• Analytical Science and Technology
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• v.28 no.5
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• pp.323-330
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• 2015

Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

• Analytical Science and Technology
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• v.29 no.2
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• pp.94-103
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• 2016

An analytical method was developed to determine the amount of spinetoram (spinetoram J and spinetoram L) in livestock samples. The spinetoram was extracted with acetonitrile and purified through a primary secondary amine (PSA) sorbent. The spinetoram residues were then quantified and confirmed using a liquid chromatography–tandem mass spectrometer (LC-MS/MS) in the positive ion mode using multiple reactions monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/kg) into a blank extract with r² > 0.994. The limits of detection and quantification were 0.002 and 0.01 mg/kg, respectively. The recovery results of spinetram ranged between 81.9-106.4% at different concentration levels (LOQ, 10LOQ, 50LOQ, n=5) with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003). An interlaboratory study was conducted to validate the method. The proposed analytical method proved to be accurate, effective, and sensitive for spinetoram determination. The method will be used as an official analytical method in Korea.

• Analytical Science and Technology
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• v.29 no.2
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• pp.57-64
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• 2016

Many phthalic acid esters (PAEs), including DMP, DEP, DBP, BBP, and DEHP, as well as DEHA are widely used as plasticizers in plastics. An analytical method was developed and used to analyze these compounds at 41 industrial facilities. The coefficient of determination (R²) for each constructed curve was higher than 0.98. The method detection limit (MDL) values were 0.4–0.7 μg/L for PAEs and 0.6 μg/L for DEHA. In addition, the recovery rate was shown to be 77.0–92.3%, while the relative standard deviation was shown to be in the range of 5.8-10.5%. DMP (n = 3), DEP (n = 2), DBP (n = 2), BBP (n = 2), and DEHA (n = 3) were detected in the range of 2.2-11.1% in the influent. DEHP was a predominant compound and was detected at > MDL in both the influent (n = 16, 35.6%) and the effluent (n = 4, 10.0%) at a high removal efficiency (92–100%). The highest levels of residue in industrial wastewater influent were 137.4 μg/L of DEHP at plastic products manufacturing facility, 12.5 μg/L of DEHA at a chemical manufacturing facility, and 14.0 μg/L of DEP at an electronics facility. The highest concentration of effluent was 12.5 μg/L of DEHP at a chemical manufacturing facility, which indicated that the effluent was below the allowable concentration (800 μg/L). Therefore, the levels of PAEs and DEHA that are discharged into nearby streams could not influence the health of the ecosystem.

• Analytical Science and Technology
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• v.23 no.1
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• pp.1-14
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• 2010

It is of importance that all countries in worldwide, including EU and China, have adopted the Restrictions on the use of certain Hazardous Substances (RoHS) for all electronics. IEC62321 document, which was published by the International Electronics Committee (IEC) can have conflicts with the standards in the market. On the contrary Publicly Accessible Specification (PAS) for sampling published by IEC TC111 can be adopted for complementary application. In this work, we tried to find a route to disassemble and disjoint cellular phone sample, based on PAS and compare the screening methods available in the market. For this work, the cellular phone produced in 2001, before the regulation was born, was chosen for better detection. Although X-ray Fluorescence (XRF) showed excellent performance for screening, fast and easy handling, it can give information on the surface, not the bulk, and have some limitations due to significant matrix interference and lack of variety of standards for quantification. It means that screening with XRF sometimes requires supplementary tool. There are several techniques available in the market of analytical instruments. Laser ablation (LA) ICP-MS, energy dispersive (ED) XRF and scanning electron microscope (SEM)-energy dispersive X-ray (EDX) were demonstrated for screening a cellular phone. For quantitative determination, graphite furnace atomic absorption spectrometry (GF-AAS) was employed. Experimental results for Pb in a battery showed large difference in analytical results in between XRF and GF-AAS, i.e., 0.92% and 5.67%, respectively. In addition, the standard deviation of XRF was extremely large in the range of 23-168%, compared with that in the range of 1.9-92.3% for LA-ICP-MS. In conclusion, GF-AAS was required for quantitative analysis although EDX was used for screening. In this work, it was proved that LA-ICP-MS can be used as a screening method for fast analysis to determine hazardous elements in electrical products.

