• 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.

• Analytical Science and Technology
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• v.25 no.6
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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.

• 한국신재생에너지학회:학술대회논문집
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• 2009.06a
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• pp.781-781
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• 2009

We demonstrate that trasition metal catalyst nanoparticle (NP) attached to carbon nitride nanotubes (CNNTs) show selective catalytic activities on hydrogen generation from the water solution including chemical hydride negative ions. The natural bonding orbitals (NBO) obtained from the first-principle calculations shows that the catalysts attached on CNNTs are quite differently polarized when they play for hydrogen generation from chemical hydride ions and hydrogen of water. For Co and Ni nanoparticles attached on CNNTs, their charges are more positively polarized when they interact with $BH_4^-Na^+$ and $H_2O$ while Pt atoms are less positively charged. In this matter, the increased positive charges on catlyst nanoparticles are proven to be more efficient in attracting hydride negative ions, thus improving hydrogen generate rates. Consequently, this result implies that these different charge polarization leads to selective catalytic activities of NPs-CNNTs. In the hydrogen generation experiments, Co-CNNTs shows the highest hydrogen generation rate when the similar amounts of catalyst nanoparticles (Co, Ni, and Pt) are dispersed on the sidewalls of CNNTs.

• 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.

• 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 $0.03{\mu}g/L$.

• 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.

• Analytical Science and Technology
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• v.14 no.5
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• pp.410-415
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• 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.

• Analytical Science and Technology
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• v.5 no.1
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• pp.51-56
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• 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.

• Korean Journal of Metals and Materials
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• v.48 no.8
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• pp.717-723
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• 2010

The degradation behavior of fuel cladding is a very import concern in nuclear power generation, because the operation of nuclear plants can be limited by fuel cladding degradation. In order to evaluate the hydride effect on failure of zirconium fuel claddings, a ring tensile test for the circumferential direction was carried out at room temperature for claddings having different hydride characteristics such as density and orientation; microstructural evaluation was also performed for those claddings. The circumferential failure of the claddings was promoted by increasing the hydride concentration in the matrix; however, the failure of the claddings was affected by the hydride orientation rather than by the hydride concentration in the matrix. From fracture surface observation, the cladding failure during the ring tensile test was matched with the hydride orientation.

• Analytical Science and Technology
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• v.13 no.2
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• pp.151-157
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• 2000

Effects of acids and pre-reductants in the analysis of arsenic have been studied by hydride generation-atomic absorption spectrometry. The analytical results were strongly dependent on the acid concentrations. All the pre-reductants was very effective to observe the arsenic signal at strong acid concentrations (3 M-5 M). However, at the low acid condition (${\leq}0.1M$), L-cysteine only showed a reasonable effect on the absorption signal. When the sample was treated with the nitric acid, absorption signal was unstable and was also decreased. Although interference effects were observed from metal ions such as $Cr^{6+}$ and $Br^{5+}$ at low acid condition, the generation of hydride could be increased by the strong acid condition.