any other property, either chemical or physical. Recovery by
the treated plants accompanied dissipation of the oil deposit.
Four commercial-type oils were field-tested to determine the re
lation of oil heaviness and refinement to phytotoxic effects. Early-
season application failed to induce oil blotch although the fruit were
in the most highly susceptible stage, 0.75 to 1.50 inches in diameter.
However, considerable leaf and fruit drop followed this application and
the extent of drop was apparently related inversely to oil heaviness
and refinement.
A late-season application of the same oils was made on the same
trees to study the relation of oil type to adverse effect on degreening


99
A direct linear relationship exists between degreening as measured
by this method and exposure to ethylene gas up to 72 hours, but a tend
ency toward curvilinearity after 48 hours was indicated. This is shown
graphically in Figures 17 and 18 where per cent absorbance is plotted
against degreening time in hours. The degreening rate for the fruit
from each treatment was calculated as the regression coefficient of the
respective curves in these 2 graphs. This is the "b" value in the re
gression equations presented in Table 16. The greater the negative
value for "b," the faster is the degreening rate. Ninety-five per cent
confidence limits were calculated for each "b" value and where these do
not overlap the degreening rates are considered significantly different.
The four 40-fruit samples for each treatment were graded for pack-
out with respect to color after the 72-hour degreening period. The per
cent pack-out for each treatment on the basis of the 160 fruit is given
in the last column under each of the sampling dates in Table 15. These
values indicate the relationship between the absorbance readings and
pack-out. The critical value for 987 or better pack-out appears to be
about 307o absorbance. On the basis of this apparent relationship, the
regression equations for each treatment were used to calculate the hours
degreening time required for the fruit to attain the 307o absorbance
level. These values are presented in Table 16. To supplement the
numerical data on degreening rates, a pictoral record was also obtained.
The photographs in Figure 19 show the appearance of 16-fruit samples
for each treatment on the 2 sampling dates degreened for 0, 24, 48, and
72 hours.
Discussion.--The data presented in Table 15 support the long-
recognized fact that late oil sprays affect the degreening rate of


VISCOSITY, SSU AT 100 F
Figure 8. Efficiency in relation to viscosity for 3 series of narrow-boiling petroleum frac
tions against adult female Florida red scale.
Ui


106
temperature of 40 F during the first 3 days.
Extension of the regression equations in Table 16 to the calcula
tion of the number of hours of ethylene degreening required for the
fruit to acquire satisfactory color shows further evidence that oil
heaviness is a factor in the adverse effect of oil sprays on degreening
rate. Although all oil-treated fruit required a considerably longer
period to degreen than the checks, the difference between the light and
heavy oils was also wide, in favor of the light oil. This becomes es
pecially important for the early sample since the fruit from the light-
oil plots attained the 307 absorbance level in 72 hours (normal maximum
time for commercial degreening) and the fruit from the heavy-oil plots
did not. The difference in effect on degreening between the light and
heavy oils is reflected in per cent pack-out after 72 hours degreening
(Table 15). The photographs in Figure 20 reveal a little more green
color after 72 hours degreening in the fruit treated with the heavy oil
than in the fruit from the other treatments, even in these very limited
samples.
Internal fruit quality
Results.The results of the fruit quality analyses are presented
in Table 17. These include per cent soluble solids, per cent acid,
solids/acid ratio, and per cent juice for all treatments on the 4
sampling dates, and the average fruit diameter for each treatment for
the first 3 sampling dates. Significance of the differences between
means on a given date are indicated. No differences occurred for any
of the factors measured other than solids. The rate of increase in
soluble solids for each treatment with time after spraying is shown
graphically in Figure 20. The horizontal broken line in this graph


