Citation
Characterization of Vanadium, Copper, and Iron Adsorption Kinetics in Ion Exchange Resins: Part II

Material Information

Title:
Characterization of Vanadium, Copper, and Iron Adsorption Kinetics in Ion Exchange Resins: Part II
Creator:
Creagan, Jesse
Brenton, Ryan
Publication Date:
Language:
English

Subjects

Subjects / Keywords:
Adsorbents ( jstor )
Adsorption ( jstor )
Flasks ( jstor )
Inlets ( jstor )
Ions ( jstor )
Isotherms ( jstor )
Kinetics ( jstor )
Resins ( jstor )
Vanadium ( jstor )
Velocity ( jstor )
Chemical kinetics
Copper
Iron
Vanadium
Genre:
Undergraduate Honors Thesis

Notes

Abstract:
The main goal of this experimentation is to characterize an ion exchange column that is used to remove Cu, V, and Fe from an acidic stream that contains a mixture of organic acids and develop kinetics models that support previously collected data. In order to do this it is necessary to develop a characteristic differential equation that expresses the concentration as a function both of position and time in the column. This equation, in conjunction with the equilibrium data for the metals with the resin and empirically obtained run data, can be used to develop kinetics models that accurately represent the adsorption and desorption process. To develop these it will also be necessary to obtain the exhaustion data (i.e. complete saturation) of the resins. ( en )
General Note:
Jesse Creagan awarded Bachelor of Science in Chemical Engineering; Graduated May 8, 2012 summa cum laude. Major: Chemical Engineering
General Note:
College/School: College of Engineering
General Note:
Ryan Brenton awarded Bachelor of Science in Chemical Engineering; Graduated May 8, 2012 summa cum laude. Major: Chemical Engineering
General Note:
Legacy honors title: Only abstract available from former Honors Program sponsored database.
General Note:
Advisor: Spyros Svoronos

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Source Institution:
University of Florida
Holding Location:
University of Florida
Rights Management:
Copyright Jesse Creagan and Ryan Brenton. 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.

Full Text

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Characterization of Vanadium, Copper, and Iron Adsorption Kinetics in Ion Exchange Resins : Part II Author : Jesse Creagan Coauthor: Ryan Brenton

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Contents 1 Introduction ................................ ................................ ................................ ............................. 3 1.1 Background: ................................ ................................ ................................ ..................... 3 1.2 Purpose: ................................ ................................ ................................ ............................ 4 2 Experimental P rocedure ................................ ................................ ................................ .......... 4 3 Modeling and Characterization ................................ ................................ ............................... 6 3.1 Column Characterization ................................ ................................ ................................ .. 6 3.2 Rate Constants ................................ ................................ ................................ .................. 7 4 Isotherm analysis using Equilibrium data: ................................ ................................ .............. 8 5 Results : ................................ ................................ ................................ ................................ .... 8 6 Figures: ................................ ................................ ................................ ................................ .. 10 7 SOP ................................ ................................ ................................ ................................ ........ 25 8 Bibliography ................................ ................................ ................................ .......................... 29 F IGURE 1: V ANADATE I ON ................................ ................................ ................................ ................................ ............... F IGURE 2: V ANADATE I ON M M I NTERACTION ................................ ................................ ................................ ............... F IGURE 3: V 2 O 7 4 C OMPLEX ................................ ................................ ................................ ................................ ......... 10

