• Title, Summary, Keyword: hydride generation method

Search Result 28, Processing Time 0.037 seconds

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
    • /
    • v.25 no.2
    • /
    • pp.233-236
    • /
    • 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.

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

  • Park, Chang Joon;Song, Sun Jin;Lee, Dong Soo
    • Analytical Science and Technology
    • /
    • v.14 no.5
    • /
    • pp.410-415
    • /
    • 2001
  • An analytical method has been developed which determines lead in steel samples by inductively coupled plasma mass spectrometry (ICP-MS) with sample introduction by the hydride generation. The lead hydride is not stable and requires and oxidant for the oxidation into metastable Pb(IV) before reduction to $PbH_4$ with $NaBH_4$. A study was carried out to find and optimum lead hydride generation condition for a sample solution with more than $1000{\mu}g/mL$ Fe matrix. $K_2Cr_2O_7$ was found to work as an efficient oxidant when more than $10{\mu}g/mL$ Fe matrix was present. Lactic acid was used with the oxidant as a complexing agent of the metastable Pb(IV) to enhance sensitivity. Optimum concentrations of the sample acidity, oxidant and lactic acid were different depending on the matrix concentration. The isotope dilution method was employed for the quantitation of lead. The determined Pb concentrations of the NIST steel SRM 361 and 362 were in good agreement with the certified values within the uncertainty range.

  • PDF

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

  • Lim, Hyuneui;Lee, Yeunhee;Kim, Sun-Tae;Kim, Young-Sang;Kim, Kang-Jin
    • Analytical Science and Technology
    • /
    • v.14 no.1
    • /
    • pp.34-43
    • /
    • 2001
  • The present work is aimed to evaluate the conditions of the hydride generation (HG) for germanium analysis by inductively coupled plasma (ICP)-atomic emission spectrometry (AES). Twelve different kinds of acids were used such as phosphoric, hydrochloric, nitric, sulfuric, perchloric, boric, tartaric, malic, oxalic, tannic, citric, and acetic acid. It was found that phosphoric acid yielded the maximum efficiency of hydride generation. Also, efficient hydride generation was obtined with the buffer solutions containing phosphate ions over a wide range of pH. In addition, in the presence of phosphoric acid the interference caused by metals was suppressed in the hydride generation of germanium. As the concentrations of a reducing agent and a stabilizing increased the hydride generation efficiency and the acid concentration proviaing the maximum intensity were increased. By using an analytical method developed in this study, the contents of germanium in water and rock samples were determined. The detection limit of germanium in the presence of phosphoric acid was $0.03{\mu}g/L$.

  • PDF

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

  • Choi, Beom Suk;Lee, Dong Kee
    • Analytical Science and Technology
    • /
    • v.9 no.1
    • /
    • pp.26-34
    • /
    • 1996
  • A method to determine the trace amount of Se and Bi in the scalp hair using the hydride generation inductively coupled plasma atomic emmission spectrometry was studied. The optimum operation conditions of ICP for hydride generation are 0.6~0.8L/min for the carrier gas flow rate, and 6mm above the induction coil for the observation height. Hydrochloric acid concentrations for the optimum hydride generation conditions were greater than 1.5M when 2.5% $NaBH_4$ and NaOH were used, and greater than 0.5M when 2.5% $NaBH_4$ and 0.1% NaOH were used. Severe interference effects are observed from transition metals such as Cu and Ni, and they could be circumvented by the coprecipitation with lanthanum hydroxide.

  • PDF

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

  • 이용근;최건형;이동수;황규자
    • Journal of Korean Society for Atmospheric Environment
    • /
    • v.6 no.2
    • /
    • pp.147-154
    • /
    • 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.

  • PDF

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

  • Park, Hyung-Shin;Kim, Sun-Tae;Jin, Hyoun-Chul;Ryoo, Si-Saeng;Choi, Beom-Suk
    • Analytical Science and Technology
    • /
    • v.5 no.1
    • /
    • pp.51-56
    • /
    • 1992
  • A method to determine the trace level of arsenic in scalp hair by the hydride generation(HG)-inductively coupled plasma(ICP) spectrometry is described. The optimum conditions for the generation of arsine($AsH_3$), and the interference effects from the concomitant ions were studied. Severe interference effect from Ni(II) is circumvented by the coprecipitation of arsenic with $La(OH)_3$. The detection limit of arsenic is 0.3ppm and the arsenic contents in scalp hair ranged 10~20ppb.

  • PDF

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

  • Lee, Jong-Wha;Lee, Ui-Seon;Hong, Sung-Chul;Jang, Bong-Ki
    • Journal of Environmental Health Sciences
    • /
    • v.35 no.5
    • /
    • pp.402-410
    • /
    • 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
    • Analytical Science and Technology
    • /
    • v.8 no.4
    • /
    • pp.419-425
    • /
    • 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.

  • PDF

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

  • Lee, Hyo-Geun;Seo, Hyo-Ryong;Kim, Gyeong-Hun;Park, Min-Won;Yu, In-Keun
    • Proceedings of the KIEE Conference
    • /
    • /
    • pp.1306-1307
    • /
    • 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.

  • PDF

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

  • Lee, Hyo-Guen;Seo, Hyo-Ryong;Kim, Gyeong-Hun;Park, Min-Won;Yu, In-Keun
    • The Transactions of The Korean Institute of Electrical Engineers
    • /
    • v.61 no.1
    • /
    • pp.80-84
    • /
    • 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.