122
13. Dallyn, E. L. 1953. Herbicidal action of oils. Cornell Agr.
Exp. Sta. Memoir 316:1-43.
14. Dean, H. A., and J. C. Bailey. 1961. Properties of spray oils
for grapefruit in the Rio Grande Valley of Texas for 1961. J.
Rio Grande Valley Hort. Soc. 15:10-11.
15. Dean, H. A., and J. C. Bailey. 1963. Control of Texas citrus
mites with various spray oil fractions. J. Rio Grande Valley
Hort. Soc. 17:116-122.
16. Dean, H. A., and J. C. Bailey. 1963. Responses of grapefruit
trees to various spray oil fractions. J. Econ. Entomol. 56
(5):547-551.
17. Dean, H. A., E. L. Wilson, J. C. Bailey, R. W. White, and L. A.
Riehl. 1964. A field technique for oil deposit determination
on citrus through colorimetric analysis. J. Econ. Entomol.
57(4):458-461.
18. DeOng, E. R. 1926. Technical aspects of petroleum oils and oil
sprays. J. Econ. Entomol. 19(5):733-745.
19. DeOng, E. R., H. Knight, and J. C. Chamberlin. 1927. A pre
liminary study of petroleum oil as an insecticide for citrus
trees. Hilgardia 2(9):351-384.
20. Duncan, D. B. 1955. Multiple range and multiple F tests.
Biometrics 11:1-42.
21. Ebeling, W. 1932. Experiments with oil sprays used in the con
trol of the California red scale, Chrysomphalus aurantii
(Maskell) (Homoptera: Coccidae) on lemons. J. Econ. Entomol.
25 (5):1007-1012.
22. Ebeling, W. 1936. Effect of oil spray on California red scale
at various stages of development. Hilgardia 10(4):95-125.
23. Ebeling, W. 1945. Properties of petroleum oils in relation to
toxicity to potato tuber moth larvae. J. Econ. Entomol. 38
(1):26-34.
24. Ebeling, W. 1950. Spray oils, p. 165-215. In W. Ebeling, Sub
tropical entomology. Lithotype Press Co., San Francisco.
25. Ebeling, W. 1959. Spray oils, p. 57-66. In W. Ebeling, Sub
tropical fruit pests. Univ. California Div. Agr. Sci., Los
Angeles.
26. Finney, D. J. 1952. Probit analysis. Second edition. Cam
bridge Univ. Press, London. 318 p.


78
Table 10. Respiratory rates of oil-sprayed 'Pineapple'
seedlings expressed as per cent of the check.
Each value is the mean of 6 determinations.
Oils were applied at 70 to 80 |ag/cm2
Oil
Days after
treatment
1
3
7
14
P-305
105.1
100.5
98.6
87.4
P-365
112.4
94.4
88.2
97.6
N-305
92.7
98.8
96.2
102.4
N-365
85.2
101.8
96.5
103.4


MATERIALS AND METHODS
Oil Specifications
The oils used in these studies were obtained from the following
major oil companies: Humble Oil and Refining Company; Gulf Oil Corpora
tion; Sun Oil Company; Shell Oil Company; Texaco, Incorporated; and the
American Oil Company. Of these, Humble was by far the largest con
tributor, providing 23 narrow-distilling, experimental fractions and 10
commercial oils. The other companies contributed both experimental and
commercial products. Specifications on important properties of these
oils appear in Table 3. The 3 narrow-boiling^- series provided by
2
Humble were comprised of paraffinic, naphthenic, and "reformed" frac
tions. These oils provided wide ranges of molecular weight, viscosity,
and distillation temperature in which to study insecticidal, ovicidal,
C
and phytocidal properties. The commercial-type oils included most of
the oils presently used on Florida citrus plus several experimental
materials. Specification data were provided by the oil companies; the
methods hy which the data were obtained are indicated by footnotes to
Table 3.
^-"Boiling" is used synonomously with "distilling" throughout this
paper and refers to the 10 to 90% distillation range, unless otherwise
specified. "Narrow-boiling" is a relative term applying to the first
23 oils listed in Table 3; the remaining oils are commercial products
of wider distillation ranges.
o
The word "reformed" in this paper refers to spray oils which have
received special treatment to alter the component hydrocarbons; the
reformed oils are predominantly paraffinic.
23


