Pre-treatment of polychlorinated biphenyl analysis in mineral oils or oily waste muds.

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Other Title
  • 鉱油及び廃油中のポリ塩化ビフェニル分析の前処理法
  • コウユ オヨビ ハイユチュウ ノ ポリ エンカ ビフェニル ブンセキ ノ マエ

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Abstract

To keep the marine environment clean, an analytical method for PCB concentration in waste oils had to be devised to meet the requirement for disposal treatment. The legal criterion of marine disposal which can be dumped into ocean and the incinerated on board has provided that the highest contamination of PCB in the waste oil or waste muds must be within 0.15μ/g. But usual technique of PCB analysis does not detect such a low level in waste substances including large amount of mineral oil because the usual pre-treatment by simple combination of silica gel and florisil column chromatography can not remove the large amount of hydrocarbons sufficiently. The partitioning extraction by dimethylsulfoxide (DMSO) and washing by fuming sulfuric acid were added to the scheme of the refining procedure, that is, florisil dry column clean up, DMSO partitioning extraction, digestion by potassium hydroxide-ethanol solution, silica gel column clean up and washing by fuming sulfuric acid were convined in the final pre-treatment system. Experimantal results using the carrier of fuel oils were able to determine 0.1 ppm of PCB, with 87% of recovery. The partitioning extraction using DMSO was given extremely higher recovery than the acetonitrile-hexane partitioning extraction and washing by fuming sulfuric acid was effective treatment for the removal of organochloric pestisides and phthalate esters originated from environmental contamination. The chromatogram of a PCB-spiked waste oil sample was almost the same as that of the mixed standard of PCB.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 34 (11), T143-T147, 1985

    The Japan Society for Analytical Chemistry

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