• 제목/요약/키워드: standard analytical method

검색결과 903건 처리시간 0.028초

유도결합 플라즈마 발광분광기의 매트릭스 보정법에 의한 구리 중납, 카드뮴 및 크롬 분석에 관한 연구 (The Study on Analytical Method of Lead, Cadmium and Chromium in Copper Metal by Matrix Matching Method of Inductively Coupled Plasma Atomic Emission Spectrometer)

  • 주성균;김준;정남용;임규철;최영환;김상경
    • 대한화학회지
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    • 제53권3호
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    • pp.293-301
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    • 2009
  • 일정 농도의 Pb, Cd 및 Cr이 첨가된 합성 Cu표준시료용액 (RMs)을 ICP로 여러 파장에서 Cu매트릭스 미 보정 검정곡선에 준하여 분석한 결과 모든 원소가 전 파장에서 Cu매트릭스의 영향을 받아 정확도 (Pb 140$\sim$1 090%)가 떨어졌다. Pb, Cd 및 Cr의 각각 일정 농도에 Cu의 농도를 변화시켜 분석한 결과 Cu 0.05 wt/v % (0.05 g/100 mL) 이상을 함유하면 실제 Pb, Cd 및 Cr이 첨가된 농도보다 Cu의 농도가 증가함에 따라 일정함수의 비로 감소하거나 증가하여 Cu매트릭스의 영향이 심함을 볼 수 있었다. Cu매트릭스 보정법에 의한 합성 Cu표준시료용액 (RMs)을 분석한 결과 99.9% 이상의 정확도를 보여주었다.

Qualitative and quantitative determination of oleanolic acid in a scalp tonic products by HPLC using response surface methodology for extraction optimization

  • Cai, Lin Xi;Cho, Chong Woon;Zhao, Yan;Kang, Jong Seong;Kim, Kyung Tae;Jung, Sang-Hun
    • 분석과학
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    • 제32권2호
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    • pp.48-55
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    • 2019
  • The simple and effective analytical method for the quality control of a novel scalp tonic formulation has been developed and optimized in terms of HPLC conditions and sample preparation method, meanwhile, the optimization of preparation condition was using response surface methodology (RSM) based on central composite design (CCD). Oleanolic acid was selected as marker compound because of its bioactivities for alopecia therapy. The developed analytical method and extraction condition were successfully qualified. Coefficient of determination ($r^2$) for the calibration was 0.9997 with a line passing through the origin point in the range of 0.1-100 mg/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) were 17.5 ng/mL and 55.0 ng/mL, respectively. The intra-day and inter-day precision of the method were 0.5-1.4 % and 0.7-1.8 % in relative standard deviation, respectively, while those accuracy were 99.5-100.9 % and 100.0-102.2 %, respectively. The repeatability of oleanolic acid in samples ranged of 0.3-1.9 % based on peak area and 0.3-0.7 % for retention time. Recoveries from samples were 95.0-99.4 % with lower than 1.8 % in relative standard deviation. Overall, the developed analytical method will be used for quality control of this commercial scalp tonic products successfully.

Indirect Determination of Nitrite by Flame Atomic Absorption Spectrometry Using a Lead(IV) Dioxide Oxidant Microcolumn

  • Noroozifar, Meissam;Khorasani Motlagh, Mozhgan;Taheri, Aboozar;Homayoonfard, Marjan
    • Bulletin of the Korean Chemical Society
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    • 제27권6호
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    • pp.875-880
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    • 2006
  • A new, simple and fast flow injection analysis (FIA) method has been developed for the indirect determination of nitrite. The proposed indirect automatic method is based on the oxidation of nitrite to nitrate using a lead(IV) dioxide oxidant microcolumn where the flow of the sample through the microcolumn reduces the $PbO_2$ solid phase reagent to Pb(II), which is measured by flame atomic absorption spectrometry. The absorbance of Pb(II) are proportional to the concentration of nitrite in the samples. The calibration curve was linear up to 30 mg $L ^{-1}$, with a detection limit of 0.11 mg $L ^{-1}$ for a 400 mL injected sample volume and a sampling rate of about 80 $h ^{-1}$. The results exhibit no interference from the presence of large amounts of ions. The developed procedure was found to be suitable for the determination of nitrite in foodstuffs and wastewaters. A relative standard deviation better than 0.9% was obtained in a repeatability study. The reliability of the method was established by parallel determination against the standard method.

유도결합 플라스마 질량분석법에 의한 모발의 다원소 분석 (Multi - elemental Analysis of Hair by Inductively Coupled Plasma/Mass Spectrometry)

  • 차명진;강준모;박창준
    • 분석과학
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    • 제15권4호
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    • pp.335-340
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    • 2002
  • 유도결합 플라스마 질량분석법 (ICP-MS)을 이용하여 모발 중 다원소 동시 정량법을 확립하였다. 0.05 g의 모발 시료에 내부표준물질인 In을 가하고 질산 1.5 mL와 함께 테플론 가압분해 용기에 넣어 마이크로파를 이용하여 분해하는 시료전처리법을 사용하였다. 측정값의 정확도 및 신뢰도를 확인하기 위하여 모발 인증표준물질인 GBW 09101을 반복 분석하였는데 측정값은 인증값과 불확도 범위 내에서 잘 일치하는 결과를 얻었다.

