Flammable gas safety program. Analytical methods development: FY 1993 progress report

Abstract

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 components 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.