• Title/Summary/Keyword: HRGC/ECD

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Analysis of PCBs in Food by Dual Column-HRGC/ECD (Dual Column-HRGC/ECD를 이용한 식품 중 PCBs 오염 실태조사)

  • Suh, Junghyuck;Kim, Jungmi;Hong, Mooki;Kim, Changmin;Choi, Dongmi
    • Analytical Science and Technology
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    • v.16 no.2
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    • pp.166-173
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    • 2003
  • To determine levels of PCBs in food, beef, pork, chicken, egg, mackerel, yellow croaker, anchovy, common squid and little neck clam were chosen and collected at markets in Seoul, Busan and Kwangju. Among 209 PCB congeners, 7 congeners (#28, #52, #101, #118, #138, #153 and #180) were selected as target compounds that were known as indicator congeners. Samples were homogenized, treated in alkali solution for 1 hour, and extracted with organic solvents. After extraction, extracts were cleaned up by sulfuric acid, purified on silica gel column chromatography, analyzed by dual column-HRGC/ECD and then confirmed by HRGC/MSD. As results, PCBs were detected in fish samples ranged from 0.0002 to 0.001 mg/kg. Both PCB #101 and PCB #118 were the major contributors among 7 congeners.

PCBs concentration and congener distribution in transformer insulation oil samples using GC/ECD and HRGC/HRMS analysis (GC/ECD와 HRGC/HRMS 분석을 이용한 변압기 절연유 중 PCBs 농도 및 이성체 분포)

  • Kim, Kyoung-Soo;Kim, Hyoung-Seop;Song, Byung-Joo;Jeong, Mi-Jeong;Kim, Jong-Guk;Park, Seok-Un;Shin, Sun-Kyoung
    • Analytical Science and Technology
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    • v.18 no.3
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    • pp.232-240
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    • 2005
  • The total PCBs level in the transformer insulation oil samples using GC/ECD and HRGC/HRMS were ranged from 0.087 to $223.6{\mu}g/g$ and ranged from N.D. to $154.04{\mu}g/g$, respectively. The calculated TEQ values were ranged from 0.00067 to 6.8 ng WHO-TEQ/g. Among the samples, 6 samples showed higher than 2 ppm concentration (specific waste criterion of Korea). A variety in the concentration of total PCBs were observed between ECD and HRMS analysis. This is maybe due to quantification mehtod. The Aroclor 1248 wasn't present in the samples. The distribution pattern of Co-PCB congeners showed that the ratio of monoortho substituted congeners were higher than non-ortho substituted congeners. Among that, PCB-167 congener was predominant. In addition, the distribution of Co-PCBs congeners was different with that of flue gas and ambient air samples as well as commercial PCB formulations (Aroclor, Kanechlor).

PYE [2-(1-pyrenyl)ethyldimethylsilylated silica] Column HPLC and HR-GC-(micro) ECD in the Accurate Determination of Toxic Co-planar PCBs and Polybrominated Diphenyl Ethers (PBDEs)

  • Kannan, Narayanan;Hong, Sang-Hee;Oh, Jae-Ryoung;Yim, Un-Hyuk;Li, Donghao;Shim, Won-Joon
    • Bulletin of the Korean Chemical Society
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    • v.26 no.4
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    • pp.529-536
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    • 2005
  • Measurement of toxicologically relevant polychlorinated biphenyl (PCB) congeners such as non-ortho(IUPAC#) 77, 81, 126, 169 and mono-ortho 105, 114, 118, 123, 156, 157, 189 and di-ortho 170, 180 and polybrominated diphenyl ethers (PBDEs) such as 47, 66, 85, 99, 100, 138, 153, 154 in environmental samples become almost mandatory in several countries now. However, most of the available methods involve expensive instrumentations such as HRGC-HRMS or ECNI-LRMS, apart from expensive extraction and clean-up (with large volume of solvents) steps. A method has been devised combining the analytical separation power of PYE [2-(1-pyrenyl)ethyldimethysilylated silica] column HPLC and high-resolution gas chromatographic techniques including micro-electron capture detection (ECD) and two dimensional gas chromatograpy-ECD techniques to determine these eco-toxic substances at parts-per-trillion (ppt) levels. This combination resolves co-elution of congeners that occur in disproportionate ratios (e.g. CB-110 and -77) and allows accurate congener-specific determination of target compounds. This method is cost effective as it requires only hexane, that in small quantities (10 mL) and GC-ECD. The elution and analysis time are optimized to less man hours. This method is effectively utilized in the analysis of co-planar PCBs and PBDEs from archived solvent extracts of samples previously analyzed for pesticides and PCBs. Structure based separation of contaminant classes improves GCECD determination at ppt levels.

Contamination level and congener profiles of PCBs, Co-PCBs and PCDD/DFs in transformer insulation oil samples (변압기 절연유 중 PCBs, Co-PCBs 및 PCDD/PCDFs 오염수준 및 이성체 분포)

  • Kim, Kyoung-Soo;Kim, Jong-Guk;Shin, Sun-Kyoung;Kim, Kyoung-Sim;Song, Byung-Joo
    • Analytical Science and Technology
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    • v.19 no.3
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    • pp.263-271
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    • 2006
  • The levels of total PCBs, Co-PCBs and PCDD/Fs in the transformer insulation oil samples obtained using GC/ECD and HRGC/HRMS were ranged from N.D. to 77.3 ppm, from 0.0863 to 2.49 ppm and from N.D. to 0.00241 ppm, respectively. In terms of WHO-TEQ values, Co-PCBs and PCDD/Fs were ranged from 23.3 to 600 pgTEQ/g and from N.D. to 128 pgTEQ/g, respectively (${\Sigma}Co$-PCBs+PCDD/Fs concentration was calculated 24.4~728 pgTEQ/g). Although, the contribution of PCDD/Fs was below 12% in total TEQ concentration, it is suggested contamination of PCDD/Fs in transformer insulation oils. Among 10 samples, 4 samples showed higher concentration than 2 ppm (specific waste criterion of Korea) and Aroclor 1242, 1248, 1254 and 1260 was detected in samples as a single or mixture of Aroclor. It was shown reliable relationship between concentration of Co-PCBs and those of PCDD/Fs (p<0.003), however, was not shown between production year of transformer and concentration of PCBs. The distribution pattern of Co-PCB congeners showed that the ratios of mono-ortho substituted congeners were higher than non-ortho substituted congeners. Among that, PCB-118 congener was predominant. In addition, the OCDD congener was predominated in PCDD/Fs congeners as above 53%. Moreover, the congener pattern of Co-PCBs was similar to that of Aroclor as well as ambient air, which suggested that PCBs volatilization from transformer insulation oil affected the pattern of Co-PCBs in ambient air.