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1

Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 104  

SciTech Connect

A sample of solids was obtained from tank 104 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprenel tubing (Phthalate free). The sample obtained in a glass jar with Teflon 2 lid, was analyzed for PCBs as Aroclor mixtures. A soxhlet extraction procedure was used to extract the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). The extraction method closely follows SW-846 method 3540C and the analysis follows SW-846 method.

Ross, G.A.

1998-03-27T23:59:59.000Z

2

Method and apparatus for controlling gas evolution from chemical reactions  

DOE Patents (OSTI)

The present invention is directed toward monitoring a thermally driven gas evolving chemical reaction with an acoustic apparatus. Signals from the acoustic apparatus are used to control a heater to prevent a run-away condition. A digestion module in combination with a robotic arm further automate physical handling of sample material reaction vessels. The invention is especially useful for carrying out sample procedures defined in EPA Methods SW-846.

Skorpik, James R. (Kennewick, WA); Dodson, Michael G. (Richland, WA)

1999-01-01T23:59:59.000Z

3

Method and apparatus for controlling gas evolution from chemical reactions  

DOE Patents (OSTI)

The present invention is directed toward monitoring a thermally driven gas evolving chemical reaction with an acoustic apparatus. Signals from the acoustic apparatus are used to control a heater to prevent a run-away condition. A digestion module in combination with a robotic arm further automate physical handling of sample material reaction vessels. The invention is especially useful for carrying out sample procedures defined in EPA Methods SW-846. 8 figs.

Skorpik, J.R.; Dodson, M.G.

1999-05-25T23:59:59.000Z

4

SALTSTONE 1QCY14 TCLP RESULTS  

SciTech Connect

A Saltstone waste form was prepared in the Savannah River National Laboratory (SRNL) from a Tank 50H sample and Z-Area premix material for the first quarter of calendar year 2014 (1QCY14). After a 64 day cure, samples of the saltstone were collected, and the waste form was shown to meet the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24 and R.61-79.268.48(a) requirements for a nonhazardous waste form with respect to RCRA metals and underlying hazardous constituents. These analyses met all quality assurance specifications of USEPA SW-846.

Miller, D.

2014-06-19T23:59:59.000Z

5

SALTSTONE 4QCY13 TCLP RESULTS  

SciTech Connect

A Saltstone waste form was prepared in the Savannah River National Laboratory (SRNL) from a Tank 50H sample and Z-Area premix material for the fourth quarter of calendar year 2013 (4QCY13). After a 62 day cure, samples of the saltstone were collected, and the waste form was shown to meet the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24 and R.61-79.268.48(a) requirements for a nonhazardous waste form with respect to RCRA metals and underlying hazardous constituents. These analyses met all quality assurance specifications of USEPA SW-846.

Miller, D.

2014-04-23T23:59:59.000Z

6

Inorganic and Radiochemical Analysis of AW-101 and AN-107 Tank Waste  

SciTech Connect

This report presents the inorganic and radiochemical analytical results for AW-101 and AN-107 as received materials. The analyses were conducted in support of the BNFL Proposal No. 30406/29274 Task 5.0. The inorganic and radiochemical analysis results obtained from the as received materials are used to provide initial characterization information for subsequent process testing and to provide data to support permit application activities. Quality Assurance (QA) Plan MCS-033 provides the operational and quality control protocols for the analytical activities, and whenever possible, analyses were performed to SW-846 equivalent methods and protocols.

