• Ceramist
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• v.5 no.2
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• pp.30-36
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• 2002

• Analytical Science and Technology
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• v.5 no.3
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• pp.277-283
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• 1992

Acid effects on the ICP-AES signals are studied as the concentrations of nitric acid, hydrochloric acid, sulfuric acid, and 1:1 mixture of nitric acid and hydrochloric acid are changed. Almost all analyte signals are depressed. The extent of the depression due to the pressence of the acids became to be pecular when the acid concentration was over 1%. Among the acids used, the suppression due to sulfuric acid is most severe and unexpectable. The ratios of the analyte signal to Ar signal and the Mg II signal to Mg I signal are measured as the concentration of the acids changed. In this study, it is proved that the main reason of the signal reduction is the change in the nebulization efficiency, for example, droplet size distribution, viscosity and surface tension variation, not the alteration of plasma excitation characteristics. There was no relationship found between ionization potential and analyte signal reduction in ICP-MS.

• The Journal of the Petrological Society of Korea
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• v.20 no.3
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• pp.161-172
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• 2011

Open beaker digestion method is routinely used as the sample preparation technique for trace element determination of rock samples by inductively coupled plasma mass spectrometry, With this method, however, dissolution of Zr and Hf is not always guaranteed especially when the samples contain refractory minerals. In this study, glass bead digestion technique was compared with conventional open beaker digestion technique for the sample preparation of three USGS rock standards such as AGV-2, BHVO-2, and G-3. Thirty trace elements including rare earth elements were analysed by ICP-MS and ICP-AES. There were no clear differences in analytical results for the AGV-2 and BHVO-2 standards between the two techniques, but Zr, Hf, Y, and middle- to heavy- rare earth element concentrations of the G-3 standard prepared by open beaker digestion technique were significantly lower than the recommended values. This can be attributed to the presence of refractory mineral zircon. On the contrary, all the analytical results of the G-3 standard prepared by glass bead digestion technique were in good agreement with the recommended values, indicating complete dissolution of zircon. The analytical results show that the volatile elements such as Pb and Zn were not lost during the preparation of glass bead. Low dilution glass bead digestion technique described here will be very helpful to enhance precision and accuracy of trace element analysis for geological samples containing refractory minerals.

• Journal of Radiation Protection and Research
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• v.35 no.3
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• pp.117-123
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• 2010

Plutonium is by far the most important of the transuranic elements which have been released into the environment due to radio-toxicity and long term radiation effects on humans. And Pu isotope ratio ($^{240}Pu/^{239}Pu$) is of great interest because this ratio is used as a fingerprint for different sources. Mass spectrometry has been used as an useful atom counting technique with several advantages over decay counting techniques for the determination of Pu isotopes. It enables a determination of Pu isotope ratio in the environmental samples with a low detection limit and a short determination time. An ICP-MS is the representative mass spectrometry for Pu determination. In this study, the precision of $^{240}Pu/^{239}Pu$ isotope ratio was improved by using 4 multiple ion counters of MC-ICP-MS. The detection limit of $^{239}Pu$ and $^{240}Pu$ were $0.10\;fg\;ml^{-1}$ ($0.24\;{\mu}Bq\;ml^{-1}$), $0.12\;fg\;ml^{-1}$ ($0.97\;{\mu}Bq\;ml^{-1}$), respectively. The relative standard deviation of $^{240}Pu/^{239}Pu$ isotope ratio was less than 1 % in trace level. The various reference materials (seawater, soil and sediment) were analyzed to verify this method and their analytical results were in good agreement with the certified (or recommended value) value.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.3 no.1
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• pp.99-99
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• 1993

혈액 및 생체시료 중 필수원소 혹은 독극성 원소의 극미량상분 정밀측정과 동위원소비율측정에 널리 사용되는 유도결합플라즈마 질량분석기(ICP-MS)의 기본원리를 소개하고 ICP-SM를 이용한 혈액중 낮은 ppb수준의 Cd, Hg 그리고 Pb의 정밀분석법을 소개한다. 혈액은 많은 양의 유기물을 포함하고 있으므로 digestion bomb에 질산과 과산화수소를 넣어 microwave oven에서 고온고압 상태로 분해시켜 많은 용액을 얻어 이 용액을 플라즈마에 주입시켜 분석한다. 그리고 수온은 tin(II) chloride 용액을 환원제로하여 생성시킨 수은원소증기를 membrane liquid-gas separator를 이용하여 뽑아내어 플라즈마에 주입시켜 낮은 ppt 수준의 검출한계를 얻는다. 또한 높은 정밀도와 정확도와 극미량 원소 측정에 사용되는 동위원소 회석법율 소개하고 실제 혈액분석에의 응용방법을 제시한다.

