• Journal of Environmental Health Sciences
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• v.44 no.5
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• pp.491-501
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• 2018

Objectives: The aims of this study were to compare concentrations and the correspondence of human blood cadmium by using graphite furnace atomic absorption spectrometry (GF-AAS) and inductively coupled plasma-mass spectrometry (ICP-MS), which are representative methods of heavy metal analysis. Methods: We randomly selected 79 people who agreed to participate in the research project. After confirming the linearity of the calibration curves for GF-AAS and ICP-MS, the concentrations of cadmium in a quality control standard material and blood samples were measured, and the correlation and the degree of agreement were compared. Results: The detection limit of ICP-MS (IDL: $0.000{\mu}g/L$, MDL: $0.06{\mu}g/L$) was lower than that of GF-AAS (IDL: $0.085{\mu}g/L$, MDL: $0.327{\mu}g/L$). The coefficient of variation of the quality control standard material showed stable values for both ICP-MS (clinchek-1: 5.35%, clinchek-2: 6.22%) and GF-AAS (clinchek-1: 7.92%, clinchek-2: 5.22%). Recovery was relatively high for both ICP-MS (clinchek-1: 95.1%, clinchek-2: 92.8%) and GF-AAS (clinchek-1: 91.4%, clinchek-2: 98.8%), with more than 90%. The geometric mean, median, and percentile of blood samples were all similar. The agreement of the two instruments compared with the bias of the analytical values found that about 81% of the analytical values were within ${\pm}30%$ of the deviation from the ideal reference line (y=0). As a result of the agreement limit, the value included in the confidence interval was about 94%, which shows high agreement. Conclusion: In this study, we confirmed there was no significant difference in concentrations of a quality control standard material and blood samples. Since ICP-MS showed lower concentrations than GF-AAS at concentrations below the method detection limit of GF-AAS, it is expected that more precise results will be obtained by analyzing blood cadmium with ICP-MS.

• Analytical Science and Technology
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• v.27 no.3
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• pp.140-146
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• 2014

An internal standard was used in PCID (post column isotope dilution) to improve the accuracy and precision in quantification of various chemical species. The error occurring in the column was the largest in HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry) when PCID and other traditional quantification methods were compared with each other. Internal standard was effective in correcting the loss of sample in the column to improve accuracy and precision. When applied to SeMet, using MeSecys or $Se^{4+}$ as an internal standard, relative errors were reduced from 31% and 13% to less than 1%, while standard deviations were reduced from 5.1% and 6.9% to 1.5% and 0.2%, respectively. Positive aspects of using an internal standard in PCID were compared with other quantitative techniques and discussed in detail.

• Bulletin of the Korean Chemical Society
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• v.26 no.3
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• pp.440-446
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• 2005

A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

• Mass Spectrometry Letters
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• v.4 no.4
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• pp.87-90
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• 2013

Isotope amount ratios of lead in a bronze sample have been successfully determined using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS). Matrix separation conditions were tested and optimized using ion exchange chromatography with anion-exchange resin, AG1-X8, and sequential elution of the 0.5 M HBr and 7 M $HNO_3$ to separate lead from very high contents of copper and tin in bronze matrix. Mercury was also removed efficiently in the optimized separation condition. The instrumental isotope fractionation of lead in the MC-ICP-MS measurement was corrected by the external standard sample bracketing method using an external standard, NIST SRM 981 lead common isotope ratio standard followed by correction of procedure blank to obtain reliable isotope ratios of lead. The isotope ratios, $^{206}Pb/^{204}Pb$, $^{207}Pb/^{204}Pb$, $^{208}Pb/^{204}Pb$, and $^{208}Pb/^{206}Pb$, of lead were determined as $18.0802{\pm}0.0114$, $15.5799{\pm}0.0099$, $38.0853{\pm}0.0241$, and $2.1065{\pm}0.0004$, respectively, and the determined isotope ratios showed good agreement with the reference values of an international comparison for the same sample within the stated uncertainties

• Bulletin of the Korean Chemical Society
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• v.25 no.2
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• pp.233-236
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• 2004

Total impurity analysis of a primary standard solution is one of the essential procedures to determine an accurate concentration of the standard solution by the gravimetry. Bi impurity is determined in Pb standard solutions by inductively coupled plasma mass spectrometry (ICP-MS). The direct nebulization of the Pb standard solution produces a significant amount of the Pb matrix-induced molecular ions which give rise to a serious spectral interference to the Bi determination. In order to avoid the spectral interference from the interferent $^{208}PbH^+$, the hydride generation method is employed for the matrix separation. The Bi hydride vapor is generated by reaction of the sample solution with 1% sodium borohydride solution. The vapor is then directed by argon carrier gas into the ICP after separation from the mixture solution in a liquid-gas separator made of a polytetrafluoroethylene membrane tube. The presence of 1000 ${\mu}$g/mL Pb matrix caused reduction of the bismuthine generation efficiency by about 40%. The standard addition method is used to overcome the chemical interference from the Pb matrix. Optimum conditions are investigated for the hydride-generation ICPMS. The detection limit of this method is 0.5 pg/mL for the sample solutions containing 1000 ${\mu}$g/mL Pb matrix.