MW Urie; JJ Wagner; LR Greenwood; OT Farmer; SK Fiskum; RT Ratner; CZ Soderquist

1999-11-11T23:59:59.000Z

7

INVESTIGATION OF THE TOTAL ORGANIC HALOGEN ANALYTICAL METHOD AT THE WASTE SAMPLING CHARACTERIZATION FACILITY (WSCF)  

SciTech Connect

Total organic halogen (TOX) is used as a parameter to screen groundwater samples at the Hanford Site. Trending is done for each groundwater well, and changes in TOX and other screening parameters can lead to costly changes in the monitoring protocol. The Waste Sampling and Characterization Facility (WSCF) analyzes groundwater samples for TOX using the United States Environmental Protection Agency (EPA) SW-846 method 9020B (EPA 1996a). Samples from the Soil and Groundwater Remediation Project (S&GRP) are submitted to the WSCF for analysis without information regarding the source of the sample; each sample is in essence a 'blind' sample to the laboratory. Feedback from the S&GRP indicated that some of the WSCF-generated TOX data from groundwater wells had a number of outlier values based on the historical trends (Anastos 2008a). Additionally, analysts at WSCF observed inconsistent TOX results among field sample replicates. Therefore, the WSCF lab performed an investigation of the TOX analysis to determine the cause of the outlier data points. Two causes were found that contributed to generating out-of-trend TOX data: (1) The presence of inorganic chloride in the groundwater samples: at inorganic chloride concentrations greater than about 10 parts per million (ppm), apparent TOX values increase with increasing chloride concentration. A parallel observation is the increase in apparent breakthrough of TOX from the first to the second activated-carbon adsorption tubes with increasing inorganic chloride concentration. (2) During the sample preparation step, excessive purging of the adsorption tubes with oxygen pressurization gas after sample loading may cause channeling in the activated-carbon bed. This channeling leads to poor removal of inorganic chloride during the subsequent wash step with aqueous potassium nitrate. The presence of this residual inorganic chloride then produces erroneously high TOX values. Changes in sample preparation were studied to more effectively remove inorganic chloride from the activated carbon adsorption tubes. With the TOX sample preparation equipment and TOX analyzers at WSCF, the nitrate wash recommended by EPA SW-846 method 9020B was found to be inadequate to remove inorganic chloride interference. Increasing the nitrate wash concentration from 10 grams per liter (g/L) to 100 g/L potassium nitrate and increasing the nitrate wash volume from 3 milliliters (mL) to 10 mL effectively removed the inorganic chloride up to at least 100 ppm chloride in the sample matrix. Excessive purging of the adsorption tubes during sample preparation was eliminated. These changes in sample preparation have been incorporated in the analytical procedure. The results using the revised sample preparation procedure show better agreement of TOX values both for replicate analyses of single samples and for the analysis of replicate samples acquired from the same groundwater well. Furthermore, less apparent column breakthrough now occurs with the revised procedure. One additional modification made to sample preparation was to discontinue the treatment of groundwater samples with sodium bisulfite. Sodium bisulfite is used to remove inorganic chlorine from the sample; inorganic chlorine is not expected to be a constituent in these groundwater samples. Several other factors were also investigated as possible sources of anomalous TOX results: (1) Instrument instability: examination of the history of results for TOX laboratory control samples and initial calibration verification standards indicate good long-term precision for the method and instrument. Determination of a method detection limit of 2.3 ppb in a deionized water matrix indicates the method and instrumentation have good stability and repeatability. (2) Non-linear instrument response: the instrument is shown to have good linear response from zero to 200 parts per billion (ppb) TOX. This concentration range encompasses the majority of samples received at WSCF for TOX analysis. (3) Improper sample preservation: ion-chromatographic analysis of several samples wit

DOUGLAS JG; MEZNARICH HD, PHD; OLSEN JR; ROSS GA; STAUFFER M

2008-09-30T23:59:59.000Z

8

Cementitious Barriers Partnership (CBP): Using the CBP Software Toolbox to Simulate Sulfate Attack and Carbonation of Concrete Structures - 13481  

