US EPA

2153851 

Journal Article 

COLUMN CHROMATOGRAPHIC SEPARATION OF POLYCHLORINATED BIPHENYLS FROM CHLORINATED HYDROCARBON PESTICIDES, AND THEIR SUBSEQUENT GAS-CHROMATOGRAPHIC QUANTITATION IN TERMS OF DERIVATIVES 

Berg, OW; Rees, GAV; Diosady, PL 

1972 

Yes 

Bulletin of Environmental Contamination and Toxicology
ISSN: 0007-4861
EISSN: 1432-0800 

NIOSH/00168645 

7 

6 

338 

English 

4205507 

WOS:A1972M971700003 

https://search.proquest.com/docview/45331132?accountid=171501
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A technique for the separation and quantitation of polychlorinated-biphenyl (1336363) (PCB) from organochlorine pesticides based on column chromatography was described. A separation technique based on activated charcoal was developed to overcome problems associated with commercial silica gels found to be contaminated with PCBs of the Aroclor-1254 (11097691) type. PCBs adsorbed onto charcoal were removed quantitatively with cold benzene. Organochlorine pesticides were eluted from the charcoal column with an ether/acetone mixture. Fisher coconut charcoal for decolorizing was determined to be the most suitable for the separation. Approximately 1.1 gram of charcoal was used for 5 micrograms of PCBs and 0.5 microgram of each of the DDT type pesticides. Identification and quantitation of the PCBs in terms of their derivatives were based on conversion into bicyclohexyl or decachlorobiphenyl using catalytic dechlorination and perchlorination reactions. Quantitative dechlorination utilized hydrogen over platinum or palladium catalysts. The conversions were better than 95 percent at the 10 microgram level. The main disadvantage of this technique according to the authors was that the PCB had to be determined with gas chromatography (GC)/flame ionization detection at a low level of sensitivity. Perchlorination to decachlorobiphenyl, which could be determined with GC electron capture detection, proved to be more adaptable to analytical problems. The perchlorination reaction involved treatment of the PCBs with antimony-pentachloride under elevated temperatures and anhydrous conditions. Yields were better than 85 percent for 1 microgram PCB. The decachlorobiphenyl chromatographic peak was well removed from the other pesticide peaks. The system as described was used for the isolation and quantitation of PCBs in samples from ducks, seagulls, porpoise blubber, sewage sediments, bottom fauna, and water samples. 

article; Animals; Catalysis; Charcoal; Chromatography, Gas; Dichlorodiphenyl Dichloroethylene; Dichlorodiphenyldichloroethane; Insecticides; Methods; Polychlorinated Biphenyls; Solvents; Spectrophotometry, Infrared; pesticides