• The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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• v.18 no.1
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• pp.40-46
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• 2013

The isotope ratios of $^{13}C/^{12}C$ and $^{18}O/^{16}O$ for a sample in a mass spectrometer are measured relative to those of a pure $CO_2$ reference gas (i.e., laboratory working standard). Thus, the calibration of a laboratory working standard gas to the international isotope scales (Pee Dee Belemnite (PDB) for ${\delta}^{13}C$ and Vienna Standard Mean Ocean Water (V-SMOW) for ${\delta}^{18}O$) is essential for comparisons between data sets obtained by other groups on other mass spectrometers. However, one often finds difficulties in getting well-calibrated standard gases, because of their production time and high price. Additional difficulty is that fractionation processes can occur inside the gas cylinder most likely due to pressure drop in long-term use. Therefore, studies on laboratory production of pure $CO_2$ isotope standard gas from stable solid calcium carbonate standard materials, have been performed. For this study, we propose a method to extract pure $CO_2$ gas without isotope fractionation from a solid calcium carbonate material. The method is similar to that suggested by Coplen et al., (1983), but is better optimized particularly to make a large amount of pure $CO_2$ gas from calcium carbonate material. The $CaCO_3$ releases $CO_2$ in reaction with 100% pure phosphoric acid at $25^{\circ}C$ in a custom designed, evacuated reaction vessel. Here we introduce optimal procedure, reaction conditions, and samples/reactants size for calcium carbonate-phosphoric acid reaction and also provide the details for extracting, purifying and collecting $CO_2$ gas out of the reaction vessel. The measurements for ${\delta}^{18}O$ and ${\delta}^{13}C$ of $CO_2$ were performed at Seoul National University using a stable isotope ratio mass spectrometer (VG Isotech, SIRA Series II) operated in dual-inlet mode. The entire analysis precisions for ${\delta}^{18}O$ and ${\delta}^{13}C$ were evaluated based on the standard deviations of multiple measurements on 15 separate samples of purified $CO_2$. The pure $CO_2$ samples were taken from 100-mg aliquots of a solid calcium carbonate (Solenhofen-ori $CaCO_3$) during 8-day experimental period. The multiple measurements yielded the $1{\sigma}$ precisions of ${\pm}0.01$‰ for ${\delta}^{13}C$ and ${\pm}0.05$‰ for ${\delta}^{18}O$, comparable to the internal instrumental precisions of SIRA. Therefore, we conclude the method proposed in this study can serve as a way to produce an accurate secondary and/or laboratory $CO_2$ standard gas. We hope this study helps resolve difficulties in placing a laboratory working standard onto the international isotope scales and does make accurate comparisons with other data sets from other groups.

• Analytical Science and Technology
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• v.28 no.6
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• pp.417-424
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• 2015

In this study, the relationship between selenoprotein concentrations in blood and stomach cancer have been searched for Korean. The concentration of each selenoprotein in blood serum was analyzed and the correlation between the concentration and stomach cancer was studied to find a potential for using Selenium as a biomarker. In concentration determination, a simple calibration curve method was used with the monitoring of m/z 78 without the use of solid phase extraction. This is a lot more simple than the method using SPE with post column isotope dilution. The result obtained from the analysis of CRM BCR-637, 72.20±3.35 ng·g⁻¹, showed similar value of reference value (81±7 ng·g⁻¹). The total concentration of Se for the controlled group, cardiovascular patients group, was 105.70±21.20 ng·g⁻¹. This value was the same as normal healthy person reported earlier. Each selenoprotein concentration of GPx, SelP and SeAlb was 26.12±7.84, 65.15±14.50, 14.43±6.99 ng·g⁻¹, respectively. The distribution of each selenoprotein was 24.7%, 61.6%, and 13.7%, which was similar to the normal person. The result of stomach cancer patients, the total concentration of Se was 76.11±28.12 ng·g⁻¹ and each concentration of GPx, SelP and SeAlb was 15.41±9.01, 50.83±17.91, and 9.87±5.21 ng·g⁻¹, respectively. The total and each selenoprotein concentration level showed significant decrease for the stomach cancer patients. The level of decrease was 41.0% for GPx, 22.0% for SelP, and 31.6% for SeAlb. However, the distribution of each selenoprotein was not much different. Either total Selenium or each selenoprotein could be used as a possible index for the diagnosis of cancer. However, in age group study, it is shown that young age group (30's-40's) did not show much difference.

