• The Journal of the Petrological Society of Korea
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• v.23 no.3
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• pp.221-227
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• 2014

With the advent of multi collector-inductively coupled plasma mass spectrometry, stable isotopic variations of non-traditional metal elements have provided important constraints on the sources of geologic materials. This review introduces the principles of magnesium isotopic fractionation and analytical methods. Recent case studies are also reviewed for the use of magnesium isotope signatures to decipher the source materials of I-, S-, and A-type granitoids in western North America, Australia, and China.

• Analytical Science and Technology
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• v.15 no.5
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• pp.433-438
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• 2002

Trace elements in two air filters (V-50, P-50) artificially loaded with urban dust provided from IAEA were determined non-destructively using instrumental neutron activation analysis. Standard reference material (Urban Particulate Matter, SRM 1648) of National Institute of Standard and Technology was used for analytical quality control. About 20 elements in both of loaded filter samples were determined. To evaluate inter-laboratory comparison and proficiency test, analytical data were statistically treated with the results which collected from 49 laboratories, 40 countries participated in this study using neutron activation analysis, particle induced X-ray emission, inductively coupled plasma mass spectroscopy, etc,. From the results of statistical treatment, Z-scores are within ${\pm}2$. Furthermore, accuracy and precision of obtained analytical values are passed according to the criteria of the proficiency test. Consequently, it was proved that analytical quality for air dust samples being performed has been controlled properly.

• Analytical Science and Technology
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• v.26 no.6
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• pp.375-380
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• 2013

Ammonium biflouride ($NH_4HF_2$) digestion was studied for germanium analysis in rock and sediment by inductively coupled plasma mass spectrometry (ICP/MS). QLO-1 and SDO-1 are used for reference materials from USGS. Sediment, basalt and ball clay for GeoPT were chosen as real samples. The loss of germanium in open vessel digestion was well known which can be caused by easy transformation to volatile compounds. But ammonium bifluoride digestion could suppress loss of germanium in open vessel digestion. Germanium recovery was not influenced by hydrogen peroxide with ammonium bifluoride digestion. Furthermore, the new method was simple and rapid in germanium analysis by ICP/MS. MDL(method detection limit) was 0.015 ${\mu}g/g$ and germanium recovery was 106~128%.

• Journal of Korean Society of Environmental Engineers
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• v.28 no.10
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• pp.1038-1045
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• 2006

A series of experiments was conducted to test the compatibilities of two different techniques to determine elemental concentrations by INAA and ICP-MS based on both the NIST SRM 2783(air particulate on filter media) and the field samples for PM10. For NIST SRM the results of INAA were more accurate and precise for all target elements than those of ICP-MS. The comparative data set for PM10 samples collected in an industrial complex area showed that mean of concentration ratio, derived for the two different methods such as C(INNA/ICP-MS), were distinguished from each other: (1) Ba, Cu, K Mg, Na, and Sb: $0.9{\sim}1.1$; (2) Al, Co, Fe, and Mn: $0.8{\sim}1.2$; and (3) Se, Ti, and Zn: >1.3. When the results obtained from both methods were evaluated in terms of regression analysis, paired t-test, and Wilcoxon signed-rank test, the results of many elements determined from PM10 samples(such as Al, Ba, Co, Cu, Fe, K, Mn, Nd, and Sb) exhibited a fairly good agreement between the two methods, despite a wide range of variation.

• Economic and Environmental Geology
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• v.49 no.2
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• pp.89-95
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• 2016

Mo isotope, one of highly redox-sensitive isotopes, has been shown to be useful tracers of geochemical processes. Many studies for Mo isotope have documented with the help of recently developed analysis tools, but it has not yet been documented in the Korea. In this study, we introduce two-stage column separation method of Mo using column tube (BioRad PolyPrep(R) column, 10 ml) and anion exchange resin (BioRad Resin AG(R) 1-X8, 200-400 mesh). Mo isotope ratios in the solid SRMs (BHVO-2, SDO-1, PACS-2) and liquid SRM (IAPSO) were measured on MC-ICP-MS (Multi-collector Inductively Coupled Plasma Mass Spectrometer) and then compared with reference Mo isotope ratios. Mo isotope ratios in our study overlap with reference Mo isotope ratios within analytical error.

• Korean Journal of Environmental Agriculture
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• v.30 no.3
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• pp.288-294
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• 2011

BACKGROUND: Methylmercury is analyzed by HPLC-ICP/MS because of the simplicity for sample preparation and interference. However, most of the pre-treatment methods for methylmercury need a further pH adjustment of the extracted solution and removal of organic matter for HPLC. The purpose of this study was to establish a rapid and accurate analytical method for determination of methylmercury in fish by using HPLC-ICP/MS. METHOD AND RESULTS: We conducted an experiment for pre-treatment and instrument conditions and analytical method verification. Pre-treatment condition was established with aqueous 1% L-cysteine HCl and heated at $60^{\circ}C$ in microwave for 20 min. Methylmercury in $50{\mu}L$ of filtered extract was separated by a C18 column and aqueous 0.1% L-cysteine HCl + 0.1% L-cysteine mobile phase at $25^{\circ}C$. The presence of cysteine in mobile phase and sample solution was essential to eliminate adsorption, peak tailing and memory effect problems. Correlation coefficient($r^2$) for the linearity was 0.9998. The limits of detection and quantitation for this method were 0.15 and $0.45{\mu}g/kg$ respectively. CONCLUSION: Result for analytical method verification, accuracy and repeatability of the analytes were in good agreement with the certified reference materials values of methylmercury at a 95% confidence level. The advantage of the established method is that the extracted solution can be directly injected into the HPLC column without additional processes and the memory effect of mercury in the ICP-MS can be eliminated.