94
distillation point the 2 light oils were similar, but the low-refined
oil had a viscosity of 71.7, due mainly to the aromatic content (13.670)
and to the heavy components in the upper portion of the 10 to 907o dis
tillation range. Comparisons may be made, therefore, on the basis of 2
important oil properties--heaviness and refinement.
With respect to oil heaviness, increased leaf drop was associated
with an increase in oil heaviness from the light to the medium range
but not from medium to heavy. This is in agreement with Thompson's
(84) report that no increase in leaf drop on Florida citrus occurred
with increase in viscosity from 72 to 100 SSU. However, the data in
Table 13 indicates less leaf drop in favor of the 60-SSU oil in the
first 4-week period. Riehl et al. (51) reported that increase in leaf
drop following oil sprays may accompany increase in oil heaviness from
200 to 350 mol wt. Smith (72) found that the amount of leaf drop was
related to the weight of the oil as indicated by the distillation
range, and to the quantity of oil deposited on the foliage by the spray
mixture. The data for the light, low-refined oil is in agreement with
reports of California workers (24) that leaf drop is indirectly related
to UR, or refinement, although Thompson (84) reported no difference be
tween oils of low and high UR with respect to "shock to the tree" in
Florida. However, he worked with oils of 70 viscosity and higher and
any effect on leaf drop due to refinement might have been masked by the
effect of oil heaviness.
The data for the fifth-week count of leaf drop are interesting in
that the checks showed a significantly high drop rate. This, plus the
fact that the rate of leaf drop effected by the heavy oils and the low-
UR oil had diminished to a significantly low level by the fifth week,


86
significant increase in transpiration on certain days beyond the twenty-
fifth .
The results discussed above are in general agreement with reports
of other workers. Wedding et al. (98) reported significant reduction
in both respiration and photosynthesis in 'Washington' navel orange
o
leaves with a California medium-grade naphthenic oil at 150 (ig/cm .
Photosynthesis was affected to a greater extent than was respiration.
However, Riehl and Wedding (57) reported no consistent inhibition of
photosynthesis in lemon or lime leaves by California light-medium or
medium-grade spray oils at the same deposit level. But a definite re
lationship between inhibition of photosynthesis and increasing oil de
posit was established (57, 59). Recovery was faster in plants sprayed
with naphthenic oils than in those treated with paraffinic oils, but
the paraffinic oils used were of a higher boiling range and the de
posits were probably more persistent.
Riehl et al. (56) obtained a two-thirds reduction of transpiration
in citrus by a California medium-grade naphthenic oil. They concluded
that the effect on transpiration was due to physical interference by
the spray oil on or in the leaf tissue and that recovery of transpi
ration occurred with dissipation of the oil from the leaves. Full re
covery occurred in 3 to 5 weeks after application (56). Recovery was
faster in plants sprayed with a naphthenic oil than in plants sprayed
with a paraffinic oil of comparable molecular weight (58). However,
the paraffinic oil had a 507 distillation temperature of 663 F while
that of the naphthenic oil was only 642 F. Table 3 shows that the 507
distillation points of the 285, 320, and 365 molecular weight fractions
used in the present study were 1) naphthenic: 635 F, 689 F, and 738 F;


92
of drop. Except for the third week, the low-UR, 72-SSU oil, BR-2,
effected an intermediate rate of drop.
The significance of the differences between the means for- the
weekly drop rates and the totals for the 4- and 5-week periods are
shown in Table 13. The differences were greater in the 4-week period
than in the 5-week period. This can be attributed to the relatively
high rates of leaf drop that occurred in the check plots and R-60 plots
during the fifth week. These tended to equalize the total drop for the
4 oils. All 4 oils effected a significantly higher leaf drop during
the first week than the check. During succeeding weeks the differences
became less significant.
The weekly fruit drop in numbers per 4-tree plot is presented in
Table 14. No significant difference was detected the first week, but
after this time, P-96 and BR-2 effected significant drop throughout the
5-week period. The light, highly-refined oil, R-60, caused no signifi
cant drop at any time. The relationship between treatment and fruit
drop seemed to be the same as that for leaf drop. However, there was
no indication that the total amount of drop in the check plots would
eventually equal that of the oil-sprayed plots.
Discussion.Although no evidence of oil blotch was obtained in
this experiment, considerable leaf and fruit drop was effected by the
various oils. With respect to distillation temperatures, the 4 oils
consisted of 2 light oils (R-60 and BR-2), 1 medium oil (P-96) and 1
heavy oil (BR-1). Of the 2 light oils, 1 was highly refined (96.1 UR)
and the other was of low refinement (85.0 UR); the medium (74.3 vis
cosity) and heavy (92.5 viscosity) oils were both highly refined (95.6
and 94.0 UR, respectively). With respect to molecular weight and 507


