• 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.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 %.

• Analytical Science and Technology
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• v.26 no.2
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• pp.135-141
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• 2013

The purpose of this study is to determine the quantity of selenium in grains by hydride generation-inductively coupled plasma mass spectrometry. Two sample preparation methods, beaker and microwave digestions, are compared and the former shows better result. The optimum condition for hydride generation is 4.0 M for HCl, 3% for $NaBH_4$ with the sample flow of 0.6 mL/min. The detection limit is 0.02 ${\mu}g/kg$($3{\sigma}$) and improved by 10 times. Isobaric interferences on Se is removed by Octopole Reactoin Cell and $H_2$ (3.8 mL/min) shows better performance over He. However, in case Br exists in a matrix, $H_2$ could induce interferences on m/z 80 and 82 ($^{80}[BrH]^+$ and $^{82}[BrH]^+$). The accuracy of this experiment is examined successfully by analyzing several reference materials. The results for several domestic grain analysis show that the concentrations are between 12.7 ${\mu}g/kg$ and 29.6 ${\mu}g/kg$.

• Journal of the Korean Chemical Society
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• v.54 no.6
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• pp.696-700
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• 2010

Yeast is immobilized upon $100{\mu}m$ CPG(controlled pore glass bead) to separate $Sb^{3+}$ and $Sb^{5+}$. Continuous hydride generation is performed after the bio-column. The optimum conditions are 0.8 M nitric acid as an eluent with the flow rate of 1.0 mL $min^{-1}$ and the optimum conditions for the generation of hydride are 2 M HCl, 3% (w/v) $NaBH_4$ with the flow rate of 0.83 mL $min^{-1}$, Ar carrier gas flow rate of 50 mL $min^{-1}$. Two species are separated at 112 and 354 seconds each. The sensitivity is enhanced by 10 times for $200{\mu}L$ of sample and the detection limits are 3.0 ppb and 7.0 ppb for $Sb^{3+}$ and $Sb^{5+}$, respectively. When compared with the standard samples, this method showed accurate results.

• 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.

• Journal of the Korean Society for Nondestructive Testing
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• v.23 no.4
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• pp.334-341
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• 2003

When the pressure tubes(f are in contact with the calandria tube(CT) in the pressurized heavy water reactor(PHWR), the temperature difference between inner and outer wall of W results in a thermal diffusion of hydrogen (deuterium) and hydride blisters are formed on the outer surface of PT. Because the hydride blisters and zirconium matrix are acoustically continuous, it is not easy to distinguish the blisters from the matrix with conventional ultrasonic method. An ultrasonic velocity ratio method was developed to detect small hydride blisters on the zirconium pressure tube. Hydride blisters were grown in the PT specimen using a steady state thermal diffusion device. The flight times of longitudinal echo and reflected shear echo from the outer surface were measured accurately. The velocity ratio of the longitudinal wave to the shear wave was calculated and displayed using contour plot. Compared to the conventional flight time method of longitudinal wave, the velocity ratio method shows superior sensitivity to detect smaller blisters as well as better images for the blister shapes. Detectable limit of the outer shape of the hydride blisters was conservatively estimated as $500{\mu}m$, with the same specifications of ultrasonic transducer used in the actual PHWR pressure tube inspection.

• 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.

• Resources Recycling
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• v.27 no.5
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• pp.30-37
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• 2018

For recylcing of high purity tantalum (Ta) scrap, We investigated manufacture of tantalum powder using hydride-dehydride (HDH) process. Tantalum had excellent properties such as ductile, hardness and high melting point. Usually these properties made difficult to make a powder. In this study, Tantalum powder was manufactured using Tantalum hydride via hydridation. Tantalum hydride was formed at $500^{\circ}C$, 5 hr/$700^{\circ}C$, 3 hr and it is easy to make a tantalum hydride powder because hydrogen in the tantalum act as a defect dislocation and lattice expansion. The powder was pulverized to a size of less than $10{\mu}m$ under a condition of 1300 rpm, 30 min using a ring mill, and tantalum powder with less than 50 ppm hydrogen was prepared through dehydridation in an Ar and low vacuum atmosphere.

• 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.