• The Journal of the Petrological Society of Korea
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• v.3 no.1
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• pp.41-48
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• 1994

Three USGS rock standards (G-2, W-2, and BHVO-1) are decomposed by three different methods, such as open beaker, microwave oven, and alkali fusion method, to compare the effect of decomposition methods for trace elememt analysis in the rock samples. Solubilized trace elements are measured with inductively coupled plasma mass spectrometer (ICP-MS). Generally the analytical results of trace elements between open beaker and microwave digestion method are not different. In case of alkali fusion method, some volatile elements such as Pb, Cu, and Rb are considerably lost. Using acid digestion method, Zr and Hf concentrations are lowered in case that these elements are concentrated in refractory minerals. The concentrations of rare earth elements are generally consistent with the recommended values, but due to large dilution factor, there are some analytical problems in alkali fusion method.

• Analytical Science and Technology
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• v.27 no.2
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• pp.92-99
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• 2014

Interferences were removed using anion exchange solid phase extraction (AE SPE) in quantification of selenoproteins in Korean human blood serum with affinity high performance liquid chromatography (AF HPLC)-inductively coupled plasma/mass spectrometry (ICP/MS). The average selenium level obtained for healthy Koreans was $94.3{\pm}2.3ngg^{-1}$ using isotope dilution method. AE SPE was coupled to AF column to separate 3 selenoproteins, glutathione peroxidase GPx, selenoprotein SelP, and selenoalbumin SeAlb. Post column isotope dilution was employed to quantify the proteins. The certified reference material of human blood serum BCR-637 was analyzed to give total selenoprotein concentration of $85.4{\pm}3.4ngg^{-1}$, which agreed well with the reference value of $81{\pm}7ngg^{-1}$. The pooled concentration of GPx, SelP, and SeAlb from healthy Koreans (n=20) was $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, and $20.0{\pm}1.9ngg^{-1}$, respectively. The sum of selenoproteins is $89.3ngg^{-1}$, which is about the same as the total selenium concentration of $94.3ngg^{-1}$. The fact suggests that selenium in blood serum is mostly consisted of selenoproteins. After the removal of interference, GPx showed a significant decrease (more than 50%) from $25.0ngg^{-1}$ to $12.1ngg^{-1}$. It was identified that the interference in blood serum was mostly from GPx and the use of AE SPE was proven to be efficient in eliminating Cl and Br that cause interference to GPx.

• Korean Chemical Engineering Research
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• v.53 no.3
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• pp.372-381
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• 2015

The effect of preparation method on the catalytic activities of the $Ni/Al_2O_3$ catalysts on steam reforming of ethylene glycol was investigated. The catalysts were prepared with various preparation methods such as an incipient wetness impregnation, wet impregnation, and coprecipitation method. In the case of coprecipitation method, various precipitants such as KOH, $K_2CO_3$, and $NH_4OH$ were compared. The prepared catalysts were characterized by using $N_2$ physisorption, inductively coupled plasma-atomic emission spectroscopy, X-ray diffraction, temperatureprogrammed reduction, pulsed $H_2$ chemisorption, temperature-programmed oxidation, scanning electron microscopy, and thermogravimetric analysis. Among the catalysts reduced at 773 K, the $Ni/Al_2O_3$ catalyst prepared by a coprecipitation with KOH or $K_2CO_3$ as precipitants showed the best catalytic performance. The preparation method affected the particle size of Ni, reducibility of nickel oxides, catalytic performance (activity and stability), and types of coke formed during the reaction. The $Ni/Al_2O_3$ catalyst prepared by a coprecipitation with KOH showed the increasing catalytic activity with an increase in the reduction temperature from 773 to 1173 K because of an increase in the reduction degree of Ni oxide species even though the particle size of Ni increased with increasing reduction temperature.

• Journal of the Mineralogical Society of Korea
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• v.29 no.4
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• pp.221-227
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• 2016

Copper is an essential transition metal involving in various biogeochemical processes. With the recent advances in analytical techniques and mass spectrometry, such as MC-ICP-MS, it is possible to measure Cu isotopes, which allows us to understand various biogeochemical processes in detail. Nonetheless, few studies have been performed in South Korea. In this study, we compared two purification methods previously reported using an anion exchange resin ($AG^{(R)}$ MP-1M), developed the best method in our lab environment, and then verified it by measuring Cu isotopic compositions in two USGS geological reference materials (BHVO-2 and BIR-1a). Although all matrix cations causing mass bias were effectively removed through both two methods with the yield of better than 95%, the method using the mixture of HCl and $H_2O_2$ only displays Cu isotopic compositions, in excellent agreement with reported values within the error. The method developed in this study is expected to be commonly applied to earth and environmental sciences.