• Title/Summary/Keyword: Dilute Phase

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Rapid Determination of Caffeine in Forensic Aqueous Sample by Dilute and Shoot LC-MS/MS (시료 희석 직접 주입 LC-MS/MS를 이용한 법화학 수용액 시료 중 카페인 신속 분석)

  • Choi, Yun Jeong;Kim, Hee Seung;In, Moon Kyo;Kim, Jin Young
    • YAKHAK HOEJI
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    • v.60 no.3
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    • pp.112-117
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    • 2016
  • A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of caffeine in forensic aqueous sample. The centrifuged sample ($100{\mu}l$) was diluted 50-fold with distilled water. The diluted sample ($400{\mu}l$) was then diluted further with $200{\mu}l$ of 0.1% formic acid solution and $400{\mu}l$ of acetonitrile containing 500 ng of caffeine-(3-methyl-$^{13}C_3$) prior to LC-MS/MS analysis. The mobile phase was composed of 0.1% formic acid in distilled water (A) and acetonitrile (B). Chromatographic separation was performed by using a Zorbax SB-C18 ($100mm{\times}2.1mm$ i.d., $3.5{\mu}m$) column and caffeine was eluted within 1.1 min. Linear least-squares regression with a 1/x weighting factor was used to generate a calibration curve with the coefficients of determination ($r^2=0.9983$). The lower limit of quantification was $25ng/ml$ for the analyte. The process efficiency was 98.6~100.1%. Intra- and inter-day precisions were not more than 2.1% and 1.7%, while intra- and inter-day accuracies were ranged from -6.8 to 4.5%, respectively. The suitability of the method was examined by analyzing unknown forensic aqueous samples.

Fluorescence Microscopy of Condensed DNA Conformations of Bacterial Cells

  • Suleymanoglu, Erhan
    • Journal of Microbiology
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    • v.40 no.4
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    • pp.319-326
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    • 2002
  • Cellular DNA in prokaryotes is organized in nucleic acid-protein self-assemblies referred to as the nucleoid. The physical forces responsible for its stability inside the poor solvent properties of the cytoplasm and their functional implications are not understood. Studies on the organisation and functioning of the cytosol of cells largely rely on experimental protocols performed in highly dilute solutions using biochemically purified molecules, which is not a reliable substitute for the situation existing in vivo. Our current research interest is focused on the characterization of biological and physical forces determining the compaction and phase separation of DNA in Escherichia coli cytoplasm. We have emphasized the effect of excluded volume in solutions with high macromolecular concentrations (macromolecular crowding) upon self-association patterns of reactions. The prokaryotic cytosol was simulated by addition of inert polymer polyethylene glycol (PEG) (average molecular weight 20000), as an agent which afterwards facilitates the self-association of macromolecules. Fluorescence microscopy was used for direct visualization of nucleoids in intact cells, after staining with DAPI (4',6-diamidino-2-phenylindole dihydrochloride). Addition of the crowding agent PEG 20,000, in increasing concentrations generated progressively enhanced nucleoid compaction, the effect being stronger in the presence of 0.2 M NaCl and 5 mM MgCl$\_$2/. Under these conditions, the nucleoids were compacted to volumes of around 2 ㎛$\^$3/ or comparable sizes with that of living cells.

Analysis of Carbendazim and Carbaryl by Micro-HPLC (Micro-HPLC에 의한 Carbendazim과 Carbaryl의 분석)

  • Choi, Kyoung-Sook;Lee, Hoe-Yeon;Lee, Duck-Hee;Byun, Woon-Ki
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.421-425
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    • 1994
  • A micro-high performance liquid chromatography(Micro-HPLC) techniquie with solid phase extraction was reported which detected carbendazim and carbaryl at picogram levels. They were separated on microbore packed $C_{18}$ column($1.0mm\;I.\;D{\times}150mm$, $d_f=5{\mu}m$) using a 50% methanol mobile phase and detected at UV 220nm(${\alpha}=2.94$, $R_s=4.71$), while they were not resolved on analtical HPLC system(${\alpha}=1.27$, $R_s=0.76$). The detection thresholds of carbendazim and carbaryl were 0.5ng and 0.1ng on Micro-HPLC, therefore Micro-HPLC system was 20~40 told more sensitive than anayltical HPLC system. Sep-Pak $C_{18}$ catridge was found to be efficient in enriching carbendazim and carbaryl from dilute aqueous solution with 97.0% and 97.8% recoveries of them. The Sep-Pak $C_{18}$ catridge followed by the Micro-HPLC had been applied to the quantitative analysis of carbendazim and carbaryl in spiked juices and a commercial drinking water.

