• Title/Summary/Keyword: Packed-capillary

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Gas-chromatographic determination of methylthiohydantoin amino acid as N(O)-butyldimethylsilyl derivatives in amino acid sequencing with methylisothiocyanate (Methylisothiocyanate를 이용한 아미노산 배열결정시 N(O)-butyldimethylsilyl 유도체로서의 methylthiohydantoin 아미노산의 기체 크로마토그래피에 의한 분석)

  • Woo, Kang-Lyung
    • Applied Biological Chemistry
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    • v.35 no.2
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    • pp.132-138
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    • 1992
  • For effective determination of methylthiohydantoin amino acids(MTHs) by gas liquid chromatography in the protein sequencing, derivatization with N-methyl-N-(tert.-butyl-dimethylsilyl)trifluoroacetamide(MTBSTFA), a new silylating reagents, was attempted instead of trimethylsilyl(TMSi) derivatives by N,O-bis(trimethylsilyl)trifluoroacetamide(BSTFA) used up to the present and N(O)-butyldimethylsilyl MTHs derivatized by MTBSTFA were analysed on HP-1 capillary column. Twenty one protein amino acids except cystine were indentified. Especially arginine that did not detected with TMSi derivative on packed column until now was resolved by derivatization with MTBSTFA. N(O)-butyldimethylsilyl MTHs showed multiple peaks by MTBSTFA were proline, isoleucine, glycine and tyrosine and hydroxyproline especially showed several extraneous peaks more than two. Calibration curves of N(O)-butyldimethysilyl MTHs of amino acids in the range of $2.5\;nmol{\sim}7.5\;nmole$ showed good linearity. however, those of lysine, histidine and arginine showed linearity in the range of $5.0\;nmole{\sim}15.0\;nmole$. Correlation coefficients and regression coefficients of all calibration curves were highly significant(p<0.001).

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Relative Anticipated Erythrocyte Sedimentation Rate of Cattle Blood, as Measured by 45 Degree-Angled Capillary Hematocrit Tube, for Ambient Temperature and PCV Value (소 혈액의 45도 경사 모세관에 의한 ESR측정에 있어서 환경온도 및 PCV에 상관하는 관계적 예기ESR치)

  • Lee, Bang-whan
    • Korean Journal of Veterinary Research
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    • v.27 no.2
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    • pp.339-345
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    • 1987
  • Each of twenty blood samples taken from apparently healthy Korean Cows was used to produce five different mixtures of autologous plasma and blood corpuscles such that their values of packed cell volume (PCV) lay between 10 to 50ml/l00ml. The measurements of erythrocyte sedimentation rate (ESR) using 45 degree-angled capillary hematocrit tube, 1.1-1.2mm bore, ($45^{\circ}-micro-ESR$) were practised for the blood of various levels of PCV under the ambient temperature of ${10^{\circ}C}$, ${20^{\circ}C}$ and ${30^{\circ}C}$. Correlation of ESR to ambient temperature showed linear regression each in five levels of PCV. ESR increased with ascending ambient temperature, and magnitude of the increase of ESR became greater as the level of PCV lowered. Correlation of ESR, of which values were transformed by the linear regression equation correlated to ambient temperature to PCV showed curvilinear regression each in three levels of ambient temperature, and ESR was increased with decreasing PCV. The data were statistically analysed and a list of relative anticipate $45^{\circ}-micro-ESR$ values for PCV and ambient temperature was presented.

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Immobilization of Styrene-acrylamide Co-polymer on Either Silica Particles or Inner Surface of Silica Capillary for the Separation of D-Glucose Anomers

  • Ali, Faiz;Kim, Yune Sung;Cheong, Won Jo
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.539-545
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    • 2014
  • Styrene-acrylamide co-polymer was immobilized on porous partially sub-$2{\mu}m$ silica monolith particles and inner surface of fused silica capillary ($50{\mu}m$ ID and 28 cm length) to result in ${\mu}LC$ and CEC stationary phases, respectively, for separation of anomeric D-glucose derivatives. Reversed addition-fragmentation transfer (RAFT) polymerization was incorporated to induce surface polymerization. Acrylamide was employed to incorporate amide-functionality in the stationary phase. The resultant ${\mu}LC$ and CEC stationary phases were able to separate isomers of D-glucose derivatives with high selectivity and efficiency. The mobile phase of 75/25 (v/v) acetonitrile (ACN)/water with 0.1% TFA, was used for HPLC with a packed column (1 mm ID, 300 mm length). The effects of pH and ACN composition on anomeric separation of D-glucose in CEC have been examined. A mobile phase of 85/15 (v/v) ACN/30 mM sodium acetate pH 6.7 was found the optimized mobile phase for CEC. The CEC stationary phase also gave good separation of other saccharides such as maltotriose and Dextran 1500 (MW~1500) with good separation efficiency (number of theoretical plates ~300,000/m).

