P. R. Monson, N. C. Bell, and S. M. Serkiz
Westinghouse Savannah River Site
Aiken, SC 29808

This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof.

This report has been reproduced directly from the best available copy.

Available for sale to the public, in paper, from:  U.S. Department of Commerce, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161,  phone: (800) 553-6847,  fax: (703) 605-6900,  email:  orders@ntis.fedworld.gov   online ordering:  http://www.ntis.gov/support/ordering.htm

Available electronically at  http://www.osti.gov/bridge/

Available for a processing fee to U.S. Department of Energy and its contractors, in paper, from: U.S. Department of Energy, Office of Scientific and Technical Information, P.O. Box 62, Oak Ridge, TN 37831-0062,  phone: (865 ) 576-8401,  fax: (865) 576-5728,  email:  reports@adonis.osti.gov

During recent operation of the H-Area Water Treatment Unit (WTU) problems have been encountered in meeting the Underground Injection Control permit requirements for mercury in the WTU effluent.

This study investigated the ability of seven ion exchange (IX) resins, some of which were mercury specific, to remove mercury in H-Area WTU waters from three sources (Reverse Osmosis (RO) Feed, RO Permeate from Train A, and a mercury "hot spot" extraction well HEX 18). Seven ion exchange resins, including ResinTech CG8 and Dowex 21K (the cation and anion exchange resins currently used at the H-Area WTU) were screened against five alternative ion exchange materials plus an experimental blank. Mercury decontamination factors (DFs), mercury breakthrough, and post-test contaminant concentrations of IX resins were determined for each IX material tested.

Generally, the experimental approach for this study consisted of passing H-Area WTU waters through a small-scale column packed with one of 7 different ion exchange resins. Effluent water from these experiments was analyzed for total mercury concentration at the SREL by the CVAFS method. Analysis of time-dependent concentration data was used to determine the mercury breakthrough and DF characteristics of each resin.

The following are the major findings and recommendations resulting from this study.

1. The thiol- and dithiol-based resins SR-4, GT73, and SIR-200 were the most effective tested in this study. Results indicate that little or no mercury breakthrough occurred for each of the three influent waters tested over the course of the experiments (equal to approximately 20 days of operational time). If more efficient mercury removal is necessary for the H-Area WTU, then further pilot-scale testing for mercury removal should focus on these three resins.
2. The CG8 and Chelex 20 resins showed early and continuous mercury breakthrough for all three water streams. These two resins should, therefore, be eliminated from further testing for mercury removal from H-Area WTU streams.
3. The S-920 and Dowex 21K resins showed mixed results. Low-levels of breakthrough were observed in most cases, but only for a subset of the influent streams (mainly RO permeate) where these resins intermittently exhibited significant breakthrough.
4. Given the high mass loading of mercury from a small number of wells, treatment of mercury in these "hot spot" wells should be evaluated to reduce operational and material costs if additional mercury removal is necessary.
5. The TCLP results are below the RCRA limits for all RCRA constituents analyzed. The mercury analyses on these extracts were not conducted due to project resource problems. TCLP mercury concentrations need to be determined prior to operation of these resins at the water treatment unit.

Key Words: H-Area Seepage Basin, groundwater treatment, ion exchange, mercury

Recent mercury concentrations measured in injection water collected from the H-Area WTU are in excess of the Underground Injection Control (UIC) Permit limit for mercury of 2 mg/L (ppb).¹ Total mercury concentrations measured in injection well water for the H-Area WTU (HIN600TK) are summarized in Table 2-1. Analytical data² (see Table 2-2) obtained from water samples collected during further mercury characterization sampling conducted after the 6/99 and 7/99 UIC compliance samples also exceeded the permit limit. These data indicate:

• The average concentration of Hg in the RO feedwater was approximately 3.50 mg/L.
• The two extraction wells sampled, HEX-9 and HEX-18, which contribute about 25% to the total water volume extracted from the well field, contributed about 70% of the Hg loading on a mass basis.
• Rejection of Hg by the RO membrane is low and, therefore, a significant quantity of Hg is observed in the RO permeate (approximately 2.4 mg/L, about 70% of the average Hg concentration measured in the RO feedwater).
• Hg in the RO Concentrate stream was adequately removed to levels below detection limit by the existing process.
• Although the speciation of mercury in the influent water to the WTU is not known, the high concentrations of Hg found in the RO permeate indicate that the mercury is likely in a low- or neutrally-charged form (e.g., Hg-Cl₂) and not in the ionic Hg²⁺ specie.