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Rheology and morphology of concentrated immiscible polymer blends

  • Mewis, Jan;Jansseune, Thomas;Moldenaers, Paula
    • Korea-Australia Rheology Journal
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    • v.13 no.4
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    • pp.189-196
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    • 2001
  • The phase morphology is an important factor in the rheology of immiscible polymer blends. Through its size and shape, the interface between the two phases determines how the components and the interface itself will contribute to the global stresses. Rheological measurements have been used successfully in the past to probe the morphological changes in model blends, particularly for dilute systems. For more concentrated blends only a limited amount of systematic rheological data is available. Here, viscosities and first normal stress differences are presented for a system with nearly Newtonian components, the whole concentration range is covered. The constituent polymers are PDMS and PIB, their viscosity ratio can be changed by varying the temperature. The data reported here have been obtained at 287 K where the viscosities of the two components are identical. By means of relaxation experiments the measured stresses are decomposed into component and interfacial contributions. The concentration dependence is quite different for the two types of contribution. Except for the component contributions to the shear stresses there is no clear indication of the phase inversion. Plotting either the interfacial shear or normal stresses as a function of composition produces in some cases two maxima. The relaxation times of these stresses display a similar concentration dependence. Although the components have the same viscosity, the stress-component curves are not symmetrical with respect to the 50/50 blend. A slight elasticity of one of the components seems to be the cause of this effect. The data for the more concentrated blends at higher shear rates are associated with a fibrillar morphology.

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Hydrodynamic Characteristics of the Rectangular Type Circulating Fluidized Bed (4각 순환유동층의 수력학적 특성)

  • Hyun, Sang Yeol;Rhee, Kwan Seok
    • Journal of the Korean Society for Heat Treatment
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    • v.10 no.4
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    • pp.232-236
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    • 1997
  • A rectangular type circulating fluidized bed (CFB) with an internal nozzle and two partition walls was proposed. In this modified CFB, an internal nozzle and two slanted partition walls were additionally set in the riser. This cold mode apparatus was made of acrylic resin; the riser was 1500mm high and $1000{\times}1000mm^2$ in the cross sectional area, the internal nozzle was 200mm high and 10mm in the inner diameter, and the partition wall was 7mm thick. Glass beads of $91{\mu}m$ in the mean diameter were employed as bed materials. In the cold mode by using the proposed CFB with an internal nozzle, it was possible to change the particle hold up by changing the gas flow ratio of the nozzle to the total(Qn/Qt). It was found that the inflection point which devided the bed structure between the dense and the dilute phase in the riser varied with Qn/Qt.

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Investigation on Polyacrylonitrile/Cellulose Acetate Blends

  • Barani, Hossein;Bahranmi, Seyad Hajir
    • Macromolecular Research
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    • v.15 no.7
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    • pp.605-609
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    • 2007
  • The molecular interactions of polyacrylonitrile (PAN) and cellulose acetate (CA) were investigated thoroughly via dilute solution viscometry in dimethylformamide (DMF) as a common solvent at $30^{\circ}C$. The intrinsic viscosities and viscometric interaction parameters were experimentally determined for both binary (polymer/dimethylformamide) and ternary (PAN/CA/dimethylformamide) systems. As all investigated PAN/CA ternaries evidenced negative viscometric interaction parameter values $({\Delta}b\;&{\Delta}k<0)$, the existence of repulsive intermolecular interactions was deduced, and PAN/CA blends were assigned as immiscible. Moreover, the results of microscopy photograph analysis indicated that pure PAN film evidences a homophasic structure, and the size of the phase domain increases gradually with increases in CA. In DSC analysis, it was determined that the glass transition temperature of the blend film increased slightly with increases in the CA content of the blend film.

A review of chromatographic analysis for rare-earth elements with focus on Ln resin

  • Jihye Kim;Kihwan Choi
    • Analytical Science and Technology
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    • v.36 no.6
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    • pp.259-266
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    • 2023
  • The demand for rare-earth elements (REEs) is increasing owing to their significance as prominent materials in electronics, high-tech industries, geological research, nuclear forensics, and environmental monitoring. In general, the utilization of REEs in various applications requires the use of chromatographic techniques to separate individual elements. However, REEs have similar physicochemical properties, which makes them difficult to separate. Recently, several studies have examined the separation of REEs using LN resin as the stationary phase and aqueous nitric acid and hydrochloric acid solutions as eluents. Using this method, light REEs have been separated using dilute acid solutions as the eluent, whereas heavy REEs are separated using solutions with high acid concentrations. To increase the separation resolution between different REEs, either the column length or resin size is changed. In addition, the suggested methods are implemented to decrease the analysis time. This review presents technical information on the chromatographic separation of REEs using the LN resin and discusses the optimal experimental conditions.