SciTech Connect

The Cementitious Barriers Partnership (CBP) Project is a multi-disciplinary, multi-institutional collaboration supported by the U.S. Department of Energy Office of Tank Waste Management. The CBP project has developed a set of integrated modeling tools and leaching test methods to help improve understanding and prediction of the long-term hydraulic and chemical performance of cementitious materials used in nuclear applications. State-of-the-art modeling tools, including LeachXS{sup TM}/ORCHESTRA and STADIUM{sup R}, were selected for their demonstrated abilities to simulate reactive transport and degradation in cementitious materials. The new U.S. Environmental Protection Agency leaching test methods based on the Leaching Environmental Assessment Framework (LEAF), now adopted as part of the SW-846 RCRA methods, have been used to help make the link between modeling and experiment. Although each of the CBP tools has demonstrated utility as a standalone product, coupling the models over relevant spatial and temporal solution domains can provide more accurate predictions of cementitious materials behavior over relevant periods of performance. The LeachXS{sup TM}/ORCHESTRA and STADIUM{sup R} models were first linked to the GoldSim Monte Carlo simulator to better and more easily characterize model uncertainties and as a means to coupling the models allowing linking to broader performance assessment evaluations that use CBP results for a source term. Two important degradation scenarios were selected for initial demonstration: sulfate ingress / attack and carbonation of cementitious materials. When sufficient sulfate is present in the pore solution external to a concrete barrier, sulfate can diffuse into the concrete, react with the concrete solid phases, and cause cracking that significantly changes the transport and structural properties of the concrete. The penetration of gaseous carbon dioxide within partially saturated concrete usually initiates a series of carbonation reactions with both dissolved ions and the hydrated cement paste. The carbonation process itself does not have a negative effect, per se, on the paste physical properties and can even result in reduced porosity and can help form a protective layer at the surface of concrete. However, carbonation has been shown to increase leaching of some constituents and can potentially have a detrimental effect on reinforced concrete structures by lowering pH to ca. 9 and de-passivating embedded steel (e.g. rebar) and accelerating corrosion, which are important processes related to high-level waste tank integrity and closure evaluations. The use of the CBP Software Toolbox to simulate these important degradation phenomena for both concrete vaults and high-level waste tanks are demonstrated in this paper. (authors)

Brown, K.G.; Kosson, D.S.; Garrabrants, A.C.; Sarkar, S. [Vanderbilt University, School of Engineering, CRESP, Nashville, TN 37235 (United States)] [Vanderbilt University, School of Engineering, CRESP, Nashville, TN 37235 (United States); Flach, G.; Langton, C.; Smith, F.G.III; Burns, H. [Savannah River National Laboratory, Aiken, SC 29808 (United States)] [Savannah River National Laboratory, Aiken, SC 29808 (United States); Van der Sloot, H. [Hans Van der Sloot Consultancy, Dorpsstraat 216, 1721BV Langedijk (Netherlands)] [Hans Van der Sloot Consultancy, Dorpsstraat 216, 1721BV Langedijk (Netherlands); Meeussen, J.C.L. [Nuclear Research and Consultancy Group, Westerduinweg 3, Petten (Netherlands)] [Nuclear Research and Consultancy Group, Westerduinweg 3, Petten (Netherlands); Seignette, P.F.A.B. [Energy Research Center of The Netherlands, Petten (Netherlands)] [Energy Research Center of The Netherlands, Petten (Netherlands); Samson, E. [SIMCO Technologies, Inc., Quebec (Canada)] [SIMCO Technologies, Inc., Quebec (Canada); Mallick, P.; Suttora, L. [U.S. Department of Energy, Washington, DC (United States)] [U.S. Department of Energy, Washington, DC (United States); Esh, D.; Fuhrmann, M.; Philip, J. [U.S. Nuclear Regulatory Commission, Washington, DC (United States)] [U.S. Nuclear Regulatory Commission, Washington, DC (United States)

