• Analytical Science and Technology
• /
• v.25 no.6
• /
• pp.339-344
• /
• 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.

• 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 $0.03{\mu}g/L$.

• 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.

• Journal of the Korean Chemical Society
• /
• v.38 no.12
• /
• pp.891-897
• /
• 1994

A method has been investigated for the determination of Selenium in Ginseng radix, Ganoderma Lucidum and Garlic using hydride generation atomic absorption spectrometry (HG-AAS). The effects of several acids and sodium tetrahydroborate concentration and their flow rate on the determination of Selenium for the hydride generation 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 were studied. In the optimum conditions, we obtained calibration curve in the range 0-40 ppb. The analytical data of Garlic, Ganoderma Lucidum and Ginseng radix are 289, 296, 198 ppb, respectively.

• Analytical Science and Technology
• /
• v.16 no.5
• /
• pp.399-406
• /
• 2003

This study was conducted to find out the analysis condition of selenium(Se) in oil refinery wastewater with a high concentration of Se using the atomic absorption spectrometry with hydride generation system (HG-AAS). From various experiments that reduced Se(VI) to Se(IV), the optimum pretreatment condition was determined to be a sample volume of 10 mL, HCl 10 mL, with a 30 min heating time in a water bath. In oil refinery wastewater, as the concentration of organics and constitution became higher, the recovery rates of Se decreased. Therefore, three acid digestion methods ($HNO_3/HClO_4$ digestion, $KMnO_4$ digestion, and microwave acid digestion) were tested on the recovery rates of Se in reference to the digestion of organics, petroleum and oxidation from organic Se(org.), Se(IV) to Se(VI). The experiment results showed that the average recovery rate of Se was the highest in microwave acid digestion, although all of the digestions were more than 90%. In consequence, the pretreatment procedure of microwave digestion followed by HCl addition was the most suitable for selenium analysis in oil refinery wastewater by using HG-AAS.

• 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.

• Analytical Science and Technology
• /
• v.13 no.2
• /
• pp.189-193
• /
• 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.

• Journal of Environmental Health Sciences
• /
• v.41 no.5
• /
• pp.289-298
• /
• 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
• /
• v.15 no.5
• /
• pp.439-444
• /
• 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
• /
• v.48 no.6
• /
• pp.583-589
• /
• 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.