Influent streams tested in this study were the RO feedwater, RO permeate, and one of the mercury "hot spot" wells, HEX-18. TCLP testing of the spent IX materials was performed to evaluate the potential for producing a mixed waste and for aiding in decisions on secondary waste disposal.

For simplicity, this report will use the term ion exchange resin to include both anionic and cationic ion exchange functional groups and chelating functional groups.

This section describes the materials and methods used to evaluate IX resins for mercury removal from H-Area WTU water streams. Included in this section are the selection of IX materials; collection and characterization of process water samples; the experimental approach and setup; and sample analysis.

IX materials evaluated in this study were selected based on the results of a literature review for mercury specific resins as well as the customer request to test the CG8 and Dowex 21K cation and anion resins currently in use at the H-Area WTU. Concurrence from appropriate Environmental Restoration Department/Environmental Restoration Engineering technical representatives on the selected materials was also obtained. A literature review of supplier information (e.g., recommendation of flow rates, exchange capacity, and application), material safety data sheets, existing WTU performance data, and trade journal data were used in this evaluation process.

The selected ion exchange materials are listed in Table 3-1 and fall into three categories: (1) those used in the current system; (2) weak-acid cationic materials; and (3) mercury-specific resins.

Water was obtained from three sources throughout this study: (1) a mercury "hot spot" extraction well, HEX-18, which contributes feedwater to the H-Area Extraction Tank HEX500TK, (2) RO Feed from the Sand Filter Discharge Sample Valve (SF-SMV-SP6), and (3) RO Train A Permeate from RO Train A Sample Valve (RO-SMV-SP8). For the RO Feed and the RO permeate samples were collected several times a day in individual 4-liter mercury-free glass bottles on an as needed basis to keep the column feed bottles filled. Columns feed samples (three to four 4-Liter mercury free glass bottles) from well HEX-18 were filled once a day.

Individual experimental blanks were conducted with each of the three influent streams. This approach allowed for characterization of the feed waters during the experiment as well as an evaluation of experimental artifacts. These experimental blanks were prepared using the same 26-mL glass column used in the resin columns. Blank columns consisted of glass wool packing at the top and a preinstalled fabric fritted disc in the bottom. Effluent samples from the blank columns were collected and analyzed in the same manner as the resin column effluent samples.

All column testing was conducted using established test methods and the general approach contained in the following procedures.

• ASTM D 1782-91, "Test Methods for Operating Performance of Particulate Cation-Exchange Materials"
• ASTM D 2187-94, "Standard Test Methods for Physical and Chemical Properties of Particulate Ion Exchange Resins"

Because this study was designed for the rapid screening of the performance of a large number of resin materials rather than a detailed characterization of the materials, modifications to the field conditions and ASTM procedures (column dimensions, mass of resin, and flow rate) were necessary.

A schematic of the experimental setup is presented in Figure 3-1 with a photograph of the setup in Figure 3-2.

Glass columns, 26-mL in volume, with a fritted disc at the bottom were filled with 26-mL of each of the resin materials. A small glass-wool plug was placed on the top of the resin and in the experimental blank column.

Two 24-head Masterflex™ peristaltic (tubing) pumps were used to pump the feed streams in an up-flow configuration through each of the 24 26-ml columns (3 streams x 7 resins + blank for each stream). Fourteen-gauge silicone tubing was used to transfer the influent from the 4-L glass feed bottle, through the pump and into the bottom of the column. We had a difficult time in adjusting the flowrate through each of the columns to the same rate. As a result, the flowrate was about 4.7 ± 1.0 ml/min resulting in a column retention time of about 5.5 minutes.

Prior to feeding process water to the resins, columns were conditioned by washing each with a minimum of 1,000-mL DI water at a flow rate of 4.7 mL/min.

Column effluent samples were collected in sequential 5-L intervals until a total volume of 30 L had been eluted through each column. Seven volume-discrete samples were taken from each column at 0.6 L (start of test), 5 L, 10 L, 15 L, 20 L, 25 L and 30 L. Experiments were conducted only during the day and at the end of each day, all feed bottles were capped, both pumps were turned off and the valve at the bottom of each column was turned to the closed position.

