• 제목/요약/키워드: capillary column

검색결과 188건 처리시간 0.024초

Determination of Pd(II) and Pt(II) Metal Cyano Complexes Using Capillary Electrophoresis

  • Lee, Hue-Jin;Lee, Sang-Ho;Chung, Koo-Soon;Lee, Kwang-Woo
    • Bulletin of the Korean Chemical Society
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    • 제15권11호
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    • pp.945-949
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    • 1994
  • Mixtures of cyano complexes of palladium(II) and platinum(II) were separated by capillary electrophoresis using a fused silica capillary as a separation column and 30 mM phosphate buffer (pH 7) containing 15 wt. % acetonitrile as a running buffer. By virtue of the high ionic mobilities of the negatively charged cyano complexes of Pd(II) and Pt(II), they were separated using a cathodic injection and anodic detection scheme. The metal complexes eluted through the capillary were detected by direct UV absorption at 214 nm. A linear relationship between peak area and concentration was obtained for both ions and the detection limit was lower than $10^{-14}$ mole. The proposed method was applied to real sample, e.g., anode slime obtained from an electrolytic copper refinary, as a method for the simultaneous determination of palladium and platinum.

Capillary Electrochromatography with Liquid Crystal Crown Ether Modified Hybrid Silica Monolith for Analysis of Imidacloprid and Carbendazim in Tomatoes

  • Wang, Mingming;Feng, Rui;Shen, Jing;Chen, Hao;Zeng, Zhaorui
    • Bulletin of the Korean Chemical Society
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    • 제33권7호
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    • pp.2224-2228
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    • 2012
  • This study describes the ability of capillary electrochromatography (CEC) for the determination of imidacloprid and carbendazim in tomato samples. A novel liquid crystal crown ether modified hybrid silica monolithic column was synthesized, characterized and developed as separation column for the first time. Baseline separation of imidacloprid and carbendazim could be achieved using a mobile phase containing 90% (v/v) 20 mmol/L phosphate buffer (pH 7.0) and 10% (v/v) acetonitrile. The matrix matched calibration curves were linear with correlation coefficient $r^2$ > 0.9998 in the range of 0.20-10.00 mg/L. The limits of detection for imidacloprid and carbendazim were 0.061 and 0.15 mg/kg, respectively, which were below the maximum residue limits established by the European Union as well as Codex Alimentarius. Average recoveries for imidacloprid and carbendazim varied from 101.6-108.0% with relative standard deviations lower than 6.3%. This method was applied to the analysis of tomatoes collected from local markets.

국내수집 달맞이꽃 종실의 감마-리놀렌산 함량(Ⅵ보) (Gamma-linolenic Acid Content of Evening Primrose(Oenothera odorata Jacq.) in Korea)

  • 임웅규
    • 한국작물학회지
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    • 제35권2호
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    • pp.176-178
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    • 1990
  • 한국에서 자생군락이 비교적 큰 3지역에서 채집한 달맞이꽃 종자의 필수 지방산을 Capillary column gas chromatography로 분석하였다. 각 지방산의 조성 함량은 palmitic acid가 6.19-6. 73%, stearic acid가 1.84-l.99%, oleic acid 가 6.73-9.10%, linoleic acid가 74.41-75.53%이었다. 특히 prostaglandin의 전구체인 GLA는 청주가 9.14%, 제천이 9.32%이고, 안동이 8.31%이었다. 따라서 한국의 자생 달맞이꽃은 GLA자원으로 유용한 것으로 생각된다.

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Gas Chromatograph에 의한 Arylmethy Halides의 정량 (Determination of Arylmethyl Halides by Gas Chromatograph)

  • 오도석;최호춘
    • 한국산업보건학회지
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    • 제4권1호
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    • pp.25-32
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    • 1994
  • Arylmethyl halides(benzyl chloride, BZYC; benzal chloride, BZYA; benzotrichloride, BZTC) and related compounds(benzyl alcohol, BZYA; benzoyl chloride, BZOC) were determined by GC using capillary column. Detailed results are as follows. 1. Stability In methanol benzotrichloride slowly transferred to benzoyl chloride by hydrolysis(ca. 7.5% for 5 days), but the others were stable. Therefore, benzotrichloride solution should be prepared just before analysis. 2. GC analysis Tenax-GC was used to absorbent and desorption solvents were $CCl_4$ and MeOH. Arylmethyl halides were analyzed within 7.5min without interference with related compounds. The calibration curve(ca. 15-80 ppm in soln), repeatability(n=10) and the desorption efficiency were good. Limit of detection by NIOSH method was about 0.003 ppm for arylmethyl halide, respectively. To analyze arylmethyl halides and related compounds in working places GC using capillary column is anticipated to be used effectively.

