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Title: Organic analysis and analytical methods development: FY 1995 progress report

Abstract

This report describes the status of organic analyses and developing analytical methods to account for the organic components in Hanford waste tanks, with particular emphasis on tanks assigned to the Flammable Gas Watch List. The methods that have been developed are illustrated by their application to samples obtained from Tank 241-SY-103 (Tank 103-SY). The analytical data are to serve as an example of the status of methods development and application. Samples of the convective and nonconvective layers from Tank 103-SY were analyzed for total organic carbon (TOC). The TOC value obtained for the nonconvective layer using the hot persulfate method was 10,500 {mu}g C/g. The TOC value obtained from samples of Tank 101-SY was 11,000 {mu}g C/g. The average value for the TOC of the convective layer was 6400 {mu}g C/g. Chelator and chelator fragments in Tank 103-SY samples were identified using derivatization. gas chromatography/mass spectrometry (GC/MS). Organic components were quantified using GC/flame ionization detection. Major components in both the convective and nonconvective-layer samples include ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), succinic acid, nitrosoiminodiacetic acid (NIDA), citric acid, and ethylenediaminetriacetic acid (ED3A). Preliminary results also indicate the presence of C16 and C18 carboxylic acids in the nonconvective-layer sample. Oxalic acidmore » was one of the major components in the nonconvective layer as determined by derivatization GC/flame ionization detection.« less

Authors:
; ;  [1]
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  1. and others
Publication Date:
Research Org.:
Pacific Northwest Lab., Richland, WA (United States)
Sponsoring Org.:
USDOE, Washington, DC (United States)
OSTI Identifier:
120865
Report Number(s):
PNL-10776
ON: DE96000808; TRN: 95:007835
DOE Contract Number:
AC06-76RL01830
Resource Type:
Technical Report
Resource Relation:
Other Information: PBD: Sep 1995
Country of Publication:
United States
Language:
English
Subject:
05 NUCLEAR FUELS; HANFORD RESERVATION; RADIOACTIVE WASTE MANAGEMENT; RADIOACTIVE WASTES; UNDERGROUND STORAGE; CHEMICAL ANALYSIS; TANKS; MONITORING; SAMPLING; ORGANIC COMPOUNDS; VOLATILE MATTER; GAS CHROMATOGRAPHY; MASS SPECTROMETERS

Citation Formats

Clauss, S.A., Hoopes, V., and Rau, J. Organic analysis and analytical methods development: FY 1995 progress report. United States: N. p., 1995. Web. doi:10.2172/120865.
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Clauss, S.A., Hoopes, V., & Rau, J. Organic analysis and analytical methods development: FY 1995 progress report. United States. doi:10.2172/120865.
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Clauss, S.A., Hoopes, V., and Rau, J. Fri . "Organic analysis and analytical methods development: FY 1995 progress report". United States. doi:10.2172/120865. https://www.osti.gov/servlets/purl/120865.
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@article{osti_120865,
title = {Organic analysis and analytical methods development: FY 1995 progress report},
author = {Clauss, S.A. and Hoopes, V. and Rau, J.},
abstractNote = {This report describes the status of organic analyses and developing analytical methods to account for the organic components in Hanford waste tanks, with particular emphasis on tanks assigned to the Flammable Gas Watch List. The methods that have been developed are illustrated by their application to samples obtained from Tank 241-SY-103 (Tank 103-SY). The analytical data are to serve as an example of the status of methods development and application. Samples of the convective and nonconvective layers from Tank 103-SY were analyzed for total organic carbon (TOC). The TOC value obtained for the nonconvective layer using the hot persulfate method was 10,500 {mu}g C/g. The TOC value obtained from samples of Tank 101-SY was 11,000 {mu}g C/g. The average value for the TOC of the convective layer was 6400 {mu}g C/g. Chelator and chelator fragments in Tank 103-SY samples were identified using derivatization. gas chromatography/mass spectrometry (GC/MS). Organic components were quantified using GC/flame ionization detection. Major components in both the convective and nonconvective-layer samples include ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), succinic acid, nitrosoiminodiacetic acid (NIDA), citric acid, and ethylenediaminetriacetic acid (ED3A). Preliminary results also indicate the presence of C16 and C18 carboxylic acids in the nonconvective-layer sample. Oxalic acid was one of the major components in the nonconvective layer as determined by derivatization GC/flame ionization detection.},
doi = {10.2172/120865},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Fri Sep 01 00:00:00 EDT 1995},
month = {Fri Sep 01 00:00:00 EDT 1995}
}
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Technical Report:
View Technical Report (3.38 MB)
DOI:  10.2172/120865
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  • ; ;
    This report describes the work performed during FY 1995 by Pacific Northwest Laboratory in developing and optimizing analysis techniques for identifying organics present in Hanford waste tanks. The main focus was to provide a means for rapidly obtaining the most useful information concerning the organics present in tank waste, with minimal sample handling and with minimal waste generation. One major focus has been to optimize analytical methods for organic speciation. Select methods, such as atmospheric pressure chemical ionization mass spectrometry and matrix-assisted laser desorption/ionization mass spectrometry, were developed to increase the speciation capabilities, while minimizing sample handling. A capillary electrophoresismore » method was developed to improve separation capabilities while minimizing additional waste generation. In addition, considerable emphasis has been placed on developing a rapid screening tool, based on Raman and infrared spectroscopy, for determining organic functional group content when complete organic speciation is not required. This capability would allow for a cost-effective means to screen the waste tanks to identify tanks that require more specialized and complete organic speciation to determine tank safety.« less

