• Title/Summary/Keyword: 크로마토그래피

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Determination of Sulfur Compounds in Gaseous Fuel by Gas Chromatography-Sulfur Chemiluminescence Detection (GC-SCD를 이용한 가스연료 중 황화합물의 정량)

  • Do, Lee Joo;Koh, Jae Suk;Kim, Ho Jin
    • Journal of the Korean Chemical Society
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    • v.43 no.5
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    • pp.517-521
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    • 1999
  • Gas chromatography using sulfur chemiluminescence detection (GC-SCD) which exhibits very good selectivity, linearity, and sensitivity was applied to the analysis of suIfur compounds in gaseous fuel. The expectmental method used in this study was to resolve the problems of repeatability and reproducibility by means of the adsorption of sulfur compounds, which is different from the existing analysis method of these compounds by GC-SCD. The calibration curves of the standard gases including dimethyl sulfide, t-butylmercaptan and ethyl methyl sulfide exhibited an excellent linearity. As the result of precision tests for the above three compounds, the high reproducibility for tests showed while repeating three times during four days, respectively. In addition, the coefficient of variation was less than 3%. In consequence, the expectmental method of this study is very effective not only with low uncertainty but also with better accuracy, which can quickly determine the concentration of gas odorants in LPG (Liquefied Petroleum Gas) from oil reservoirs and filling stations.

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GC/MS Analysis of Ethylene Glycol in the Contaminated Lubricant Oil Through Solvent Extraction Followed by Derivatization using Bistrimethylsilyltrifluoroacetamide (BSTFA) (엔진윤활유 중 Ethylene Glycol의 용제추출후 bistrimethylsilyltrifluoroacetamide(BSTFA)를 이용한 GC/MS 분석에 관한 연구)

  • Lee, Joon-Bae;Kwon, O-Seong;You, Jae-Hoon;Shon, Shungkun;Sung, Tae-Myung;Paeng, Ki-Jung
    • Tribology and Lubricants
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    • v.28 no.6
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    • pp.315-320
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    • 2012
  • For proper functioning, general machines usually need lubricant oil as a cooling, cleaning, and sealing agent at points of mechanical contact. The quality of lubricant oil can deteriorate during operation owing to various causes such as high temperature, combustion products and extraneous impurities. In this study, a heavy load stopped during operation, and the oil was analyzed to check whether any impurities were added. Extraction using acetonitrile followed by reaction with BSTFA(bistrimethylsilyl trifluoroacetamide) showed that, trimethylsilylated ethylene glycol was present in the lubricant oil. To quantify the ethylene glycol in the oil, deuterium-substituted ethylene glycol, which acted as an internal standard, was added to the sample and then extracted with the solvent. Next, the extract was reacted with the derivatizing agent(BSTFA) and then analyzed with GC/MS. The detection limit of this method was found to be $0.5{\mu}g/g$ and the recovery of oil containing $20,000{\mu}g/g$ of ethylene glycol was measured to be 94.8%. A damaged O-ring and eroded cylinder liner were found during the overhaul, which implied the leakage of coolant containing ethylene glycol into the lubricating system. The erosion of the cylinder liner was assumed to be due to cavitation of the coolant in the cooling system.

Effects of Steeping on Physicochemical Properties of Waxy Rice (수침이 찹쌀의 이화학적 성질에 미치는 영향)

  • Kim, Kwan;Lee, Yong-Hyun;Kang, Kil-Jin;Kim, Sung-Kon
    • Korean Journal of Food Science and Technology
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    • v.25 no.5
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    • pp.535-540
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    • 1993
  • Effects of steeping of waxy rice in water at $20^{\circ}C$ for 6 or 30 hr on physicochemical properties of rice flour and molecular structure of starch were examined. pH of the steep water was decreased upon steeping. The lightness of the flour was gradually increased, while redness and yellowness were decreased as steeping time increased. The protein content was linearly decreased during steeping period. The fat content was sharply decreased from 18hr of steeping. The ash content rapidly decreased up to 12hr of steeping. The water-binding capacity was increased up to 12hr of steeping and decreased thereafter. The swelling power at $80^{\circ}C$ was consistently increased during steeping period. The amylograph peak viscosity showed a linear relationship with the steeping time. The molecular structure of starch was not affected by steeping.

