• Title/Summary/Keyword: Separation flow

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Optimizing analytical method in Health Functional Food code with adjustable chromatographic parameters: A case study of vitamin C (건강기능식품공전 시험법의 크로마토그래프법 조건의 조정 및 비타민C에 대한 적용성 평가 연구)

  • Junghoon Shin;Yooseong Jeong;Yong Seok Choi;Sang Beom Han;Dong-Kyu Lee
    • Analytical Science and Technology
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    • v.37 no.3
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    • pp.143-154
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    • 2024
  • In this study, we improved the vitamin C test method and reviewed data on the adjustable range of chromatography conditions for quantification. First, we adjusted the mobile phase conditions such as solvent composition, salt concentration, pH and column temperature and in particular, it was confirmed through an improved test method that the peak derived from the buffer solution could be clearly separated from the target component, vitamin C by adjusting the pH. The retention time of vitamin C was partially changed by adjusting the column diameter, length and particle size but the number of theoretical plates indicated similar values and did not affect the separation and quantitative analysis of the target component. The flow rate according to the column specifications was derived from the equation proposed by the U.S. FDA (Food and Drug administration) and the Korean MFDS (Ministry of Food and Drug Safety), and evaluation of the applicability to vitamin complexes showed high selectivity for vitamin C even with altered stationary phase conditions and flow rates. In conclusion, vitamin C can be optimally separated and detected by changing the chromatographic method conditions and it was confirmed that the mobile and stationary phase conditions of liquid chromatography can be slightly adjusted in case the assay method uses an isocratic elution.

New Analytical Method to Identify Chromium Species, Cr(III) and Cr(VI), and Characteristic Distribution of Chromium Species in the Han River (한강수계해서의 크롬(III,VI) 종(species) 분포 및 분석방법 정립)

  • Jeong, Gwan-Jo;Kim, Dok-Chan;Park, Hyeon
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.6
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    • pp.590-598
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    • 2005
  • An adequate method to identify chromium separation, Cr(III) and Cr(VI), in water samples were studied by using High Performance Liquid Chromatography(HPLC) coupled with Inductively Coupled Plasma Mass Spectometer(ICP-MS) equipped with Dynamic Reaction Cell(DRC). The characteristic distribution of Cr(III) and Cr(VI) in the raw water taken at the six water intake stations in Seoul, was analyzed by the method developed by the authors. The chromium species separated by HPLC was isocratically conducted by using tetrabutylammonium phosphate monobasic(1.0 mM TBAP), ethylenediaminetetraacetic acid(0.6 mM EDTA) and 2% v/v methanol as the mobile phase. 5% v/v methanol was used as flushing solvent. A reactive ammonia($NH_3$) gas was used to eliminate the potential interference of $ArC^+$. Several Parameters such as solvent ratio, pH, flow rate and sample injection volume were optimized for the successful separation and reproducibility. Although it has been reported thai the separation sensitivity of Cr(III) is superior to that of Cr(VI), the authors observed Cr(VI) was more sensitive than Cr(III) when ammonia($NH_3$) gas was used as the reaction gas. It took less than 3 minutes to analyze chromium species with this method and the estimated detection limits were $0.061\;{\mu}g/L$ for Cr(III) and $0.052\;{\mu}g/L$, for Cr(VI). According to the results from the analysis on chromium species in the raw water of the six intake stations, the concentrations of Cr(III) ranged from 0.048 to $0.064\;{\mu}g/L$(ave. $0.054\;{\mu}g/L$) while that of Cr(VI) ranged from 0.014 to $0.023\;{\mu}g/L$(ave. $0.019\;{\mu}g/L$). Recovery ratio was very high($90.1{\sim}94.1%$). There were two or three times more Cr(III) than Cr(VI) in the raw water.