• Analytical Science and Technology
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• v.28 no.6
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• pp.385-397
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• 2015

Harmful and potentially harmful constituents (HPHCs) are chemical compounds in tobacco smoke that cause harm to smokers and non-smokers. This study established and validated methods for the analysis of HPHCs from mainstream cigarette smoke. The analyzed HPHCs were categorized into seven groups: aromatic amines, volatile organic compounds (VOCs), heavy metals, tobacco specific nitrosamines (TSNAs), benzo[a]pyrene (B[a]P), ammonia, and carbonyl compounds. The methods were validated by specificity, linearity, limit of detection (LOD), accuracy, precision, and recovery. These validated methods were then applied to the reference cigarettes (1R5F, 3R4F). The correlation coefficients (r²) for the calibration curves of the seven groups were over 0.995. The LODs showed values of 0.01-0.04 ng/cig cig for aromatic amines, 0.01-0.16 μg/cig for VOCs, 0.01-1.27 ng/cig for heavy metals, 0.06-0.28 ng/cig for TSNAs, 0.04 ng/cig for benzo[a]pyrene, 0.08 μg/cig for ammonia, and 0.78-1.77 μg/cig for carbonyl compounds. The precisions obtained from the intra and inter-day batches were less than 15%. The accuracy and the recovery range were less than 15% and 79.2-117.5%, respectively. The proposed methods can therefore be applied for determining HPHCs in tobacco mainstream smoke.

• Korean Journal of Environmental Agriculture
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• v.36 no.2
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• pp.113-118
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• 2017

BACKGROUND: The carbon (C) isotope ratio (${\delta}^{13}C$) of dissolved organic C (DOC) is an indicator of water pollution source. In this study, the potential use of two pre-treatments for the ${\delta}^{13}C$ analysis, alkaline persulfate oxidation coupled with carbonate precipitation (precipitation) and freeze drying (drying), were compared to suggest a more feasible pre-treatment method. METHODS AND RESULTS: Two reference materials with different ${\delta}^{13}C$ values were used for the experiments; chemical grade glucose ($-12.0{\pm}0.02$‰) and pig manure compost extract ($-23.3{\pm}0.04$‰). In the precipitation method, the measured ${\delta}^{13}C$ values were consistently lower than the theoretically calculated values as dissolved $CO_2$ could not be removed due to the alkaline property of the reagents and the dissolution of air $CO_2$ into the alkaline solution. The drying method also resulted in more negative ${\delta}^{13}C$ than the calculated ${\delta}^{13}C$; however, the difference was systematic ($3.9{\pm}0.3$‰) and there was a strong correlation (${\delta}^{13}C_{calculated}=0.87{\times}{\delta}^{13}C_{measured}-0.624$, $r^2=0.98$) between the calculated and measured ${\delta}^{13}C$. Calibration of ${\delta}^{13}C$ using the relationship between the calculated and the measured ${\delta}^{13}C$ values produced reliable and accurate ${\delta}^{13}C$ values. CONCLUSION: Our results suggest that the drying method is more accurate pre-treatment method to minimize the influence of air $CO_2$ compared to the precipitation method for the determination of ${\delta}^{13}C$ of DOC.

• Journal of Korean Society of Environmental Engineers
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• v.31 no.2
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• pp.153-160
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• 2009

A PM10 (aerodynamic diameter${\leq}$10 ${\mu}m$) sampler is used to quantify the potential human exposure to suspended particulate matter (PM) and to comply with the governmental regulation. This study was conducted to compare and evaluate the same PM10 cutpoint and different slopes between United States Environmental Protection Agency (USEPA) PM10 sampling criterion and American Conference of Governmental Industrial Hygienists/$Comit\acute{e}$ $Europ\acute{e}en$ de Normalization/International Organization for Standardization thoracic PM10 sampling criterion through theory and experiment. Four PM10 samplers according to the USEPA criterion and one RespiCon sampler in accordance with the thoracic PM10 criterion were used in the present study. In addition, one DustTrak monitor was used to measure real time PM10 mass concentrations. All six aerosol samplers were tested in a PM generation chamber using polydisperse fly ash. Theoretical mass concentrations were calculated by applying the measured particle size distribution characteristics (geometric mean = 6.6 ${\mu}m$, geometric standard deviation = 1.9) of fly ash to each sampling criterion. The measured mass concentrations through a chamber experiment were consistent with theoretical mass concentrations in that a RespiCon sampler with the thoracic PM10 criterion collected less PM than a PM10 sampler with the USEPA criterion. The overall chamber experiment results indicated, when a PM10 sampler was used as a reference sampler, that (1) a RespiCon sampler had a normalizing factor of 1.6, meaning that this sampler underestimated an average 60% of PM10 mass sampled from a PM10 sampler, and (2) a DustTrak real-time monitor using a PM10 inlet had a calibration factor of 2.1.

• Korean Journal of Food Science and Technology
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• v.36 no.5
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• pp.701-710
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• 2004

Uncertainty was quantified to evaluate calcium determination result in infant formula with AAS (Atomic Absorption Spectrometry) and ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry). Uncertainty sources in measurand, such as sample weight, final volume of sample, sample dilution and the instrumental result were identified and used as parameters for combined standard uncertainty based on the GUM (Guide to the expression of uncertainty in measurement) and Draft EURACHEM/CITAC Guide. Uncertainty components of each sources in measurand were identified as resolution, reproducibility and stability of chemical balance, standard material purity, standard material molecular weight, standard solution concentration, standard solution dilution factor, sample dilution factor, calibration curve, recovery, instrumental precision, reproducibility, and stability, Each uncertainty components were evaluated by uncertainty types and included to calculate combined uncertainty. The kinds of uncertainty sources and components in the analytical method by AAS and ICP-AES were same except sample dilution factor for AAS. The analytical results and combined standard uncertainties of calcium content were estimated within the certification range $(367{\pm}20\;mg/100g)$ of CRM (Certified Reference Material) and were not significantly different between method by AAS followed by ashing and method by ICP-AES followed by acid digestion as $359.52{\pm}23.61\;mg/100g\;and\;354.75{\pm}16.16\;mg/100g$, respectively. Identifying uncertainty sources related with precision, repeatability, stability, and maintaining proper instrumental conditions as well as personal proficiency was needed to reduce analytical error.