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Thermostability of Polygalacturonase from Chinese Cabbage (배추 Polygalacturonase의 열안정성)

  • Cheong, Tae-Kyou;Moon, Tae-Wha;Park, Kwan-Hwa
    • Korean Journal of Food Science and Technology
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    • v.25 no.5
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    • pp.576-581
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    • 1993
  • Polygalacturonase(PG) was extracted from Chinese cabbage and partially purified by ammonium sulfate fractionation and ion-exchange chromatography. Three fractions, D-PG, C-1 PG, and C-2 PG, were separated by CM-Sephadex C-25 column chromatography and FPLC Mono Q HR 5/5 or Mono S HR 5/5 column and their physicochemical characteristics were investigated. All three fractions had optimum pH and temperature of 4.5 and $65^{\circ}C$, and were stable in the range of pH $4.5{\sim}8.0$. These fractions were inhibited by 0.8mM $CaCl_2$ or 0.6M NaCl. In the thermal inactivation of PC isozymes at $65{\sim}80^{\circ}C$, z-values were $8.4{\sim}9.3^{\circ}C$ and D-values at $80^{\circ}C$ were In the range of $120{\sim}126s$. Thermodynamic constants were calculated from thermal inactivation data of the isozymes and were applicable to estimation of thermal process time of retort pouched Kimchi.

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Studies on the Composition and Chemical Structure of Desmethylsterols from Torreya nucifera Seeds (비자(榧子)의 Desmethylsterol 조성(組成) 및 구조(構造)에 관한 연구(硏究))

  • Joh, Yong-Goe;Kim, Kyeng-Ja;Bark, Kui-Sun;Jeong, Tae-Myung
    • Korean Journal of Food Science and Technology
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    • v.13 no.2
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    • pp.127-132
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    • 1981
  • Studies on the physico-chemical properties of acetone-solubles from Torreya nucifera seeds, the composition, and chemical structure of desmethylsterol from the lipids are summarized as follows; 1. The acetone-soluble lipids and moisture content of Torreya nucifera seeds amounted to 46.6% and 9.3%, respectively. 2. The unsaponifiable content, iodine value, and saponification value of the lipids were 0.3%, 122 and 189.3, respectively. 3. The desmethylsterols comprised three components, whose Rrts (1.5% OV-17 to ${\beta}$-sitosterol) corresponded to 1.09 (trace), 1.16 (trace) and 1.33 (98%). 4. From IR, mass and NMR spectrometric features, the prominent desemethylsterol appears to be 24(?)-ethylcholesta-5-en-3${\beta}$-ol.

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Studies on Biological Activity of Wood Extractives(V) - Identification of Flavonoids from the Heartwood of Larix leptolepis and Their Antioxidative Activities - (수목추출물의 생리활성에 관한 연구(V) - 일본잎갈나무 심재부의 플라보노이드 성분 분리 및 항산화활성 -)

  • Yoon, Sun-Young;Lee, Hak-Ju;Lee, Sung-Suk;Choi, Don-Ha;Paik, Ki-Hyon
    • Journal of the Korean Wood Science and Technology
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    • v.28 no.3
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    • pp.78-84
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    • 2000
  • Two flavanones and one flavone were isolated from the diethylether soluble fraction of ethanol extract of Larix leptolepis heartwood. These compounds were identified 3,3',4',5,7-pentahydroxyflavanone(taxifolin), 3,4',5,7-tetrahydroxyflavanone(aromadendrin) and 3,3',4',5,7-pentahydroxyflavone(quercetin) by instrumental analyses using UV, IR, MS and NMR spectrometries. Antioxidative activies of these compounds were investigated by 1,1-diphenyl-2-picrylhydrazyl(DPPH) free radical scavenging activity. Quercetin and taxifolin indicated high free radical scavenging activities compared to ${\alpha}$-tocopherol and BHT(butylated hydroxytoluene).

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Determination of Stereochemical Structure of a Grandidentatin Isomer from Populus alba × glandulosa Bark (현사시나무 수피에서 분리한 Grandidentatin Isomer의 입체구조결정)

  • Kwon, Dong-Joo;Kim, Hyun-Seok;Lee, Phil-Ho;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.37 no.1
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    • pp.114-120
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    • 2009
  • The bark of Populus alba ${\times}$ glandulosa was collected, air-dried and extracted with 70% aqueous acetone. Then it was successively partitioned with n-hexane, $CH_2Cl_2$, EtOAc and $H_2O$. Repeated Sephadex LH-20 column chromatography and preparative TLC on the EtOAc soluble fraction gave a grandidentatin isomer. The structure was elucidated as grandidentatin A (cis-2-hydroxycyclohexyl 6-O-p-coumaroyl-${\beta}$-D-glucopyranoside) on the basis of spectroscopic evidences such as $^1H$-NMR, $^{13}C$-NMR, 2D-NMR and MALDI TOF-MS spectrum followed by acid hydrolysis. Grandidentatin A was identified here for the first time in Populus alba ${\times}$ glandulosa bark, and to the bset of our knowledge it has not been reported in any other literature.

