• 제목, 요약, 키워드: hydride generation method

검색결과 28건 처리시간 0.039초

Determination of Bi Impurity in Lead Stock Standard Solutions by Hydride-generation Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.233-236
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    • 2004
  • Total impurity analysis of a primary standard solution is one of the essential procedures to determine an accurate concentration of the standard solution by the gravimetry. Bi impurity is determined in Pb standard solutions by inductively coupled plasma mass spectrometry (ICP-MS). The direct nebulization of the Pb standard solution produces a significant amount of the Pb matrix-induced molecular ions which give rise to a serious spectral interference to the Bi determination. In order to avoid the spectral interference from the interferent $^{208}PbH^+$, the hydride generation method is employed for the matrix separation. The Bi hydride vapor is generated by reaction of the sample solution with 1% sodium borohydride solution. The vapor is then directed by argon carrier gas into the ICP after separation from the mixture solution in a liquid-gas separator made of a polytetrafluoroethylene membrane tube. The presence of 1000 ${\mu}$g/mL Pb matrix caused reduction of the bismuthine generation efficiency by about 40%. The standard addition method is used to overcome the chemical interference from the Pb matrix. Optimum conditions are investigated for the hydride-generation ICPMS. The detection limit of this method is 0.5 pg/mL for the sample solutions containing 1000 ${\mu}$g/mL Pb matrix.

수소화물 발생-유도결합플라스마 질량분석법에 의한 철강 중의 납의 정량 (Determination of Lead in Steels by Hydride generation-Inductively Coupled Plama/Mass Spectrometry)

  • 박창준;송선진;이동수
    • 분석과학
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    • v.14 no.5
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    • pp.410-415
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    • 2001
  • 철강 시료 중의 납 분석을 위하여 수소화물 발생법을 플라스마에 납을 선택적으로 주입하고 유도결합플라스마 질량분석법으로 측정하는 분석법을 개발하였다. 납 수소화물 $PbH_4$의 생성을 위해서는 $NaBH_4$와 반응 전에 먼저 준안정 상태의 Pb(IV)로 만들어주기 위하여 산화제가 필요하다. $1000{\mu}g/mL$ 이상의 철 매질을 함유하는 시료용액으로 납 수소화물을 발생시키기 위한 최적조건을 찾는 연구를 수행하였다. 철 매질이 $10{\mu}g/mL$ 이상 존재할 때는 $K_2Cr_2O_7$이 효과적인 산화제로 작용하였으며 젖산을 가하여 감도를 향상시켰다. 시료용액의 산농도 그리고 산화제와 젖산 농도의 최적값은 철 매질의 농도에 따라 달랐다. 동위원소 희석법을 사용하여 납을 정량하였으며 철강 표준물질 NIST SRM 361, 362 분석결과는 불확도 범위안에서 검정값과 잘 일치하였다.

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HG-ICP-AES를 이용한 Germanium 분석에 있어서 보조산에 대한 연구 (Investigation of Acids on the Germanium Analysis by HG-ICP-AES)

  • 임현의;이연희;김선태;김영상;김강진
    • 분석과학
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    • v.14 no.1
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    • pp.34-43
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    • 2001
  • 수소화물생성법-유도결합플라스마-원자방출분광법으로 게르마늄을 분석할 때 보조산으로 phosphoric acid의 사용은 nitric acid, hydrochloric acid, sulfuric acid, perchloric acid, boric acid, tartaric acid, malic acid, oxalic acid, acetic acid, tannic acid, citric acid의 사용보다 높은 수소화물 생성효율을 보였고, 같은 pH영역이라도 phosphate ion이 존재하는 buffer의 사용이 더 높은 생성효율을 보였다. 또한, 2.5M phosphoric acid를 이용한 결과, 시료용액 내에 잔류하는 산이나 공존원소의 영향이 감소하였다. 환원제와 안정제의 농도가 증가할수록 수소화물 생성효율은 증가되었으며, 최대방출세기를 나타내는 산의 세기는 높은 쪽으로 이동했고 농도영역은 넓어졌다. 인산 존재 하에서의 게르마늄의 검출한계는 $0.03{\mu}g/L$이었다.