• The Korean Journal of Nuclear Medicine
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• v.34 no.4
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• pp.336-343
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• 2000

Purpose: Thallous-201 chloride produced at Korea Cancer Center Hospital(KCCH) is used in detecting cardiovascular disease and cancer. Thallium impurity can cause emesis, catharsis and nausea, so the presence of thallium and other metal impurities should be determined. According to USP and KP, their amounts must be less than 2 ppm in thallium and 5 ppm in total. In this study, the detection method of trace amounts of metal impurities in $[^{201}Tl]$TICI injection with polarography was optimized without environmental contamination. Materials and Methods: For the detection of metal impurities, Osteryoung Square Wave Stripping Voltammetry method was used in Bio-Analytical System (BAS) 50W polarograph. The voltammetry was composed of Dropping Mercury Electrode (DME) as a working electrode, Ag/AgCl as a reference electrode and Pt wire as a counter electrode. Square wave stripping method, which makes use of formation and deformation of amalgam, was adopted to determine the metal impurities, and pH 7 phosphate buffer was used as supporting electrolyte. Results: Tl, Cu and Pb in thallous-201 chloride solution were detected by scanning from 300 mV to -800 mV Calibration curves were made by using $TINO_3,\;CuSO_4\;and\;Pb(NO_3){_2}$ as standard solutions. Tl was confirmed at -450 mV peak potential and Cu at -50 mV Less than 2 ppm of Tl and Cu was detected and Pb was not detected in KCCH-produced thallous-201 chloride injection. Conclusion: Detection limit of thallium and copper is approximately 50 ppb with this method. As a result of this experiment, thallium and other metal impurities in thallous-201 chloride injection, produced at Korea Cancer Center Hospital, are in the regulation of USP and KP Polarograph could be applied for the determination of metal impurities in the quality control of radiopharmaceuticals conveniently without environmental contamination.

• Journal of the Korean Association of Geographic Information Studies
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• v.22 no.2
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• pp.82-96
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• 2019

This study evaluated the status of watershed health in Geum River Basin by SWAT (Soil and Water Assessment Tool) hydrology and water quality. The watershed healthiness from watershed hydrology and stream water quality was calculated using multivariate normal distribution from 0(poor) to 1(good). Before evaluation of watershed healthiness, the SWAT calibration for 11 years(2005~2015) of streamflow(Q) at 5 locations with 0.50~0.77 average Nash-Sutcliffe model efficiency and suspended solid (SS), total nitrogen(T-N), and total phosphorus(T-P) at 3 locations with 0.67~0.94, 0.59~0.79, and 0.61~0.79 determination coefficient($R^2$) respectively. For 24 years (1985~2008) the spatiotemporal change of watershed healthiness was analyzed with calibarted SWAT and 5 land use data of 1985, 1990, 1995, 2000, and 2008. The 2008 SWAT results showed that the surface runoff increased by 40.6%, soil moisture and baseflow decreased by 6.8% and 3.0% respectively compared to 1985 reference year. The stream water quality of SS, T-N, and T-P increased by 29.2%, 9.3%, and 16.7% respectively by land development and agricultural activity. Based on the 1985 year land use condition. the 2008 watershed healthiness of hydrology and stream water quality decreased from 1 to 0.94 and 0.69 respectively. The results of this study be able to detect changes in watershed environment due to human activity compared to past natural conditions.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.13-21
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• 2019

A method was developed for the simultaneous detection of an antibiotic fungicide, streptomycin, and its metabolite (dihydrostreptomycin) in agricultural products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using methanol adjusted to pH 3 using formic acid, and purified with a HLB (Hydrophilic lipophilic balance) cartridge. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.001 to 0.1 mg/kg, and linearity of five agricultural products (hulled rice, potato, soybean, mandarin, green pepper), with coefficients of determination $(R^2){\geq}0.9906$, for streptomycin and dihydrostreptomycin. The mean recoveries at three fortification levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) were from 72.0~116.5% and from 72.1~116.0%, and relative standard deviations were less than 12.3% and 12.5%, respectively. The limits of quantification (LOQ) were 0.01 mg/kg, which are satisfactory for quantification levels corresponding with the Positive List System. All optimized results satisfied the criteria ranges requested in the Codex guidelines and the Food Safety Evaluation Department guidelines. The present study could serve as a reference for the establishment of maximum residue limits and be used as basic data for detection of streptomycin and dihydrostreptomycin in food.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.235-241
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• 2019

An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.