• Title/Summary/Keyword: PT/GC

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Determination of Cr(Ⅵ) by Glassy Carbon and Platinum Electrodes Modified With Polypyrrole Film (폴리피롤 막으로 변성시킨 유리질 탄소 및 백금 전극에서 Cr(Ⅵ) 이온의 정량)

  • Yoo, Kwang Sik;Woo, Sang Beom;Jyoung, Jy Young
    • Journal of the Korean Chemical Society
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    • v.43 no.4
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    • pp.407-411
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    • 1999
  • Studies have been carried out on the fabrication of PPy/GC and PPy/Pt electrode modified with polypyrrole film and determination of Cr(VI) by using 3-electrode system with modified electrodes. Modified electrodes were able to easily fabricated by cyclic voltammetry scanned from +1.0V to -1.0V(vs. Ag/AgCl) at 50 mV/sec. Film thickness could be controlled at same condition by the number of cycling up to 26 times. Reduction behaviour of Cr(VI) at PPy/GC electrode could be seen at wide potential ranges from +0.6V to -0.5V(vs. Ag/AgCl), and maximum reduction peak potential of the ion was observed at -0.25V(vs.Ag/AgCl). Calibration graph at its potential was linear from 0.1 ppm to 80.O ppm. Slope factor and relative coefficient were 1.75 mA/ppm and 0.998, respectively. Reduction behaviour of Cr(VI) at PPy/Pt electrode was similar to PPy/GC electrode, Calibration graph was linear from l.0 ppm to 60.0 ppm. Slope factor and relative coefficient were 0.5mA/ppm and 0.923, respectively. But PPy/GC modified electrode had about 3 times higher sensitivity than PPy/Pt modified electrode. Reduction behaviour of Cu(II), As(IlI), Pb(II), and Cd(II) couldn't be seen at PPy/GC electrode,Its metals had not lnterfered with Cr (VI) determination.

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Development of a Simultaneous Detection and Quantification Method of Anorectics in Human Urine Using GC-MS and its Application to Legal Cases (GC-MS를 이용한 사람 뇨시료 중 비만치료제 분석 및 비만치료제 남용 현황의 법과학적 고찰)

  • Choi, Hyeyoung;Lee, Jaesin;Jang, Moonhee;Yang, Wonkyung;Kim, Eunmi;Choi, Hwakyung
    • YAKHAK HOEJI
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    • v.57 no.6
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    • pp.420-425
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    • 2013
  • Phentermine (PT) and phenmetrazine (PM) have been widely used as anti-obesity drugs. These drugs should be used with caution due to its close relation to amphetamine in its structure and toxicity. PT and PM, amphetamine-type anorectics, have recently been considered as alternatives for methamphetamine abuse in Korea. In addition, the misuse and abuse of PT and PM obtained by illegal sources such as the internet become a serious social problem. In the present study, a simultaneous detection and quantification method for determining PT and PM in human urine was developed and validated according to the international guidelines. The urine samples were screened using a fluorescence polarization immunooassay and analyzed by gas chromatography mass spectrometry (GC-MS) after extraction using automatic solid phase extraction (SPE) with a mixed-mode cation exchange cartridge and derivatization with pentafluoropropionic anhydride (PFPA). The validation results for selectivity, linearity, limits of detection (LOD) and quantification (LOQ), intra- and inter-assay precision and accuracy and recovery were satisfactory. The validated method was successfully applied to authentic urine samples collected from 38 drug abuse suspects. PT and/or PM were identified with or without methamphetamine in urine samples. Abuse of PT and PM have increased continuously in Korea, therefore, closer supervision of the inappropriate use of anoretics is necessary.