A 5-10 ml sample was collected for mercury analysis in a 125-ml mercury-free glass bottle as each column reached its prescribed volume-discrete sampling interval. Each sample was preserved by adding 50 mL of BrCl (bromine monochloride oxidizes all mercury compounds to the soluble Hg⁺² state) to each sample.

At the same time the mercury samples were collected, a 30-mL sample of each feed stream was placed in a 60-mL plastic bottle and submitted to the F-Area Water Quality Lab for a Rad Screen and Tritium analysis. The samples were stored at the WTU until rad screen results were obtained. All rad screen results (see Table 3-2) were below the Department of Transportation limits (£ 1 d/m/mL alpha, £ 1 c/m/mL beta/gamma, and less than 2 nC_i/mL tritium) for shipping as radioactive samples. These effluent samples were then transported to SREL and placed in a freezer until analyzed (typically within 4-6 weeks).

Additionally, at the end of the experiment, each feed solution (RO Feed, RO Permeate, and "hot spot" well HEX-18) was analyzed by the Analytical Development Section of SRTC for major and trace elements by ion coupled plasma emission spectroscopy and ion chromatography. The results of these analyses are tabulated in Table 3-3. As expected, RO Permeate concentrations are all lower than the corresponding RO Feed and HEX-18 values.

A series of six bottles of DI water were left open to the atmosphere in the vicinity of experiments for two weeks during the test to investigate uptake of mercury from the air. These samples showed no detectable mercury.

The procedure for daily operation of the system is given in Appendix A.

After the 30-L of process waters had been passed through the column, spent resin from each of the columns was divided into approximately 3 equal portions (Top (column outlet), Middle and Bottom (column inlet)). The Top and Bottom portions were submitted to the ADS for microwave digestion, leaching by the EPA Toxicity Characteristic Leaching Procedure (TCLP), and analysis of the digestion/leaching solutions (Rad Screen, and ICP-ES). The Middle portion was archived.

All samples were allowed to warm to room temperature prior to analysis for mercury at SREL using a Brooks-Rand Model II CVAFS (Cold Vapor Atomic Fluorescence Spectrometer). This analysis was run in accordance with "EPA Method 1631, Revision B: Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry".³ Each day the instrument was calibrated using mercury standards preserved with a stock BrCl solution (oxidizes all mercury compounds to the Hg⁺² state) prepared by SREL graduate students. A three-point calibration curve using random triplicates of each mercury concentration was generated and a linear least squares regression line was fit to the data. Calibrations were repeated until an r-squared value of at least 0.99 was obtained. The standard was #021600, which was 10.00 µg Hg/L preserved with BrCl and made from stock solution #090399. For the CVAFS analysis, the mercury in the samples and standards was reduced to the volatile Hg⁰ by adding 1.2 mL of 10% stannous chloride in 7% HCl just prior to bubbling the sample into the CVAFS. The actual samples were each run once with 3 random samples duplicated for each of the seven sample sets. The minimum detectable concentration of mercury was 0.1µg/L (0.1 ppb). A standard was run after every 12 samples as a check of calibration.

The results of mercury screening of the IX resins tested with H-Area WTU streams is presented in this section.

Table 4-1 is a tabulation of the results of the mercury analysis of column effluent from each of the 24 columns (seven resins and experimental blank for three process waters) and for each of the sample intervals. The table includes the sample ID, liters of water eluted and corresponding number of bed volumes. The mercury values are the single values measured or the average of replicates. The number of bed volumes is calculated as the volume of influent passed through the column in liters divided by the resin volume in liters (0.026L). The nomenclature for the sample ID is SS-ABC-MAT where SS is the stream number corresponding to the pump head location, ABC is the feed source (ROF for RO Feed, ROP for RO Permeate, and HEX-18 for extraction well HEX-18), and MAT is the resin material with BLK being the no resin glass-wool experimental blank.

Influent mercury concentrations for each of the process waters are assumed to be represented by the experimental blank data. In all cases the higher mercury concentrations were found in the extraction well water (HEX-18) followed by the RO Feed and lowest in the RO permeate (see Table 4-1). Temporal variations in these concentrations varied by up to a factor of three for the influent streams. As expected, the RO Feed and RO Permeate streams exhibited smaller temporal variations than did extraction well HEX-18. As previously reported¹, rejection of mercury by the RO membrane was poor.