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F IGURE 4: V 4 O 12 4 C OMPLEX ................................ ................................ ................................ ................................ ....... 10 F IGURE 5: V3O93 C OMPLEX ................................ ................................ ................................ ................................ ....... 11 F IGURE 6: MO V ANADATE ................................ ................................ ................................ ................................ ........... 11 F IGURE 7: P OLYMATH C ODE ................................ ................................ ................................ ................................ ...... 12 F IGURE 8: R ESIN D V ANADIUM I SOTHERM ................................ ................................ ................................ ................... 13 F IGURE 9: R ESIN T V ANADIUM I SOTHERM ................................ ................................ ................................ ................... 13 F IGURE 10: R ESIN D C OPPER I SOTHERM ................................ ................................ ................................ ...................... 14 F IGURE 11: R ESIN T C OPPER I SOTHERM ................................ ................................ ................................ ....................... 14 F IGURE 12: R ESIN D F E I SOTHERM ................................ ................................ ................................ ............................... 15 F IGURE 13: R ESIN T F E I SOTHERM ................................ ................................ ................................ ............................... 15 F IGURE 14: I NVERSE L ANGMUIR I SOTHERM R ESIN D C OPPER ................................ ................................ ...................... 16 F IGURE 15: I NVERSE L ANGMUIR I SOTHERM FOR R ESIN T C OPPER ................................ ................................ ............... 16 F IGURE 16: F REUNDLICH I SOTHERM FOR R ESIN D V ANADIUM ................................ ................................ .................... 17 F IGURE 17: F REUNDLICH I SOTHERM FOR R ESIN T V ANADIUM ................................ ................................ ..................... 17 F IGURE 18: G RAPH D ISPLAYING E XPERIMENTALLY C OLLECTED D ATA WITH F ITTED C URVE FOR THE O UTLET V C ONCENTRATION OF A C OLUMN WITH 100 M L OF R ESIN T WITH I NLET C ONCEN TRATION 57 PPM ....................... 19 F IGURE 19: P OLYMATH M ODEL OF C OLUMN DESCRIBED BY F IGURE 18 ................................ ................................ ...... 19 F IGURE 20: G RAPH D ISPLAYING E XPERIMENTALLY C OLLECTED D ATA WITH F ITTED C URVE FOR THE O UTLET V C ONCENTRATION OF A C OLUMN WITH 100 M L OF R ESIN D WITH I NLET C ONCENTRATION 57 PPM ....................... 20 F IGURE 21: P OLYMATH M ODEL OF C OLUMN DESCRIBED BY F IGURE 20 ................................ ................................ ...... 20 F IGURE 22: G RAPH D ISPLAYING E XPERIMENTALLY C OLLECTED D ATA WITH F ITTED C URVE FOR THE O UTLET C U C ONCENTRATION OF A C OLUMN WITH 30 M L OF R ESIN D WITH I NLET C ONCENTRATION 21 PPM ......................... 21 F IGURE 23: P OLYMATH M ODEL OF C OLUMN DESCRIBED BY F IGURE 22 ................................ ................................ ...... 21 F IGURE 24: G RAPH D ISPLAYING E XPERIMENTALLY C OLLECTED D ATA WITH F ITTED C URVE FOR THE O UTLET V C ONCENTRATION OF A C OLUMN WITH 30 M L OF R ESIN D WITH I NLET C ONCENTRATION 36 PPM ......................... 22 F IGURE 25: P OLYMATH M ODEL OF C OLUMN DESCRIBED BY F IGURE 24 ................................ ................................ ...... 22 F IGURE 26:G RAPH D ISPLAYING E XPERIMENTALLY C OLLECTED D ATA WITH F ITTED C URVE FOR THE O UTLET C U C ONCENTRATION OF A C OLUMN WITH 30 M L OF R ESIN T WITH I NLET C ONCENTRATION 21 PPM ......................... 23 F IGURE 27: P OLYMATH M ODEL OF C OLUMN DESCRIBED BY F IGURE 26 ................................ ................................ ...... 23 F IGURE 28: G RAPH D ISPLAYING E XPERIMENTALLY C OLLECTED D ATA WITH F ITTED C URVE FOR THE O UTLET V C ONCENTRATION OF A C OLUMN WITH 30 M L OF R ESIN T WITH I NLET C ONCENT RATION 36 PPM ......................... 24 F IGURE 29: P OLYMATH M ODEL OF C OLUMN DESCRIBED BY F IGURE 28 ................................ ................................ ...... 24 1 Introduction 1.1 Background: The term AMLS refers to Aqueous Mother Liquor Stream, and is a byproduct in the production of Nylon 6 6. Ascend Performance Materials, one of the leaders in U.S. production