유도결합 플라스마-질량분석법과 고체-액체 추출법을 이용한 해수중 미량금속의 분석에 관한 연구 (A Study on the Analytical Method of Trace Metal Ions in Sea Water by Inductively Coupled Plasma - Mass Spectrometry using Solid-Liquid Extraction Technique)

  • 이원;박경수;김은경;허영회
    • 분석과학
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    • 제11권6호
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    • pp.499-504
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    • 1998
  • An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in sea water has been investigated by Inductively Coupled Plasma-Mass Spectrometry. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Recoveries of 99.8% for Cu, 99.6% for Sn, and 97.9% for Bi were obtained for the standard spiked sample. The developed method was applied to analysis of trace metals in sea water.

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Determination of Boron Steel by Isotope-Dilution Inductively Coupled Plasma Mass Spectrometry after Matrix Separation

  • Park, Chang-J.
    • Bulletin of the Korean Chemical Society
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    • 제23권11호
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    • pp.1541-1544
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    • 2002
  • The concentration of B in steels is important due to its influence on mechanical properties of steel such as hardenability, hot workability, and creep resistance. An analytical method has been developed to determine B in steel samples by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). National Institute of Standard and Technology Standard Reference Material (NIST SRM) 348a was analyzed to validate the analytical method. The steel sample was digested in a centrifuge bottle with addition of aqua regia and $^{10}B$ spike isotope. Sample pH was then adjusted to higher than 10 to precipitate most matrix elements such as Fe, Cr, and Ni. After centrifugation, the supernatant solution was passed through a cation exchange column to enhance the matrix separation efficiency. B recovery efficiency was about 37%, while matrix removal efficiency was higher than 99.9% for major matrix elements. The isotope dilution method was used for quantification and the determined B concentration was in good agreement with the certified value.

PVC 제품에서의 염화비닐 단량체 정량분석 방법에 관한 연구 (Development of the testing method for vinyl chloride monomer (VCM) in polyvinyl chloride(PVC) samples)

  • 권덕준;최기인;엄희정;이재인;최철호
    • 분석과학
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    • 제25권6호
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    • pp.395-401
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    • 2012
  • 본 연구에서는 PVC 제품에 잔류하는 염화비닐 단량체(VCM)에 대한 정량분석방법을 제시하였다. 용출용매의 경우, 에탄올, THF, 아세톤에서 유사한 추출효율을 나타내었으나, 노말헥산을 이용한 경우에는 상대적으로 낮은 추출효율을 보였다. 분쇄 PVC 시료에 VCM 표준용액을 주입한 분석시료에 대한 VCM 함유량 측정 결과, GC/MS를 이용한 직접주입법이나 헤드스페이스법 모두 양호한 결과를 나타내었다. PVC 제품의 중간물질인 스펀지에서의 VCM 분석과 관련하여 5 개 시험전문기관의 시험소간 비교시험 결과, 각 시험소간 결과 편차가 크지 않은 것으로 나타나 본 연구에서 제시한 전처리 및 분석방법에 대한 플라스틱 제품내의 VCM 정량방법이 유효한 것으로 판단되었다.

적분법을 이용한 와전류신호의 해석적 모델 (An Analytical Model of Eddy Current Signal using Integral Method)

  • 정용무
    • 비파괴검사학회지
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    • 제11권2호
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    • pp.7-14
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    • 1991
  • The integral model for the eddy current phenomena has been suggested. The model could lift the limitations of the previously well-known analytical model of eddy current theory. The model could be applied to two-dimentional, arbitary shaped defects. The computer programs have been developed in order to calculate the eddy current signal with the suggested integral method. The eddy current signals by the model calculations have been shown similar patterns to the actual experimental data from the real defects in the calibration standard tubes.

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GC/ECD 및 GC/MS를 이용한 트리클로산 정량분석에 관한 기초 연구 (Fundamental study on the development of the testing method of Triclosan with GC/ECD and GC/MS)

  • 정희재;이재인;권덕준;엄희정;최철호;최기인
    • 분석과학
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    • 제25권6호
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    • pp.410-415
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    • 2012
  • 본 연구에서는 현재 항균제, 세정제 및 살균제의 형태로 가장 많이 사용되는 물질 중 하나인 트리클로산에 대한 전처리 방법 및 정량분석 방법을 확립하기 위한 기초적인 연구를 수행하였다. 노말헥산을 추출용매로 하여 속실렛 추출기에서 8 시간 추출할 경우, 가장 높은 추출효율을 보였으며, 분석장비는 GC-ECD와 GC-MS 모두 양호한 분석결과를 보였다. 본 연구에서 조제한 종이 여과지 시료 및 솜 시료를 각각 30 개씩 분석한 결과, 높은 트리클로산 추출효율, 낮은 분석 편차, 일원배치법에 따른 분산분석 결과를 고려할 때, 본 연구에서 조제한 시료 및 본 연구에서 제시한 추출 및 분석방법은 종이 및 섬유시료 내 트리클로산 분석에 유효하게 적용할 수 있을 것으로 판단되었다.

흑연로 원자흡수분광광도법에 의한 뇨시료 중 흔적량 원소의 정량 (Determination of Trace Elements in Urine Samples by Graphite Furnace Atomic Absorption Spectrophotometry)

  • 최종문;최희선;박창준;김영상
    • 분석과학
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    • 제7권4호
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    • pp.555-561
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    • 1994
  • A method was described for the graphite furnace atomic absorption spectrophotometric determination of trace cadmium, copper, chromium and lead in urine samples. The elements were directly determined without any other treatments. The ash temperature was intensively optimized to improve the large background by the removal of organic materials and alkali and alkali earth metals in urine samples. Two kinds of standard solutions were used to plot calibration curves. From the recovery data, it could be confirmed that the analytical results with the synthetic urine matrix similar to real urine were more accurate than with a deionized water matrix.

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