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Analyses of phenolics in cigarette smoke by GC-MS with the multiple ion selction technique

  • Park, Jeen-Woo
    • Archives of Pharmacal Research
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    • 제5권2호
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    • pp.71-77
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    • 1982
  • Improvements in the analytical methodology used in the gas chromatographic/mass spectral analysis of phenolic compounds from cigarette smoke are described. For the direct analysis of crude samples, pyridine extraction and the glass capillary column GC was used for the separation of phenolics as trimethylsilyl derivativatives. The separations of cigarette smoke on Carbowax 20M and SE-54 wall coated open tubular columns are given. Improved methodology for the routine quantitation of the identified components using the computer-controlled multiple ion selection technique of MS presented. Considerations pertaining to routine analyses of a multitude of complex smoke samples are also discussed.

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수용성 매체로부터 휘발성 유리 지방산의 미량 농축에 관한 연구 (Trace Enrichment of Volatile Free Acids from Aqueous Samples)

  • 김경례;최동미
    • 대한화학회지
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    • 제31권3호
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    • pp.244-249
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    • 1987
  • 미생물의 대사산물 중에서 각각의 균주에 특징있게 생성되는 탄소수 $C_2-C_5$인 휘발성 유리산의 정성 정량 분석자료는 혐기성 미생물을 확인하는 정보를 준다. 수용성 매체에 용해되어 있는 미생물의 대사산물을 처리함에 있어서 흡착제로 Chromosorbp를 사용한 liquid-solid extraction 방법에 대하여 조사 검토하였다. Chromosorb P는 친수성인 흡착제이므로 그 표면에 간섭물질인 수용성 성분들이 흡착되어 남아있는 반면에 비이온화성인 휘발성 유리산들은 ether에 의해서 정량적으로 회수가 된다. 이와 같이 신속하며 효율적으로 처리된 시료를 5% Carbowax 20M/0.75% $H_3PO_4$로 coating 된 stainless steel capillary column 으로 정성 정량분석하였다.

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Comparison between Head Space Gas Sampling and Purge & Trap Sampling in Water Analysis

  • Nagayanagi, Yutaka;Nakagawa, Katsuhiro;Saito, Yoshihiro;Kim, Poongzag
    • 분석과학
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    • 제8권4호
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    • pp.739-744
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    • 1995
  • The two main methods to prepare water samples for analyzing volatile organic compounds(VOC's) were investigated. One is the purge and trap(PT) method and another is the head space(HS) sampling method. Both methods were effective to transfer the low boiling point components from the water sample onto the capillary column. The cryo-focusing at the top of the main capillary column was an effective way to obtain the sharpness of the chromatographic peaks but could be avoided when a semi-wide bore column was used. The recovery from the same amount of the sample was better in PT than in HS but a larger sample volume in HS method could compensate the lower efficiency. Therefore PT is suitable to the analysis of drinking water where the very low concentration must be determined. HS is suitable to waste water analysis because of the easiness of the operation. The repeatability was good and similar in both methods. For the contamination of the former sample, both methods were tough and could be used without any problems. The matrix effect which could change the equilibrium parameters in HS method was find negligible in many components. The actual samples such as tap water and river water were analyzed with both methods concerning 16 components regulated in Korea.

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모세관전기영동을 이용한 수용성비타민의 분석 (Determination of Water-Soluble Vitamins by Free Solution Capillary Electrophoresis)

  • 최원균;조재선
    • 한국식품과학회지
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    • 제26권1호
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    • pp.18-22
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    • 1994
  • 7종의 수용성 비타민 즉, 티아민, 리보플라빈, 피리독신, 시아노코발라민, 아스코르브산, 엽산, 니코틴산을 free solution capillary electrophoresis로 정량분석하였다. 최적 분리조건 설정을 위해 완충용액의 pH, 모세관의 온도 그리고 적용한 전압에 대해 실험한 결과 완충용액의 pH는 6에서는 겹치는 peak가 있었으며 pH 8에서는 최적의 분리를 보여주었고 pH가 더 올라갈수록 분리도는 저하되었다. 모세관의 온도와 적용한 전압은 둘 다 높아질수록 분리시간은 단축되었으며 온도 $25^{\circ}C$, 전압 20 kV에서 최적분리능을 보여주었고 그 이상의 각 조건에서는 두 경우 모두 분리능이 저하되었다. 앞의 최적조건에서 수용성비타민은 8분내에 분리되었으며 각 peak의 migration time의 편차는 $0.01{\sim}0.1$분(CV : 0.9%)이었다.

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