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of Nylon 6 6, has provided samples of AMLS for the analysis of this project. This untreated AMLS contains traces of Copper, Vanadium, and Iron. Ascend Performance Materials tasked an IPPD team under Dr. Svoronos to remove these metal ions while retaining t he organics in the aqueous solution. After two semesters of experimentation and elimination of possible removal methods, the team focused their efforts on two ion exchan ge resins, labeled D and T These provided the best consistent metal removal. This dete rmination was made on data collected for varying superficial velocities and metal concentrations of the feed stream, as well as for different bed heights of resin. The continuation of this project seeks to further analyze the data collected in the previou s two semesters and utilize it creat e new models based on the resin s kinetics An extended look into the possibility of anionic complexes, their kinetic effect on adsorption, and the feasibility of column characterization using equilibrium data is explore d. 1.2 Purpose: The main goal of this experimentation is to characterize an ion exchange column that is used to remove Cu, V, and Fe from an acidic stream that contains a mixture of organic acids and develop kinetics models that support previously collected data. In order to do this it is necessary to develop a characteristic differential equation that expresses the concentration as a function both of position and time in t he column. This equation, in conjunction with the equilibrium data for the metals with the resin and empirically obtained run data, can be used to develop kinetics models that accurately represent the adsorption and desorption process. To develop these it will also be necessary to obtain the exhaustion data (i.e. complete saturation) of the resins. The secondary objective of this experimentation is to examine the possibility of the presence of anionic Vanadium matrices, and to determine whether they can be removed via adsorption to a basic ion exchange resin The objective was chosen becaus e, during ion removal with cationic resins, Vanadium was consistently the hardest metal to remove. It is known that the acidic solution contains the higher oxidation states of Vanadium including Vanadium(V) These higher oxidation states of Vanadium typic ally form complex matrices in aqueous solutions that may affect the overall rate of adsorption and desorption for Vanadium on the resin. Seeing as this is a preliminary analysis into the possibility of this type of matrix forming it will not assume or prop ose that any one type of complex forms, but rather empirically determine whether any could exist. The project will therefore reference different complexes and their properties that are known to exist, rather than hypothesize that any one in particular. 2 Experimental Procedure The experimental procedure for the data collection was similar to that of the IPPD project (see SOP) There were three primary pieces of data that needed to be collected in order to attempt to meet the experiments objectives.

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The fi rst set of data required exhausting the resin to its fullest saturation capacity. This would be the point at which all of the solution running through the column would be in equilibrium with the resin for the entire height of the column. This would mean th at a mass balance on this system would yield no accumulation of metals on the resin. In order to do this 100mL of both resins were run at a rate of 24 bv/h for 75 bed volumes. This was chosen as an overshoot estimate for the saturation limits of the resins and was based on previous data obtained from the IPPD experiment. The analysis of the data from these runs showed that even the Vanadium, the metal which most easily breaks through, was still having marginal removal. The other metals, Copper and Iron, we re still having significant removal. Another run was conducted at a resin volume of 30 mL and at a rate o 24 bv/h for 66 bed volumes. It was intended for both resins to again be run to 75+ bed volumes however due to a lack of solution 66 was the max that could be reached. The analyzed data for this set of runs showed breakthrough and saturation for both the Copper and the Vanadium, however the Iron, was still strongly being adsorbed. The second set of data required obtaining equilibrium data between the resins and the metals. In order to do this 20 mL of resin was added to 5 different concentrations of solution. The different concentrations were obtained by dilution of the original solution. The analysis of this data showed that nearly all of the metals w ere adsorbed in all 10 test samples. In order to obtain proper equilibrium data the samples were spiked with 1000ppm standards of Vanadium and 10,000ppm standards of Copper. Unfortunately there was no pure standard of Iron within the ppm range needed to do pe the samples. The third set of data needed is that for the anionic resin to determine whether negatively charged complexes of Vanadium can exist in the solution. The anionic resin was run in a similar fashion to the data collected during the screening p rocess of the IPPD project. Seven bed volumes of solution were run at a rate of 10 bv/h and at a resin volume of 100mL. All seven bed volumes were collected for analysis.