A Study of the Development of Liquid-liquid Static Contactor Using Capillary Phenomena Induced by Highly Packed Fiber Bundle and its Characteristics (고밀집 섬유 집합체에 의해 유도된 모세관 현상을 이용한 정적 액-액 접촉장치의 개발과 그 특성 연구)

  • Kim, Kwang-Wook;Byeon, Kee-Hoh;Lee, Eil-Hee;Yoo, Jae-Hyung;Park, Hyun-Soo
    • Applied Chemistry for Engineering
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    • v.7 no.4
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    • pp.743-749
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    • 1996
  • A new static contractor using capillary phenomena induced by a highly packed fiber bundle was developed for the solvent extraction. When two immiscible phases being cocurrently and forcedly fed into the packed fiber bundle, the contactor brings about a very large liquid-liquid contact area for mass transfer within a small definite space without any turbulence and drop phenomena. In order to test the characteristics and stability of the static contractor system, continuous extraction experiments of TBP-uranyl ion-nitric acid system were done and compared with the batch extraction experiment of the same chemical system. The performance of the static contractor were the same as that of the ideal batch extractor with the same extraction condition. For the increase of the extraction yield by the contactor, the increase of organic flow rate was required at a fixed aqueous flow rate, and a certain residence time of the aqueous phase flow within the contactor system had to be maintained to meet the performance of the batch system of the same phase ratio. The residence time in the case of TBP-uranyl ion-nitric acid system was about 1.9 minutes. This system was confirmed to be effective and stable enough for purposes of the kinetic study of solvent extraction as well as the mutual separation and purification of ordinary materials because of good reproducibility and the stable and large static liquid-liquid contact area.

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Studies on Simultaneous Analysis of Organophosphorus Pesticide Residues in Crops by Gas-Liquid Chromatography (II). Separation of Pesticides by Capillary Column (기체-액체 크로마토그래피에 의한 농작물 중 유기인제 잔류농약의 동시 분석에 관한 연구 (제 2 보). 모세관 컬럼에 의한 분리)

  • Kim, Taek-Jae;Eo, Yun-Woo;Kim, Young-Sang
    • Journal of the Korean Chemical Society
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    • v.31 no.3
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    • pp.236-243
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    • 1987
  • The optimum resolution condition of 11 organophosphorus pesticides by gas-liquid chromatography was studied using a capillary column. The injection modes and types of vaporization tubes were evaluated in relation to pesticide analysis. The best reproducibility of peak heights of pesticides was obtained by the split mode with the vaporization tube packed with quartz wool. A 25m SE-30 capillary column provided better resolution than SE-54 column for their optimum resolution. The column at $200^{\circ}C$ initially was heated by $5^{\circ}C/min\;to\;230^{\circ}C$ followed by $10^{\circ}C/min\;to\;270^{\circ}C$ and the temperatures were held constant for 5 minutes at $230^{\circ}C\;and\;270^{\circ}C$, respectively. The relative standard deviations of their retention times were less than 0.19%.

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Indirect calculation for volume of packed red cell(VPRC) by means of erythrocyte sedimentation rate (ESR) of blood diluted with isotonic dextrose solution in cattle (소에 있어서 등장 dextrose액으로 희석한 혈액의 적혈구 침강율(ESR) 측정에 의한 적혈구 침층용적(VPRC)치의 간접계산법)

  • Lee, Bang-whan;Bahk, Young-woo;Min, Byeong-man
    • Korean Journal of Veterinary Research
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    • v.30 no.1
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    • pp.107-112
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    • 1990
  • The purpose of this study is to derive indirect values of volume of packed red cell(VPRC), without centrifugation, from erythrocyte sedimentation rate(ESR) of blood diluted with isotonic dextrose solution in cattle. Each of ten blood samples taken from apprently healthy Korean cows and Holstein cows was used to produce eight different mixture of autologous plasma and blood corpuscles such that their values of VPRC lay between 15 to 50ml/100ml, and then each of the blood mixture was again diluted with 5% dextrose solution. The measurements of ESR using 45 degree-angled capillary hematocrit tube, 1.1~1.2mm bore, ($45^{\circ}$-micro-ESR) were practised for the diluted blood of various levels of VPRC under the ambient temperature of $10^{\circ}$, $20^{\circ}$ and $30^{\circ}C$. Reliable values of VPRC on the basis of the correlating linear regressive equation to the ESR could be derived from the values of $45^{\circ}$-micro-ESR/hr in the mixture of one part of whole blood and one part of 5% dextrose solution(1:1). For an aid of practical use, authors suggested a list of the $45^{\circ}$-micro-ESR/hr values of the diluted blood equivalent to VPRC of whole blood.

