• 제목/요약/키워드: HPLC-Hydride generation

검색결과 4건 처리시간 0.017초

HPLC-ICPMS를 이용한 셀레늄 화학종의 연구에서 화학적 및 광화학적 수소화물 발생법의 비교 (Comparison of chemical and photochemical generation of hydrides in Se speciation study with HPLC-HG-ICPMS)

  • 지하나;박용남
    • 분석과학
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    • 제25권6호
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    • pp.339-344
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    • 2012
  • In this research, hydride generation in HPLC-ICPMS for the selenium speciation was investigated. Chemical and photochemical vapor generation techniques were compared for the effective generation of selenium vapour. $HBr/KBrO_3$ was used for the chemical reduction and a UV lamp was used for the photochemical reduction. It was found out that the photochemical reduction was more effective than the chemical reduction in all of selenium species studied. The optimum conditions for the generation of vapour are 0.4% KI, 2.5% $NaBH_4$, and 1.0 M HCl. The enhancement factor using a photochemical hydride generation was from 6.3 to 16.7 times for inorganic and organic selenium species.

이이스트 고정 bio칼럼을 이용한 Sb의 화학종분리 및 연속적 수소화물발생법에 의한 감도개선 (Separation and Sensitive Determination of Sb Species using Yeast Bonded Bio-column with Continuous Hydride Generation)

  • 이정옥;권효식;박용남
    • 대한화학회지
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    • 제54권6호
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    • pp.696-700
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    • 2010
  • 매우 작은 유리구슬(직경 $100{\mu}m$이하)위에 이이스트를 공유결합시킨 bio컬럼을 제작하여 $Sb^{3+}$$Sb^{5+}$를 선택적으로 분리하고 연속적 수소화물 발생법을 이용하여 감도를 개선하였다. 최적 용리조건은 용리액 0.8 M 질산으로 흐름속도 1.0 mL $min^{-1}$이며 수소화물 발생의 최적조건은 HCl 2 M, 환원제로 $NaBH_4$ 3% (w/v), 흐름속도는 0.83 mL $min^{-1}$, 수소화물을 운반하는 아르곤기체의 흐름속도는 50 mL $min^{-1}$ 이었다. 이러한 조건에서 두 화학종의 분리시간은 각각 112초와 354초였다. $200{\mu}L$의 시료를 사용하였을 때 감도는 10 여배 개선되었고 검출한계는 $Sb^{3+}$$Sb^{5+}$에 대하여 각각 3.0 ppb와 7.0 ppb 이었다. 표준시료를 제작하여 분석한 결과, 정확한 결과를 얻을 수 있었다.

FI-HG-AAS를 이용한 전처리 과정에서 사용되는 예비환원제의 종류에 따른 요중 비소 분석결과 비교 (Comparisons of Urinary Arsenic Analysis by Pre-reductant for Preconditioning via the FI-HG-AAS Method)

  • 최승현;최재욱;조용민;배문주
    • 한국환경보건학회지
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    • 제41권5호
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    • pp.289-298
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    • 2015
  • Objectives: The method of analyzing urinary arsenic by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS) is generally used because it shows relatively greater sensitivity, low detection limits, low blocking action, and is simple to operate. In this study, the results of analysis according to three pre-reductants commonly used in the FI-HG-AAS method were compared with each other. Methods: To analyze urinary arsenic, nineteen urine samples were collected from adults aged 43-79 years old without occupational arsenic exposure. Analysis equipment was FI-HG-AAS (AAnalyst 800/FIAS 400, Perkin- Elmer Inc., USA). The three pre-reductants were potassium iodide (KI/AA), C3H7NO2S (L-cysteine), and a mixture of KI/AA and L-cysteine (KI/AA&L-cysteine). Results: In the results of the analysis, the recovery rate of the method using KI/AA was 82.3%, 95.7% for Lcysteine, and 123.5% for KI/AA and L-cysteine combined. When compared with the results by use of high performance liquid chromatography inductively-coupled plasma mass spectrometry (HPLC-ICP-MS), the method using L-cysteine was the closest to those using HPLC-ICP-MS ($98.57{\mu}g/L$ for HPLC-ICP-MS; $74.96{\mu}g/L$ for L-cysteine; $69.23{\mu}g/L$ for KI/AA and L-cysteine; $13.06{\mu}g/L$ for KI/AA) and were significantly correlated (R2=0.882). In addition, they showed the lowest coefficient of variation in the results between two laboratories that applied the same method. Conclusion: The efficiency of hydride generation is considered highly important to the analysis of urinary arsenic via FI-HG-AAS. This study suggests that using L-cysteine as a pre-reductant may be suitable and the most rational among the FI-Hg-AAS methods using pre-reductants.

HPLC-AFS를 이용한 해산물 중 비소 화학종 분리정량 (Quantification of Arsenic Species in Some Seafood by HPLC-AFS)

  • 정승우;이채혁;이종화;장봉기
    • 한국환경보건학회지
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    • 제47권5호
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    • pp.496-503
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    • 2021
  • Background: Considering the expenses of and difficulties in arsenic speciation by high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), alternative measurement methods should be useful, especially for large-scale research and projects. Objectives: A measurement method was developed for arsenic speciation using HPLC-atomic fluorescence spectrometry (HPLC-AFS) as an alternative to HPLC-ICP-MS. Methods: Total arsenic and toxic arsenic species in some seafoods were determined by atomic absorption spectrometry coupled with hydride vapor generation (AAS-HVG) and HPLC-AFS, respectively. Recovery rate of arsenic species in seafood was evaluated by ultra sonication, microwave and enzyme (pepsin) for the optimal extraction method. Results: Limits of detection of HPLC-AFS for As3+, dimethylarsinate (DMA), monomethylarsonate (MMA) and As5+ were 0.39, 0.53, 0.60 and 0.64 ㎍/L, respectively. The average accuracy ranged from 97.5 to 108.7%, and the coefficient of variation was in the range of 1.2~16.7%. As3+, DMA, MMA and As5+ were detected in kelp, the sum of toxic arsenic in kelp was 40.4 mg/kg. As3+, DMA, MMA and As5+ were not detected in shrimp and squid, but total arsenic (iAS and oAS) content in shrimp and squid analyzed by AAS-HVG were 18.1 and 24.7 mg/kg, respectively. Conclusions: HPLC-AFS was recommendable for the quantitative analysis method of arsenic species. As toxic arsenic species are detected in seaweeds, further researches are needed for the contribution degree of seafood in arsenic exposure.