• Title/Summary/Keyword: Hydride generation ICP-AES

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Determination of Trace Amount of Germanium in Rocks and Sediments by Hydride Vapor Generation-ICP-AES (수소화합물 발생법-유도결합플라스마 원자방출 분광기를 이용한 암석및 퇴적물중 미량의 게르마늄 분석)

  • Shin, Hyung Seon;Choi, Man Sik;Kim, Kang Jin
    • Journal of the Korean Chemical Society
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    • v.41 no.8
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    • pp.399-405
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    • 1997
  • We examined the determination of trace amount of germanium in rocks and sediments by hydride vapor generation-ICP-AES. Germanium is formed volatile compounds with various types of acid reagents, but volatilizing of germanium was decreased in the presence of $H_3PO_4$. Sediments and rocks can be dissolved by mixed acids of $HF-HNO_3-H_3PO_4$ without volatilizing loss of germanium in open digestion system and it was possible to determine germanium by hydride generation-ICP-AES without further sample treatment. Detection limit of Ge is reached to 0.08 ppb under the condition of 5M $H_3PO_4$ and 1% $NaBH_4$ as a supporting acid and a reducing reagent, respectively. The measured values by hydride generation-ICP-AES agreed well with the reference values of SRMs as well as the values determined by solution nebulization-ICP-MS.

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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
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    • v.14 no.1
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    • pp.34-43
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    • 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 $0.03{\mu}g/L$.

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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
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    • v.9 no.1
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    • pp.26-34
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    • 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.

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Effect of NaBH4 and HCl on signal intensity of As, Se, Ge with on-line hydride generation system and E-O-V ICP-AES (수소화물 발생장치와 유도 결합 플라스마 원자화 방출 분광법 이용 시 비소와 셀레늄 및 게르마늄의 신호세기에 대한 NaBH4와 HCl의 영향)

  • Nam, Sang-Ho;Han, Soung-Sim
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.439-444
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    • 2002
  • DE-O-V ICP-AES has been studied for the analytical characteristics of As, Se, and Ge with PN, USN and HG. Effect of $NaBH_4$ and HCl on the signal intensity of As, Se and Ge with HG and E-O-V ICP-AES were closely investigated. The sensitivities of As, Se and Ge with HG were much greater than those with PN and USN. Accordingly, the detection limits of the elements with HG were lower by a factor of 100 and 10 than PN and USN, respectively.

Direct Determination of Tellurium in Simulated Nuclear Spent Fuels by Hydride Generation-Inductively Coupled Plasma Atomic Emission Spectrometry (수소화물 생성-유도결합플라스마 원자방출분광법을 이용한 모의사용후 핵연료 중의 텔루르 분석)

  • Choi, Kwang Soon;Lee, Chang Heon;Han, Sun Ho;Joe, Kih Soo;Kim, Won Ho
    • Analytical Science and Technology
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    • v.13 no.6
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    • pp.781-788
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    • 2000
  • Tellurium in simulated nuclear spent fuels (SIMFUEL) has been determined by hydride generation-inductively coupled plasma atomic emission spectrometry (HG-ICP-AES). Parameters such as concentrations of HCl and $NaBH_4$, flow rate of HCl and $NaBH_4$ were optimized and then the effects of U, Mo, Pd, Rh and Ru on the Te intensity were investigated. A thiourea as a masking agent was used to eliminate or minimize such interferences specially caused by palladium. Tellurium was measured by HG-ICP-AES and ICP-MS after separation of tellurium from SIMFUEL with cation exchange chromatography. The relative deviation between direct measurement and separation method was less than 6% based on the data by ICP-MS.