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3 Modeling and Characterization 3.1 Column Characterization Column Characterization Equation: D L axial dispersion coefficient, m/s V superficial velocity, m/s p particle density, kg/m3 q p concentration adsorbed on the particle, mg/g The equation above represents the overall balance for a column with resin that exhibits non competitive characteristics. For the basis of initial calculations the assumption is being made that the amount of diffusion throug hout the column is minimal in comparison to the other terms in the equation. Also the change in superficial velocity with respect to the change in height is extremely small in comparison with the other terms. The simplified model used in the characterizat ion of the column is dependent only on the change in concentration of a given species with respect to both time and the position in the column, and is zero at equilibrium. This equation can also be obtained by taking the total derivative of the concentration: The first term on left side is the change in concentration with respect to time multiplied by the velocity. The concentration derivative will be approximated by a first order Tayl or expansion. The second term is simply the rate equation for the adsorption reaction. The resulting numerical model is of the form:

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C1 concentration at point 1 C2 and C3 are the concentration entering and exiting the control volume around point 1 V superficial velocity r rate equation The resin and liquid concentrations at various times and locations were solved for by cascading this equation; the indices are incremented, and one equation feeds the next. Increasing t he number of equations can be used to either increase the resolution of the column characterization or increase the column height by an equivalent number of control volumes with no subsequent loss in resolution. 3.2 Rate Constants Were proper equipment availa ble, experiments would have been conducted to determine the rate constants for each of the adsorption reactions. The accuracy and time sensitivity necessary for such experimentation could not be provided by ICP. Alternatively, it was proposed that the rat e constants could be solved for using the data from the exhaustion experiments. By using the above equations and Polymath differential equation solver, it would be possible to back solve for the k values. First, the data was organized based on column hei ght, resin, and inlet ion concentration. Both exhaustion experiments were conducted at the same flow rate, but varied in each of the other aspects mentioned. This data was graphed as outlet concentration versus time. Visual inspection indicated that the d ata followed a sigmoid function. A best fit model following a sigmoid response was then calc ulated for each of set of data. These graphs were then used as boundary conditions for the differential model in Polymath. The results of these program outputs can be seen in Figures 18 29.

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4 Isotherm analysis using Equilibrium data: In order to find the equilibrium relations for adsorbents it is important to determine what type of adsorption isotherm they follow. Generally the ratio q, mass weight of adsorbate over adsorbent, is plotted against the mass concentration of adsorbate. The most common and strongly favored type of isotherm follows the Langmuir model, which generates some kind of log curve. There is a theoretical basis for the Langmuir isotherm and it can be shown to follow in which q o and K are empirical constants th at are determined via a plot of 1/q versus 1/c, the slope of this is K/q o and the intercept is 1/q o A nother favorable type of isotherm is the Freundlich model which follows a power law equation that follows where K and n are determined via a plot of the log log data for q and c. 5 Results : The equilibrium data for both resin D and T shows that the Vanadium has a tendency to follow the Freundlich model (Figures 7 8) where as the Copper tends to form a Langmuir isotherm (Figures 9 10). Iron concentrations above the lower limits of the ICP machine were not achieved. Therefore, equilibrium data was not obtained, and no isotherm could be determined wi thout further testing (Figures 11 12). The plots of 1/q vs. 1/c for the Cu Langmuir curves and the log log plots of q vs. c for the V Freundlich curve are shown in (Figures 13 16). Using the above equations the constant values for K, qo, and n can be calc ulated. Seven 100 mL samples were run through the resin. The experimental results show a disappointingly large amount of Vanadium in the samples that were in contact with the resin. Although some of the samples appear to be slightly lower in concentration, the variability and accuracy of the ICP machine is such that they should all be considered to be equivalent. It can be concluded from this evidence that the pH of the AMLS solution in conju n ction with the presence of the highly oxidizing Nitric acid resul ts in Vanadium that either does not form complexes or forms only cationic or neutral species. The kinetics model describing the ion exchange column could not be fully solved for. The model used was an over simplification of the actual process and would n eed more data in order to accurately characterize the system. In addition it would require more computational power, and possibly a better differential equation solver than polymath. The model does appear to be able to characterize the column for the cases in which there is data, because this allows the

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specification of both inlet and outlet conditions. At present it does not allow for a predicative model.

