• Analytical Science and Technology
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• v.15 no.6
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• pp.489-495
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• 2002

In this study, we determined distribution status of organonitrogen pesticides such as trifluralin, atrazine, metribuzin, alachlor, malathion, nitrofen, permethrin, cypermethrin, fenvalerate, and parathion accumulated in the fresh water fishes and amphibians. We collected those samples at 31 sites from the basin of major rivers, and separated the muscular tissue as a final sample for analysis. In the pretreatment process, lipid was eliminated by using acetonitrile and n-hexane, and pesticides were reextracted with dichloromethane. The extract was dehydrated and concentrated, and then cleaned it up by passing the Florisil column, and pesticide content was finally determined by using a GC-MS system after introducing isotope labelled references. The accumulation level was observed in the range of $0.17{\sim}6.8{\mu}g/kg$ in amphibians and $0.26{\sim}16{\mu}g/kg$ in fishes including cypermethrin as $16{\mu}g/kg$.

• Analytical Science and Technology
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• v.17 no.5
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• pp.381-387
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• 2004

To characterize chemically a spent pressurized water reactor (PWR) fuel, an analytical method for trace amounts of tritium ($^3H$) in it has been established. Considering the effective management of radioactive wastes generated through the whole experimental process and the radiological safety for analysts, a separation condition under which $^{14}C$ and $^3H$ can be sequentially recovered from a single fuel sample was optimized using simulated spent PWR fuel dissolved solutions. $^{14}CO_2$ evolved during dissolution of the spent PWR fuels with nitric acid was trapped in an aliquot of 1.5 M NaOH. $^{129}I_2$ which was volatilized along with $^{14}CO_2$ was removed using a silver nitrate-impregnated silica gel absorbent. $^3H$ remaining in the fuel dissolved solution as $^3H_2O$ was selectively recovered by distillation. Its recovery yield was 97.9% with a relative standard deviation of 0.9% (n=3). $^3H$ in a spent PWR fuel with burnup value of 37,000 MWd/MtU was analyzed, reliability of this analytical method being evaluated by standard addition method.

• Archives of Pharmacal Research
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• v.14 no.1
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• pp.35-40
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• 1991

(R) (+) and (S) (-) $4-^2H$-phenytoin have been used as substrates for the determination of the percentage of deuterium retention (NIH shift) after para-hydroxylation of the substrates in rat. By using GC-MS analyses, the percentages of deuterium retention were found to be 69% and 70% for the (R) and (S) phenyl rings, respectively. The results add additional evidence for the involvement of arene oxide in the oxidation of the pro (R) and pro (S) phenyls of phenytoin. The oxidation process of each ring could be mediated by independent enzyme systems, a rapid oxidative enzyme for the pro (S) phenyl and a slow oxidative enzyme for the pro (R) phenyl.

• Analytical Science and Technology
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• v.8 no.2
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• pp.131-138
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• 1995

We have discussed on the structural transition and its effect on the electrical property of Li-GFDICs and Li-PCDICs occuring during the deintercalation process of Li-Graphite Fiber Intercalation Compounds(Li-GFICs) and Li-Petroleum Cokes Intercalation Compounds(Li-PCDICs) synthesized under pressure and temperature by spontaneous oxidation by air circulation. The analytical results were obtained by X-ray diffraction and electrical specific resistivity measurements. According to X-ray analysis, we have found that the major stage of Li-GFICs was stage 2 and those of Li-PCICs were stage 1 and stage 2, respectively. And from this results of the deintercalation process, we have found that the deintercalation process did not occur any more after 5th week of Li-GFDICs and after 3rd week of Li-PCDICs. According to the results of the electrical specific resistivity measurements, Li-GFDICs showed little variation to 3rd week and rising in the steady curve after 4th week, while Li-PCDICs showed a rising in the steady curve to 3rd week and a declining curve after 3rd week. Therefore from these results, we can consider that graphite fiber and petroleum cokes as a substrate can be also used as an anode material of battery because they have good intercalation-deintercalation reactivity with lithium.

• Analytical Science and Technology
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• v.15 no.2
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• pp.97-101
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• 2002

Co(II) complexes with tridentate Schiff base-NOIPH and tetradentate Schiff base-$NOTDH_2$ and $TNBPH_4$ were synthesized. The redox process of the complexes in DMF solution containing 0.1M TBAP was investigated at glassy carbon electrode by cyclic voltammetry and differential pulse voltammetry techniques. Reduction step of [Co(II)$(NOIP)_2$] and [Co(II)$(H_2O)_2$] complexes were observed in two step as one electron process of irreversible or quasi-reversible and diffusion-controlled reaction. [$Co(II)_2$(TNBP)] complex was observed in one step as one electron process of quasi-reversible and diffusion-controlled reaction.