8
results obtained by other authors reporting on the subject.
Nelson (40) reported that kerosene penetrated throughout the tra
cheal system and eventually into muscles and nerve ganglia. Woglum
(101) and Woglum and LaFollette (102) found that the residual oil film
killed scale crawlers through inhibition of settling and concluded that
this was an important means by which oil controlled California red
scale.
Smith (73) pointed out that in many instances the oil does not
reach the tracheal system of scale insects, in which case, "...if the
insect succumbs, death is apparently caused by a prolonged impairment
of physiological processes such as might be induced by the presence of
the oil film in the scale covering or in contact with the derm of the
insect's body."
Ebeling (22) corroborated the reports of Woglum (101) and Woglum
and LaFollette (102) concerning inhibition of settling of scale
crawlers and of Smith (73) as to the effect of oil in the scale cover
ing. Ebeling (22) established that crawler settling is inhibited,
whitecap mortality is high where settling does occur, young stages are
more easily killed than adults, and tracheal penetration is the chief
cause of adult mortality but death can occur without it. In addition,
he found adult scales were much more vulnerable to oil treatments where
the margins of their armors were loosened from the substratum. The
scales that survived the treatment gave birth to a high percentage of
dead embryos and dead crawlers. Scales on the branches of the tree
were harder to control because of the absorptive nature of the rough
bark.



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Table 12. Transpiration rate of 'Pineapple' seedlings sprayed with 1.57 concentration of low, medium,
and high molecular weight fractions of paraffinic and naphthenic oils
Days from Water loss
treatment from check3
in mg/cm^
Transpiration rate of oil sprayed plants as per cent of check3
Paraffinic oils
Naphthenic oils
P-285 P-320 P-365 N-285 N-320 N-365
-14
9.8
a
115.8
a
89.6
a
85.3
a
86.3
a
91.0
a
92.0
a
-13
17.2
a
109.2
a
97.5
a
116.8
a
104.5
a
83.3
a
101.6
a
-12
14.0
a
110.3
a
103.5
a
102.3
a
111.7
a
115.5
a
92.5
a
- 8
17.1
a
98.0
a
100.1
a
105.6
a
104.1
a
97.3
a
94.3
a
Sprayed
28 October
1
1964
15.3
a
91.4
ab
68.0
c
98.0
a
76.4
be
67.7
c
76.4
be
2
24.3
a
61.8
b
37.2
c
60.2
be
68.9
b
46.1
be
53.7
be
3
17.2
a
63.8
b
33.3
c
51.5
be
65.1
b
40.6
be
43.4
be
4
24.3
a
78.6
ab
34.4
d
56.2
bed
73.6
abc
50.1
cd
44.5
d
5
16.8
a
74.7
be
52.1
c
68.0
be
81.8
ab
54.9
c
56.5
c
6
15.6
a
73.3
b
46.9
c
59.6
be
73.5
b
62.4
be
54.5
c
7
24.0
a
70.6
b
37.1
d
52.5
bed
68.0
be
51.1
cd
50.6
cd
8
8.4
: a
74.0
b
64.7
b
71.3
b
77.7
b
70.3
b
76.6
b
9
8.2
a
87.0
a
89.4
a
79.0
a
78.1
a
81.4
a
90.6
a
10
25.5
a
82.6
ab
43.3
c
63.6
be
86.0
ab
63.4
be
55.7
c
11
26.4
a
75.4
ab
45.9
c
54.1
be
98.8
a
61.6
be
40.2
c
12
15.7
a
79.5
be
54.5
d
61.5
cd
81.1
b
69.2
bed
51.0
d
13
22.2
a
79.0
b
47.4
d
56.5
cd
80.6
be
70.7
b
47.0
d
14
22.8
a
78.8
abc
54.2
c
62.6
be
85.4
ab
68.5
be
53.6
c
15
22.1
a
76.4
be
61.5
cd
66.4
cd
89.6
ab
70.7
bed
52.5
d
16
22.9
a
77.5
be
57.6
d
61.1
cd
85.1
ab
72.2
bed
54.4
d
00
o