2013-07-01T23:59:59.000Z

9

SALTSTONE 2QCY08 TCLP RESULTS  

SciTech Connect

A Saltstone waste form was prepared in the Savannah River National Laboratory from a Tank 50H sample and Z-Area premix material for the second quarter of calendar year 2008 (2QCY08). After the prescribed 28 day cure, samples of the saltstone were collected, and the waste form was shown to meet the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24 and R.61-79.268.48(a) requirements for a nonhazardous waste form with respect to RCRA metals and underlying hazardous constituents. These analyses met all quality assurance specifications of USEPA SW-846. The Saltstone Production Facility (SPF) receives waste from Tank 50H for treatment. In the second quarter of the 2008 calendar year (2QCY08), Tank 50 accepted transfers of approximately 21 kgal from the Effluent Treatment Project (ETP) waste, approximately 3 kgal from Tank 710--the H-Canyon General Purpose Evaporator, and approximately 23 kgal form the Modular Caustic Side Solvent Extraction Unit (MCU) Decontaminated Salt Solution Hold Tank (DSS-HT). The Saltstone Grout Sampling plan provides the South Carolina Department of Health and Environmental Control (SCDHEC) with the chemical and physical characterization strategy for the salt solution which is to be disposed of in the Z-Area Solid Waste Landfill (ISWLF). During operation, samples were collected from Tank 50H and grout samples prepared to determine the non-hazardous nature of the grout to meet the requirements of the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24(b) and R.61-79.268.48(a). SRNL was asked to prepare saltstone from a sample of Tank 50H obtained June 5, 2008, during 2QCY08 processing to determine the non-hazardous nature of the grout. The samples were cured and shipped to Babcock & Wilcox Technical Services Group-Radioisotope and Analytical Chemistry Laboratory (B&WTSG-RACL) to perform the Toxic Characteristic Leaching Procedure (TCLP)2 and subsequent extract analysis on saltstone samples for the analytes required for the quarterly analysis saltstone sample. In addition to the eight toxic metals-arsenic, barium, cadmium, chromium, mercury, lead, selenium and silver-analytes included the underlying hazardous constituents (UHC) antimony, beryllium, nickel, and thallium which could not be eliminated from analysis by process knowledge.3 B&WTSG-RACL provided subsamples to GEL Laboratories, LLC for analysis for the UHCs benzene, phenols and total and amenable cyanide.

Cozzi, A

2009-03-23T23:59:59.000Z

10

SALTSTONE 3QCY09 TCLP RESULTS  

SciTech Connect

A Saltstone waste form was prepared in the Savannah River National Laboratory (SRNL) from a Tank 50H sample and Z-Area premix material for the third quarter of calendar year 2009 (3QCY09). After the prescribed 28 day cure, samples of the saltstone were collected, and the waste form was shown to meet the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24 and R.61-79.268.48(a) requirements for a nonhazardous waste form with respect to RCRA metals and underlying hazardous constituents. These analyses met all quality assurance specifications of USEPA SW-846. The Saltstone Production Facility (SPF) receives waste from Tank 50H for treatment. In the third quarter of the 2009 calendar year (3QCY09), Tank 50H accepted transfers of approximately 37 kgal from the Effluent Treatment Project (ETP) waste, approximately 5 kgal from Tank 710 - the H-Canyon General Purpose Evaporator, approximately 26 kgal from Tank 221H, approximately 319 kgal from the Modular Caustic Side Solvent Extraction Unit (MCU) Decontaminated Salt Solution Hold Tank (DSS-HT), and approximately 358 kgal from Tank 23H. The Saltstone Grout Sampling plan provides the South Carolina Department of Health and Environmental Control (SCDHEC) with the chemical and physical characterization strategy for the salt solution which is to be disposed of in the Z-Area Solid Waste Landfill (ISWLF). During operation, samples were collected from Tank 50H and grout samples prepared to determine the non-hazardous nature of the grout to meet the requirements of the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24(b) and R.61-79.268.48(a). Savannah River National Laboratory (SRNL) was asked to prepare saltstone from a sample of Tank 50H obtained August 5, 2009 during 3QCY09 to determine the non-hazardous nature of the grout. The samples were cured and shipped to Babcock & Wilcox Technical Services Group-Radioisotope and Analytical Chemistry Laboratory (B&WTSG-RACL) to perform the Toxic Characteristic Leaching Procedure (TCLP) and subsequent extract analysis on saltstone samples for the analytes required for the quarterly analysis saltstone sample. In addition to the eight toxic metals-arsenic, barium, cadmium, chromium, mercury, lead, selenium and silver-analytes included the underlying hazardous constituents (UHC) antimony, beryllium, nickel, and thallium which could not be eliminated from analysis by process knowledge. B&WTSG-RACL provided subsamples to GEL Laboratories, LLC for analysis for the UHCs benzene, phenols and total and amenable cyanide.