Photodecomposition of Concentrated Ammonia over Nanometer-sized TiO2, V-TiO2, and Pt/V-TiO2 Photocatalysts

  • Choi, Hyung-Joo;Kim, Jun-Sik;Kang, Mi-Sook
    • Bulletin of the Korean Chemical Society
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    • v.28 no.4
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    • pp.581-588
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    • 2007
  • To enhance the photodecomposition of concentrated ammonia into N2, Pt/V-TiO2 photocatalysts were prepared using solvothermal and impregnation methods. Nanometer-sized particles of 0.1, 0.5 and 1.0 mol% V-TiO2 were prepared solvothermally, and then impregnated with 1.0 wt% Pt. The X-ray diffraction (XRD) peaks assigned to V2O5 at 30.20 (010) and Pt metal at 39.80 (111) and 46.20 (200) were seen in the 1.0 wt% Pt/ 10.0 mol% V-TiO2. The particle size increased in the order: pure TiO2, V-TiO2 and Pt/V-TiO2 after thermal treatment at 500 °C, while their surface areas were in the reverse order. On X-ray photoelectron spectroscopy (XPS), the bands assigned to the Ti2p3/2 and Ti2p1/2 of Ti4+-O were seen in all the photocatalysts, and the binding energies increased in the order: TiO2 < Pt/V-TiO2 < V-TiO2. The XPS bands assigned to the V2p3/2 (517.85, 519.35, and 520.55 eV) and V2p1/2 (524.90 eV) in the V3+, V4+ and V5+ oxides appeared over V-TiO2, respectively, while the band shifted to a lower binding energy with Pt impregnation. The Pt components of Pt/ V-TiO2 were identified at 71.60, 73.80, 75.00 and 76.90 eV, which were assigned to metallic Pt 4f7/2, PtO 4f7/2, PtO2 4f7/2, and PtO 4f5/2, respectively. The UV-visible absorption band shifted closer towards the visible region of the spectrum in V-TiO2 than in pure TiO2 and; surprisingly, the Pt/V-TiO2 absorbed at all wavelengths from 200 to 800 nm. The addition of vanadium generated a new acid site in the framework of TiO2, and the medium acidic site increased with Pt impregnation. The NH3 decomposition increased with the amount of vanadium compared to pure TiO2, and was enhanced with Pt impregnation. NH3 decomposition of 100% was attained over 1.0 wt% Pt/1.0 mol% V-TiO2 after 80 min under illumination with 365 nm light, although about 10% of the ammonia was converted into undesirable NO2 and NO. Various intermediates, such as NO2, -NH2, -NH and NO, were also identified in the Fourier transform infrared (FT-IR) spectra. From the gas chromatography (GC), FT-IR and GC/mass spectroscopy (GC/MS) analyses, partially oxidized NO and NO2 were found to predominate over V-TiO2 and pure TiO2, respectively, while both molecules were reduced over Pt/V-TiO2.

Selective Production of Monomeric Phenols from Lignin via Two-step Catalytic Cracking Process (2단계 촉매 분해공정을 이용한 리그닌 유래 선택적 페놀화합물 생산)

  • Kim, Jae-Young;Heo, Sujung;Park, Shin Young;Choi, In-Gyu;Choi, Joon Weon
    • Journal of the Korean Wood Science and Technology
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    • v.45 no.3
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    • pp.278-287
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    • 2017
  • In this study, lignin was efficiently degraded via two-step catalytic cracking process and lignin-oil, char, and gas was produced as lignin degraded products. Three kinds of catalysts (MgO, CaO, and Pt/C) were used in first catalytic cracking step and the highest lignin-oil yield (76.2 wt%) was obtained in Pt/C catalyst with the smallest char formation (4.1 wt%). GC-MS/FID analysis revealed that 18 kinds of monomeric phenols existed in lignin-oil and sum of them was the highest in Pt/C condition (97.8 mg/g lignin). Meanwhile, relatively lower yield of monomeric phenols was produced in MgO and CaO condition because of their absorption on catalysts. Lignin-oil produced over Pt/C was introduced to second catalytic cracking process with porous Pd/activated carbon aerogel catalyst. From this process, four kinds of monomeric phenols such as 4-ethylguaiacol, 4-propylguaiacol, 4-ethylsyringol, 4-propylsyringol were selectively produced at 0.89 - 1.82 wt% level.

