• Title/Summary/Keyword: PCBs analytical method

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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.

Analysis of all PCB Congeners in Air Samples by HRGC/HRMS (대기 시료 중 PCBs 전 이성체 분석에 관한 연구)

  • Kim, Kyoung-Soo;Song, Byung-Joo;Kim, Jong-Guk
    • Analytical Science and Technology
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    • v.16 no.4
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    • pp.309-319
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    • 2003
  • This study was performed to describe analysis method of 209 PCB congeners in ambient air samples. The samples were collected by high volume air sampler in Chonju city. Extracted samples were cleaned by silicagel cleanup modified with sulfuric acid and activated carbon cleanup processing. The cleaned samples were analyzed by high resolution gas chromatography and high resolution mass spectrometry (HRGC/HRMS) with DB-5 column (60 m, 0.25 mm i.d., 0.25 m film thickness) to analyze the 209 kinds of PCB congeners. PCBs levels of air samples were detected to the range between 0.003 and $0.163pg-TEQ/m^3$. The PCBs congener of 162 kinds were detected in samples analysed using DB-5 column and 37 kinds peaks were overlapped with congeners more than one. It is difficult to isolate PCB 118/106 and PCB 105/127 in coplanar PCB, so it is likely to overestimate the concentration.. The distribution of coplanar-PCB congeners in origin source samples (Kanechlor and exhaust gas from incinerator) was compared with that in air samples, and PCB 81, PCB 77, PCB 126, and PCB 169 were higher in incinerator samples.

Distribution and exposure assessment of indicator PCBs in Food (식품 중 indicator PCBs의 분포와 노출평가)

  • Oh, Keum-Soon;Suh, Jung-Hyuck;Paek, Ok-Jin;Park, Seong-Soo;Na, Young-Joon;An, Yeong-Sun;Kim, Mee-Hye;Lee, Kwang-Ho
    • Analytical Science and Technology
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    • v.23 no.3
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    • pp.312-321
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    • 2010
  • Seven indicator PCBs (IUPAC nos 28, 52, 101, 118, 138, 153, 180 congeners) concentrations were measured in food samples including cereal (polished rice), meats, eggs, milk and dairy products, and fisheries and products as representation for the general Korean populations during 2006-2007, and was analyzed using isotopic dilution method. Fishes had the highest average level as 39.8 ng/g, 1.4 ng/g for milk and dairy products, and 0.9 ng/g for meats. The hairtail out of fishes was contaminated at the level of 15.4 ng/g, 5.4 ng/g for pacific mackerel and spanish mackerel, and 4.5 ng/g for yellow croaker. The ratio for indicator PCBs in overall food was contributed as follows; 35.8% for PCB-153, 16.2% for PCB-138, 16.1% for PCB-101, 13.4% for PCB-118, 8.8% for PCB-180, 6.9% for PCB-52, and 2.9% for PCB-28. The hexa-CBs including PCB-153 and 138 were more predominated, and the next was penta-CBs including PCB-101 and 118 in food. For estimated daily intake (EDI) in average and $95^{th}$ percentile, fishes and products out of overall food were taken to represent over 50%. However, it was estimated that there was no adverse health effect for Korean.

Introduction of the Rapid Analysis Method for PCBs in Insulating Oils and Its Comparison Study to the Analysis Method in Korea

  • Hong, Jang-Ho;Takahashi, Tomohumi;Ishizaka, Takahiro;Toita, Hideki;Min, Byung-Yoon;Honda, Katsuhisa
    • Environmental Engineering Research
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    • v.16 no.1
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    • pp.11-18
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    • 2011
  • The aim of this research was to introduce a new rapid analysis method (heating of the multi-layer silica gel column/alumina column) for polychlorinated biphenyls in insulating oils, and to compare our new method with the analytical method currently used in Korea. The entire pretreatment procedure was completed within 2 hr, using about only 20 mL of solvents via our rapid analytical method. Furthermore, the pretreatment procedure can always be uniformly performed, regardless of oil type (JIS 1~JIS 7 and KS 1~KS 7). The recovery rates were more than 89%, with relative standard deviations below 6.0%. In conclusion, this rapid analytical method could reduce the pretreatment time and solvent usage by 1/10 and between 1/25 and 1/50, respectively, compared to analytical method currently used in Korea.

The Development of Rapid analytical Method for PCBs in Transformer Oils (변압기 절연유 중 PCBs 신속분석법 개발)

  • Park, Seok-Un;Nam, Chang-Hyun;Park, Hyun-Joo
    • Proceedings of the KIEE Conference
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    • 2008.11a
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    • pp.136-138
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    • 2008
  • PCBs는 잔류성유기오염물질(POPs) 중 하나로 변압기 절연유 등에 주로 사용되어 왔으나 환경 및 인체유해성이 밝혀짐에 따라 생산 및 사용이 금지된 물질로써 국내에서는 절연유 중 PCBs 분석이 전력산업과 변압기 절연유의 재활용 및 처리 분야에서 매우 중요한 문제로 대두되고 있다. 그러나 현행 폐기물공정시험방법은 분석절차가 까다롭고 고가의 분석비용이 소모되며 고도로 훈련된 분석인력이 필요하다. 이에 본 연구에서는 보다 저렴한 비용으로 신속하게 PCB를 분석할 수 있는 간이 분석법을 개발하고자 하였다. 현행 폐기물공정시험방법에 대한 기술적 검토를 수행하여 복잡한 전처리 절차를 축소하고 번거로운 정성 및 정량작업을 간소화한 결과, 분석비용은 약 1/2, 분석시간은 약 1/3로 줄일 수 있었다. 본 연구에서 개발한 간이 분석법을 현행 공정시험법과 적절히 병행하여 사용 할 경우 폐 변압기의 신속한 분석이 가능하여 분석비용 절감에 따른 큰 경제적 효과가 있을 것으로 예상된다.

