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1

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

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. 8 figs.

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

1999-05-25T23:59:59.000Z

3

Saltstone 3QCY12 TCLP Results  

SciTech Connect (OSTI)

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 2012 (3QCY12). After a 34 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.

Eibling, R. E.

2012-12-19T23:59:59.000Z

4

Saltstone 1QCY13 TCLP Results  

SciTech Connect (OSTI)

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 2013 (1QCY13). After a 49 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.

Eibling, R. E.

2013-07-08T23:59:59.000Z

5

SALTSTONE 1QCY14 TCLP RESULTS  

SciTech Connect (OSTI)

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

6

SALTSTONE 4QCY10 TCLP RESULTS  

SciTech Connect (OSTI)

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 2010 (4QCY10). 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.

Reigel, M.

2011-03-31T23:59:59.000Z

7

Saltstone 2QCY13 TCLP Results  

SciTech Connect (OSTI)

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 second quarter of calendar year 2013 (2QCY13). After a 49 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.

Reigel, M. M.

2013-10-29T23:59:59.000Z

8

SALTSTONE 4QCY13 TCLP RESULTS  

SciTech Connect (OSTI)

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

9

Saltstone 4QCY12 TCLP results  

SciTech Connect (OSTI)

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 2012 (4QCY12). After a 48 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.

Reigel, M. M.

2013-03-14T23:59:59.000Z

10

Saltstone 3QCY13 TCLP Results  

SciTech Connect (OSTI)

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 2013 (3QCY13). After a 63 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. H.

2013-12-20T23:59:59.000Z

11

A DOE manual: DOE methods for evaluating environmental and waste management samples  

SciTech Connect (OSTI)

DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) is a guidance/methods document supporting environmental restoration (ER) and waste management (WM) (collectively referred to as EM) sampling and analysis activities at US Department of Energy (DOE) sites. DOE Methods is intended to supplement existing guidance documents (e.g., the US Environmental Protection Agency`s Test Methods for Evaluating Solid Waste, SW-846), which apply to low-level or non-radioactive samples, and the complexities of waste and environmental samples encountered at DOE sites. The document contains quality assurance (QA), quality control (QC), safety, sampling, organic analysis, inorganic analysis, and radio-analytical guidance as well as sampling and analytical methods. It is updated every six months (April and October) with additional methods. As of April 1994, DOE methods contained 3 sampling and 39 analytical methods. It is anticipated that between 10 and 20 new methods will be added in October 1994. All methods are either peer reviewed and contain performance data, or are included as draft methods.

Goheen, S.C.; Fadeff, S.K.; Sklarew, D.S.; McCulloch, M.; Mong, G.M.; Riley, R.G.; Thomas, B.L.

1994-08-01T23:59:59.000Z

12

Qualitative vs. quantitative data: Controls on the accuracy of PID field screening in petroleum contamination assessment applications  

SciTech Connect (OSTI)

The use of photoionization detectors (PIDs) for field screening of soils for volatile organic contaminants has become a standard industry practice. PID screening data is generally utilized as a qualitative basis for selection of samples for laboratory analysis to quantify concentrations of specific contaminants of concern. Both qualitative field screening data and quantitative laboratory analytical data were reviewed for more than 100 hydrogeologic assessment sites in Ohio to evaluate controls on the effectiveness of field screening data. Assessment data evaluated was limited to sites at which the suspected contaminant source was a gasoline underground storage tanks system. In each case, a 10.0 eV (or greater) PID calibrated for benzene was used to screen soils which were analyzed for benzene, toluene, ethylbenzene and xylene (BTEX) by SW 846 method 8020. Controls on field screening which were evaluated for each site included (1) soil classification, (2) soil moisture, (3) weather conditions, (4) background levels, (5) equipment quality, (6) screening methodology, and (7) laboratory QA/QC. Statistical data analysis predictably indicated a general overestimate of total BTEX levels based on field screening (gasoline is approximately 25 weight percent BTEX). However, data locally indicated cases of both significant (i.e., more than an order of magnitude difference) over- and under-estimation of actual BTEX concentrations (i.e., quantitative laboratory data) by field screening data.

