• Title/Summary/Keyword: 가스크로마토그래피 /질량분석기

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Material Analysis and Conservation Treatment of Sangryangmun in Jinnamgwan, Yeosu (여수 진남관 상량문의 재질분석 및 보존처리)

  • Imn, Se Yeon;Yu, Ji A;Lee, Jae Sung;Jeong, Hee Won
    • Journal of Conservation Science
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    • v.36 no.3
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    • pp.213-224
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    • 2020
  • This research conducted a component analysis and conservation treatment of "Sangryangmun," a material which had been written in 1965 and was discovered during the repair project for "Jinnamgwan" in Yeosu. The "Sangryangmun" has been stored in a cylindrical metal storage; however, defects, discolorations, hardening, and damages caused by pollutants were found. Based on the XRF analysis, rust in the cylindrical metal storage, which was made of Cu, was stuck on the surface of the "Sangryangmun". Using FT-IR and Pyrolysis-GC/MS analyses, carbonyl and compounds of fatty acids were detected; the organic material on the surface of the "Sangryangmun" was identified to have belonged to oil-based components. Therefore, it was presumed that the bast fibers of a mulberry was used in the paper. To determine the conservation materials, component analysis, condition survey, and preliminary test on adhesives were conducted. Moreover, the missing parts and partial linings were filled using mulberry-fiber paper, methyl cellulose, etc.

Analysis of all PCB Congeners in Air Samples by HRGC/HRMS (대기 시료 중 PCBs 전 이성체 분석에 관한 연구)

  • Kim, Kyoung-Soo;Song, Byung-Joo;Kim, Jong-Guk
    • Analytical Science and Technology
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    • v.16 no.4
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    • pp.309-319
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    • 2003
  • This study was performed to describe analysis method of 209 PCB congeners in ambient air samples. The samples were collected by high volume air sampler in Chonju city. Extracted samples were cleaned by silicagel cleanup modified with sulfuric acid and activated carbon cleanup processing. The cleaned samples were analyzed by high resolution gas chromatography and high resolution mass spectrometry (HRGC/HRMS) with DB-5 column (60 m, 0.25 mm i.d., 0.25 m film thickness) to analyze the 209 kinds of PCB congeners. PCBs levels of air samples were detected to the range between 0.003 and $0.163pg-TEQ/m^3$. The PCBs congener of 162 kinds were detected in samples analysed using DB-5 column and 37 kinds peaks were overlapped with congeners more than one. It is difficult to isolate PCB 118/106 and PCB 105/127 in coplanar PCB, so it is likely to overestimate the concentration.. The distribution of coplanar-PCB congeners in origin source samples (Kanechlor and exhaust gas from incinerator) was compared with that in air samples, and PCB 81, PCB 77, PCB 126, and PCB 169 were higher in incinerator samples.

Determination of Additives Content in Aviation Turbine Fuel Using Multi-dimensional GC-MS (Multi-dimensional GC-MS를 이용한 항공터빈유의 첨가제 분석)

  • Youn, Ju Min;Jang, Yoon Mi;Yim, Eui Soon;Kim, Seong Lyong;Kang, Yong
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.4
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    • pp.1260-1268
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    • 2018
  • To improve fuel performance and specific characteristics of long storage and moving through fuel systems additives should be added in kerosene type aviation turbine fuel (AVTUR) such as antioxidant, fuel system icing inhibitor (FSII), electric conductivity improvers and so on. The dosage of additives has to be analyzed qualitatively and quantitatively due to inspect the quality of abnormal fuel and distinguish other petroleum products. Multi-dimensional GC-MS (MDGC-MS) with Deans switching technique are applied the determination of antioxidant and FSII, which are added with AVTUR containing complex mixture of hydrocarbons. Antioxidant and FSII in the range of 2.5-20 mg/L was quantitatively and qualitatively analyzed using MDGC-MS and the detection limit was about twice as low as that of the 1-dimensional GC-MS results. The method in this study has been higher peak resolution compared with GC-MS and could be simultaneously analyzed different two additives without sample pre-treatment.