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수소화물발생 유도결합플라즈마 원자방출분광법에 의한 머리카락 시료 중 미량의 Se와 Bi의 분석에 관한 연구 (A study on the Determination of Trace Se and Bi in the Scalp Hair by Hydride Generation- Inductively Coupled Plasma Atomic Emission Spectrometry)

  • 최범석;이동기
    • 분석과학
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    • v.9 no.1
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    • pp.26-34
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    • 1996
  • 수소화물 발생장치를 사용한 유도결합플라즈마 원자방출분광법(ICP-AES)으로 머리카락 시료 중에 함유된 미량의 Se와 Bi의 분석에 관해 연구하였다. 기체상태의 수소화물 측정시 ICP의 최적 측정조건은 시료운반기체의 유속은 0.6~0.8L/min, 관측위치는 유도코일로부터 6mm 높이였다. 수소화물 생성효율이 최대를 나타내는 염산농도는 $NaBH_4$와 NaOH를 각각 2.5% 사용할 때 1.5M 이상일 때였으며, 2.5% $NaBH_4$와 0.1% $NaBH_4$를 사용할 때는 약 O.5M 이상일 때였다. 분석과정에서 Cu와 Ni 같은 전이금속으로부터의 심한 방해영향이 관찰되었고, lanthanum hydroxide로 Se와 Bi를 공침시켜 방해영향을 제거하였다.

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환원기화 원자 흡광광도법에 의한 대기분진중의 총 셀렌의 정량 (Hydride Generation-Atomic Absorption Spectrophotometric Determination of Total Selenium in Atmospheric Particulate)

  • 이용근;최건형;이동수;황규자
    • 한국대기환경학회지
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    • v.6 no.2
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    • pp.147-154
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    • 1990
  • A sensitive method for the determination of total selenium in aerosol particles is described. The method involves dissolution of aerosol particles by $HNO_3-HClO_4$ mixed acids, pre-reduction of Se (VI) to Se (IV) by boiling hydrochloric acid, and hydride generation followed by atomic absorption detection. Dissolved Se (IV) in 4M hydrochloric acid is reacted with $NaBH_4$ to form $H_2Se$, which is subsequently collected in an U-tube cooled in liquid nitrogen. Upon the completion of $H_2Se$ generation, the collected $H_2Se$ is rapidly vaporized into a quartz cuvette burner by removing the U-tube from liquid nitrogen, atomized, and then detected by an atomic absorption spectrophotometer. The absolute sensitivity of the method is 0.49 ng/0.0044 Abs. The accuracy of the method evaluated by analyzing standard reference materials for urban aerosol is better than 10%. Analytical results for urban and rural aerosol particles are reported.

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수소화물 생성-유도 결합 플라즈마 분광법에 의한 머리카락 중 비소의 분석 (Determination of Arsenic in Human Scalp Hair by Hydride Generation-Inductively Coupled Plasma Spectrometry)

  • 박형신;김선태;진현철;류시생;최범석
    • 분석과학
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    • v.5 no.1
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    • pp.51-56
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    • 1992
  • 수소화물 생성-유도결합플라즈마 분광법으로 머리카락 중 비소를 정량하는 방법에 대해 연구하였다. Arsine의 생성시 최적 조건과 머리카락에 공존하는 원소에 의한 방해영향을 조사하였다. Ni(II)이 arsine의 생성에 큰 방해영향을 주므로 비소를 $La(OH)_3$에 의한 공침법으로 분리하였다. 본 방법에 의한 비소의 검출한계는 0.3ppb이며 머리카락 중 비소의 함량은 약 10~20ppb였다.