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Power Integrity and Shielding Effectiveness Modeling of Grid Structured Interconnects on PCBs

  • Kwak, Sang-Keun;Jo, Young-Sic;Jo, Jeong-Min;Kim, So-Young
    • JSTS:Journal of Semiconductor Technology and Science
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    • v.12 no.3
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    • pp.320-330
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    • 2012
  • In this paper, we investigate the power integrity of grid structures for power and ground distribution on printed circuit board (PCB). We propose the 2D transmission line method (TLM)-based model for efficient frequency-dependent impedance characterization and PCB-package-integrated circuit (IC) co-simulation. The model includes an equivalent circuit model of fringing capacitance and probing ports. The accuracy of the proposed grid model is verified with test structure measurements and 3D electromagnetic (EM) simulations. If the grid structures replace the plane structures in PCBs, they should provide effective shielding of the electromagnetic interference in mobile systems. An analytical model to predict the shielding effectiveness (SE) of the grid structures is proposed and verified with EM simulations.

Analytical Head-space Supercritical Fluid Extraction Methodology for the Determination of Organochlorine Compounds in Aqueous Matrix

  • Ryoo, Keon-Sang;Ko, Seong-Oon;Hong, Yong-Pyo;Choi, Jong-Ha;Kim, Yong-gyun;Lee, Won-Kyoung
    • Bulletin of the Korean Chemical Society
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    • v.27 no.5
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    • pp.649-656
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    • 2006
  • The proposed head-space supercritical fluid extraction (SFE) methodology as an alternative to an existing conventional procedure was explored for the determination of organochlorine compounds in aqueous matrix. In this study, polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) were utilized as target analytes. To enhance the recovery efficiency, the factors such as the $CO _2$ density, the extraction time, and the extraction mode were investigated. Furthermore, the analytical procedures and the results obtained were compared with those provided by the conventional method (the U.S. EPA method 8080). Under the optimized conditions, i.e., a combination of static with dynamic SFE mode at 2,000 psi and 40 ${^{\circ}C}$, the head-space SFE methodology gave equivalent or better to the conventional method in recovery efficiencies with clear advantages such as simple sample treatment and fast analysis time as well as reduced solvent and reagent consumption.

Analytical Method for Dioxin and Organo-Chlorinated Compounds : (I) Pretreatment of Milk Samples for Dioxin Analysis

  • 양정수;김진영;최용욱;이대운
    • Bulletin of the Korean Chemical Society
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    • v.19 no.6
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    • pp.619-624
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBS) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

The Analysis of Dioxin-like PCBs in Fishes and Shellfishes using Accelerated Solvent Extraction (ASE) System and Multilayer Column Chromatography (가속용매추출장치(ASE) 및 다층크로마토그래피를 이용한 어패류 중의 dioxin-like PCBs의 분석)

  • Oh, Keum-Soon;Park, Seong-Soo;Chung, So-Young;Sho, You-Sub;Kim, Jung-Soo;Jang, Seoung-Chul;Lee, Jong-Ok;Kim, Hee-Yun;Woo, Gun-Jo;Suh, Jung-Hyuck
    • Korean Journal of Food Science and Technology
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    • v.39 no.2
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    • pp.122-127
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    • 2007
  • In this study, an analytical method was optimized for detecting dioxin-like PCBs in fish and shellfish. Here, homogenized samples were extracted using an accelerated solvent extraction (ASE) system with 33 mL cell size. Multilayer column chromatography, which consisted of acidic, basic and neutral silica gels, was used for the clean up of the extracts. The instrumental analysis was executed by HRGC/HRMS to a resolution of 10,000 using 4 window multiple ion detection (MID) mode. For the results, the average recoveries ranged from 94.1 to 104.1% (${\pm}8.4$) and the limit of detection was approximately 0.1 pg/g at S/N ratio >3. Finally, the detected concentrations of dioxin-like PCBs for fish and shellfish were in the range of 0.030-1.836 pg TEQ/g.

Sample Pretreatment and HRGC/HRMS Analysis for Determination of Dioxins in Environmental Samples (환경시료 중 다이옥신류의 정량을 위한 시료전처리방법의 개선 및 고분해능 GC/MS 분석에 관한 연구 Ⅰ)

  • Kim, Jin Yeong;Jang, Yun Seok;Lee, Dae Un
    • Journal of the Korean Chemical Society
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    • v.38 no.11
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    • pp.819-826
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    • 1994
  • This study described a simple, rapid and cost effective analytical technique for the ultra-trace analysis of dioxins in environmental samples. Liquid-Liquid extraction methods were used for the initial extraction and enrichment of the analyte. Subsequent clean-up procedures were achieved by using strong cation exchanger, silica and Florisil cartridges. Extracts were analysed by HRGC/HRMS-SIM. The efficiency of these analytical methods was tested by recovery and selectivity for elimination of interferences such as phenols, pesticides and PCBs in each step. The mean recovery of 1,2,3,4-TCDD spiked at 10 ppt in sea water was about 92(${\pm}$1.6)%. This analytical method was applied to Kwangyang sea water and 4.5pg/L of 2,3,7,8-TCDD was determined.

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