• Analytical Science and Technology
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• v.26 no.4
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• pp.287-297
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• 2013

The optimization of analytical method for the thermal desorption of seven VOCs (volatile organic compounds) by TD-GC/MS (thermal desorption-gas chromatograph-mass spectrometer) with solid phase sorbent tube, and comparative analysis for the determination of VOCs plotted by standard sorbent tubes prepared using both gas phase and liquid phase materials were investigated. The result of paired t-test showed that a liquid phase standard sorbent tube method was in agreement with a gas phase standard sorbent tube method for six species of VOCs including benzene, toluene, ethylbenzene, o-, m-, and p-xylene except for styrene at the significance level (${\alpha}=0.01$), while the 15.6% of difference in response factor between both of gas phase and liquid phase standard plotting for the determination of styrene showed that both methods were significantly different at the significance level. Therefore, the liquid phase standard plotting method was employed to reduce erroneous data for the determination of styrene including BTEX. Under the optimized analytical method by liquid phase standard sorbent tube, recovery was between $100{\pm}5%$ for 7 species of VOCs, reproducibility ranged from 0.3 to 7.7%, and method detection limit (MDL) ranged from $0.01{\mu}g/m^3$ for o-xylene to $0.27{\mu}g/m^3$ for toluene. The optimized standard method was applied to determine VOCs VOCs from indoor air of of dormitory, one bedroom apartment, and a new car.

• Analytical Science and Technology
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• v.31 no.2
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• pp.96-105
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• 2018

This study aimed to improve the method for detecting eight secondary aliphatic amines (SAAs), so as to measure their concentrations in fresh water and tap water samples. NaOH (8 mL, 10 M) and benzenesulfonyl chloride (2 mL) were added to a water sample (200 mL), and the mixture was stirred at $80^{\circ}C$ for 30 min. An additional NaOH solution (10 mL) was added and the stirring was continued for another 30 min. The pH of the cooled mixture was adjusted to 5.5-6.0 by adding HCl (35 %), and the SAAs were extracted using dichloromethane (50 mL). This extraction was repeated once. The extract was then washed with $NaHCO_3$ (15 mL, 0.05 M) and dried over $Na_2SO_4$ (4 g). The extract was finally concentrated to 0.1 mL, of which $1{\mu}L$ was analyzed for SAAs by GC-MS. The linearity of the spike calibration curves was high ($r^2=0.9969-0.9996$). The detection limits of the method ranged from 0.01 to $0.20{\mu}g/L$, and its repeatability and reproducibility (expressed as relative standard deviation) were both less than 10 % (6.6-9.4 %). Its accuracy (measured in percentage error) ranged between 2.4 % and 6.1 %. The established method was applied to the analysis of five surface water and 82 tap water samples. Dimethylamine was the only SAA detected in all the water samples, and its average concentration was $0.79{\mu}g/L$ (range: $0.20-2.54{\mu}g/L$). Therefore, this study improved the analytical method for SAAs in surface water and tap water, and the regional and seasonal concentration distributions were obtained.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.8 no.4
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• pp.311-318
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• 2010

U. S. NRC Regulation Guide 1.52 regulating ESF ACS in nuclear power plants has been revised to revision 3. To apply reduction of operability test time, allowance of alternative challenge agents for in-place leak test of HEPA filters, and upgrade of Methyl Iodide penetration acceptance criterion in activated carbon performance test suggested in Reg. Guide 1.52(Rev.3) on Yonggwang units 5 and 6 ESF ACSes, technical feasibility study was carried out with on-site experiments as well as experiments with a lab-scale model. It was confirmed that the moisture in the system returned to the level before the test in 1 or 4 days even though the moisture was removed during the operability test lasting more than 10 hours. Therefore, it is appropriate to perform monthly operability test in 15 minutes just long enough to check the operability of equipment. To change challenge material for in-place HEPA filter leak test, size of aerosol, production rate, and leak detection capability were compared for DOP and PAO. It was concluded that PAO can be substituted for DOP in nuclear power plants. The upgrade of Methyl Iodide penetration acceptance criterion from 0.175 % to 0.5 % in active carbon filter bed deeper than 4 inches was to conform to the change of activated carbon performance test method to ASTM D3803(1989). It was confirmed that Methyl Iodide penetration acceptance criterion of 0.5 % under $30^{\circ}C$, relative humidity 95 % condition was conservatively good enough for testing performance of active carbon insitu. The licence change of Yonggwang units 5 and 6 has been completed based on this study.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.31 no.3
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• pp.429-436
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• 1998