123
27. Fiori, B. J., E. H. Smith, and P. J. Chapman. 1963. Some factors
influencing the ovicidal effectiveness of saturated petroleum
oils and synthetic isoparaffins. J. Econ. Entomol. 56(6):885-
888.
28. Ginsburg, J. M. 1931. Penetration of petroleum oils into plant
tissue. J. Agr. Res. 43(5):469-474.
29. Gray, G. P., and E. R. DeOng. 1925. Laboratory and field tests
of California petroleum insecticides. Ind. Eng. Chem. 18:175-
180.
30. Green, J. R., and A. H. Johnson. 1931. Effect of petroleum oils
on the respiration of bean leaves. Plant Physiol. 6:149-159.
31. Green, J. R. 1936. Effect of petroleum oils on the respiration
of bean plants, apple twigs and leaves, and barley seedlings.
Plant Physiol. 11:101-113.
32. Grierson, W., and W. F. Newhall. 1960. Degreening of Florida
citrus fruits. Univ. Florida Agr. Exp. Sta. Bull. 620. 80 p.
33. Grierson, W., M. F. Oberbacher, and W. L. Thompson. 1960. Fruit
color, grove practices, and fresh fruit pack-out with particu
lar reference to tangerines. Proc. Florida State Hort. Soc.
73:96-100.
34. Harding, P. L. 1953. Effects of oil emulsion and parathion
sprays on composition of early oranges. Proc. Amer. Soc.
Hort. Sci. 61:281-285.
35. Hubbard, H. G. 1885. Insects affecting the orange. U. S.
Government Printing Office, Washington, D. C. 227 p.
36. Knight, H., J. C. Chamberlin, and C. D. Samuels. 1929. On
some limiting factors in the use of saturated petroleum oils
as insecticides. Plant Physiol. 4:299-321.
37. McMillan, R. T., and J. M. Riedhart. 1964. The influence of
hydrocarbons on photosynthesis of citrus leaves. Proc.
Florida State Hort. Soc. In Press.
38. Merrin, G. A. 1929. The effect of oil sprays on the transpi
ration of citrus. Proc. Florida State Hort. Soc. 42:219-224.
39. Minshall, W. H., and V. A. Helson. 1949. Herbicidal action of
oils. Proc. Amer. Soc. Hort. Sci. 53:294-298.
Nelson, F. C. 1927. The penetration of a contact oil spray into
the breathing system of an insect. J. Econ. Entomol. 20(4):
632-635.
40.


PROBIT OF PER CENT KILL
54
Figure 6. Regression of per cent kill on deposit level for 3 series of
narrow-boiling petroleum fractions tested against adult female
Florida red scale. The number on each line indicates the average
molecular weight of the fraction.
PER CENT KILL OF ADULT FEMALE FLORIDA RED SCALE


Figure 16. Accumulated leaf drop from 'Hamlin' orange trees in the 5-week period
following application of 4 oils on 6 May 1964.


Table 3--Continued
Oil
No.a Name^
Avg
mol
wt
Viscosity,
SSU at UR,
100 Fc %
Chemical composition*^
API
gravity6
Temper ature, F,
for distillation
(760 mm Hg) of:^
10-90%
distillation
range, F
7oC.
A
%CN
7oCp
! 10%
50%
90%
46
G-5
384
103.0
93.0
4.0
44.0
52.0
28.5
643
700
756
113
47
S-l
-
61.8
91.0
16.2
-
-
37.5
613
671
711
98
48
S-2
310
69.6
95.0
4.0
32.0
64.0
33.9
644
688
696
52
49
S-3
-
86.5
94.0
-
-
-
32.6
666
695
723
57
50
A-1
-
85-98
89.0
-
-
-
30.0
-
-
-
-
51
NG-1
310
76.5
88+
12.0
24.0
64.0
671
717
750
79
52
NG-2
312
56.0
92+
12.0
22.0
66.0
-
628
651
690
62
53
SL-1
275
58.8
94.8
-
-
-
31.1
582
640
692
110
54
SL-2
275
57.6
93.6
-
-
-
30.7
582
630
688
106
55
P-60