Mercury effluent concentration data for the seven resins and three process waters tested in this study are summarized in Table 4-1 and these data are graphically represented as a function of number of bed volumes in Figures 4-1 to 4-3 for RO Feed, RO Permeate and HEX-18 process waters respectively. For all three process streams the resins that removed mercury to the lowest concentrations, also those with the highest DF values, were all thiol based (i.e., SR-4 (selective chelating agent), SIR-200 (weak-acid cationic resin) and GT73 (weak-acid cationic resin)). The resins with the poorest mercury removal were the CG8 (strong-acid cationic resin) and the Chelex 20 (iminodiacetic, weak-acid cationic). Although this study was not designed to determine the speciation of the mercury in the various streams, the fact that significant quantities of mercury are present in the RO Permeate suggests that mercury specie(s) other than Hg⁺² exists in the RO Feed. This is because the Reverse Osmosis process should be very effective in rejecting the +2 cationic species.

Figure 4-1. Total Mercury Concentration in Effluent for ROF versus
Bed Volume for all Resins (note: ng/mL = µg/L) .

An alternative approach to analyzing the effluent data is to normalize the effluent data from each column to its corresponding experimental blank (i.e., influent) concentration. The ability of a process to remove contaminants is often quantified by the decontamination factor (DF) that is defined by the treated water concentration divided by the influent concentration. The DF value is, therefore, the inverse of the influent normalized data. Tables 4-2 and 4-3 are the influent normalized and DF data respectively for the mercury data in Table 4-1.

When plotted in this manner the data often gives a clearer picture of the resin performance. The data are presented graphically in Figures 4-4 to 4-6 for the influent normalized data of the RO Feed, RO Concentrate, and HEX-18 respectively and Figures 4-7 to 4-9 for the DF data of the RO Feed, RO Concentrate, and HEX-18 respectively.

A general trend is for resins is for the DF to decrease as a function of volume processed as a greater fraction of the available IX sites are unavailable for exchange due to the presence of other exchanged contaminants. This trend is evident form the data in Table 4-3 with the higher DF values occurring earlier in the experiment. The small rate of decrease in DF values for the thiol-based resins, however, suggests that these resins were not close to breakthrough even at the end of the test (equivalent of about 20 days of unit operational time).

There seems to be effect of waste stream on DF values, notice that the ROF and ROP streams have about the same incoming mercury concentrations but the DF is noticeably greater for the ROF stream. This could be due to some fractionation of the mercury species and some complex neutral mercury species passing through the RO system giving higher mercury concentrations in the RO Permeate.

Figure 4-6. H-Area WTU Normalized Mercury Concentration (unitless) for HEX-18
versus Bed Volume for all Resins (note: ng/mL = µg/L).

This section is a summary of the results of the resin solids analysis at the end of the column testing. Generally, resins solids were digested or leached using standard protocols and the extracts were analyzed for elemental composition using ICP-MS. Solids analysis is designed to provide information on the secondary-waste characteristics of potential resins and may, also, provide insight in to resin performance (e.g., competing sorption effects).

Total microwave dissolution of the resins at the end of testing was conducted by the ADS. Liquid samples from this dissolution process were analyzed by ICP-ES. Solid-phase (resin) concentrations in mg/Kg (ppm) are summarized in Tables 4-4 to 4-6 for the RO Feed, RO Permeate, and HEX-18 tests respectively. The concentrations generally correspond to the relative elemental concentrations of the effluent water given in Table 3-3 with sodium, calcium and magnesium being in the higher proportions in the effluent water than in the digested resin. The higher sodium concentrations in the spent CG8 resins could be due to the fact that this resin is supplied in the sodium form. The non-thiol based cation resins (i.e., CG8 and Chelex 20) exhibited much higher divalent cation concentrations (e.g., Ca and Mg) suggesting that the poor performance for these materials could be attributed to sorption competition from major ions in the waste stream and lack of resin specificity for mercury sorption.

The USEPA TCLP (Toxicity Characteristic Leaching Procedure – Method 1311) is an acetic acid extraction used to determine if solids are Resource Conservation and Recovery Act (RCRA) hazardous.

