• Analytical Science and Technology
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• v.18 no.5
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• pp.396-402
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• 2005

We try to look for optimum conditions of pre-reductants like L-Cysteine, KI and $FeSO_4$ when analyzing inorganic arsenic by using hydride generation-atomic absorption spectrometry, and run a comparative study of effect in the analysis of them. Also, we separated and analyzed only inorganic arsenic by using $H_2SO_4$-trap to eliminate organic arsenic which are MMA(monomethylarsonate) and DMA(dimethylarsinate). Under the conditions of mixture acid of 1.8 M HCl and 0.08 M $HNO_3$, arsenic standard solution of 20 ppb have more higher absorbance than without adding acid. In case of L-Cysteine, As(V) completely reduces into As(III) when 0.5 g of L-Cysteine is reacted more than 30 mins. in weak acid condition of approximately 0.07 M $HNO_3$ or HCl. In the event of KI, As(V) completely reduces into As(III) when 3 g of KI is reacted more than 1hour in acid condition of 0.8 M $HNO_3$. On the occasion of $FeSO_4$, the inside of tube is blocked by precipitation by mixture reaction of $NaBH_4$ and $Fe^{2+}$, therefore, comparing to other pre-reductants, reproducibility of efficiency of reducing As(V) to As(III) is low. To evaluate the accuracy of the analytical results, we use NIST SRM 1643C Trace Elements in Water ($82.1{\pm}1.2ng/mL$). The results are satisfactory.

• Journal of Environmental Health Sciences
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• v.41 no.5
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• pp.289-298
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• 2015

Objectives: The method of analyzing urinary arsenic by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS) is generally used because it shows relatively greater sensitivity, low detection limits, low blocking action, and is simple to operate. In this study, the results of analysis according to three pre-reductants commonly used in the FI-HG-AAS method were compared with each other. Methods: To analyze urinary arsenic, nineteen urine samples were collected from adults aged 43-79 years old without occupational arsenic exposure. Analysis equipment was FI-HG-AAS (AAnalyst 800/FIAS 400, Perkin- Elmer Inc., USA). The three pre-reductants were potassium iodide (KI/AA), C3H7NO2S (L-cysteine), and a mixture of KI/AA and L-cysteine (KI/AA&L-cysteine). Results: In the results of the analysis, the recovery rate of the method using KI/AA was 82.3%, 95.7% for Lcysteine, and 123.5% for KI/AA and L-cysteine combined. When compared with the results by use of high performance liquid chromatography inductively-coupled plasma mass spectrometry (HPLC-ICP-MS), the method using L-cysteine was the closest to those using HPLC-ICP-MS ($98.57{\mu}g/L$ for HPLC-ICP-MS; $74.96{\mu}g/L$ for L-cysteine; $69.23{\mu}g/L$ for KI/AA and L-cysteine; $13.06{\mu}g/L$ for KI/AA) and were significantly correlated (R2=0.882). In addition, they showed the lowest coefficient of variation in the results between two laboratories that applied the same method. Conclusion: The efficiency of hydride generation is considered highly important to the analysis of urinary arsenic via FI-HG-AAS. This study suggests that using L-cysteine as a pre-reductant may be suitable and the most rational among the FI-Hg-AAS methods using pre-reductants.

• Analytical Science and Technology
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• v.21 no.4
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• pp.316-325
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• 2008

An inductively coupled plasma mass spectrometry (ICP-MS) instrument equipped with flow injection-hydride generation system was used for the determination of trace arsenic in seawater sample. The accuracy in this method was verified by the analysis of certified reference materials (CRM) of seawater (CASS-4, NASS-5). The analytical results agreed with certified value within the range of uncertainty. The expanded uncertainties for CASS-4 and NASS-5 in this experiment were ranged from 6.2% to 6.8% obtained from repeated analyses of the CRMs (n=5). The detection limit of $As^+$ (m/z=74.9216) in this method was confirmed about 0.01 ug/kg. Linearity obtained from calibration curve of arsenic was excellent ($R^2=1$). The detection at $As^+$ (m/z=74.9216) and $AsO^+$ (m/z=90.9165) by using oxygen reaction gas in DRC mode was compared. Sensitivity at $AsO^+$ (m/z=90.9165) was decreased about 25-fold, but the analytical results are the same that at $As^+$ (m/z=74.9216).