• 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 ${\mu}g/kg$.

• Analytical Science and Technology
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• v.25 no.3
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• pp.190-196
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• 2012

The human exposure of lead has usually detected the amount of lead in the whole blood, however, this method has a shortcoming to give the information on the short-term exposure to lead. In that sense, it is desirable to estimates the level of lead in plasma to draw the chronic bio-marker of lead exposure even though it is difficult to measure lead of several ng/L. An inductively coupled plasma-mass spectrometry (ICP-MS) method was developed for determining lead in plasma as the chronic bio-marker of lead of workers. To minimize the contamination of lead from the environment, we constructed class 1,000 clean room and compared the amount of floating dust before and after the operation of the clean room. The limit of detection (LOD) and the limit of quantification (LOQ) of lead in fetal bovine serum were 4.3 ng/L and 12.2 ng/L by NIOSH method (statistical calculation method) and 7.0 ng/L and 22.1 ng/L by signal/noise ratio, respectively. The accuracy was in a range of 92.3-101.3%, and the precision of the assay was less than 4% in the samples spiked in the concentration of 20 ng/L and 2,000 ng/L. The method was simple, reproducible and sensitive enough to permit reliable analysis of lead to the ng/L level in plasma and/or serum. The method was also useful for the biological monitoring of chronic exposure to lead.

• Analytical Science and Technology
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• v.16 no.2
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• pp.152-158
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• 2003

This study was conducted to evaluate two sample digestion procedures and instrumental determination parameters for analysis of lead in bone. Amputated human legs were treated by acid digestion or microwave dissolution prior to spectrometric analysis. Inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GF-AAS) were used for determining bone lead levels. Recovery efficiencies using standard reference material from acid digestion measured by ICP-MS were in good agreement with those of the certified value, but in cases of acid digestion by GF-AAS and microwave digestion by both two methods, recovery underestimated and overestimated, respectively. For the bone samples, the lead concentrations obtained by ICP-MS after acid digestionwere in good agreement with those by GF-AAS (correlation coefficient = 0.983), but GF-AAS gave systematically higher values than ICP-MS. While a good agreement between two analytical methods after microwave digestion was also obtained (correlation coefficient = 0.950), bone lead concentrations from microwave were relatively higher than those from acid digestion. In conclusion, the use of the simple nitric acid digestion procedure at an ambient temperature coupled to ICP-MS seems to be efficient for the determination of lead in bone in consideration for both the convenience and validity.

• The Journal of the Petrological Society of Korea
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• v.24 no.2
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• pp.141-147
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• 2015

Using laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), we evaluated the reliability of trace element abundance data measured from the silicate rock references of JR-3, JG-3, JGb-1 and JB-1b using glass discs made by alkali fusion. For 28 elements including rare earth elements, relative standard deviations (RSD) are better than 7% in case when the concentrations of the elements in the rock samples are greater than 10 ppm. However, RSD shows somewhat increased values for the concentrations less than 10 ppm, but never exceeds 25%. Compared with previously reported averages of the compiled abundance data, our data display satisfactory results for the most cases with differences less than 10%. We suggest that LA-ICP-MS analysis using fused glass beads is a reliable, precise and time-saving method of trace element analysis for the silicate rocks spanning from mafic to felsic compositions.

• Analytical Science and Technology
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• v.7 no.1
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• pp.1-10
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• 1994

A survey was made on detection limit, reproducibility, matrix effect, linear dynamic range and the memory effect of yttrium and europium in order to analyze rare earth elements which exist as impurities in the rare earth oxide which is raw materials of fluorescent substance. When analysing a certain amount of thulium quantitatively using inductively coupled plasma mass spectrometry, it was found that the analysis was interfered with $EuO^+$ which is one of polyatomic ions caused by plasma. As the intensity of thulium linearly proportional to the europium concentration, it was possible to the determine the actual concentration of thulium.