• The Journal of the Petrological Society of Korea
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• v.25 no.2
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• pp.107-119
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• 2016

Trace element abundances in the igneous rocks are important data for petrogenetic interpretation. Their concentrations are generally measured using ICP-MS from the dissolved solution. The acid digestion of rock powder can be performed by conventional teflon vial or pressure bomb. In this paper, we investigated a problem that happened during acid digestion experiment using conventional teflon vial or pressure bomb of BCR2 and GSP2 USGS rock standard materials. The results show that the measured concentrations of the elements like Cr, Ni, Zn, Ta, W in the BCR2 are different from the recommended values of USGS whereas those of the elements like Rb, Sr, Zr, Hf, Ta, W in the GSP2 are different from those values. Our experiment shows that defect of specific elements like Cr, Ni may happen during the sample digestion. Our results also indicate that the Cr, Ni, W, Zr, Hf, Ta concentration obtained based on an acid digestion of geological samples need to be careful in their geochemical interpretation.

• Analytical Science and Technology
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• v.15 no.1
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• pp.15-19
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• 2002

The pretreatment of tungsten added $BaTiO_x$ ceramics was performed to improve the recovery of Ba, Ti and W. $BaTiO_x$ ceramics were digested with HF : HCl ( 1 : 2 ) mixture in an acid digestion bomb at $220^{\circ}C$ for 3 hrs. The concentration of Ba, Ti and W were determined by ICP-AES. Recoveries of Ba, Ti and W were 99.6%, 99.8% and 99.2%, respectively. And their C.V. values were 1.02%, 0.73% and 1.79%. Using this method, the analytical results of Ba, Ti and W for a real sample were obainted to be 25.9% (w/w), 38.8% (w/w) and 3.31% (w/w), respectively.

• Analytical Science and Technology
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• v.13 no.6
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• pp.731-735
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• 2000

The acid digestion bomb pretreatment method for the determination of antimony in a commercial fire retardant material sample (DBDPE-$Sb_2O_3$) was studied. DBDPE-$Sb_2O_3$ sample was digested with $H_2SO_4:HCl$(1:2) mixture in digestion bomb at $220^{\circ}C$ for 2 hrs. and antimony was determined by atomic absorption spectrophotometry. Recovery of 99.6-99.8% and C.V. of 0.94-1.07% for Sb was obtained for spiked real samples. In the present method, the analytical results obtained for antimony were 40.3 and 36.3% (w/w), respectively.

• Analytical Science and Technology
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• v.15 no.4
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• pp.335-340
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• 2002

An analytical method has been developed to determine multi-elements in human hair samples by inductively coupled plasma mass spectrometry (ICP-MS). 0.05 g of hair sample was added to the Teflon digestion bomb together with 1.5 mL of nitric acid and an appropriate amount of In as an internal standard. The sample was then decomposed in the microwave digestion system. The hair certified reference material, GBW 09101, was analyzed for the validation of the analytical method. The determined values were in good agreement with the certified values within the uncertainty range.

• Analytical Science and Technology
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• v.10 no.1
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• pp.35-42
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• 1997

The sample pretreatment technique using a high pressure acid digestion bomb for the analysis of ceramic capacitor materials, such as barium titanate and PZT, was studied. When the concentrations of hydrochloric acid were varied with the addition of nitric acid or distilled water, quantitative measurements for those samples were carried out using inductively coupled plasma atomic emission spectrometry. From this experiment the results indicate that most of elements, such as Ba, Mn, Zn, Si, etc., aren't affected by the concentration of hydrochloric acid but Nb and Zr are very susceptable to it. It however turns out that the digestion time relatively gave little effects on the analytical result. In case of Nb the ratio of hydrochloric acid to water should be greater than 3:1(v / v) for the best analytical result. For the Pb determination use of diluted hydrochloric acid compared to the mixture of nitric acid and hydrochloric acid showed a better analytical result.