• Korean Journal of Metals and Materials
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• v.50 no.2
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• pp.183-190
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• 2012

Hydrogen was generated by the reaction of metal hydride with water. The variation of hydrogen generation with the kind of powders (milled $MgH_2$, and $MgH_2$ milled with various contents of MgO, $MgCl_2$ or $Ni+Nb_2O_5$) was investigated. $MgH_2$ powder with a hydrogen content of 6.05 wt% from Aldrich Company was used. Hydrogen is generated by the reaction of Mg as well as $MgH_2$ with water, resulting in the formation of byproduct $Mg(OH)_2$. For about 5 min of reaction time, milled $95%MgH_2+5%MgO$ has the highest hydrogen generation rate among milled $MgH_2+x%MgO$ (x=0, 5, 10, 15 and 20) samples. Milled $90%MgH_2+10%MgCl_2$ has the highest hydrogen generation rate among all the samples.

• Journal of the Korean Society for Aeronautical & Space Sciences
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• v.41 no.3
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• pp.226-232
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• 2013

A compact hydrogen generation device of fuel cell system using chemical hydride storage technique was designed to fit the propulsion device requirement of a small unmanned aerial vehicle(SUAV). For high efficient, compact, and lightweight hydrogen generation control device, the Co-B catalyst hydrogen conversion rate by $NaBH_4$ aqueous solution flux is measured so that the proper amount of Co-B catalyst for maximum hydrogen generation of 100W stack was proposed. A compact hydrogen generation device is controlled by pump's on/off using its own internal pressure and consumes fuel in high efficiency through a dead-end type fuel cell. The fuel cell system has stable operation for a planed flight profile. The system operates up to maximum 7 hours and at least 4 hours for tough flight profiles.

• Applied Chemistry for Engineering
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• v.8 no.4
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• pp.667-672
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• 1997

Thermal behavior of high capacity Nickel/Metal hybride battery in analyzed using the NISA software which is based on the three dimensional finite element method. Differential energy balance equation is used for the conduction heat transfer of the battery, while convective heat transfer equation is used for the interface between the battery and air. Heat generation rate and convective heat transfer coefficient are tested as variables to investigate thermal behavior, and the generalized equation for maximum temperature inside the battery is developed. The abrupt rise of the battery temperature due to the quick charge or discharge can be prevented from the use of metallic cooling fin. In addition, temperature augmentation of the battery is negligible when the low thermal conductive and thin insulating material is used outside of the battery case.

• 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.

• Journal of the Korean Chemical Society
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• v.54 no.4
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• pp.447-450
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• 2010

In this study, the improved large-scale synthetic route for epinastine hydrochloride, the second-generation antihistamine, was developed. The original synthetic route involves the synthesis of an aminomethyl derivative, the main intermediate, and in this process hazardous materials such as very toxic phosgene and sodium cyanide along with the explosive and expensive aluminum chloride and lithium aluminum hydride were used. In order to improve the synthetic route, we developed industrially very useful process to prepare the aminomethyl intermediate by the synthesis of the phthalimidomethyl derivative first and easy removal of the phthalyl group using hydrochloric acid or methyl hydrazine, and hazardous materials and expensive reagents were excluded in this process.

• 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.

• Analytical Science and Technology
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• v.12 no.6
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• pp.484-489
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• 1999

The extraction of trace amounts of Se in volcanic rock was investigated using the hydride generation method and atomic absorption spectrophotometry. The powdered rock, 1.0 g, was decomposed with the mixture of $HClO_4$, $HNO_3$ and HF in an acid digestion bomb at $140^{\circ}C$ for 2 hours. For the reduction of Se(VI) to Se(IV) in the solution, 10 mL of 6 M HCl and 0.2 mL of 1 M KBr were added to the solution and the mixture was heated for 30~45 minutes. $H_2Se$ was produced by adding 3% $NaBH_4$ as a strong reducing agent, extracted by nitrogen gas, and was absorbed twice into $KMnO_4$solution. The contents of Se in the solution were determined by generation/AAS. According to the proposed method, 1.0 ng or more of Se was quantitatively extracted and Se levels of 2.5 ng/g or more in rock samples could be determined. For example, Se in a rhyolite was determined with the precision of $19.5{\pm}1.3ng/g$(95% confidence, n=6).