Characteristics of Formaldehyde Emission from Small Gasoline Engine and Its Reduction Technology (소형 가솔린엔진의 포름알데히드 배출특성 및 저감법에 관한 연구)

  • Choi, B.C.;Lee, N.S.
    • Journal of Power System Engineering
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    • v.3 no.2
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    • pp.20-25
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    • 1999
  • Experiments were carried out to investigate the characteristics of formaldehyde emission from the small gasoline engine and its reduction technologies. Catalytic converters used are Pt/Rh, Pd/Rh, Pd/Pt, $62cell/cm^2$ monolith type. The measurement of formaldehyde was conducted by using the method of DNPH-GC. From the experimental results, formaldehyde emission increased in a lean mixture due to incomplete combustion of the hydrocarbons. The order of catalytic activity of formaldehyde oxidation was Pt/Rh > Pd/Rh > Pd/Pt. As the distance from the exhaust manifold to the inlet of the catalyst became far, in spite of lower catalyst temperature, formaldehyde concentration decreased because of the adsorption of formaldehyde.

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Enhanced Electrocatalytic Activity of Platinized Carbon Electrode via NaBH4 Treatment (NaBH4 화학적 처리를 통한 백금화 카본 전극의 촉매반응 향상)

  • Yun, Changsuk;Hwang, Seongpil
    • Applied Chemistry for Engineering
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    • v.31 no.5
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    • pp.581-584
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    • 2020
  • The effect of a chemical pretreatment on the surface carbon was investigated using a scanning electron microscope (SEM) and electrochemical methods. Primitive carbon has a reducing power likely due to incompletely oxidized functional groups on the surface. We aim to control this reducing power by chemical treatment and apply for the spontaneous deposition of nanoparticles (NPs). Highly ordered pyrolytic graphite (HOPG) was initially treated with a reducing agent, NaBH4 or an oxidizing agent, KMnO4, for 5 min. Subsequently, the pretreated carbon was immersed in a platinum (Pt) precursor. Unexpectedly, SEM images showed that the reducing agent increased spontaneous PtNPs deposition while the oxidizing agent decreased Pt loading more as compared to that of using bare carbon. However, the amount of Pt on the carbon obviously decreased by NaBH4 treatment for 50 min. Secondly, spontaneous reduction on pretreated glassy carbon (GC) was investigated using the catalytic hydrogen evolution reaction (HER). GC electrode treated with NaBH4 for a short and long time showed small (onset potential: -640 mV vs. MSE) and large overpotential for the HER, respectively. Although the mechanism is unclear, the electrochemistry results correspond to the optical data. As a proof-of-concept, these results demonstrate that chemical treatments can be used to design the shapes and amounts of deposited catalytic metal on carbon by controlling the surface state.

Determination of Survival of Gastric Cancer Patients With Distant Lymph Node Metastasis Using Prealbumin Level and Prothrombin Time: Contour Plots Based on Random Survival Forest Algorithm on High-Dimensionality Clinical and Laboratory Datasets

  • Zhang, Cheng;Xie, Minmin;Zhang, Yi;Zhang, Xiaopeng;Feng, Chong;Wu, Zhijun;Feng, Ying;Yang, Yahui;Xu, Hui;Ma, Tai
    • Journal of Gastric Cancer
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    • v.22 no.2
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    • pp.120-134
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    • 2022
  • Purpose: This study aimed to identify prognostic factors for patients with distant lymph node-involved gastric cancer (GC) using a machine learning algorithm, a method that offers considerable advantages and new prospects for high-dimensional biomedical data exploration. Materials and Methods: This study employed 79 features of clinical pathology, laboratory tests, and therapeutic details from 289 GC patients whose distant lymphadenopathy was presented as the first episode of recurrence or metastasis. Outcomes were measured as any-cause death events and survival months after distant lymph node metastasis. A prediction model was built based on possible outcome predictors using a random survival forest algorithm and confirmed by 5×5 nested cross-validation. The effects of single variables were interpreted using partial dependence plots. A contour plot was used to visually represent survival prediction based on 2 predictive features. Results: The median survival time of patients with GC with distant nodal metastasis was 9.2 months. The optimal model incorporated the prealbumin level and the prothrombin time (PT), and yielded a prediction error of 0.353. The inclusion of other variables resulted in poorer model performance. Patients with higher serum prealbumin levels or shorter PTs had a significantly better prognosis. The predicted one-year survival rate was stratified and illustrated as a contour plot based on the combined effect the prealbumin level and the PT. Conclusions: Machine learning is useful for identifying the important determinants of cancer survival using high-dimensional datasets. The prealbumin level and the PT on distant lymph node metastasis are the 2 most crucial factors in predicting the subsequent survival time of advanced GC.