A Comparison Study of Radiostrontium Chelation with Chitin, Chitosan, EDTA and DTPA (카이틴, 카이토산, EDTA, DTPA의 방사성스트론튬(Sr-85) 착화물 형성에 관한 비교 연구)

  • Bom, Hee-Seung;Kim, Young-Ho;Kim, Ji-Yeul
    • The Korean Journal of Nuclear Medicine
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    • v.32 no.4
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    • pp.391-395
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    • 1998
  • Purpose: Chitin and chitosan are nontoxic natural chelators that chelate radiostrontium effectively. The purpose of this study was to compare radiostrontium chelation of chitin and chitosan with that of well known chemical chelators, namely EDTA and DTPA. Materials and Methods: The chelaton rates of chitin, chitosan, EDTA and DTPA were compared using a column chromatography method (Sephadex G-25M, Sweden). Three kinds of chitins and four kinds of chitosans were used. All of them were water soluble. Results: Phosphated chitosan showed the highest chelation yield of 97% at pH 7. All of chitins, chitosans, EDTA and DTPA showed chelation yield of more than 90% independent of varing pH level. Conclusion: Chitin and chitosan have similar chelation rate as compared with EDTA and DTPA.

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Exposure to Styrene in the Lamination Processes with Fiberglass-Reinforced Plastics: Health Diagnosis Case Report (유리섬유강화 플라스틱을 이용한 적층공정 근로자들의 스티렌 노출 평가: 보건진단 사례)

  • Choi, Sangjun;Jeong, Yeonhee
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.25 no.2
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    • pp.126-133
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    • 2015
  • 연구목적: 이 연구는 노동부의 보건진단 명령에 의해 유리섬유 강화플라스틱(FRP)을 이용한 이중벽 탱크 제조 사업장의 적층 공정 근로자들을 대상으로 스티렌 노출 특성을 평가하기 위해 수행되었다. 연구방법: 스티렌의 주요발생원 파악을 위해 불포화 폴리에스테르 수지(UPR), 경화제, 조색제, 세척액 등의 원료 내 스티렌 함유량을 가스크로마토그래피 질량분석기(GC-MS)를 이용하여 분석하였다. FRP 적층 공정에 근무하는 작업자들을 대상으로 NIOSH 1501 공정시험법에 의해 공기 중 스티렌 노출 농도에 대한 개인노출 평가를 실시하였고, 생물학적 노출 지표로 뇨 중 만델릭산을 채취한 후 고성능액체크로마토그래피(HPLC)로 분석하였다. 또한 각 직무 특성과 단위작업 중심으로 스티렌에 대한 단시간 노출평가를 수행하였다. 연구결과: 스티렌의 함유량이 가장 많은 주요 원료는 중량비율로37%의 스티렌이 함유된 UPR이었다. 적층 공정의 FRP분무 작업자와 보조 작업자들 모두 스티렌의 8시간 가중평균 노출기준(20 ppm)을 초과하였다. 단시간 노출평가 결과 FRP분무 작업자의 경우 45.9 ppm에서 86.1 ppm 수준으로 FRP를 사용하지 않는 작업보다 통계적으로 유의하게 높은 수준이었다(P<0.01). 가장 높은 수준의 스티렌에 노출되는 단위작업은 FRP를 이용하여 1차 코팅 하는 작업으로 특별한 관리가 필요하였다. 결론: 보건진단을 위해 실시한 이중벽 탱크 제조 사업장의FRP 적층 공정 작업자의 스티렌 노출수준은 노출기준을 초과할 정도로 높은 수준이었다. 그러나 탱크를 천장에 매달고 돌리면서 적층작업을 수행하기 때문에 적절한 국소환기 시스템을 구축하는데 어려움이 있다. 따라서 적절한 방독마스크 착용으로 스티렌 노출 예방이 필요하였다.

Failure Analysis on Scale Formation of Thermostat Housing and Development of Accelerated Test Methodology (써모스타트 하우징의 침전물 생성에 관한 고장분석 및 가속시험법 개발)

  • Cho, In-Hee;Hyung, Sin-Jong;Choi, Kil-Yeong;Weon, Jong-Il
    • Applied Chemistry for Engineering
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    • v.20 no.2
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    • pp.177-185
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    • 2009
  • The failure analysis of scales deposited on automotive thermostat housing has been carried out. Observations using energy dispersive spectroscopy and electron probe micro analyzer indicate that the main components of scales are some of additives of coolant used. For a detailed investigation of organic matters pyrolysis-GC/MS is employed. The result shows that the main organic component is benzoic acid and furthermore, a small amount of acetophenone, benzene and phenyl group is detected. Based on the results of failure analysis performed, the scales on automotive thermostat housing appear due to the deposition of coolant components, followed by crevice corrosion, into gap between housing and rubber horse. New accelerated test methodology, which could mimic the scale formation and the crevice corrosion on thermostat housing, is developed considering the above results. In order to reproduce the real operating conditions, the accelerating factors, i.e. temperature and humidity, are changed and programmed. The reproducibility of the accelerated test proposed is confirmed after analyzing the scales obtained from the accelerated test.