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Simultaneous Analytical Method of Organochlorine and Pyrethroid Pesticides using GC(ECD) (GC-ECD를 이용한 유기염소계 밑 Pyrethroid계 농약 동시 분석법)

  • 김우성;이선화;김재이;정지윤;이명자;박영채;이영자;정성욱;이봉헌
    • Journal of Environmental Science International
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    • v.12 no.4
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    • pp.477-480
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    • 2003
  • Pesticides were extracted from samples with 70% acetone and methylene chloride in order, and then cleaned up via open-column chromatography apparatus packed with florisil, and finally analyzed simultaneously the organochlorine and pyrethroid pesticides using GC(ECD). An ultra-2 fused silica capillary column was used to separate and identify the products. The resolution between the last isomeric peak of cypermethrin(59.987min) and the first isomeric peak of flucythrinate(60.043min) was not satisfactory. The last isomeric peak of fenvalerate(62.344min) and the first isomeric peak of fluvalinate(62.397min) were overlapped. Recoveries of soybean sample fer the most pesticides were 73.3% to 102.4%. Detection limits were between 0.004 and 0.063 ${\mu}$g/mg when this method was used.

Development of Simultaneous Analytical Method for Various Residual Pesticides Using GC-ECD (GC-ECD를 이용한 잔류 농약 다성분 동시 분석법 개발)

  • 김우성;손영욱;정지윤;안경아;홍무기;임무혁;이홍재;이봉헌;박흥재
    • Journal of Environmental Health Sciences
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    • v.27 no.1
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    • pp.88-92
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    • 2001
  • The simultaneous analytical method for 37 residual pesticides was developed by a gas chromatography with $^{63}$ Ni electron capture detector. Pesticides added in soybean sample were extracted with 70% acetone in water and methylene chloride in oder, and then cleaned up via open-column apparatus packed with florisil and alumina N. The Ultra-2 fused capillary column was used to separate the products. The resolution between the last isomeric peak of cypermethrin (56.398 min) and the first isomeric peak of flucythrinate (56.421 min) was not satisfactory and the last isomeric peak of fenvalerate(58.783 min) and the first isomeric peak of fluvalinate(58.835 min) was overlapped. Except for $\alpha$-BHC, dichlofluanid, captan, and captafol, most recoveries were showed over 70%.

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Simultaneous Analysis of Multi-residual pesticides using GC/NPD (GC/NPD를 이용한 다성분 잔류농약의 동시분석)

  • 김우성;이선화;김상엽;정동윤;김재이;이영자;이홍재;정성욱;박흥재
    • Journal of Environmental Science International
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    • v.12 no.10
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    • pp.1117-1120
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    • 2003
  • Pesticides were extracted from samples with 70% acetone and methylene chloride in order, and then cleaned up via open-column chromatography apparatus packed with florisil, and finally analyzed simultaneously the organophosphorus pesticides using GC/NPD. Ultra-2 and Ultra-1 fused silica capillary columns were used to separate and identify the products. Recovery of most analytes from soybean sample, taken from pesticide residues well, was greater than(80%) for all except(6) analytes. This method can simultaneously determine multiple pesticides with a high degree of accuracy and precision.

Study on dryout heat flux of axial stratified debris bed under top-flooding

  • Wenbin Zou;Lili Tong;Xuewu Cao
    • Nuclear Engineering and Technology
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    • v.56 no.2
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    • pp.636-643
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    • 2024
  • The coolability of the debris bed with a simulant of solidified corium is experimentally studied, focusing on the effects of the structure of the axial stratified debris bed on the dryout heat flux (DHF). DHF was obtained for the four structures with different particle sizes for the axial stratified debris bed under top flooding. The experimental results show that the dryout position of the axial stratified debris bed is formed at the stratified interface indicated by the temperature rise, and the DHF of the axial stratified bed is much lower than that of the homogeneous bed packed with the upper small particles. To predict the dryout heat flux of the stratified debris beds, by considering the properties of the mixed area, a one-dimensional dryout heat flux model of the porous medium is derived from a water and vapor momentum equation for porous medium, two-phase permeability modifications, interfacial drag, and the correlation between capillary pressure and liquid saturation and verified with the experimental data. The modified model can give reasonable results under different structures.