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• 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 components detected were ethylenediaminetetraacetie 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, glyeolic, 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.

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This report describes the work performed during FY 1997 by Pacific Northwest National Laboratory in optimizing analysis techniques for identifying organic components in Hanford waste tank samples. The work was conducted for the Flammable Gas and Organic Tanks Waste Safety Programs. The major focus during FV 1997 was the analysis of actual tank wastes. The methods developed during this task are illustrated by their application to samples listed below. S U-107"' BY-105 c108 segl (BY-105 1) A-102 Auger (A-102) U-105 grab (U-105 grab) U-105 c136 seg7 (U-105 s) BY-104 c117 (BY-104) U-106 c148 seg2 (U-106 s) AW-101 c139 seg21 (AW-101) C-105 c76 segl (C-105 1) U-106 c148 seg2 (U-106 1) U-102 c144 seg6 (U-102) AN-107 s-102 c = number, seg = segment number, 1= liquid, s= solid The samples from U-107 and AN-107 were grab samples; core and segment numbers do not apply. Samples C-105 c76 segl, BY-105 c108 segl, U-106 c148 seg2, and U-105 grab were liquid samples, and the rest were primarily solids. The methodology has been extended to the analysis of samples from Tank S-102 for Flammable Gas Generation Studies and analysis of simulated wastes to support Organic Waste Aging studies. The results reported here are from the most recent organic analyses and require further validatioxdverification. Table S. 1 lists the samples received by Pacific Northwest National Laboratory (PNNL) for analyses, the jarhial numbers, and associated laboratory identification numbers from the chain of custody (See also Appendix B).

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