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Simultaneuous Determination of As(III) and As(V) in Disused Mine Tailing Samples by Hydride Generation-Inductively Coupled Plasma-Atomic Emission Spectrometry (수소화물 발생-유도결합 플라스마 원자 방출 분광법을 이용한 폐광산 광미 시료 중의 As(III)와 As(V)의 동시 정량)

  • Kim, Sun-Tae;Lim, Yoo-Ree;Park, Kyung-Su;Chung, Jin-Ho
    • Analytical Science and Technology
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    • v.13 no.2
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    • pp.189-193
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    • 2000
  • Arsenic (III) and arsenic (V) in disused mine tailing samples have been determined simutaneuously by hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-AES). Total arsenic was determined using 2% $NaBH_4$ and 6 M HCl after prereduction of As(V) to As(III) with) 1M KI. Arsenic (III) was determined selectively using citrate/citric acid buffer with range of pH 5-6, it was determined by HG-ICP-AES. Arsenic (V) can be evaluated by the differences. According to the results, arsenic (V) was over 90% among the total arsenic extracted from disused mine tailing samples.

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Continuous Coprecipitantion Preconcentration-Hydride Generation for Arsenic in Inductively Coupled Plasma-Atomic Emission Spectrometry (연속적 공침 선농축-수소화물 발생법을 이용한 ICP-AES에서의 비소의 감도 개선)

  • Kim, Chang-Gyu;Pak, Yong-Nam
    • Journal of the Korean Chemical Society
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    • v.48 no.6
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    • pp.583-589
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    • 2004
  • In a stream of aqueous sample, trace arsenic ions were quantitatively coprecipitated and detected in ICP-AES through hydride generation. In was used as a coprecipitating reagent. The precipitate was collected on a filter and dissolved by HCl. The eluted As was sent into the reaction coil to generate hydrides and analyzed by ICP. With optimal conditions, and with a sample of 0.3 mL, an enrichment of 70 was obtained with the sampling speed of 10/hr. When compared with coprecipitation and hydride generation technique, the sensitivity was increased by 7 and 10 times, respectively. The limit of detection limit$(3{\sigma})$ was 0.020 ${\mu}g\;L^{-1}$ and the precision was 7-10%. Separation of $As^{3+}\;and\;As^{5+}$ were possible using citric acid in hydride generation.

Arsenic Speciation Aanalysis in Bamboo Salts by Hydride Generation-ICP-AES (수소화물 발생-유도결합 플라즈마 원자 방출 분광법을 이용한 죽염중의 비소 종분리 분석)

  • Yu, Byung-Kyu;Lyu, Mu-Sang;Sun, Yle-Shik;Cho, Ki-Sung
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.41 no.5
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    • pp.674-680
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    • 2012
  • As(III) and As(V) were analyzed in bamboo salts by hydride generation ICP-AES. In order to quantify the total amount of As in bamboo salts, $AsH_3$ was producted by reacting with 6 mol/L hydrochloric acid and $NaBH_4$, which was then analyzed by hydride generation ICP-AES. As(V) was quantified simultaneously after selectively quantifying As(III). As(III) was quantified by determining the total amount of As and then correcting for the amount of As(III). To improve the reliability of the analysis we repeated the experiment several times to check the detection limit, quantification limit, and measurements of our testing methods. According to the result of our quantification analysis of As existing in bamboo salt, the range of total As content was 0.05 mg/kg~0.2 mg/kg and As(V) was over 90% of the total As.

Effect of Fluoride Ion in the Analysis of Tin by HG-ICP-AES (HG-ICP-AES법에 의한 Tin 분석시 플루오르화 이온의 영향에 대한 연구)

  • Lim, Heon-Sung;Cho, Sung-Il;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.416-421
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    • 2001
  • The optimization of the reductant and acid concentration for stannane($SnH_4$) generation was investigated by using a continuous flow hydride generator combined with an inductively coupled plasma-atomic emission spectrometer. Several different prereductants were studied to remove the interfering effect of fluoride ion on the hydride generating of tin. The optimum acid concentration was 0.5-1.0 M for the 1-2% $NaBH_4$ and 1.0 M NaOH and the interfering effect of fluoride ion was minimized using boric acid and L-cysteine mixed solution as a prereductant. The reconveries of tin at 20 ng/mL level in the solution containing fluoride ion were 100~108 %.

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