  • ; ;
    The objectives of this task are to develop and document extraction and analysis methods for organics in waste tanks, and to extend these methods to the analysis of actual core samples to support the Waste Tank organic Safety Program. This report documents progress at Pacific Northwest Laboratory (a) during FY 1994 on methods development, the analysis of waste from Tank 241-C-103 (Tank C-103) and T-111, and the transfer of documented, developed analytical methods to personnel in the Analytical Chemistry Laboratory (ACL) and 222-S laboratory. This report is intended as an annual report, not a completed work.

  • The development tests and examination equipment and new analytical chemistry techniques for examining irradiated LMFBR fuel pins are described. Quality assurance requirements for FFTF materials and components are presented. The development of a fuel burnup measurement method and the development of a fuel composition determination method are reviewed. (DCC)

  • Characterization of unirradiated and irradiated LMFBR fuels by analytical chemistry methods will continue, and additional methods will be modified and mechanized for hot cell application. Macro- and microexaminations will be made on fuel and cladding using the shielded electron microprobe, emission spectrograph, radiochemistry, gamma scanner, mass spectrometers, and other analytical facilities. New capabilities will be developed in gamma scanning, analyses to assess spatial distributions of fuel and fission products, mass spectrometric measurements of burnup and fission gas constituents and other chemical analyses. Microstructural analyses of unirradiated and irradiated materials will continue using optical and electron microscopy and autoradiographic and x-raymore » techniques. Analytical quality assurance standards tasks are designed to assure the quality of the chemical characterizations necessary to evaluate reactor components relative to specifications. Tasks include: (1) the preparation and distribution of calibration materials and quality control samples for use in quality assurance surveillance programs, (2) the development of and the guidance in the use of quality assurance programs for sampling and analysis, (3) the development of improved methods of analysis, and (4) the preparation of continuously updated analytical method manuals. Reliable analytical methods development for the measurement of burnup, oxygen-to-metal (O/M) ratio, and various gases in irradiated fuels is described.« less

  • ; ; ; ...
    This report describes the status of developing analytical methods to account for the organic constituents in Hanford waste tanks, with particular emphasis on those tanks that have been assigned to the Flammable Gas Watch List. Six samples of core segments from Tank 101-SY, obtained during the window E core sampling, have been analyzed for organic constituents. Four of the samples were from the upper region, or convective layer, of the tank and two were from the lower, nonconvective layer. The samples were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry (GC/MS). The major componentsmore » detected were ethylenediaminetetraacetic acid (EDTA), nitroso-iminodiacetic acid (NIDA), nitrilotriacetic acid (NTA), citric acid (CA), succinic acid (SA), and ethylenediaminetriacetic acid (ED3A). The chelator of highest concentration was EDTA in all six samples analyzed. Liquid chromatography (LC) was used to quantitate low molecular weight acids (LMWA) including oxalic, formic, glycolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon (TOC) in the samples analyzed was accounted for by these acids. Oxalate constituted approximately 40% of the TOC in the nonconvective layer samples. Oxalate was found to be approximately 3 to 4 times higher in concentration in the nonconvective layer than in the convective layer. During FY 1993, LC methods for analyzing LWMA, and two chelators N-(2-hydroxyethyl) ethylenediaminetriacetic acid and EDTA, were transferred to personnel in the Analytical Chemistry Laboratory and the 222-S laboratory.« less