Application of Lumley's Drag Reduction Model to Two-Phase Gas-Particl Flow in a Pipe(II) - Mechanism of Heat Transfer- (고체 분말이 부상하는 2상 난류 수직관 유동에 대한 Lumley의 저항감소 모델의 적용 (II) - 열전달 기구 -)

  • 한기수;정명균;성형진
    • Transactions of the Korean Society of Mechanical Engineers
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    • v.14 no.1
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    • pp.214-224
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    • 1990
  • A "two-fluid" model using thermal eddy diffusivity concept and Lumley's drag reduction theory, is proposed to analyze heat transfer of the turbulent dilute gas-particle flow in a vertical pipe with constant wall heat flux. The thermal eddy diffusivity is derived to be a function of the ratio of the heat capacity-density products .rho. over bar $C_{p}$ of the gaseous phase and the particulate phase and also of the ratio of thermal relaxation time scale to that of turbulence. The Lumley's theory dictates the variation of the viscous sublayer thickness depending on the particle loading ratio Z and the relative particle size $d_{p}$/D. At low loading ratio, the size of viscous sublayer thickness is important for suspension heat transfer, while at higher loading, the effect of the ratio .rho. $_{p}$ over bar $C_{p}$$_{p}$/ .rho. $_{f}$ over bar $C_{p}$$_{f}$ is dominant. The major cause of decrease in the suspension Nusselt number at lower loading ratio is found to be due to the increase of the viscous sublayer thickness caused by the suppression of turbulence near the wall by the presence of solid particles. Predicted Nusselt numbers using the present model are in satisfactory agreements with available experimental data both in pipe entrance and the fully developed regions.

Study on the Separation of MAs from HLLW and Their Extraction Behavior Using New Extractants of Amido Podand

  • An, Ye-Guo;Luo, Fang-Xiang;Zhu, Zhi-Xuan;Zhang, Xiang-Ye;Zhu, Wen-Bin
    • Proceedings of the Korean Radioactive Waste Society Conference
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    • 2004.02a
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    • pp.245-256
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    • 2004
  • The extraction of three kinds of amido podands, N,N,N'N'-tetrabutyl-3-oxa-pentanedi- amide (TBDGA), N,N,N'N'-tetra-isobutyl-3-oxa-pentanediamide(TiBDGA) and N,N,N'N'-tetra- butyl-3,6-dioxa-oct-anediam- ide(TBDOODA) on U(VI),Pu(IV), Am(III), Eu(III) and other metal ions is studied in nitric acid solutions. 40%octanol-kerosene is chosen as diluents to eliminate third phase and emulsion. TBDGA and TiBDGA show extraction selectivity to An(III) and Ln(III) much higher than to U(VI) and Pu(IV). Fe, Ru and Mo is poorly extracted by the three kinds of amid podands in 2~3mol/L $HNO_3$ solutions. Aiming to eliminate interface crude when using simulated HLLW solution in the system of 0.2mol/L TBDGA/Octanol+kerosene, acetohydroxyamic acid was adapted. Distribution ratio of zirconium was decreased when adding acetohydroxyamic acid in aqueous solution, and interface crude disappeared as mixing extractant with HLLW. The counter-current extraction test is carried out in a set of miniature mixer-settler, with 0.2mol/L TBDGA/ 40% octanol-kerosene as extractant to separate U(VI), Pu(IV), Am(III) and Eu(III) from simulated high level liquid waste(HLLW) solution. In battery A, lanthanides and actinides are coextracted into organic phase with the recovery of 99.98% for U(Ⅵ), >99.99% for Pu(IV), and >99.99% for Am(III) and Eu(III) respectively. In battery R1, 99.99% U, 86.2% Pu and a part of Am or Eu are stripped into aqueous phase by 0.2mol/L acetohydroxyamic acid (AHA) in 0.01mol/L $HNO_3$ solution. In battery $R_2$, Am, Eu and remained Pu are completely back-extracted by 0.2mol/L AHA. This separation process contains no salt reagent, and it is not necessary to dilute HLLW feed.

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Magnetism in Fe-implanted ZnO

  • Heo, Y.W.;Kelly, J.;Norton, D.P.;Hebard, A.F.;Pearton, S.J.;Zavada, J.M.;Park, Y.D.
    • JSTS:Journal of Semiconductor Technology and Science
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    • v.4 no.4
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    • pp.312-317
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    • 2004
  • High dose ($3{\times}10^{16}cm^{-2}$) implantation of Fe or Ni ions into bulk, single-crystal ZnO substrates was carried out at substrate temperature of ${\sim}350^{\circ}C$ to avoid amorphization of the implanted region. The samples were subsequently annealed at $700^{\circ}C$ to repair some of the residual implant damage. X-Ray Diffraction did not show any evidence of secondary phase formation in the ZnO. The Ni implanted samples remained paramagnetic but the Fe-implanted ZnO showed evidence of ferromagnetism with an approximate Curie temperature of ${\sim}$240K. Preliminary X-Ray Photoelectron Spectroscopy measurements showed the Fe to be ill the 2+ oxidation state. The earrler density in the implanted region still appears to be too low to support carrier-meditated origin of the ferromagnetism and formation of bound magnetic polarons may be one potential explanation for the observed magnetic properties, No evidence of the Anomalous Hall Effect could be found in the Fe-implanted ZnO, but its transport properties were dominated by the conventional or ordinary Hall effect.