Effect of Volatile Matter and Oxygen Concentration on Tar and Soot Yield Depending on Coal Type in a Laminar Flow Reactor (LFR에서 탄종에 따른 휘발분과 산소농도가 타르와 수트의 발생률에 미치는 영향)

  • Jeong, Tae Yong;Kim, Yong Gyun;Kim, Jin Ho;Lee, Byoung Hwa;Song, Ju Hun;Jeon, Chung Hwan
    • Korean Chemical Engineering Research
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    • v.50 no.6
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    • pp.1034-1042
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    • 2012
  • This study was performed by using an LFR (laminar flow reactor), which can be used to carry out different types of research on coal. In this study, an LFR was used to analyze coal flames, tar and soot yields, and structures of chars for two coals depending on their volatile content. The results show that the volatile content and oxygen concentration have a significant effect on the length and width of the soot cloud and that the length and width of the cloud under combustion conditions are less than those under a pyrolysis atmosphere. At sampling heights until 50 mm, the tar and soot yields of Berau (sub-bituminous) coal, which contains a large amount of volatile matter, are less than those of Glencore A.P. (bituminous) coal because tar is oxidized by the intrinsic oxygen component of coal and by radicals such as OH-. On the other hand, at sampling heights above 50 mm, the tar and soot yields of Berau coal are higher than those of Glencore A.P. coal by reacted residual volatile matter, tar and light gas in char and flame. With above results, it is confirmed that the volatile matter content and the intrinsic oxygen component in a coal are significant parameters for length and width of the soot cloud and yields of the soot. In addition, the B.E.T. results and the images of samples (SEM) obtained from the particle separation system of the sampling probe support the above results pertaining to the yields; the results also confirm the pore development on the char surface caused by devolatilization.

Performance Evaluation of Hydrocyclone Filter for Treatment of Micro Particles in Storm Runoff (Hydrocyclone Filter 장치를 이용한 강우유출수내 미세입자 제거특성 분석)

  • Lee, Jun-Ho;Bang, Ki-Woong;Hong, Sung-Chul
    • Journal of Korean Society of Environmental Engineers
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    • v.31 no.11
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    • pp.1007-1018
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    • 2009
  • Hydrocyclone is widely used in industry, because of its simplicity in design, high capacity, low maintenance and operational cost. The separation action of a hydrocyclone treating particulate slurry is a consequence of the swirling flow that produces a centrifugal force on the fluid and suspended particles. In spite of hydrocyclone have many advantage, the application for treatment of urban stormwater case study were rare. We conducted a laboratory scale study on treatable potential of micro particles using hydrocyclone filter (HCF) that was a combined modified hydrocyclone with perlite filter cartridge. Since it was not easy to use actual storm water in the scaled-down hydraulic model investigations, it was necessary to reproduce ranges of particles sizes with synthetic materials. The synthesized storm runoff was made with water and addition of particles; ion exchange resin, road sediment, commercial area manhole sediment, and silica gel particles. Experimental studies have been carried out about the particle separation performance of HCF-open system and HCF-closed system. The principal structural differences of these HCFs are underflow zone structure and vortex finder. HCF was made of acryl resin with 120 mm of diameter hydrocyclone and 250 mm of diameter filter chamber and overall height of 800 mm. To determine the removal efficiency for various influent concentrations of suspended solids (SS) and chemical oxygen demand (COD), tests were performed with different operational conditions. The operated maximum of surface loading rate was about 700 $m^3/m^2$/day for HCF-open system, and 1,200 $m^3/m^2$/day for HCF-closed system. It was found that particle removal efficiency for the HCF-closed system is better than the HCF-open system under same surface loading rate. Results showed that SS removal efficiency with the HCF-closed system improved by about 8~20% compared with HCF-open system. The average removal efficiency difference for HCF-closed system between measurement and CFD particle tracking simulation was about 4%.