60.0
-

-
Oil numbers were drawn from a larger table of specifications,
bp = paraffinic; R = reformed; N = naphthenic; all other letters are code numbers for convenient reference.
cConverted from Kinematic to Saybolt Universal, in accordance with ASTM D-446, or similar methods,
d
CA aromatic carbons; Cjg = naphthenic carbons; Cp = paraffinic carbons.
eBy ASTM D-287, or similar methods.
Converted from 10 mm Hg in accordance with Note 2 of ASTM D-1160, or similar methods.
K>
O'


Table 2. Specifications for
oils applied to fruit and shade
trees in New
York3
100-second
superior oil
70-second
superior oil
60-second
superior oil
Saybolt Universal
viscosity at 100 F
90-120
66-74
56-62
Gravity, API
(minimum)
31
33
34
Unsulfonated residue
(minimum), %
90
92
92
Pour point, F
(maximum)
30
20
20
Distillation temperature, F,
at 760 mm Hg
(a relatively narrow
distillate portion of
petroleum)
507, point
670 + 10
645 + 8
107-907 range
(maximum)
90
75
Compiled from Chapman and Pearce (7), Chapman (8), and Chapman et al. (9).


2
requirements. Although the available oils are quite diverse in their
properties, their use by Florida citrus growers over the past few years
has not generally resulted in excessive damage. However, damage from
oil sprays is not uncommon even though it is not always striking.
Where problems do occur, information about oil properties, formulation,
and application, sufficient to establish a probable cause, is seldom
available. Information pertaining to the relationship between chemical
and physical properties of spray oils and performance on Florida citrus
is needed.
The objective of the work reported herein was to establish the re
lationship of physical and chemical properties of petroleum oil to in
secticidal and ovicidal efficiency, and to phytotoxicity to citrus,
under Florida conditions. Three series of narrow-distillation range,
experimental fractions and numerous commercial oils provided wide
ranges of the various properties for study. The oils were tested in
the laboratory against adult female Florida red scale, Chrysomphalus
aonidum (L.), and against eggs of the citrus red mite, Panonychus citri
(McGregor), to establish the effective ranges of the various properties
for insecticidal and ovicidal efficiency. Phytotoxicity studies were
conducted under both laboratory and field conditions to relate oil
heaviness, refinement, and chemical composition to various adverse
effects on citrus. The results obtained may serve as a guide for ad
ditional field studies, leading eventually to more rigid specifications
for petroleum oils used on citrus in Florida.


105
ETHYLENE DEGREENING
OCTOBER 1. 1904
Figure 19. 'Hamlin' oranges from plots receiving late-season applica
tion of 4 oils and degreened for 0, 24, 48, and 72 hours; sampled
4 and 8 weeks after treatment. Sprays applied 18 September 1964.


114
effect on solids at the time of harvest after mid-October. This would
be of great importance to growers with large acreages who sometimes
find difficulty in completing their summer oil applications by the
1 August deadline. However, extensive field testing is necessary be
fore recommendations for oil specifications can be presented. The
specifications desired are those which combine full pesticidal effi
ciency with minimum phytotoxic effects.