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6 Figures: Figure 3 : V 2 O 7 4 Complex Figure 4 : V 4 O 12 4 Complex Figure 1 : Vanadate Ion Figure 2 : Vanadate Ion M M Interaction

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Figure 5 : V3O93 Complex Figure 6 : MO Vanadate

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Figure 7 : Polymath Code y = 0.0943x 0.3137 R = 0.9367 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0 10 20 30 40 50 q (kg adsorbate/kg adsorbent) Concentration V Resin D Vanadium Isotherm Dowex V Power (Dowex V)

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Figure 8 : Resin D Vanadium Isotherm Figure 9 : Resin T Vanadium Isotherm y = 0.1098x 0.3366 R = 0.9389 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45 0.5 0 10 20 30 40 50 q (kg adsorbate/ kg adsorbent) Concentration V Resin T Vanadium Isotherm Series1 Power (Series1)

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Figure 10 : Resin D Copper Isotherm Figure 11 : Resin T Copper Isotherm y = 0.3754ln(x) + 0.5868 R = 0.9807 0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2 0 10 20 30 q (kg adsorbate / kg adsorbent) Concentration Cu Resin D Copper Isotherm Dowex Cu Log. (Dowex Cu) y = 0.3642ln(x) + 1.1823 R = 0.8087 0 0.5 1 1.5 2 2.5 3 0 10 20 30 40 q (kg adosrbate/ kg adsorbent) Concentration Cu Resin T Copper Isotherm Series1 Log. (Series1)

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Figure 12 : Resin D Fe Isotherm Figure 13 : Resin T Fe Isotherm 0 0.01 0.02 0.03 0.04 0.05 0.06 0 0.05 0.1 0.15 0.2 0.25 0.3 q (kg adsorbate/kg adsorbent) Concentration Fe Resin D Fe Isotherm Series1 0 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0 0.1 0.2 0.3 0.4 0.5 q (kg adsorbate/kg adsorbent) Concentration Fe Resin T Fe Isotherm Series1

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Figure 14 : Inverse Langmuir Isotherm Resin D Copper Figure 1 5 : Inverse Langmuir Isotherm for Resin T Copper y = 1.9297x + 0.4825 R = 0.98 0 0.2 0.4 0.6 0.8 1 0 0.05 0.1 0.15 0.2 0.25 1/q 1/c Inverse Langmuir Isotherm for Resin D Copper Series1 Linear (Series1) y = 1.4886x + 0.3238 R = 0.975 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0 0.05 0.1 0.15 0.2 1/q 1/c Inverse Langmuir Isotherm for Resin T Copper Series1 Linear (Series1)

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Figure 16 : Freundlich Isotherm for Resin D Vanadium Figure 17 : Freundlich Isotherm for Resin T Vanadium y = 0.0943x 0.3137 R = 0.9367 0.01 0.1 1 0.1 1 10 Log_10 of q Log_10 of c Freundlich Isotherm of q vs c for Resin D Vanadium Series1 Power (Series1) y = 0.1098x 0.3366 R = 0.9389 0.1 1 0.1 1 10 100 Log_10 of q Log_10 of c Freundlich Isotherm of q vs c for Resin T Vanadium Series1 Power (Series1)

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Table 1 : Experimentally Determined Equilibrium Constants K Values Using PSSA (mg resin*L/mol^2) Resin Cu V Fe Dowex 0.003037356 0.000884 N/A Thermax 0.009649013 0.00032 N/A Table 2 : Experimentally Determined Freundlich and Langmuir Coefficients K, q0, n Values Using Freundlich and Langmuir Isotherms Resin Cu V Fe K q0 K n Dowex 4.005 2.072 0.0943 0.3137 N/A Thermax 4.59728 3.088 0.1098 0.3366 N/A

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Figure 18 : Graph Displaying Experimentally Collected Data with Fitted Curve for the Outlet V Concentration of a Column with 100mL of Resin T with Inlet Concentration 57ppm Figure 19 : Polymath Model of Column described by Figure 18 -10 0 10 20 30 40 50 60 0 50 100 150 200 100mL Resin T C_V=57 Thermax T-46ish Fitted Model(30mL)