Instrumental Analysis of Deposits on Paper Machine and Holes/Spots in Paper (제지공정 침착이물질 및 종이내 불순물 성분의 기기분석)

  • Ma, Geum-Ja;Lee, Bok-Jin
    • Applied Chemistry for Engineering
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    • v.9 no.1
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    • pp.135-140
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    • 1998
  • The constituents of deposits on paper machine and holes/spots in paper have been analyzed by a combination of analytical techniques, such as FTIR, Py-GC-MS, and EDS. FTIR spectroscopy was used prior to Py-GC-MS and EDS analysis, as a preliminary analysis. The analysis of organic components was carried out with a pyrolysis unit connected to a GC-MS, and inorganic components in ash were analyzed by SEM equipped with an EDS analyzer after pyrolysis at $590^{\circ}C$. The deposits on the dryer section were complex pitch, which was the mixture of the organic components of fatty acid ester and starch, and the inorganic components of talc, clay, and calcium carbonate. The complex pitch was estimated to come from the coated broke. We knew the deposits on the metering rod of sym-sizer were associated with the interaction of unstable alkyl keten dimer(AKD) and $CaCO_3$. The compositions of holes or spots varied considerably and were associated with chemical interaction within the system. The holes, spots, and blotches in the finished paper were PE and PP from pulp sources, complex pitch that were caused by the interaction of the different additives in the system, polymer such as flexible PVC that was used for the prop of palette, and hot melt as adhesives that came from the inadequate handling of broke. In addition, we identified that poly(caprolactam) which is used for forming fabrics or press felts, could be mixed with the raw materials by accident and results in streaks on coating.

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Evaluation of human exposure to polychlorinated biphenyls using human serum by congener-specific analysis (혈액 중 PCBs 이성질체별 분석에 의한 인체 노출 평가)

  • Park, Hyo-Keun;Lee, Se-Jin;Jin, Guang-Zhu;Kang, Jung-Ho;Baek, Song-E;Chang, Yoon-Seok
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.73-85
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    • 2006
  • Blood serum concentrations of polychlorinated biphenyls (PCBs) were measured in employees who worked at a municipal solid waste incinerator (MSWI), members of residential community who lived near the MSWI (<0.3km) and members of residential community lived far from the MSWI (>10 km). Human blood serum samples were analyzed for all PCB congeners using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS). The mean levels of total PCBs and dioxin-like PCBs in 87 serum samples were 242.77 ng/g lipid and 8.83 TEQ pg/g lipid, respectively. The PCB homologue profiles showed that penta-, hexa-, hepta-chlorinated biphenyls contributed more than 80% of the total PCBs concentration. The most abundant congeners were PCB153, PCB138, PCB180, PCB187, PCB118. A statistical analysis was performed to determine whether there were significant correlations between PCB concentrations and specific variables such as age, gender, smoking habits, occupation, BMI (Body Mass Index) and time of residence. As a result, the age was found to be strongly correlated with serum PCB concentrations. In addition, there were strong correlations between total PCBs and PCB153 (r=0.93, p<.0001), dioxin-like PCBs and PCB118 (r=0.98, p<.0001). So these two congeners are satisfactory indicators for total PCB concentrations and dioxin-like PCBs in human blood respectively.

Development of Rapid and Simple Drug Identification and Semi Quantitative Analytical Program by Gas Chromatography-Mass Spectrometry (가스크로마토그래피/질량분석기를 이용한 약물의 확인 및 간이 정량분석 프로그램 개발)