Reigel, M.

2010-01-13T23:59:59.000Z

11

SALTSTONE 2QCY09 TCLP RESULTS  

SciTech Connect

A Saltstone waste form was prepared in the Savannah River National Laboratory from a Tank 50H sample and Z-Area premix material for the second quarter of calendar year 2009 (2QCY09). After the prescribed 28 day cure, samples of the saltstone were collected, and the waste form was shown to meet the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24 and R.61-79.268.48(a) requirements for a nonhazardous waste form with respect to RCRA metals and underlying hazardous constituents. These analyses met all quality assurance specifications of USEPA SW-846. The Saltstone Production Facility (SPF) receives waste from Tank 50H for treatment. In the second quarter of the 2009 calendar year (2QCY09), Tank 50 accepted transfers of approximately 32 kgal from the Effluent Treatment Project (ETP) waste, approximately 4 kgal from Tank 710 - the H-Canyon General Purpose Evaporator, approximately 156 kgal from the Modular Caustic Side Solvent Extraction Unit (MCU) Decontaminated Salt Solution Hold Tank (DSS-HT), and approximately 484 kgal from Tank 23. The Saltstone Grout Sampling plan provides the South Carolina Department of Health and Environmental Control (SCDHEC) with the chemical and physical characterization strategy for the salt solution which is to be disposed of in the Z-Area Solid Waste Landfill (ISWLF). During operation, samples were collected from Tank 50H and grout samples prepared to determine the non-hazardous nature of the grout to meet the requirements of the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24(b) and R.61-79.268.48(a). SRNL was asked to prepare saltstone from a sample of Tank 50H obtained May 20, 2009 during 2QCY09 to determine the non-hazardous nature of the grout. The samples were cured and shipped to Babcock & Wilcox Technical Services Group-Radioisotope and Analytical Chemistry Laboratory (B&WTSGRACL) to perform the Toxic Characteristic Leaching Procedure (TCLP) and subsequent extract analysis on saltstone samples for the analytes required for the quarterly analysis saltstone sample. In addition to the eight toxic metals - arsenic, barium, cadmium, chromium, mercury, lead, selenium and silver - analytes included the underlying hazardous constituents (UHC) antimony, beryllium, nickel, and thallium which could not be eliminated from analysis by process knowledge. B&WTSG-RACL provided subsamples to GEL Laboratories, LLC for analysis for the UHCs benzene, phenols and total and amenable cyanide.

Reigel, M.

