• Proceedings of the Korean Radioactive Waste Society Conference
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• 2018.11a
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• pp.608-609
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• 2018

• Analytical Science and Technology
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• v.37 no.2
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• pp.123-129
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• 2024

We present a rapid method for the determination of Cs, Sr, and Ba, heat generators found in highly active liquid wastes, by gas-pressurized extraction chromatography (GPEC) using a column containing a cation-exchange resin. GPEC is a microscale column chromatographic technique that uses a constant flow rate of solvent (0.07 mL/min) with pressurized nitrogen gas supplied through a valve. In particular, because this method uses a small sample volume (a few hundred microliters), it produces less chemical waste and allows for faster separation compared to traditional column chromatography. In this study, we evaluated the separation of Cs, Sr, and Ba using GPEC. The eluate from the column (GPEC or conventional column chromatography) was quantitatively analyzed using inductively coupled plasma-mass spectrometry to measure the column recovery and precision. The column reproducibility of the proposed GPEC system (RSDs of recoveries) ranged from 2.7 to 4.1 %, and the column recoveries for the three elements ranged from 72 to 98% when aqueous HCl was used as the eluent. The GPEC results are slightly different in efficiency and separation resolution compared to those of conventional column chromatography because of the differences in the eluent flow rate as well as the internal diameter and length of the column. However, the two methods had similar recoveries for Cs and Sr, and the precision of GPEC was improved by two-fold. Remarkably, the solvent volume required for GPEC analysis was five times lower than that of the conventional method, and the total analysis time was 11 times shorter.

• Bulletin of the Korean Chemical Society
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• v.34 no.6
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• pp.1689-1692
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• 2013

Food is a common source of chromium (Cr) exposure. However, it is difficult to analyze Cr in complex food matrices by using inductively coupled plasma mass spectrometry (ICP-MS) because the major isotope, $^{52}Cr$, is masked by interference generated by the sample matrix and the plasma gas. Among the systems available to minimize interference, the recently developed collision-reaction interface (CRI) has a different structure relative to that of other systems (e.g., collision cell technology, octopole reaction system, and dynamic reaction cell) that were designed as a chamber between the skimmer cone and quadrupole. The CRI system introduces collision or reaction gas directly into the plasma region through a modified hole of skimmer cone. We evaluated the use of an CRI ICP-MS system to minimize polyatomic interference of $^{52}Cr$ and $^{53}Cr$ in various foodstuffs. The $^{52}Cr$ concentrations measured in the standard mode were 2-3 times higher than the certified values. This analytical method based on an ICP-MS system equipped with a CRI of helium gas was effective for Cr analysis in complex food matrices.

• 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.3 no.2
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• pp.54-57
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• 2012

Mass spectrometric analysis was carried out using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) for the precise and accurate determination of the isotope ratios of ultratrace levels of uranium dissolved in 3% $HNO_3$. We used the certified reference material (CRM) 112-A at a trace level of 100 pg/mL for the uranium isotopic measurement. Multiple collectors were utilized for the simultaneous measurement of uranium isotopes to reduce the signal uncertainty due to variations in the ion beam intensity over time. Mass bias correction was applied to the measured U isotopes to improve the precision and accuracy. Furthermore, elemental standard solution with certified values of platinum, iridium, gold, and thallium dissolved in 3% $HNO_3$ were analyzed to investigate the formation rates of the polyatomic ions of $Ir^{40}$ $Ar^+$, $Pt^{40}$ $Ar^+$, $Tl^{40}$ $Ar^+$, $Au^{40}$ $Ar^+$ for the concentration range of 50-400 pg/mL. Those polyatomic ions have mass-to-charge ratios in the 230-245 m/z region that it would contribute to the increase of background intensity of uranium, thorium, plutonium, and americium isotopes. The effect of the polyatomic ion interference on uranium isotope measurement has been estimated.

• 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.

• Journal of Korean Society for Atmospheric Environment
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• v.15 no.4
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• pp.495-503
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• 1999

Airborne particulate matter $(PM_{10})$ collected using high volume air sampler and silica fiber filter were analyzed by Instrumental Neutron Activation Analysis(INAA), Inductively Coupled Plasma Atomic Emission Spectrometry(ICP-AES) and Atomic Absorption Spectrometry(AAS), and the results were compared with each other. 30~40 trace elements in environmental standard reference materials(NIST SRM 1648 and NIES CRM No.8) were analyzed for the analytical quality control. The relative error for two-third of elements detected was less than 10%, and the standard deviation was less than 15%. During the sampling period for 24 hours, the mass concentration of total suspended particulate was 36.1$\mu\textrm{g}$/㎥ and the value is lower than the critical level in Korea. In the results of NAA, the elements of Al, As, Ba, Fe, La, Mg, Na, Sb, Zn were well agreed with those of other methods. In statistical estimation between different methods, the deviation of Al, Ba, Cr, Fe was less than 10% and quite reliable.

• Proceedings of the Korean Society of Tobacco Science Conference
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• 2005.10a
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• pp.37-38
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• 2005

• 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.

• 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.