  • Kim, Eun-Mi;Han, Eun-Young;Hong, Hyo-Jeong;Jeong, Su-Jin;Choe, Sang-Gil;Rhee, Jong-Sook;Jung, Jin-Mi;Yeom, Hye-Sun;Lee, Han-Sun;Lee, Sang-Ki
    • YAKHAK HOEJI
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    • v.55 no.2
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    • pp.106-115
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    • 2011
  • Systematic toxicological analysis (STA) means the process for general unknown screening of drugs and toxic compounds in biological fluids. In order to establish STA, in previous study we investigated pattern of drugs & poisons in autopsy cases during 2007~2009 in Korea, and finally selected 62 drugs as target drugs for STA. In this study, rapid and simple drug identification and quantitative analytical program by gas chromatography-mass spectrometry(GC-MS) was developed. The in-house program, "DrugMan", consisted of modified chemstation data analysis menu and newly developed macro modules. Total 55 drugs among 62 target drugs were applied to this program, they were 14 antidepressants, 8 anti-histamines, 5 sedatives/hypnotics, 5 narcotic analgesics, 3 antipsychotic drugs, and etc. For calibration curves, fifty five drugs were divided into four groups of range considering their therapeutic or toxic concentrations in blood specimen, i.e. 0.05~1 mg/l, 0.1~1 mg/l, 0.1~5 mg/l or 0.5~10 mg/l. Standards spiked bloods were extracted by solid-phase extraction (SPE) with trimipramine-D3 as internal standard. Parameters such as retention times, 3 mass fragment ions, and calibration curves for each drug were registered to DrugMan. A series of identification, semi quantitation of target drugs and reporting the results were performed automatically. Calibration curves for most drugs were linear with correlation coefficients exceeding 0.98. Sensitivity rate of DrugMan was 0.90 (90%) for 55 drugs at the level of 0.5 mg/l. For standard spiked bloods at the level of 0.5 mg/l for 29 drugs, semi quantitative concentrations were ranged 0.36~0.64 mg/l by DrugMan. If more drugs are registered to database in DrugMan in further study, it will be useful tools for STA in forensic toxicology.

Estimation of Indicator PCBs Exposure in Infants via Breast-Feeding Period (수유기간에 따른 모유 중 Indicator PCBs 분석을 통한 영유아의 인체노출평가)

  • We, Sung-Ug;Yoon, Cho-Hee;Min, Byung-Yun
    • Journal of Korean Society of Environmental Engineers
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    • v.34 no.1
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    • pp.7-15
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    • 2012
  • The levels of indicator PCBs were determined in 132 human milk samples (Colostrum, 30th days after delivery, 60th days after delivery) collected in 2006 according to World Health Organization's (WHO) protocol. In addition, concentrations of indicator polychlorinated biphenyls (PCBs) were measured by the isotope dilution method with high resolution gas chromatograph/high resolution mass detector (HRGC/HRMS), which gave accurate and precise data for estimations of international trend and comparisons. Average daily intakes (ADIs) of all analytes were calculated. The median level of total indicator PCBs was 14 ng/g lipid, which is significantly lower than the level found in individuals from other countries. PCB congeners 138, 153 and 180 accounted for about 65% of the sum of the indicator congeners analyzed. The concentration of the most abundant PCB 153 is positively correlated with the concentration of the sum indicator PCBs (p<0.001). In this study, concentrations of total indicator PCBs significantly decreased with increasing number of children for a mother, indicating that parity and breast-feeding period an important role in the accumulation and elimination of these compounds in lactating women. The ADI for the median of total indicator PCBs for an infant was evaluated at $0.077{\mu}g/kg{\cdot}bw/day$ from birth to 6 months of age. The present study shows that concentrations of PCB 118 primipara breast milk have decreased 25~35 since 1998, and that this trend is continuing.