Development of Simultaneous Quantification Method of Phenylalkylamines in Oral Fluid (타액 중 페닐알킬아민유도체류의 일제분석법 확립)

  • Choi, Hye-Young;Baeck, Seung-Kyung;Jang, Moon-Hee;Choi, Hwa-Kyung;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.55 no.2
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    • pp.145-153
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    • 2011
  • A simultaneous detection and quantification method for determining the Phenylalkylamine derivatives, such as methamphetamine (MA), amphetamine (AM), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), ketamine (KT), norketamine (NKT), phentermine (PT), fenfluramine (FFA) and phenmetrazine (PM), in oral fluid was developed and validated according to international guidelines. The validated method was applied to actual oral fluid samples collected from drug abuse suspects. The recovery of phenylalkylamines from oral fluid collection devices was also assessed. Oral fluid specimens from 20 drug abuse suspects submitted by the police were collected using Salivette$^{TM}$, Quantisal$^{TM}$ or direct expectoration. The samples were screened using a biochip array analyzer. For confirmation, the samples were analyzed by GC-MS in selected-ion monitoring (SIM) mode after extraction using automated SPE with a mixed-mode cation exchange cartridge and derivatization with trifluoroacetic anhydride (TFAA). The results from the immunoassay were consistent with those from GC-MS. All the oral fluid samples gave positive results for MA, AM, PT and/or PM. The detection of phenylalkylamines in oral fluid can provide a better indication of recent use than urine or hair. Therefore, the oral fluid specimen was useful for demonstrating phenylalkylamines abuse in the driving under the influence of drug (DUID) as an alternative specimen for urine.

Development and validation of a qualitative GC-MS method for methamphetamine and amphetamine in human urine using aqueous-phase ethyl chloroformate derivatization

  • Kim, Jiwoo;Sim, Yeong Eun;Kim, Jin Young
    • Analytical Science and Technology
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    • v.33 no.1
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    • pp.23-32
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    • 2020
  • Methamphetamine (MA) is the most common and available drug of abuse in Korea and its primary metabolite is amphetamine (AP). Detection of AP derivatives, such as MA, AP, phentermine (PT), MDA, MDMA, and MDEA by the use of immunoassay screening is not reliable and accurate due to cross-reactivity and insufficient specificity/sensitivity. Therefore, the analytical process accepted by most urine drug-testing programs employs the two-step method with an initial screening test followed by a more specific confirmatory test if the specimen screens positive. In this study, a gas chromatography-mass spectrometric (GC-MS) method was developed and validated for confirmation of MA and AP in human urine. Urine sample (500 µL) was added with N-isopropylbenzylamine as internal standard and ethyl chloroformate as a derivatization reagent, and then extracted with 200 µL of ethyl acetate. Extracted samples were analysed with GC-MS in the SIM/ Scan mode, which were screened by Cobas c311 analyzer (Roche/Hitachi) to evaluate the efficiency as well as the compatibility of the GC-MS method. Qualitative method validation requirements for selectivity, limit of detection (LOD), precision, accuracy, and specificity/sensitivity were examined. These parameters were estimated on the basis of the most intense and characteristic ions in mass spectra of target compounds. Precision and accuracy were less than 5.2 % (RSD) and ±14.0 % (bias), respectively. The LODs were 3 ng/mL for MA and 1.5 ng/mL for AP. At the screening immunoassay had a sensitivity of 100% and a specificity of 95.1 % versus GC-MS for confirmatory testing. The applicability of the method was tested by the analysis of spiked urine and abusers' urine samples.