2009-10-29T23:59:59.000Z

12

SALTSTONE 3QCY09 TCLP RESULTS  

SciTech Connect

A Saltstone waste form was prepared in the Savannah River National Laboratory (SRNL) from a Tank 50H sample and Z-Area premix material for the third quarter of calendar year 2009 (3QCY09). After the prescribed 28 day cure, samples of the saltstone were collected, and the waste form was shown to meet the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24 and R.61-79.268.48(a) requirements for a nonhazardous waste form with respect to RCRA metals and underlying hazardous constituents. These analyses met all quality assurance specifications of USEPA SW-846. The Saltstone Production Facility (SPF) receives waste from Tank 50H for treatment. In the third quarter of the 2009 calendar year (3QCY09), Tank 50H accepted transfers of approximately 37 kgal from the Effluent Treatment Project (ETP) waste, approximately 5 kgal from Tank 710 - the H-Canyon General Purpose Evaporator, approximately 26 kgal from Tank 221H, approximately 319 kgal from the Modular Caustic Side Solvent Extraction Unit (MCU) Decontaminated Salt Solution Hold Tank (DSS-HT), and approximately 358 kgal from Tank 23H. The Saltstone Grout Sampling plan provides the South Carolina Department of Health and Environmental Control (SCDHEC) with the chemical and physical characterization strategy for the salt solution which is to be disposed of in the Z-Area Solid Waste Landfill (ISWLF). During operation, samples were collected from Tank 50H and grout samples prepared to determine the non-hazardous nature of the grout to meet the requirements of the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24(b) and R.61-79.268.48(a). Savannah River National Laboratory (SRNL) was asked to prepare saltstone from a sample of Tank 50H obtained August 5, 2009 during 3QCY09 to determine the non-hazardous nature of the grout. The samples were cured and shipped to Babcock & Wilcox Technical Services Group-Radioisotope and Analytical Chemistry Laboratory (B&WTSG-RACL) to perform the Toxic Characteristic Leaching Procedure (TCLP) and subsequent extract analysis on saltstone samples for the analytes required for the quarterly analysis saltstone sample. In addition to the eight toxic metals - arsenic, barium, cadmium, chromium, mercury, lead, selenium and silver - analytes included the underlying hazardous constituents (UHC) antimony, beryllium, nickel, and thallium which could not be eliminated from analysis by process knowledge. B&WTSG-RACL provided subsamples to GEL Laboratories, LLC for analysis for the UHCs benzene, phenols and total and amenable cyanide.

Reigel, M.

2009-12-14T23:59:59.000Z

13

SALTSTONE 1QCY11 TCLP RESULTS  

SciTech Connect

A Saltstone waste form was prepared in the Savannah River National Laboratory (SRNL) from a Tank 50H sample and Z-Area premix material for the first quarter of calendar year 2011 (1QCY11). After the prescribed 28 day cure, samples of the saltstone were collected, and the waste form was shown to meet the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24 and R.61-79.268.48(a) requirements for a nonhazardous waste form with respect to RCRA metals and underlying hazardous constituents. These analyses met all quality assurance specifications of USEPA SW-846. The Saltstone Production Facility (SPF) receives waste from Tank 50H for treatment. In the first quarter of the 2011 calendar year (1QCY11), Tank 50H accepted transfers of approximately 15 kgal from the Effluent Treatment Project (ETP), approximately 15 kgal from Tank 710 - the H-Canyon General Purpose Evaporator, approximately 73 kgal from the H-Canyon Super Kukla campaign, approximately 285 kgal from the Actinide Removal Process/Modular Caustic Side Solvent Extraction Unit (ARP/MCU) Decontaminated Salt Solution Hold Tank (DSS-HT), and approximately 21 kgal from other sources. The Saltstone Grout Sampling plan provides the South Carolina Department of Health and Environmental Control (SCDHEC) with the chemical and physical characterization strategy for the salt solution which is to be disposed of in the Z-Area Solid Waste Landfill (SWLF). During operation, samples were collected from Tank 50H and grout samples prepared to determine the non-hazardous nature of the grout to meet the requirements of the South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-79.261.24(b) and R.61-79.268.48(a). Savannah River National Laboratory (SRNL) was asked to prepare saltstone from samples of Tank 50H obtained January 5, 2011 during 1QCY11 to determine the non-hazardous nature of the grout. The samples were cured and shipped to Babcock & Wilcox Technical Services Group-Radioisotope and Analytical Chemistry Laboratory (B&W TSG-RACL) to perform the Toxic Characteristic Leaching Procedure (TCLP) and subsequent extract analysis on saltstone samples for the analytes required for the quarterly analysis saltstone sample. In addition to the eight toxic metals-arsenic, barium, cadmium, chromium, mercury, lead, selenium and silver-analytes included the underlying hazardous constituents (UHC) antimony, beryllium, nickel, and thallium which could not be eliminated from analysis by process knowledge. B&W TSG-RACL provided subsamples to GEL Laboratories, LLC for analysis for the UHCs benzene, phenols and total and amenable cyanide.

