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  • Effect of Pedological Characteristicson Aqueous Soil Extraction Recoveryand tert-Butyldimethylsilylation Yieldfor Gas Chromatography−MassSpectrometry of Nerve GasHydrolysis Products from Soils
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  • Detection and identification of alkyl methylphosphonate(RMPA) and methylphosphonate (MPA) are performed toverify the existence of nerve gases by gas chromatography−mass spectrometry (GC−MS) after tert-butyldimethylsilylation (TBDMS). However, it is sometimes difficult to detectRMPA and MPA in soils. This study examines therelationship between the pedological characteristics andthe aqueous extraction recoveries and TBDMS derivatizationyields of ethyl-, isopropyl- and pinacolyl methylphosphonateand MPA for 21 soil samples. The aqueous extractionrecoveries were measured directly by capillary electrophoresis. Andosols showed low extraction recoveries, whileRegosols and Fluvisols showed high recoveries. RMPAwere extracted with higher recoveries than MPA from allsoils. MPA could not be extracted from Andosols. Withinthe pedological characteristics, phosphate absorptioncoefficients showed a strong negative correlation with theextraction recoveries of all phosphonates. The levels ofRMPA and MPA in aqueous soil extracts were also determinedfor eight soils by GC−MS after TBDMS. Compared tothe aqueous extraction recoveries, the yields of TBDMSderivatives were low. Strong anion exchange led to asignificant improvement in derivatization yields. Theefficiencies of TBDMS derivatization were inversely correlatedwith the levels of alkaline earth metals extractable fromsoils when the three soils that possessed high total carbonwere excluded.
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