• Analytical Science and Technology
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• v.9 no.1
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• pp.43-51
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• 1996

We have discussed on the deintercalation process of Li-EaGICs and Li-EGICs synthesized under pressure and temperature by spontaneous oxidation reaction of those compounds based on the results of X-ray diffraction, thermal analysis and electrical specific resistivity analysis. According to the results of the X-ray analysis for the intercalation process, we have found that the stage 1 for Li-EaGICs and Li-EGICs were not completly formed, but their lower stages were formed mainly. And from this results of the deintercalation process, we have found that the deintercalation process did not occur any more after 4 weeks, and the Li-EGDICs have more residual lithium metals than LiEaGDICs between the graphite interlayers. According to the thermal decomposition analysis, Li-two compounds had included very hard exothermic reaction. And we have found that these compounds did not occrurred deintercalation reaction above $400^{\circ}C$. According to the results of the electrical specific resistivity measurements, Li-EGDICs have relatively lower electrical specific resistivity than Li-EaGDICs, and Li-EaGDICs showed a formation of the ideal curve. From these results, we can suggest that Li-EaGDICs have a better properties as an anode material secondary than Li-EGICs.

• Analytical Science and Technology
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• v.23 no.1
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• pp.60-67
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• 2010

A sensitive competitive heterogeneous bioluminescence immunoassay for serotonin was developed using photoprotein, aequorin as a label for the first time with the optimal assay conditions; especially, serotoninavidin conjugate was prepared by Mannich reaction and the synthetic process of serotonin-avidin conjugate was optimized by controlling the initial molar ratios of serotonin, formaldehyde and avidin (1:12,000:25). The developed bioluminescence immunoassay for serotonin showed good sensitivity (LOD of 0.68 ng/mL) with wide area of dynamic range ($5.0{\times}10^{-10}\;M\sim5.0{\times}10^{-7}\;M$). (cf. the range for serotonin in human blood serum is $151{\pm}45\;ng$/mL). In addition, cross-reactivity studies demonstrated that 5-methoxytryptamine showed some cross-reactivity (28.0%), whereas 3-methylindole, melatonin and 5-hydroxylindole-3-acetic acid showed no crossreactivity, and good recoveries were obtained in serum. Thus, this developed method provides a good tool to monitor serotonin in serum.

• Analytical Science and Technology
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• v.17 no.2
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• pp.173-179
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• 2004

The $BaTiO_3$ powders and thin films were prepared by an alkoxide modified sol-gel process (polymerization-complex route) using ethylene glycol. The stable starting (Ba-Ti)-mixed metal organic sol was made by addition of acetylacetone. The $BaTiO_3$ powders, which had a particle size of 40~77 nm, were crystallized from an amorphous to a tetragonal phase on annealing at 700 and $1100^{\circ}C$ for 1 h. From FT-IR, solid-state $^{13}C$ CP/MAS NMR spectroscopy and X-ray diffractometry, the trace of the Ba-Ti-oxycarbonate phase first appeared at $400^{\circ}C$. Hydrolyzed sol was spin coated on a quartz wafer at 3500 rpm for 60 s and pyrolyzed at $1100^{\circ}C$ for 1 h. After heat treatment, the coated layer became dense and smooth.

• Analytical Science and Technology
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• v.34 no.3
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• pp.128-133
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• 2021

During titration, several chemical reactions result in changes not only in the potential of chemicals, but also in the colors of the indicator. In a potentiometric titration, a titration curve is obtained by measuring the abrupt change in the potential at the endpoint. Generally, acid-base titration is performed by observing the color change caused by an indicator to determine the endpoint. The method of determining the endpoint by measuring the potential difference has been well established and commercialized; however, the devices that can obtain the endpoint by observing the color change are limited. Consequently, in this study, a simple and precise spectral endpoint detector was manufactured using a drop-counter comprising an infrared emitter and a phototransistor, a white light LED as the light source and photodetector, and an analog-to-digital converter (Arduino). Spectrator, a new named, showed excellent results in terms of the reproducibility of acid-base titration using thymol blue as an indicator. Herein, we present the results of the Spectrator-manufacturing process as well as the experimental results.

• Analytical Science and Technology
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• v.37 no.2
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• pp.98-113
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• 2024

The current investigation entails the characterization of five degradation products (DPs) formed under different stress conditions of loteprednol using liquid chromatography-tandem mass spectrometry (LC-MS/MS). In addition, this study developed a stable high-performance liquid chromatography (HPLC) method for evaluating loteprednol along with impurities. The method conditions were meticulously fine-tuned which involved the exploration of the appropriate solvent, pH, flow of the mobile phase, columns, and wavelength. The method conditions were carefully chosen to successfully resolve the impurities of loteprednol and were employed in subsequent validation procedures. The stability profile of loteprednol was exposed to stress degradation experiments conducted under five conditions, and DPs were structurally characterized by employing LC-MS/MS. The chromatographic resolution of loteprednol and its impurities along with DPs was effectively achieved using a Phenomenex Luna 250 mm C18 column using 0.1 % phosphoric acid, methanol, and acetonitrile in 45:25:30 (v/v) pumped isocratically at 0.8 mL/min with 243 nm wavelength. The method produces an accurate fit calibration curve in 50-300 ㎍/mL for loteprednol and LOQ (0.05 ㎍/mL) - 0.30 ㎍/mL for its impurities with acceptable precision, accuracy, and recovery. The stress-induced degradation study revealed the degradation of loteprednol under basic, acidic, and photolytic conditions, resulting in the formation of seven distinct DPs. The efficacy of this method was validated through LC-MS/MS, which allowed for the verification of the chemical structures of the newly generated DPs of loteprednol. This method was appropriate for assessing the impurities of loteprednol and can also be appropriate for structural and quantitative assessment of its degradation products.