In this testing, solids are extracted with a weight-based fluid to solid ratio of 20 with acetic acid for 17 hours. Solids were separated by filtration and the extracts were then analyzed by ICP-ES. All TCLP extractions and ICP-ES analytes were conducted by the ADS.

TCLP extract results for each of the spent resins (in units of mg/L), as well as the regulatory standards for those elements analyzed, are summarized in Tables 4-7 to 4-9. The TCLP results are below the RCRA limits for all RCRA constituents analyzed. The mercury analyses on these extracts were not conducted due to project resource problems. TCLP mercury concentrations need to be determined prior to operation of these resins at the water treatment units.

The results of this study indicate that commercially available thiol-based resin materials were effective in reducing mercury concentrations to below UIC regulatory standard of 1 ppb in RO Feed, RO Permeate, and the mercury "hot spot" extraction well HEX-18 from the H-Area Water Treatment Unit. In particular, SR-4, SIR-200 and GT73 thiol-based resins are recommended for further evaluation if greater mercury removal efficiency is needed. The IX materials currently used in the HWTU (CG8 and Dowex21K), however, were largely ineffective in removing mercury in these feed waters for appreciable operation times.

The test was designed to simulate approximately 20 days of operational time at the HWT and breakthrough above regulatory standards was not observed for three of the thiol-based resins (SR-4, SIR-200, and GT73). Although these resins did not show breakthrough, decontamination factors decreased as a function of the amount of water processes. In order for a meaningful economic evaluation to be completed, these resins would have to be run to breakthrough.

Two extraction wells (HEX-9 and HEX-18) contribute about 25% to the total water volume from the extraction well field and about 70% of the mass of mercury. Given the high mercury DF values for the HEX-18 in this study, treatment at the well head of these mercury "hot spot" wells should be evaluated to reduce operational and material costs if additional mercury removal is necessary.

The TCLP results are below the RCRA limits for all RCRA constituents analyzed. The mercury analyses on these extracts were not conducted due to project resource problems. TCLP mercury concentrations need to be determined prior to operation of these resins at the water treatment units.

This study was designed to be a screening study of potential materials and not a selection or design process for resins. It is recommended that scale-up studies be conducted using one or more of the better performing materials from this study (SR-4, SIR-200 and GT73) to evaluate operating parameters and costs. Additionally, data on the IX kinetics should be collected as design input in order to minimize material and construction costs if this option is implemented.

1. Kanzleiter, J. P. , to McNamee, E. et. al. "Mercury Removal- Ion Exchange Material Screening", WSRC Interoffice Memorandum, ERD-99-1-93, October 25, 1999.
2. Kanzleiter, J. P., "Sampling/Analysis for Defining H-Area WTU Mercury Removal Requirements", WRSC Interoffice Memorandum, WSRC-TCE-99-0010, August 19, 1999.
3. US EPA Method 1631, Revision B: Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-99-005, May 1999.

We would like to thank our technicians Cathy Coffey for her help in analyzing the mercury samples and Frances Wakefield for helping run the experiment in the field.

All of the H-Area WTU shift operators were instrumental in the success of this program as well as were the RCO’s. A special thanks goes to Art Gleghorn for clearing our samples and transporting them to SREL for analysis.

We express recognition to the staff and technicians at SREL for assisting with the mercury analysis. Dr. Charles Jagoe for letting us use his mercury analyzer and especially to Heather Brant and Pat Shaw-Allen for the hours of training and help with the analyzer.

1. Must be Rad Worker II Trained to work in Facility.
2. Must read WTU HASP Briefing (WSRC-RP-98-4087, Rev. 1, Briefing for the Facility Specific Health and Safety Plan for the F & H Groundwater Treatment Units) this manual is located in the control room.
3. Must sign SWRP 1 and SWRP 2 (in Rad Con trailer).
4. Safety Glasses with side shield required for all work on WTU Pad (must supply your own safety glasses).
5. Hearing Protection is required for all work on WTU Pad (Control Room and Rad Con trailer have earplugs).
6. Must wear 1 pair of Radiation Rubber Gloves (with Trifoil marking on glove) for all work with well water of WTU process water (Gloves are available in bins in RBA on WTU Pad).