127
80. Stofberg, F. J., and E. F. Anderssen. 1949. Effects of oil
sprays on the yield and quality of navel and Valencia oranges.
Union of South Africa Dept. Agr. Sci. Bull. 296:1-19.
81. Swingle, H. S., and 0. I. Snapp. 1931. Petroleum oils and oil
emulsions as insecticides, and their use against the San Jose
scale on peach trees in the south. U. S. Dep. Agr. Tech. Bull.
253. 48 p.
82. Thompson, W. L. 1942. Some problems of control of scale insects
on citrus. Proc. Florida State Hort. Soc. 55:51-59.
83. Thompson, W. L., and J. W. Sites. 1945. Relationship of solids
and ratio to the timing of oil sprays on citrus. Proc.
Florida State Hort. Soc. 58:116-123.
84. Thompson, W. L. 1948. Spray control for the control of mites and
scale insects in Florida. Lower Rio Grande Valley Citrus and
Vegetable Institute, Third Annu. Proc. p. 95-105.
85. Thompson, W. L. 1949. The relationship of timing post-bloom
sprays to certain fruit blemishes on oranges. The Citrus Ind.
30(4):5-8, 18.
86. Thompson, W. L., and J. T. Griffiths, Jr. 1949. Purple scale and
Florida red scale as insect pests of citrus in Florida. Univ.
Florida Agr. Exp. Sta. Bull. 462:33-36.
87. Thompson, W. L., J. T. Griffiths, Jr., and J. W. Sites. 1950. A
progress report on parathion as an insecticide for citrus trees
in Florida. Citrus Mag. 12(9):30-33.
88. Thompson, W. L. 1951. Important mites attacking citrus and their
control. Citrus Mag. 13(11):20-22.
89. Thompson, W. L., J. T. Griffiths, Jr., and J. W. Sites. 1951. A
comparison of oil emulsion and parathion for the control of
scale insects on citrus. Proc. Florida State Hort. Soc. 64:
66-71.
90. Thompson, W. L., R. B. Johnson, and J. W. Sites. 1954. The
status of the purple mite and its control. Proc. Florida State
Hort. Soc. 67:50-56.
91. Thompson, W. L. and E. J. Deszyck. 1957. Phosphatic insecticides
mixed with oil emulsions for scale control and their effect on
fruit quality. Proc. Florida State Hort. Soc. 70:31-38.
92. Thompson, W. L. 1959. Leaf drop following spray applications on
citrus. Proc. Florida State Hort. Soc. 72:29-34.
93. Thompson, W. L., R. F. Brooks, and M. F. Oberbacher. 1961. Re
sults of spray programs on tangerines in relation to scale con
trol and fruit color. Proc. Florida State Hort. Soc. 74:58-62.


96
cases groves appearing to be in excellent condition have suffered as
heavy drop as those which appeared to be in a poor state of vigor."
Fruit color and ethylene degreening
Results.--The fruit samples harvested 16 October and 12 November
were degreened with ethylene gas for 72 hours. The color of the fruit
was measured after 0, 24, 48, and 72 hours exposure to the gas to de
termine the degreening rate. The color values obtained for the differ
ent samples at each of the 4 readings are presented as per cent ab
sorbance in Table 15. Each value is the average of measurements on
40 fruit. Per cent absorbance is directly related to the amount of
green color in the fruit peel. As indicated by the letters adjacent
to the treatment means for each time of degreening on each sampling
date, fruit from oil-sprayed plots were significantly greener than the
check fruit at harvest, and this relationship held throughout the 72-
hour degreening period with only 2 exceptions. Fruit from trees spray
ed with P-96 degreened to the same level as check fruit in the 4-week
sample and fruit from trees treated with R-60 did likewise at the 8-
week sampling. However, the effect of P-96 should be viewed with some
skepticism since a temporary fault in the sprayer at the time of appli
cation resulted in a dilution of the spray and a low, unknown level of
oil deposit. Closer inspection of the data for the 4-week sample shows
the 72-SSU, low-UR oil, BR-2, and the 92-SSU, high-UR oil, BR-1, had
the greatest adverse effect on color. This same relation held at har
vest time for the 8-week sample but after 24 hours degreening no sig
nificant difference existed between the oils, although all oil-treated
fruit were greener than the check fruit.


14
accomplished by breaking down of the plasma membrane of the cell by the
process of solubilization. However, they pointed out that solubiliza
tion would not occur with molecules as large as those of foliage spray
oils. Other workers (10, 13, 39) have studied the penetration and
phytotoxic action of herbicidal oils. In general, the herbicidal
activity is related inversely to the heaviness of oil and directly to
the aromatic hydrocarbon content. However, the petroleum spray oils
are considerably higher-boiling and more highly-refined than the
herbicidal oils. The light herbicidal oils are considerably more pene
trating than the foliage spray oils.
Effects of oil on the physiological processes of plants
Application of oil sprays has resulted in reduced transpiration
rates of citrus trees (36, 38, 56, 58) and of deciduous fruit trees
(109). Merrin (38) reported a 25 to 30% decrease on citrus in Florida,
with very little difference between first, second, or third-flush
growth. Knight et al. (36) reported reduction of transpiration of
citrus by 50-SSU and 106-SSU oils but recovery was faster with the
light oil.
Riehl et al. (56) determined the effect of a medium-grade
California oil on transpiration of several varieties of citrus in the
laboratory. On the first day after the application of 1.75% oil in
aqueous mixture, transpiration of the oil-sprayed plants was reduced to
one-third that of untreated plants. The reduction seemed to be due to
physical interference by the oil on or in the leaf tissue and recovery
was apparently related to dissipation of the oil from the leaves.
Transpiration was restored to original levels in the treated plants in
3 to 5 weeks after treatment. Riehl and Wedding (58) studied the