• The Journal of the Petrological Society of Korea
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• v.23 no.4
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• pp.337-349
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• 2014

We measured rare earth element and Zr concentrations of USGS granite standard material GSP-2 and GSJ granite standard material JG-1a to clarify the effect of zircon during rare earth element analysis using ICP-MS. We also measured rare-earth element and zirconium (Zr) contents of zircon from granite by acid-digestion methods using conventional teflon vial and pressure-bomb. The results show that acid-digestion using teflon vial dissolved ca. 50% of zircon compared to pressure-bomb method. The Zr contents of JG-1a and GSP-2 gave ca 50% of reference value. However, rare-earth element abundance of JG-1a and GSP-2 were similar to those of reference values. This suggests that the decomposition degree of zircon might give a negligible effect on a petrological and geochemical interpretation using chondritenormalized REE pattern.

• Analytical Science and Technology
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• v.20 no.6
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• pp.524-528
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• 2007

Variations of the twenty one metal components (Mg, Al, V, Cr, Co, Sr, Ba, Na, K Mn, Fe, Cu, Zn, As, Hg, Pb, Ca, P, Mo, Cd, Sb) were analyzed in human hair sample by inductively coupled plasma mass spectrometry (ICP-MS). The effect of bleach and permanent wave manipulation on the elemental composition of hair were investigated. It was found that the composition of hair varied with hair bleach and permanent wave. Hair sample was collected from male in the age of thirties. Hair sample (0.05 g) was added to the Teflon digestion bomb together with 1.5 mL of nitric acid and an appropriate amount of In as an internal standard. The sample was then decomposed in the microwave digestion system. In normal hair, the contents of V, Cr, Mn, Fe, Co, Cu, Zn, As, Mo, Cd, Sb and P were increased in permanent wave hair, and Mg, Al, V, Co, Sr, Ba, Na and K were increased in bleached hair. But Mg, Al, Sr, Ba, Hg, Pb, Na, K, and Ca contents were decreased with permanent wave hair, Mn, Fe, Cu, Zn, As, Hg, Pb and Ca contents were decreased with bleached hair.

• Analytical Science and Technology
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• v.9 no.2
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• pp.145-160
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• 1996

Inorganic analytical laboratory of Korea Research Institute of Standards and Science participated in an interlaboratory comparison program operated by Quebec Toxicology Centre of Canada in 1994 and again in 1995. The objective of this program is to enable participating laboratories to assess reproducibility and accuracy of their analytical results for trace toxic elements in human biological fluids. This laboratory determined Cd and Pb concentrations in 3 levels of human blood samples by isotope dilution inductively coupled plasma mass spectrometry. 0.5mL of blood sample is added to the digestion bomb together with 2mL of nitric acid and enriched spike isotopes and then decomposed in the microwave digestion system. The decomposed sample is diluted to 10mL and nebulized into ICP-MS. The Cd and Pb values reported by all participating laboratories are presented and compared. The values reported by this laboratory are within the acceptable range of target values.

• Journal of the Korean Chemical Society
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• v.37 no.9
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• pp.800-805
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• 1993

An analytical method has been developed to determine trace elements in biological samples. The biological samples are added to a laboratory-bulit Teflon bomb together with nitric acid-hydrogen peroxide mixture and enriched stable isotopes. The samples are decomposed in a microwave oven. The decomposed sample solutions are analyzed by isotope dilution inductively coupled plasma mass spectrometry. The analytical results of the biological samples agree well with the reference values.

• Journal of the Korean Chemical Society
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• v.44 no.6
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• pp.526-532
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• 2000

Cation exchange separation and inductively coupled plasma atomic emission spectrometric(ICP-AES) determination of ruthenium in HCl solutions were studied to quantitatively determine ruthenium in spent nuclear fuels. Ruthenium-bearing samples were dissolved with the mixed acid solution(9 : 1 mole ratio, HCl-HNO$_3$) using an acid digestion bomb. Based on the absorption spectra and ion exchange behaviour of ruthenium in hydrochloric acid media, its possible chemical species were discussed. On a cation exchange column (0.7 ${\times}$ 8.0 cm) packed with AG 50W ${\times}$ 8(100~200 mesh) and equilibrated with 0.5 M HCl, ruthenium was eluated with 0.5 M HCl while uranium was retained on the column. The established separation method was applied to a simulated spent nuclear fuel and resulted in the recovery of 98.5% with a relative standard deviation of 0.7%.