• Title/Summary/Keyword: 표준물질

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Synthesis and Isolation of Monoacetyl-DCB and Diacetyl-DCB from 3,3대-dichlorobenzidine(DCB) (디클로로벤지딘으로부터 대사물질의 합성과 분리방법에 대한 연구)

  • Lee, Jin-Heon;Lee, Beom-Gyu
    • Journal of Environmental Health Sciences
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    • v.29 no.2
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    • pp.50-55
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    • 2003

  • 3,3-dichlorobenzidine is suspected to be cancinogenic in experimental animal and human. Several studies have investigated excretion of metabolites in urine, hemoglobin adduction and cancer incidence among workers occupationally exposed to 3,3'-dichlorobenzidine. In these researches, metabolites of 3,3'-dichlorobenzidine had a very important role, and were required as highly purity. The purpose of this study was synthesis and isolation of its metabolites from 3,3'-dichlorobenzidine. 3,3'-dichlorobenzidine was partially dissolved in benzene, ether, ethanol and methanol, and completely dissolved in 70% acetic acid on mixtures of citric acid containing less than 1% DCB, pyridine, a mixture of 0.5N NaOH and toluene(1:2), and phenol saturated with 20 mM TRIZA base. DCB, monoacetyl-DCB and diacetyl-DCB were measured by using gas chromatography/mass spectrometry(GC/MS). Detection for checking them was nitrogen phosphorous detection mode(NPD), and for identifying them was selected ion monitoring mode(SIM). The base peaks were 252 m/z in DCB, 252, and 294 m/z in monoacetyl-DCB, and 252, 294 and 336 m/z in diacetyl-DCB, respectively. Diacetyl-DCB was synthesized by titrating DCB solution of pyridine with sufficient acetyl chloride. Precipitation was diacetyl-DCB, which was purity of 98.7%. And its supernatant was composed of DCB, monoacetyl-DCB and diacetyl-DCB. By using acetic acid as controller of acetylation, monoacetyl-DCB was isolated from diacetyl-DCB . And residual pyridine was removed by using acetone. The purity of monoacetyl-DCB was 98.8%.

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Preparation of wastewater-based reference materials for heavy metal analysis and interlaboratory study (중금속분석용 폐수표준물질 제조 및 실험실간 비교평가)

  • Kim, Young-Hee;Song, Ki-Bong;Shin, Sun-Kyoung;Lee, Jung-Sub;Jeong, Gi-Taeg;Hong, Eun-Jin;Park, Jin-Ju;Yu, Suk-Min
    • Analytical Science and Technology
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    • v.23 no.3
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    • pp.295-303
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    • 2010

  • In this study, the wastewater-based reference material (RM) was prepared and certified for 7 trace metal elements with evaluation of uncertainties. The RM was distributed to 25 laboratories for the interlaboratory comparison testing. The certified values and expanded uncertainties were derived using ISO guideline 35 and the standard uncertainties for homogenieties were 0.43~2.67% of certified values. The analytical results from the interlaboratory comparison testing showed normal distributions and the robust means from the interlaboratory comparison testing were higher than the certified values of the RM for all analytes.

  • https://doi.org/10.5806/AST.2010.23.3.295 인용 PDF KSCI