A bacteriological study of sea water and oyster in Charan Bay was conducted to evaluate sanitary conditions of the bay and compliance of waters with the recommended bacteriological criteria for the designated area of shellfish cultivation, The Samples were collected at 23 sampling stations(Fig. 1 and Fig. 2) estaslished once a month from January 1997 to December 1997, During the study period, temperature ranged from 4.7 to $25.6^{\circ}C$, transparency ranged from 3.3 to 6.2m chemical oxygen demand ranged from 1.67 to 2.18 mg/$\ell$, dissolved oxygen demand ranged from 5.4 to 10.0 mg/$\ell$ dissolved nitrogen ranged from 1.65 to 7.88 $\mu$g-at/$\ell$, phosphate ranged from 0.15 to 1.16 $\mu$g-at/$\ell$, Chlorophylla-a ranged from 0.95 to 12.69mg/$\ell$. The coliform group and fecal coliform MPN's of sea water were ranged from <1.8$\~$l,600 and <1.8$\~$540, respectively. The coliform group and fecal coliform MPN's of oysters were ranged from <18$\~$16,000 and <18$\~$1,400, respectively. The viable cell counts in oyster ranged from $1.5\times10^2$ to $7.5\times10^3$. The bacteriological criteria of sea water in shellfish growing area should be less than 70 per 100 ml of sea water for median value of coliform MPN, and below $10\%$ of the samples which contain over than 230 for coliform MPN or over than 43 for fecal coliform MPN. The sea water from 432 samples were complied water coliform criteria recommended for designated shellfish growing area. The coliform group, fecal coliform, classification of coliform group with IMViC reactions and pathogenic vibrios were analyzed. During the study period, infectious bacteria such as Vibrio cholerae, Salmonella sp, and Shigella sp, were not detected from the samples, but detection ratios of Vibrio parahaemolyticus and Vibrio vulnifirus were $7\~17\%$ in summer months.

• Journal of the Institute of Electronics and Information Engineers
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• v.51 no.9
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• pp.82-90
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• 2014

In this paper, a couple of 4-channel differential transimpedance amplifier arrays are realized in a standard 0.18um CMOS technology for the applications of linear LADAR(laser detection and ranging) systems. Each array targets 1.25-Gb/s operations, where the current-mode chip consists of current-mirror input stage, a single-to-differential amplifier, and an output buffer. The input stage exploits the local feedback current-mirror configuration for low input resistance and low noise characteristics. Measurements demonstrate that each channel achieves $69-dB{\Omega}$ transimpedance gain, 2.2-GHz bandwidth, 21.5-pA/sqrt(Hz) average noise current spectral density (corresponding to the optical sensitivity of -20.5-dBm), and the 4-channel total power dissipation of 147.6-mW from a single 1.8-V supply. The measured eye-diagrams confirms wide and clear eye-openings for 1.25-Gb/s operations. Meanwhile, the voltage-mode chip consists of inverter input stage for low noise characteristics, a single-to-differential amplifier, and an output buffer. Test chips reveal that each channel achieves $73-dB{\Omega}$ transimpedance gain, 1.1-GHz bandwidth, 13.2-pA/sqrt(Hz) average noise current spectral density (corresponding to the optical sensitivity of -22.8-dBm), and the 4-channel total power dissipation of 138.4-mW from a single 1.8-V supply. The measured eye-diagrams confirms wide and clear eye-openings for 1.25-Gb/s operations.

• Journal of the Korean Society of Food Science and Nutrition
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• v.42 no.10
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• pp.1618-1628
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• 2013

Relationships between fatty acids and tocopherols in conventional and genetically modified peanut cultivars were studied by gas chromatography with flame ion detector and high performance liquid chromatography with fluorescence detection. Eight fatty acids and four tocopherol isomers in the sample set were identified and quantified. Oleic acid and linoleic acid are major fatty acids and the ratio of oleic and linoleic acids ranged from 1.11 to 16.26. Tocopherols contents were 6.76 to 12.24 for ${\alpha}$-tocopherol (T), 0.08 to 0.39 for ${\beta}$-T, 5.28 to 15.02 for ${\gamma}$-T, and 0.17 to 1.17 mg/100 g for ${\delta}$-T. Correlation coefficient (r) for fatty acids and tocopherols indicated a strong inverse relationship between oleic & linoleic acids (r=-0.97, P<0.05) and positive relationships between palmitic & linoleic acids (r=0.95, P<0.05) and ${\gamma}$-T & ${\delta}$-T (r=0.83, P<0.05). Principal component analysis (PCA) of fatty acids and tocopherols gave four significant principal components (PCs, with eigenvalues>1), which together account for 85.49% of the total variance in the data set with PC1 and PC2 contributing 45.27% and 21.33% of the total variability, respectively. Eigen analysis of the correlation matrix loadings of the four significant PCs revealed that PC1 was mainly contributed by palmitic, oleic, linoleic, and gondoic acids, while PC2 was by behenic acid, ${\beta}$-T, and ${\gamma}$-T. The score plot generated by PC1-PC2 identified sample clusters in the two spatial planes based on the oleic and linoleic acids. The score plot PC3-PC4 didn't separate sample groups.