• 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.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.18 no.4
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• pp.549-562
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• 2020

Deionized water, methanol, and ethanol were investigated for their effectiveness at dissolving LiCl-KCl-UCl3 at 25, 35, and 50℃ using inductively coupled plasma mass spectrometry (ICP-MS) to study the concentration evolution of uranium and mass ratio evolutions of lithium and potassium in these solvents. A visualization experiment of the dissolution of the ternary salt in solvents was performed at 25℃ for 2 min to gain further understanding of the reactions. Aforementioned solvents were evaluated for their performance on removing the adhered ternary salt from uranium dendrites that were electrochemically separated in a molten LiCl-KCl-UCl3 electrolyte (500℃) using scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). Findings indicate that deionized water is best suited for dissolving the ternary salt and removing adhered salt from electrodeposits. The maximum uranium concentrations detected in deionized water, methanol, and ethanol for the different temperature conditions were 8.33, 5.67, 2.79 μg·L-1 for 25℃, 10.62, 5.73, 2.50 μg·L-1 for 35℃, and 11.55, 6.75, and 4.73 μg·L-1 for 50℃. ICP-MS analysis indicates that ethanol did not take up any KCl during dissolutions investigated. SEM-EDS analysis of ethanol washed uranium dendrites confirmed that KCl was still adhered to the surface. Saturation criteria is also proposed and utilized to approximate the state of saturation of the solvents used in the dissolution trials.

• Proceedings of the Korean Vacuum Society Conference
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• 2015.08a
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• pp.156.2-156.2
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• 2015

반도체 소자의 크기가 나노사이즈로 줄어들기 때문에, 건식식각의 중요성이 강조되고 있다. dual plasma source를 사용함으로써 plasma 밀도, 이온충돌에너지, 이온플럭스를 조절 가능하다. Low frequency로 이온에너지를 조절하고, high frequency로 이온플럭스를 일반적으로 조절한다. 본 연구는 inductively coupled plasma (ICP)와 capacitively coupled plasma (CCP)를 사용하는 dual plasma source이다. ICP는 AE RPS로 2.4 MHz를 사용하고, CCP는 AE RFX-600으로 13.56 MHz이다. single L-probe는 Hiden ESPion이고, quadrupole mass spectrometer (QMS)는 INFICON CPM-300이다. chuck에 CCP가 인가되고, ICP는 SUS mesh를 거쳐서 영향을 미친다. Gas는 Ar, Ar+CF4 두 조건에서 비료를 하였다. Single L-probe를 이용하여 플라즈마를 측정한 결과 CCP만 인가하였을 때, Te 2.05 eV, Ne 4.07E+10 #/cm3, Ni 5.82E+10 #/cm3의 결과를 얻을 수 있었다. ICP를 방전하고 mesh를 통해서 chuck으로 입사하는 이온을 측정한 결과 mesh에 의해 이온이 중성화되어 거의 입사하지 않음을 확인할 수 있었다. 최종적으로 이온의 영향이 상쇄되고, 라디칼의 영향이 증가하여 높은 etch rate와 선택비를 가지며, 등방성 식각의 영향이 커질 것으로 사료된다.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2003.05a
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• pp.54-54
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• 2003

MgO layer는 POP 패빌 내 유전증을 이온의 스퍼터링으로부터 보호하여 주며, 또한 높은 이차 전자 밤출 계수의 특성을 가지고 있어 구동 및 유지 전압을 낮춰 주는 역할을 한다. 그러나. MgO layer는 $H_20,{\;}CO_2,{\;}N_2,{\;}0_2$ 그리고 $H_2$와 같은 불순물 들을 쉽게 를착하는 단점이 있어, PDP의 특성 및 수명 단축에 영향을 줄 수 있다. 따라서, 본 연구에서는 atmospheric pressure plasma cleaning 과 low pressure i inductively coupled plasma (ICP) cleaning 처리에 의하여, 보호층으로 사용이 되는 MgO layer의 outgassing 특성을 조사하고자 한다. plasma cleaning에 의한 MgO layer 표면의 roughness와 불순물의 변화를 알아보기 위 하여 atomic force microscopy(AFM)과 x-ray p photoelectron spectroscopy(XPS)를 이용하여 측정 하였다. 또한, outgassing의 특성을 분석하기 위하여 MgO layer를 $400^{\circ}C$ 까지 온도를 가하여 온도에 따른 outgassing의 특성을 quadrupole mass spectrometer(QMS)를 이용하여 알아보았다. atmospheric pressure plasma cleaning 에서는 $He/O_2/Ar/N_2$의 gas를 사용하였으며, low pressure ICP cleaning 에 서는 Ar의 gas를 사용하였다. atmospheric pressure plasma cleaning는 low pressure ICP C cleaning과 비교해 더 낮은 outgassing을 관잘 할 수 있었으나. MgO 표면의 roughness는 low pressure ICP cleaning 후 더 낮은 것을 알 수 있었다. 또한 $He/O_2/Ar/N_2$의 gas를 사용 한 atmospheric pressure plasma cleaning 과 $Ar/O_2$의 gas를 사용한 ICP cleaning에서 이 차전자방출계수(SEEC)가 약 1.5~2.5배 증가된 것을 알 수 있었다.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.21 no.1
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• pp.43-53
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• 2023

Sulfide concentrations critically affect worker safety and the integrities of underground facilities, such as deep geological repositories for spent nuclear fuel. Sulfide is highly sensitive to oxygen, which can oxidize sulfide to sulfate. This can hinder precise measurement of the sulfide concentration. Hence, a literature review was conducted, which revealed that two methods are commonly used: the methylene blue and sulfide ion-selective electrode (ISE) methods. Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used for comparison with the two methods. The sulfide ISE method was found to be superior as it yielded results with a higher degree of accuracy and involved fewer procedures for quantification of the sulfide concentration in solution. ICP-OES results can be distorted significantly when sulfide is present in solution owing to the formation of H₂S gas in the ICP-OES nebulizer. Therefore, the ICP-OES must be used with caution when quantifying underground water to prevent any distortion in the measured results. The results also suggest important measures to avoid problems when using ICP-OES for site selection. Furthermore, the sulfide ISE method is useful in determining sulfide concentrations in the field to predict the lifetime of disposal canisters of spent nuclear fuel in deep geological repositories and other industries.