Determination of polychlorinated biphenyls in waste oil by gas-liquid chromatography

Abstract

A 0.1 g portion of waste oil is cleaned up by silica gel chromatography followed by dimethylformamidehexane partitioning and chromatography on a de-activated neutral alumina column. The purified extract is examined for PCBs by either packed-column or capillary-column gas chromatography using either electon-capture or Hall electrolytic conductivity detectors. Recoveries at the 10 mg kg-1 level are in the range 66-98% and the coefficient of variation is typically 12%. A reporting limit of 5 mg kg-l is readily attainable and PCBs can be detected down to about 1 mg kg-1.

Validation of an improved European standard method for the determination of PCBs in oil samples

“…In addition to the official methods (where a combination of acidified silica/anion exchange (SiOH-H 2 SO 4 /SA) and silica adsorbent is proposed) numerous sample preparation techniques are available for PCB analysis in oil samples ranging from extraction with aprotic solvents (e.g. dimethylsulfoxide, dimethylformamide) (LARSEN et.al., 1991;LAWN and TOFFEL, 1987), enzyme immunoassay (LAMBERT et.al., 1997), HS SPME (CRIADO et.al., 2004), sulphuric acid and alkali treatment (SHIN and KIM, 2006;SHU et.al., 1995), gel permeation chromatography (SHERIDAN et.al., 1995), normal-phase (Florisil, alumina) (LULEK, 1998;NERIN and DOMENO, 1999;STORR-HANSEN et.al., 1992), reversed-phase chromatography and many surface modified silica for SPE may be in use (NH 2 , NH 2 -Cl, NH 2 -SO, SCX-2, SCX-2-NH 4 , SAX, SAX-SO 4 , CN, DIOL and PSA) for the separation of PCBs from mineral oils (TAKADA et.al. 2001;NA et.al., 2008;NUMATA et.al., 2006;NUMATA et.al., 2007;NUMATA NUMATA et.al., 2008).…”

Analysis method for PCBs in reclaimed oil using a fast-GC triple stage quadrupole mass spectrometer with the 13-component quantitation method

“…However, the aforementioned methods are extremely time-consuming in terms of performing a series involving sample preparation, GC measurement, and data analysis. Specifically, methods including sulfuric acid treatment, partition with dimethyl sulfoxide (DMSO)/hexane, partition with dimethylformamide (DMF)/hexane, florisil column cleanup, and silica gel column cleanup are used in sample preparation, and the operations require skilled technologies in terms of analysis and operation time (Copland and Gohmann 1982 ; Orazio et al 1989 ; Larsen et al 1991 ; Lawn and Toffel 1987 ; Gordon et al 1982 ; Sandra et al 1988 ; Suzuki et al 1991 ; Koizumi and Yoshimura 1984 ). Conversely, with respect to the analysis of insulation oil analysis in Japan, a few pretreatment techniques were developed to aid in performing the analysis in a more quick and easy manner (Takahashi and Honda 2010 ; Shimizu 2010 ; Hamada 2010 ).…”

Selective determination of polychlorinated biphenyls in waste oils using liquid–liquid partition followed by headspace solid-phase microextraction and gas chromatography with atomic emission detection

“…An alternative sample preparation approach consists of oil dilution with n-hexane followed by the extraction of PCBs using an aprotic and water miscible solvent, e.g. acetonitrile, dimethylformamide or dimethylsufoxide, which show the capacity to establish -interactions with the aromatic ring of the analytes [7][8][9][10][11]. Previous to the application of this procedure, some authors had recommended an oxidative treatment of the oil matrix with sulphuric acid [12].…”