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Abstract  

Ion-pair chromatography was tested for its applicability in determining monobutyl phosphate (MBP) and dibutyl phosphate (DBP), which are degradation products of tributyl phosphate, in Hanford tank wastes. In tests with simulant waste mixtures, tetrahexylammonium bromide, an ion-pairing agent, was used to complex with all three phosphate species. Recovery studies indicated that ion-pairing chromatography is quantitative for determining the analytes in spiked samples. Initial results demonstrated that DBP could be detected easily and was fairly well separated from other peaks, but MBP was frequently lost due to large negative peaks. Then a preconcentration column procedure was used to clean up the waste-sample matrix, and the negative peaks disappeared. Results indicated that 80% of MBP and 90% of DBP could be recovered. Most of the radioactivity was removed from actual waste tank samples so that additional sample preparation could be performed safely in a fume hood rather than a hot cell. Dibutyl phosphate was identified in an actual tank waste, but MBP was not found; this result was confimed by ion chromatography with conductivity detection.

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Journal of Thermal Analysis and Calorimetry
Authors:
J. Douillard
,
H. Malandrini
,
T. Zoungrana
,
F. Clauss
, and
S. Partyka

Abstract  

It is possible to estimate surface tension of high-energy solids combining the immersion microcalorimetry thermodynamics and Van Oss' model. In this study we have applied this method on talc and talc-chlorite samples in order to obtain thermodynamic values which permit to understand surface properties useful in the industrial applications of these solids. Some talcite samples are preferentially used in specific industrial applications because they are less hydrophobic or more lamellar. This method seems to be reliable to classify the solids and predict some properties.

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Abstract  

Tank wastes are usually very basic, pH>12, and extremely radioactive. An ion exchange method for removing most of the radioactive components has been developed. The sample can then be removed from the hot cell facility to be analyzed for chelator, chelator fragments, and low-molecular weight acids. The use of cation exchange resin in the sample preparation does not introduce or remove any organic carbon.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
S. Goheen
,
B. McVeety
,
T. Clauss
,
R. Lucke
,
M. Ligotke
,
J. Edwards
, and
J. Fruchter

Abstract  

Organic species from the headspace of one Hanford radioactive waste tank are described. Samples were collected either using a sorbent trap or a SUMMATM canister and were analyzed by gas chromatograph and mass spectrometry. The headspace contained several organic components, including alkanes, alkenes, ketones, aldehydes, organic nitriles, and chlorinated hydrocarbons. Sorbent trap samples were designed to collect only normal paraffin hydrocarbons (NPHs). A comparison of NPH data from sorbent traps and SUMMATM cans revealed results of 693 and 1320 mg/m3, NPH respectively. Significant differences were observed in NPH values when samples were collected at different times, or at different locations in the tank. These data suggest either the time of collection, or the position of the sampling device are important variables in the analysis of organic species from Hanford tanks.

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Abstract  

A technique has been developed for the qualitative determination of low-molecular-weight organic acids in radioactive, mixed hazardous wastes using thermospray liquid chromatography/mass spectrometry. A tank waste was analyzed, and the results indicated the presence of citric, glycolic, acetic, and nitrosoiminodiacetic acid (NIDA). Further investigation revealed NIDA was formed under acidic conditions with the reaction of iminodiacetic acid and the high nitrate/nitrite concentration present in the waste.

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