All of our work is within a special RMA within the RBA on the WTU Pad.

1. Sign in on the Visitor Accountability Log each day, get a numbered Visitor Accountability Badge and record number on Log. Read and sign the ER Accountability Briefing form the first time you enter the area, leave signed form in the Accountability Sign –In trailer. Blank copies can be obtained from the control room.
2. Check in with Control Room Operator when entering the area.

1. Put on Safety Glasses with Side Shields, Earplugs and Rubber Gloves.
2. Remove the silicone tubes from each of the 4 –250 mL wide mouth plastic bottles and place the appropriate tubes into the proper 4-L brown glass bottle (ROP-A, ROF, HEX18-1 and HEX18-4).
3. Eight (8) tubes numbered 1-8 going to the 8 columns labeled ROP-A are placed into the 4 L Brown Glass Feed Bottle labeled ROP-A. These tubes are connected to the small white Masterflex tubing pump.
4. Four (4) tubes numbered 9-12 going to 4 of the columns labeled HEX18 are placed into the 4 L Brown Glass Feed Bottle labeled HEX18-1. These tubes are connected to the small white Masterflex tubing pump (Digital Console Drive, Model 7523-30).
5. Four (4) tubes numbered 21-24 going to the other 4 columns labeled HEX18 are placed into the 4 L Brown Glass Feed Bottle labeled HEX18-4. These tubes are connected to the large blue Masterflex tubing pump (Pump #2 Digi-Stalic Model 7527-34, DOE-SRL L0030043).
6. Eight (8) tubes numbered 13-20 going to the 8 columns labeled ROF are placed into the 4 L Brown Glass Feed Bottle labeled ROF. These tubes are connected to the large blue Masterflex tubing pump.
7. Top off the liquid in each of these four 4 L Brown Glass Bottles which now contain the tubes. You can use the funnel with the same label as the bottle (ie. Funnel ROF with water ROF) of just carefully pour from the appropriate 4 L Brown Glass Storage Bottle. Use the ROP-A Storage bottle to fill ROP-A Feed Bottle ONLY. Use the ROF Storage bottle to fill ROF Feed Bottle ONLY. Use the HEX18-2,-3,-5 or-6 Storage bottles to fill HEX18-1 and HEX18-4 Feed Bottles ONLY. DO THIS CAREFULLY, TRY NOT TO OVERFLOW THE BOTTLES, IT IS BEST TO KEEP THE LEVEL JUST BEFORE THE NARROW NECK OF THE FEED BOTTLES.
8. Carefully open each of the 24 valves attached to the bottom of each column. The open position is parallel with the column.
9. Turn on each pump power and Start of Run. The white pump should display 100.0 RPM and the blue pump should display between 97-105 RPM (it varies within this range as the pump operates).
10. Record the date and Start Time in the logbook.
11. After a minute or two. Verify that water is flowing through each column by carefully lifting the tubing from each of the 24 plastic catch jugs and verifying that it is dripping liquid. If no flow is noticed, check to see if pump is on and operating (can check other columns connected to same pump) also make sure valve is open. If still no flow, troubleshoot or call for help (Paul Monson 77242).