Fundamental Studies on the Development of Axial-Flow Combine(I) -Evaluation of the Design Parameters of Grain-Straw Separator- (축류(軸流) 콤바인의 개발(開發)에 관(關)한 기초(基礎) 연구(硏究)(I) -조선별장치(粗選別裝置)의 설계변수(設計變數)의 평가(評價)-)

  • Lee, S.K.;Kim, S.T.;Choi, K.H.
    • Journal of Biosystems Engineering
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    • v.11 no.2
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    • pp.31-40
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    • 1986
  • Cylindrical and conical types of grain-straw separation equipment which has a stationary crimped sieve drum with rotating inner rotor were constructed. The developed equipments were tested to investigate the characteristics of separating performance under various mechanical conditions and crop conditions. As increase of the inclination of equipment and decrease of pitch of cover vane, the grain recovery was increased while straw rejection was decreased. The grain recovery and overall efficiency were decreased as the rotor speed and feeding velocity were increased for both varieties of rice, moisture contents, and test equipments. Conical prototype equipment performed higher straw rejection, lower grain recovery, and lower power requirement. However, separation performance of conical type equipment was more widely varied with various test conditions compared to cylindrical one. The performance of both equipments showed relatively insensitive to crop feedrate and crop properties, such as variety, moisture content, and grain-to-straw ratio.

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Optimization of HPLC Method and Clean-up Process for Simultaneous and Systematic Analysis of Synthetic Color Additives in Foods (식품 중 타르색소의 동시분석 및 계통분석을 위한 HPLC 분석조건 및 정제과정 확립)

  • Park, Sung-Kwan;Hong, Yeun;Jung, Yong-Hyun;Lee, Chang-Hee;Yoon, Hae-Jung;Kim, So-Hee;Lee, Jong-Ok
    • Korean Journal of Food Science and Technology
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    • v.33 no.1
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    • pp.33-39
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    • 2001
  • To develop a method for separation process using Sep-pak $C_18$, simultaneous and systematic analysis of 8 permitted and 11 non-permitted synthetic food colors in Korea, optimization of analysis conditions for reverse phase ion-pair high performance liquid chromatography was carried out. For the best result of Sep-pak $C_18$ separation the pH of color standard mixture solution was $5{\sim}6$ and 0.1% HCl-methanol solution were set as eluent. The colors eluated from Sep-pak $C_18$ cartridge were determined and confirmed by high performance liquid chromatography with a photodiode array detector at 420 nm for yellow colors type, at 520 nm for red colors type, at 600 nm for blue and green colors type and at 254 nm for mixed colors. Conditions for HPLC analysis were as follows: column, Symmetry $C_18$ (5 m, 3.9 mm $i.d.{\times}150\;mm$); mobile phase, 0.025 M ammonium acetate (containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (65 : 25 : 10) and 0.025 M ammonium acetate(containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (40 : 50 : 10); flow rate, 1 mL/min. It takes 35 minutes for simultaneaus analysis and 18 minutes for systematic analysis. The detection limits range of each colors were $0.01{\sim}0.05\;{\mu}g/g$.

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Characterization of Low-Temperature Pyrolysis and Separation of Cr, Cu and As Compounds of CCA-treated Wood (CCA (Chromated Copper Arsenate) 처리 목재의 저온 열분해와 CCA 유효 성분분리 특성)

  • Lim, Kie-Pyo;Lee, Jong-Tak;Bum, Jung-Won
    • Journal of the Korean Wood Science and Technology
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    • v.35 no.1
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    • pp.73-80
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    • 2007
  • This study was carried out to separate the heavy toxic metals in eco-building materials by low-temperature pyrolysis, especially arsenic (As) compounds in CCA wood preservative as a solid in char. The pyrolysis was carried out to heat the CCA-treated Hemlock at $280^{\circ}C$, $300^{\circ}C$, $320^{\circ}C$, and $340^{\circ}C$ for 60 mins. Laboratory scale pyrolyzer composed of [preheater$\rightarrow$pyrolyzer$\rightarrow$1st water scrubber$\rightarrow$2nd bubbling flask with 1% $HNO_3$ solution$\rightarrow$vent], and was operated to absorb the volatile metal compound particulates at the primary water scrubber and the secondary nitric acid bubbling flask with cooling condenser of $4^{\circ}C$ under nitrogen stream of 20 mL/min flow rate. And the contents of copper, chromium and arsenic compounds in its pyrolysis such as carbonized CCA treated wood, 1st washing and 2nd washing liquors as well as its raw materials, were determined using ICP-AES. The results are as follows : 1. The yield of char in low-temperature pyrolysis reached about 50 percentage similar to the result of common pyrolytic process. 2. The higher the pyrolytic temperature was, the more the volatiles of CCA, and in particular, the arsenic compounds were to be further more volatile above $320^{\circ}C$, even though the more repetitive and sequential monitorings were necessary. 3. More than 85 percentage of CCA in CCA-treated wood was left in char in such low-temperature pyrolytic condition at $300^{\circ}C$. 4. Washing system for absorption of volatile CCA in this experiment required much more contacting time between volatile gases and water to prevent the loss of CCA compounds, especially the loss of arsenic compound. 5. Therefore, more complete recovery of CCA components in CCA-treated wood required the lower temperature than $320^{\circ}C$, and the longer contacting time of volatile gases and water needed the special washing and recovery system to separate the toxic and volatile arsenic compounds in vent gases.

