SAMPLE PREPARATION TECHNIQUES FOR DETERMINING SEMIVOLATILE ORGANIC-COMPOUNDS IN NUCLEAR DEFENSE MATERIALS PRODUCTION WASTE

Extraction techniques for semi-volatile organic compounds in caustic a nd high-ionic-strength nuclear defense material production waste store d is presented. It was demonstrated that the nitrite ions in extracts caused degradation of chromatographic columns. Liquid-liquid extractio n, ion-exchange and two types of solid-phase extraction (SPE) adsorben t supports were investigated in this study. The SPE media were styrene -divinylbenzene and alumina. Three classes of compounds were used: aci ds, base/neutral, paraffinic hydrocarbons and alkyl phosphates. SPE wa s able to extract semi-volatile organic compounds in simulated waste s amples without significant carry-over of nitrate ion. Extraction yield s ranged from 2.3 to 97.6% (12% R.S.D.). The range of yields for each chemical class was 0-4.1%, 6.4-79.9%, 14.3-68.3% and 91.1-97.6% for th e acid, base/neutral, paraffinic hydrocarbons and alkyl phosphate comp ounds, respectively. Compounds of regulatory interest, organic semi-vo latile acid and base neutral compounds were found to be unstable in th e waste samples.