Reigel, M.

2011-05-16T23:59:59.000Z

14

INVESTIGATION OF THE TOTAL ORGANIC HALOGEN ANALYTICAL METHOD AT THE WASTE SAMPLING AND CHARACTERIZATION FACILITY  

SciTech Connect

Total organic halogen (TOX) is used as a parameter to screen groundwater samples at the Hanford Site. Trending is done for each groundwater well, and changes in TOX and other screening parameters can lead to costly changes in the monitoring protocol. The Waste Sampling and Characterization Facility (WSCF) analyzes groundwater samples for TOX using the United States Environmental Protection Agency (EPA) SW-S46 method 9020B (EPA 1996a). Samples from the Soil and Groundwater Remediation Project (SGRP) are submitted to the WSCF for analysis without information regarding the source of the sample; each sample is in essence a ''blind'' sample to the laboratory. Feedback from the SGRP indicated that some of the WSCF-generated TOX data from groundwater wells had a number of outlier values based on the historical trends (Anastos 200Sa). Additionally, analysts at WSCF observed inconsistent TOX results among field sample replicates. Therefore, the WSCF lab performed an investigation of the TOX analysis to determine the cause of the outlier data points. Two causes were found that contributed to generating out-of-trend TOX data: (1) The presence of inorganic chloride in the groundwater samples: at inorganic chloride concentrations greater than about 10 parts per million (ppm), apparent TOX values increase with increasing chloride concentration. A parallel observation is the increase in apparent breakthrough of TOX from the first to the second activated-carbon adsorption tubes with increasing inorganic chloride concentration. (2) During the sample preparation step, excessive purging of the adsorption tubes with oxygen pressurization gas after sample loading may cause channeling in the activated carbon bed. This channeling leads to poor removal of inorganic chloride during the subsequent wash step with aqueous potassium nitrate. The presence of this residual inorganic chloride then produces erroneously high TOX values. Changes in sample preparation were studied to more effectively remove inorganic chloride from the activated-carbon adsorption tubes. With the TOX sample preparation equipment and TOX analyzers at WSCF, the nitrate wash recommended by EPA SW-846 method 9020B was found to be inadequate to remove inorganic chloride interference. Increasing the nitrate wash concentration from 10 grams per liter (g/L) to 100 giL potassium nitrate and increasing the nitrate wash volume from 3 milliliters (mL) to 10 mL effectively removed the inorganic chloride up to at least 100 ppm chloride in the sample matrix. Excessive purging of the adsorption tubes during sample preparation was eliminated. These changes in sample preparation have been incorporated in the analytical procedure. The results using the revised sample preparation procedure show better agreement of TOX values both for replicate analyses of single samples and for the analysis of replicate samples acquired from the same groundwater well. Furthermore, less apparent adsorption tube breakthrough now occurs with the revised procedure. One additional modification made to sample preparation was to discontinue the treatment of groundwater samples with sodium bisulfite. Sodium bisulfite is used to remove inorganic chlorine from the sample; inorganic chlorine is not expected to be a constituent in these groundwater samples. Several other factors were also investigated as possible sources of anomalous TOX results: (1) Instrument instability: examination of the history of results for TOX laboratory control samples and initial calibration verification standards indicate good long-term precision for the method and instrument. Determination of a method detection limit of 2.3 ppb in a deionized water matrix indicates the method and instrumentation have good stability and repeatability. (2) Non-linear instrument response: the instrument is shown to have good linear response from zero to 200 parts per billion (ppb) TOX. This concentration range encompasses the majority of samples received at WSCF for TOX analysis. Linear response was checked using both non-volatile TOX species (trichlorophenol) an

JG DOUGLAS; HK MEZNARICH, PHD; JR OLSEN; GA ROSS PHD; M STAUFFER

2009-02-13T23:59:59.000Z