Luessen, M.J.; Allex, M.K.; Holzel, F.R. [ATEC Associates Inc., Cincinnati, OH (United States)

1995-09-01T23:59:59.000Z

13

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

SciTech Connect (OSTI)

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

14

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

SciTech Connect (OSTI)

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

15

SALTSTONE 3QCY11 TCLP RESULTS  

SciTech Connect (OSTI)

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 2011 (3QCY11). After the prescribed 32 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 2011 calendar year (3QCY11), Tank 50H accepted transfers of approximately 20 kgal from the Effluent Treatment Project (ETP), approximately 236 kgal from the Actinide Removal Process/Modular Caustic Side Solvent Extraction Unit (ARP/MCU) Decontaminated Salt Solution Hold Tank (DSS-HT), and approximately 25 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 July 7, 2011 during 3QCY11 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.

Bannochie, C.

2012-01-12T23:59:59.000Z

16

SALTSTONE 1QCY11 TCLP RESULTS  

SciTech Connect (OSTI)

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

17

SALTSTONE VAULT CLASSIFICATION SAMPLES MODULAR CAUSTIC SIDE SOLVENT EXTRACTION UNIT/ACTINIDE REMOVAL PROCESS WASTE STREAM APRIL 2011  

SciTech Connect (OSTI)

Savannah River National Laboratory (SRNL) was asked to prepare saltstone from samples of Tank 50H obtained by SRNL on April 5, 2011 (Tank 50H sampling occurred on April 4, 2011) during 2QCY11 to determine the non-hazardous nature of the grout and for additional vault classification analyses. 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. Additional inorganic species determined by B&W TSG-RACL include aluminum, boron, chloride, cobalt, copper, fluoride, iron, lithium, manganese, molybdenum, nitrate/nitrite as Nitrogen, strontium, sulfate, uranium, and zinc and the following radionuclides: gross alpha, gross beta/gamma, 3H, 60Co, 90Sr, 99Tc, 106Ru, 106Rh, 125Sb, 137Cs, 137mBa, 154Eu, 238Pu, 239/240Pu, 241Pu, 241Am, 242Cm, and 243/244Cm. B&W TSG-RACL provided subsamples to GEL Laboratories, LLC for analysis for the VOCs benzene, toluene, and 1-butanol. GEL also determines phenol (total) and the following radionuclides: 147Pm, 226Ra and 228Ra. Preparation of the 2QCY11 saltstone samples for the quarterly analysis and for vault classification purposes and the subsequent TCLP analyses of these samples showed that: (1) The saltstone waste form disposed of in the Saltstone Disposal Facility in 2QCY11 was not characteristically hazardous for toxicity. (2) The concentrations of the eight RCRA metals and UHCs identified as possible in the saltstone waste form were present at levels below the UTS. (3) Most of the inorganic species measured in the leachate do not exceed the MCL, SMCL or TW limits. (4) The inorganic waste species that exceeded the MCL by more than a factor of 10 were nitrate, nitrite and the sum of nitrate and nitrite. (5) Analyses met all quality assurance specifications of US EPA SW-846. (6) The organic species (benzene, toluene, 1-butanol, phenol) were either not detected or were less than reportable for the vault classification samples. (7) The gross alpha and radium isotopes could not be determined to the MCL because of the elevated background which raised the detection limits. (8) Most of the beta/gamma activity was from 137Cs and its daughter 137mBa. (9) The concentration of 137Cs and 90Sr were present in the leachate at concentrations 1/40th and 1/8th respectively than in the 2003 vault classification samples. The saltstone waste form placed in the Saltstone Disposal Facility in 2QCY11 met the SCHWMR R.61-79.261.24(b) RCRA metals requirements for a nonhazardous waste form. The TCLP leachate concentrations for nitrate, nitrite and the sum of nitrate and nitrite were greater than 10x the MCLs in SCDHEC Regulations R.61-107.19, Part I A, which confirms the Saltstone Disposal Facility classification as a Class 3 Landfill. The saltstone waste form placed in the Saltstone Disposal Facility in 2QCY11 met the R.61-79.268.48(a) non wastewater treatment standards.

Eibling, R.

2011-09-28T23:59:59.000Z

18

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

SciTech Connect (OSTI)

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