ANALYSIS OF NONYLPHENOL POLYETHOXYLATES AND THEIR DEGRADATION PRODUCTS IN RIVER WATER AND SEWAGE EFFLUENT BY GAS-CHROMATOGRAPHY ION-TRAP (TANDEM) MASS-SPECTROMETRY WITH ELECTRON-IMPACT AND CHEMICAL-IONIZATION

A method is presented for the analysis of nonylphenol polyethoxylate ( NPEO) residues and their degradation products, nonylphenol polyethoxy carboxylates and carboxyalkylphenol ethoxy carboxylates, in the sample s of river water and sewage effluent. The method involves extraction o f the samples by graphitized carbon black (GCB) cartridge, propylation by a propanol/acetyl chloride derivatization procedure, and separatio n, identification and quantitation by ion-trap GC-MS with electron imp act ionization (EI), liquid-chemical ionization (CI) and CI-MS-MS mode s. The large-volume injection technique provides high precision and se nsitivity for both NPEO residues and their degradation products, to qu antitation at greater than or equal to 0.01 mu g/l in 100 ml of water samples. Dicarboxylic acids of NPEO residues were identified by the CI -MS-MS technique with relatively high concentrations in the samples of river water and sewage effluent. Recovery of nonylphenol and octylphe noxyacetic acid in spiked water samples ranged from 81 to 107%. Relati ve standard deviations of replicate analyses ranged from 2 to 12%. (C) 1998 Elsevier Science B.V. All rights reserved.