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Figure 20 : Graph Displaying Experimentally Collected Data with Fitted Curve for the Outlet V Concentration of a Column with 100mL of Resin D with Inlet Concentration 57ppm Figure 21 : Polymath Model of Column described by Figure 20 -10 0 10 20 30 40 50 60 0 50 100 150 200 Outlet Concentration (ppm) Time(min) 100mL Resin D C_V= 57 100mL fitted(100mL)

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Figure 22 : Graph Displaying Experimentally Collected Data with Fitted Curve for the Outlet Cu Concentration of a Column with 30mL of Resin D with Inlet Concent ration 21ppm Figure 23 : Polymath Model of Column described by Figure 22 0 5 10 15 20 25 0 50 100 150 200 Outlet Concentration (ppm) Time(min) 30mL Resin D C_Cu= 21 30mL Fitted Model(30mL)

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Figure 24 : Graph Displaying Experimentally Collected Data with Fitted Curve for the Outlet V Concentration of a Column with 30mL of Resin D with Inlet Concentration 36ppm Figure 25 : Polymath Model of Column described by Figure 24 0 5 10 15 20 25 30 35 40 0 50 100 150 200 Outlet Concentration (ppm) Time(min) 30mL Resin D C_V= 36 30mL Fitted Model(30mL)

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Figure 26 :Graph Displaying Experimentally Collected Data with Fitted Curve for the Outlet Cu Concentration of a Column with 30mL of Resin T with Inlet Concentration 21ppm Figure 27 : Polymath Model of Column described by Figure 26 -5 0 5 10 15 20 25 0 50 100 150 200 Outlet Concentration(ppm) Time(min) 30mL Resin T C_Cu=21 T-46 Fitted Model(30mL)

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Figure 28 : Graph Displaying Experimentally Collected Data with Fitted Curve for the Outlet V Concentration of a Column with 30mL of Resin T with Inlet Concentration 36ppm Figure 29 : Polymath Model of Column describe d by Figure 28 0 10 20 30 40 50 0 50 100 150 200 Outlet Concentration (ppm) Time(min) 30mL Resin T C_V=36 T-46 Fitted Model(30mL)

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7 SOP 1.0. METHOD SUMMARY The capacities of ion exchange resins are tested in the laboratory using a column and variable flow rate pump. The following procedures outline the methods recommended by Dow and Purolite for testing resins using co current regeneration. Regeneration solutions are used to fill ion exchange sites within the resin and are selected based on resin characteristics. One bed volume (BV), chosen as 100 ml, of resin is added to the column. It is th en rinsed in an up flow and down flow manner to both classify the beads and remove any contaminants. These steps are followed by a regeneration step and two final rinse steps. Finally, the testing solution is pumped through the column and collected as 100 ml samples in 150 ml beakers for digestion and filtration. 2.0. EQUIPTMENT AND SUPPLIES 2.1. APARATUS AND MATERIALS 2.1.2. Glass column 2.1.3. Pump 2.1.4. 500 ml graduated cylinder 2.1.5. 500 ml Erlenmeyer flask 2.1.6. 200 ml Griffin beaker 2.1.7. 150 ml Griffin beakers 2.1.8. Parafilm 2.1.9. 100 ml resin 2.2. REAGENTS 2.2.1. Deionized Water 2.2.2. AMLS 2.2.3. Hydrochloric or Sulfuric acid

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3.0. QUALITY CONTROL To ensure good quality control the following will be carried out: Replicate Trials : Multiple test runs with the same resin will be carried out through the entire analytical process to determine precision. 4.0. PROCEDURES 4.1. PREPARATION 4.1.1. Clean and label all glassware. 4.1.2. Make 200 ml of regeneration solution according to specific resin operating conditions (Use 4% H 2 SO 4 ) 4.1.3. Collect a sample of AMLS from the 5 gal containers using a pump and acid approved tubing. 4.2. RESIN COLUMN TESTING 4.2.1. Fill the 500 ml graduated cylinder with DI water. 4.2.2. Add 100 ml of DI water to a 150 ml beaker. 4.2.3. Add 100 ml of resin to a 150 ml beaker (DO NOT COMPACT THE RESIN) 4.2.4. Pour 50 ml of the DI water into the beaker containing the resin. 4.2.5. Pour the resin slurry into the test column. 4.2.6. Use the remaining 50 ml of DI water to remove any resin left in the beaker and add it to the column. 4.2.7. Pla ce the outlet tubing in the graduated cylinder containing DI water and the outlet tubing in the empty 500 ml flask. 4.2.8. Backwash the resin with DI water in an up flow manner at a rate of 15 BV/h for 12 minutes. 4.2.9. Gradually reduce the flow to zero and allow the r esin to gravity settle.