1. Keep each of the Feed bottles topped off throughout the day.
2. ROP-A Feed water is obtained from the ROP Train A Sample Valve (Valve RO-SMV-SP8 Train A Permeate, G-782012-RO-SMV-SP8). Use black rubber bucket to carry bottle. BE CAREFUL IN FILLING THIS BOTTLE SINCE THE FLOW OF WATER FROM THIS VALVE IS COMES OUT VERY QUICKLY AND IT IS NEAR METAL PIPES. DO NOT OVERFILL THESE BOTTLES. IT IS BEST TO FILL TO WELL BELOW THE NECK AS IT IS BETTER TO MAKE MORE TRIPS THAN TO OVERFILL AND DEAL WITH A SPILL.
3. ROF Feed water is obtained from the Sand Filter Discharge Sample Valve SF-SMV-SP6, G-782012-SF-SMV-SP6). Use black rubber bucket to carry bottle. BE CAREFUL IN FILLING THIS BOTTLE SINCE THE FLOW OF WATER FROM THIS VALVE COMES OUT VERY RAPIDLY (EVEN GREATER THAN THE ROP-A VALVE). DO NOT OVERFILL THESE BOTTLES. IT IS BEST TO FILL TO WELL BELOW THE NECK AS IT IS BETTER TO MAKE MORE TRIPS THAN TO OVERFILL AND DEAL WITH A SPILL.
4. HEX18 Feed water is obtained from extraction well 18 about a half-mile behind the WTU. To fill these 3 or 4 bottles inform the control room operator several hours before you want to fill them (each bottle should last about 2.5 hours). Rad Con must accompany you or the Control Room Operator to the HEX18 well. Use the black rubber buckets to transport the glass bottles. You must take the golf cart to the well site to fill these HEX18 bottles.
5. When a column has eluted 1000mL of water as measured on the plastic jug, it is time to empty this 1000ml and record the volume removed and time in the logbook. To remove the 1000mL of water, CAREFULLY LIFT THE JUG, KEEPING THE TUBE WITHIN THE JUG AND TRANSFER THE CONTENTS INTO THE UNNUMBERED JUG. NOTE VOLUME IN UNNUMBERED JUG and ADJUST TO 1000mL BY ADDING MORE WATER FROM THE JUG THAN YOU ARE PRESENTLY EMPTYING ONLY. IF YOU HAVE ALREADY ADDED MORE THAN 1000mL FROM THE COLUMN JUG, NOTE HOW MUCH EXTRA YOU ADDED AND THE NEXT TIME YOU REACH NEAR 1000mL FOR THIS SAME NUMBER COLUMN PULL THE AMOUNT TO MAKE UP FOR THE PREVIOUSLY OVERAGE. Discard the 1000mL of water in the unnumbered jug into the CLARIFER at the top of the stair steps behind our setup.
6. Repeat STEP 5 for each of the 24 columns as they reach 1000mL. If more than one column reaches 1000mL before you can empty it, when you get to that jug just remove 1000mL and leave the remaining water in that numbered jug for the next 1000mL.
7. Continue Steps 5 and 6 until 5000mL are passed through each column. This will take 2.5-3 days of operation.
8. Once 5000mL is collected (1000mL at a time), we take a 10mL sample from each column for mercury analysis. These samples are collected by placing a tube from each column into a labeled 125 mL glass bottle for about 4-5 minutes. This can be done one column at a time, if careful several columns at a time, as they reach 5000mL. Once all 24 samples have been collected, each sample is "preserved" by adding 50 microliters of BrCl (Bromine Monochloride a strong oxidizing agent) in a well-ventilated area.
9. As soon as the 24 samples are collected, we collect 30mL from each of the three feed bottles (of their storage bottles) ROP-A, ROF and HEX18, these samples are put into 60mL plastic bottles with Red ADS Labels and given to Rad Con for smearing before Art Gleghorn (26400/13626) delivers them to the F-Area Water Quality Laboratory for a Rad Scan (Alpha, Beta/Gamma and Tritium).
10. Once the Rad Scan comes back (via FAX to the Control Room) "CLEAN" (ie Tritium < 2000 microcuries/mL), we can have Art Gleghorn deliver them to Heather Brant in Room 186 of SREL. The samples will be placed in the freezer in Room 186. Contact Heather Brant (55767) well before the samples will arrive to let her know they are coming.

1. Turn off both pumps flow and their power.
2. Close all 24 valves at the base of each column, Closed position is perpindicular to the column tube.
3. Remove the tubes from each of the four Feed Bottles and place the tubes into the appropriate 250mL wide mouth plastic bottle.
4. Put a cap on each of the 4 L Brown Glass Feed Bottles.
5. Notify the Control Room Operator that you are leaving the area for the day.
6. Sign out on the Visitor Accountability Log and Replace Visitor Badge in the Badge Rack.

Appendix B. Hg Data for 0.6L Influent Samples

Appendix C. Hg Data for 0.6L Influent Samples

Appendix D. Hg Data for 0.6L Influent Samples

Appendix E. Hg Data for 5L Influent Samples

Appendix F. Hg Data for 10L Influent Samples

Appendix G. Hg Data for 15L Influent Samples

Appendix H. Hg Data for 20L Influent Samples

Appendix I. Hg Data for 25L Influent Samples

Appendix J. Hg Data for 25L Influent Samples

Appendix K. Hg Data for 30L Influent Samples and DI Water Blank Samples