40
made 18 days after treatment. The scales killed by the oil were easily
identified by the brown discoloration of the body in contrast to the
bright lemon-yellow color of live, healthy scales. Mortality was de
termined by turning the scale armor and inspecting the condition of the
insect's body under 3X magnification. Only the scales in an equatorial
band of 2.0 to 2.5 inches were considered.
Testing the oils.--The testing of the oils against Florida red
scale included dosage-mortality tests for selected oils of the 3 nar
row-boiling series and screening of the commercial-type oils at 2
levels of application.
Dosage-mortality tests were run on 6 selected oils of the
naphthenic and paraffinic series and 5 of the reformed series. Each
oil was applied at 8 concentrations, each replicated on 3 scale-infested
fruit. Therefore each point on the dosage-mortality curves represents
the response of approximately 300 individuals. In these tests, all
dosage levels for the oils in a given series were applied on the same
day.
The dosage-mortality data were submitted to the University of
Florida Computing Center for analysis. Probit regression lines were
fitted according to the methods of Finney (26), giving the maximum like
lihood solution with adjustment for natural mortality. The input data
were oil deposit (p.g/cm^), total scales, and the number killed for each
deposit level. The computer print-out provided regression coefficients
and both LD^q and LDg^ values with their 95% confidence intervals.
The commercial oils were compared at 0.57 and 1.25% oil concentra
tion in randomized block experiments with 5 replicates for each treat
ment. Due to the large number of oils tested and differences in age of


Rohm and Haas Company is appreciated.
The author expresses special appreciation to his wife for her
understanding, encouragement, and support during the years of study
prior to the preparation of the manuscript, and for her cooperation
and assistance in preparation of the manuscript.
He wishes to thank Mrs. Cynthia Boyd Evans for performing the
final typing and assisting in the Multilith duplication of the
manuscript.
iii


Table 7. Oil deposit, number of eggs, and per cent kill with 3 series of petroleum oils in dosage-
mortality tests against citrus red mite eggs
Dosage levels, high to low deposit
Oil
1
2
3
4
5
6
7
8
9
10
11
pg/cm2
135
124
111
69
42
16
0
_
_
P-250
Eggs
421
372
408
417
431
405
430
-
-
-
-
7o kill
45
38
32
19
9
10
2.0
-
-
-
-
pg/cm2
108
90
74
43
32
18
0
-
-
-
-
P-265
Eggs
397
487
410
443
404
405
430
-
-
-
-
7o kill
71
57
71
41
34
9
2.0
-
-
-
-
pg/cm2
121
78
45
36
25
20
0
-
-
-
-
P-285
Eggs
427
550
412
392
384
419
430
-
-
-
-
% kill
99
95
85
80
34
20
2.0
-
-
-
-
pg/cm2
88
48
42
20
20
17
14
6
3
0
-
P-305
Eggs
414
443
547
453
484
491
472
448
404
442
-
7o kill
98
100
99
98
90
89
69
62
35
1.3
-
pg/cm2
84
45
36
18
15
13
9
8
4
3
0
P-320
Eggs
410
419
464
471
481
502
449
433
117
451
442
% kill
99
98
100
97
96
87
68
86
59
62
1.3
pg/cm2
78
48
47
31
18
16
8
5
3
2
0
P-365
Eggs
449
434
497
515
473
443
464
413
472
428
442
% kill
97
99
99
98
98
96
95
86
83
70
1.3
pg/cm2
82
58
48
38
26
23
19
16
14
5
0
P-435
Eggs
444
432
497
487
502
452
431
447
467
424
442
7o kill
100
95
97
96
95
97
96
92
89
82
1.3
pg/cm2
85
50
42
32
26
21
18
13
10
10
0
P-520
Eggs
485
483
474
464
429
456
439
440
395
406
442
7o kill
99
95
86
87
86
87
83
76
77
66
1.3