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4.2.10. Place the inlet tubing in the graduated cylinder containing DI water and the outlet tubing in the 500 ml flask. 4.2.11. Reverse the flow and rinse the resin in a down flow manner with DI water for 2 BV at a rate of 10 BV/h. 4.2.12. Empty the 500 ml flask. 4.2.13. Reverse the flow, and backwash the with regeneration solution at 5 BV/h for 2 BV. 4.2.14. Reverse the flow, and forward rinse the resin with DI water at 5 BV/h for 1 BV. 4.2.15. Fast rinse the resin with DI water at 10 BV/h for 1 BV. 4.2.16. Empty the 500 ml flask into t he appropriate hazardous waste container. 4.2.17. For REGENERATION see section 4.3. 4.2.18. Run AMLS through the resin at a rate of 10 BV/h. 4.2.19. Collect the first sample for testing after 200 ml of liquid has gone through the column. 4.2.20. Collect 1 BV (100 ml) samples in separat e 150 ml beakers. 4.2.21. Stop collection and cover samples with parafilm. 4.2.22. Empty waste AMLS into the appropriate hazardous waste container. 4.2.23. If running the resin to EXHAUSTION, flush resin with 3 BV of DI water at 24 BV/h. 4.2.24. Leave the resin soaking in water. 4.2.25. Repeat steps 4.2.7 through 4.2.9 4.2.26. Place the inlet tubing in the regeneration solution and the outlet tubing in the empty 500 ml flask. 4.2.27. Repeat steps 4.2.13 through 4.2.21 4.3. REGENERATION 4.3.1. Forward rinse with 3 BV of DI water at a rate of 24 BV/h. 4.3.2. Backwash with 8% H 2 SO 4 (volume) at a rate of 10 BV/h for 5BV. 4.3.3. Backwash with 1 BV of DI water at a rate of 10 BV/h. 4.3.4. Forward rinse with 3 BV of DI water at a rate of 10 BV/h. Return to step 4.2.16.

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4.4. FILTER 4.4.1. Use folded P8 filter paper in a funnel in a Nalgene bottle. 4.4.2. Pour sample into the filter, (make sure to capture at least 50 mL). 4.4.3. Label should include: Team initials, date the column is run, resin, speed of the pump, if regen: regen 1, 2, or 3. 4.5. CLEAN UP 4.5.1. Dispose of any unused acids or AMLS into their proper hazardous waste container. 4.5.2. Dispose of resin into the resin hazardous waste container. 4.5.3. Flush empty column and tubing with DI water. 5.0. REFERENCES 5.1. 5. 2. ying out Laboratory Trials on Ion Exchange Resins and

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8 Bibliography Hu, Bo Yu, Yong Jun Yuan, Chao Jiang, and Qiang Liu. "Rational Oxidation of Cyclohexane to Cyclohexanol, Cyclohexanone and Adipic Acid with Air over Metalloporphyrin and Cobalt Salt." WorldsciNet. Web. 19 Apr. 2012. . Kotrba, Pavel, Martina Mackova, and Tomas Macek. Microbial Biosorption of Metals. Dordrecht: Springer Science+Business Media, 2011. Print. 3.3.1.2 pg 25 Geankoplis, Christie J., and Christie J. Geankoplis. "Chapter 12." Transport Processes and Separation Process Principles: (includes Unit Operations). Upper Saddle River, NJ: Prentice Hall Professional Technical Reference, 2003. 760 68. Print Bird, R. Byron, Warren E. Stewart, and Edwin N. Lightfoot. Transport Phenomena. New York: J. Wiley, 2002. Print.