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HG-AAS법에 의한 요중 비소의 최적 분석법에 관한 연구 (A Study on the Optimal Analytical Method for the Determination of Urinary Arsenic by Hydride Generation-Atomic Absorption Spectrometry)

  • 이종화;이의선;홍성철;장봉기
    • 한국환경보건학회지
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    • v.35 no.5
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    • pp.402-410
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    • 2009
  • This study was carried out to examine the optimal analytical method for determination of urinary toxic arsenic (inorganic arsenic and its metabolites) by HG-AAS (hydride generation-atomic absorption spectrometry). In the analysis of SRMs (standard reference materials), method E (addition of 0.4% L-cysteine to pre-reductant and use 0.04M HCl as carrier acid) showed the most accurate results compared with the reference values. In the analysis of 30 urinary samples, analytical results were significantly different depend on the component of pre-reductant and the concentration of carrier acid. When the concentration of carrier acid was higher, the analytical result was lower. The recovery rates of MMA (monomethylarsonic acid) and DMA (dimethylarsenic acid) were varied by the concentration of pre-treatment acid and carrier acid and hydride generation reagents. When the concentration of carrier acid was 1.62 M (5% HCl), the recovery rates of DMA was 1%. The recovery rates of MMA and DMA in method E (=V) were 102% and 100%, respectively. The results of this study suggest that the component and concentration of pre-reductant and carrier acid must be carefully adjusted in the analysis of urinary arsenic, and method E is recommendable as the most precise analytical method for determination of urinary toxic arsenic.

Determination of Selenium and Tellurium by HG-AAS in Foods

  • Cha, Ki-Won;Park, Sang-Ho;Park, Kwang-Won
    • 분석과학
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    • v.8 no.4
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    • pp.419-425
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    • 1995
  • A method has been investigated for the determination of selenium and tellurium in Ginseng, Ganoderma and Garlic using hydride generation atomic absorption spectrometry(HG-AAS). The concentration effects of hydrochloric acid and sodium tetrahydroborate on the hydride generation for the determination of selenium and tellurium were investigated. The method of sample decomposition was also investigated using various mineral acids, such as nitric, perchloric and sulfuric acid in the closed system, and foreign ion effects containing in the samples were studied. The calibration curves of selenium and tellurium were obtained in the range of 0~40 ppb. The detection limits(S/N=2) of selenium and tellurium are 0.1 and 0.2 ppb. Analytical data of selenium and tellurium in Garlic, Ganoderma and Ginseng are 289, 296 and 198 ng/g for selenium and 146, 127 and 110 ng/g for tellurium, respectively.

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FPGA를 이용한 소형 태양광 발전 니켈 수소 전지 충전 시스템의 POS MPPT 제어 (FPGA based POS MPPT control for a small scale charging system of PV-nickel metal hydride battery)

  • 이효근;서효룡;김경훈;박민원;유인근
    • 대한전기학회:학술대회논문집
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    • pp.1306-1307
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    • 2011
  • Recently, the small scale photovoltaic (PV) electronic devices are drawing attention as the upcoming PV generation system. The PV system is commonly used in small scale PV applications such as LED lighting and cell phone. This paper proposes photovoltaic output sensorless (POS) maximum power point tracking (MPPT) control for a small scale charging system of PV-nickel metal hydride battery using field-programmable gate array (FPGA) controller. A converter is connected to a small scale PV cell and battery, and performs the POS MPPT at the battery terminal current instead of being at the PV cell output voltage and current. The FPGA controller and converter operate based on POS MPPT method. The experimental results show that the nickel metal hydride battery is charged by the maximum PV output power.

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FPGA를 이용한 소형 태양광 발전 니켈 수소 전지 충전 시스템의 POS MPPT 제어 (FPGA based POS MPPT Control for a Small Scale Charging System of PV-nickel Metal Hydride Battery)

  • 이효근;서효룡;김경훈;박민원;유인근
    • 전기학회논문지
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    • v.61 no.1
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    • pp.80-84
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    • 2012
  • Recently, the small scale photovoltaic (PV) electronic devices are drawing attention as the upcoming PV generation system. The PV system is commonly used in small scale PV applications such as LED lighting and cell phone. This paper proposes photovoltaic output sensorless (POS) maximum power point tracking (MPPT) control for a small scale charging system of PV-nickel metal hydride battery using field-programmable gate array (FPGA) controller. A converter is connected to a small scale PV cell and battery, and performs the POS MPPT at the battery terminal current instead of being at the PV cell output voltage and current. The FPGA controller and converter operate based on POS MPPT method. The experimental results show that the nickel metal hydride battery is charged by the maximum PV output power.