Determination of fuel marker in petroleum products using GC-MS (GC-MS를 이용한 석유제품 중의 식별제 분석)

  • Youn, Ju Min;Doe, Jin Woo;Yim, Eui Soon;Lee, Jung Min
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.4
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    • pp.1073-1080
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    • 2018
  • There are several types of petroleum products used for the fuel oil, according to their respective quality standards, grades and usage. Depending on the degree of oil tax rate by country, even the same petroleum products will have price gap. The illegal mixing of cheap petroleum products, which are subject to the lower tax rate, with relatively expensive transportation fuel causes problems such as tax evasion, environmental pollution and vehicle breakdown. In order to prevent illicit production and mixing of these different petroleum products, a small amount of markers are legally added to specific petroleum products. In Korea, markers are introduced and used to prevent illegal activity that kerosene used as fuel for house and commercial boiler are mixed with automotive diesel fuels, and marker contents are analyzed to use UV-Vis spectrophotometer and high performance liquid chromatography (HPLC). In this study, we have developed a method to qualitatively and quantitatively determine the marker added to petroleum products by gas chromatography-mass spectrometry (GC-MS) without adding developing reagent or sample pre-treatments.

Determination of fatty acid methyl esters (FAME) content in aviation turbine fuel using multi-dimensional GC-MS (Multi-dimensional GC-MS를 이용한 항공터빈유의 FAME 함량 분석)

  • Youn, Ju Min;Doh, Jin Woo;Hwang, In Ha;Kim, Seong Lyong;Kang, Yong
    • Journal of the Korean Applied Science and Technology
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    • v.34 no.4
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    • pp.717-726
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    • 2017
  • The current allowable cross-contamination level of fatty acid methyl esters (FAME) in aviation turbine fuel (AVTUR) is 50 mg/kg, due to that the presence of FAME in AVTUR can significantly impact the fuel supply system and jet engine. It has been difficult to analyze the level of FAME in AVTUR, since it is consisted of a lot of hydrocarbons. In this study, thus, a new method using multi-dimensional GC-MS (MDGC-MS) was proposed in order to determine the FAME level in AVTUR effectively. Applying to MDGC-MS with Deans switching system enabled us to detect and quantify the FAME with low carbon numbers such as those derived from coconut oil and palm kernel oil. The matrix effect of MDGC-MS method, which could shift the FAME peaks to slightly longer retention times, was reduced by 20 times compared with that of 1-dimensional GC-MS reference method. This developed method could be suitable for qualitative and quantitative analyses to determine the contamination level of trace FAME in AVTUR.

Synthesis of Long-Chain Unsaturated Acetates (장직쇄상(長直鎖狀) 불포화(不飽和) 초산화합물(醋酸化合物)의 합성(合成)에 관(關)한 연구(硏究))

  • Oh, Sung-Ki
    • Applied Biological Chemistry
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    • v.19 no.1
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    • pp.1-23
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    • 1976
  • The female moths of Lepidoptera comprising over 1,000,000 described species possess long-chain unsaturated alcohols or esters as the typical structure of potential sex attractants. In this experiment, various stereoisomers of $C_{16}-unsaturated$ acetates were synthesized for potential sex attractants; e.g., $CH_3(CH_2)_mCH=CH(CH_2)_nOR$ (m=0-12, n=1-13, R=H and $-COCH_3$). Seventeen acetates were spectrometrically examined so that the data would provide a ready catalog of gas chromatography and mass spectrometric data for comparison with natural insect sex attractants. Exclusively cis and trans isomers were obtained by the catalytic and chemical reduction methods, respectively. Commercially available $CH_3(CH_2)_mBr,\;CH_3(CH_2)_mC{\equiv}CH,\;HC{\equiv}C(CH_2)_nOH\;and\;HO(CH_2)_n\;OH$ were used for the synthetic starting material. 1-Alkynes, $CH_3(CH_2)_m\;C{\equiv}CH$ exceeding nine methylene groups did not condense with alkyl dihalides. The yield of coupling products was gradually decreased with increasing the molecular weight of diols. In the coupling reaction of $BrCH_2CH_2$ OTHP with acetylene gas, the tetrahydropyranyl ether of bromohydrin produced undesirable elimination product. In this experiment, it seems that p-toluenesulfonic acid is greatly favoured hydrolyzing agent over dilute sulfuric acid in the hydrolysis of the tetrahydropyranyl ether of long-chain alkynols.

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