Study on the Manufacture of High-purity Vanadium Pentoxide for VRFB Using Chelating Agents (킬레이트제를 활용한 VRFB용 고순도 오산화바나듐 제조 연구)

  • Kim, Sun Kyung;Kwon, Sukcheol;Kim, Hee Seo;Suh, Yong Jae;Yoo, Jeong Hyun;Chang, Hankwon;Jeon, Ho-SeoK;Park, In-Su
    • Resources Recycling
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    • v.31 no.2
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    • pp.20-32
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    • 2022
  • This study implemented a chelating agent (Ethylenediaminetetraacetic acid, EDTA) in purification to obtain high-purity vanadium pentoxide (V2O5) for use in VRFB (Vanadium Redox Flow Battery). V2O5 (powder) was produced through the precipitation recovery of ammonium metavanadate (NH4VO3) from a vanadium solution, which was prepared using a low-purity vanadium raw material. The initial purity of the powder was estimated to be 99.7%. However, the use of a chelating agent improved its purity up to 99.9% or higher. It was conjectured that the added chelating agent reacted with the impurity ions to form a complex, stabilizing them. This improved the selectivity for vanadium in the recovery process. However, the prepared V2O5 powder exhibited higher contents of K, Mn, Fe, Na, and Al than those in the standard counterparts, thus necessitating additional research on its impurity separation. Furthermore, the vanadium electrolyte was prepared using the high-purity V2O5 powder in a newly developed direct electrolytic process. Its analytical properties were compared with those of commercial electrolytes. Owing to the high concentration of the K, Ca, Na, Al, Mg, and Si impurities in the produced vanadium electrolyte, the purity was analyzed to be 99.97%, lower than those (99.98%) of its commercial counterparts. Thus, further research on optimizing the high-purity V2O5 powder and electrolyte manufacturing processes may yield a process capable of commercialization.

Average Fission Neutron Cross Section for $^{93}Nb(n,\alpha)^{90}Y$, $^{90}Zr(n,p)^{90}Y$, $^{93}Nb(n,\alpha)^{90m}Y$and $^{90}Zr(n,p)^{90m}Y$ Reactions ($^{93}Nb(n,\alpha)^{90}Y$, $^{90}Zr(n,p)^{90}Y$, $^{93}Nb(n,\alpha)^{90m}Y$$^{90}Zr(n,p)^{90m}Y$반응의 평균 핵분열 중성자 반응 단면적)

  • Chul Lee;Yung Chang Yim;Koo Soon Chung;Hae-Ill Park
    • Journal of the Korean Chemical Society
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    • v.17 no.1
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    • pp.20-24
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    • 1973
  • The average fission neutron cross sections were determined for the following reactions, $^{93}Nb(n,\alpha)^{90}Y$, $^{90}Zr(n,p)^{90}Y$,$^{93}Nb(n,\alpha)^{90m}Y$and$^{90}Zr(n,p)^{90m}Y$. The cation exchange column was used for the quantitative separation of the product nuclides using $\alpha-$hydroxyisobutyric acid as the eluent. The absolute activites of $^{90m}Y$ and $^{90}Y$were determined by the gamma ray spectrometry and a calibrated $2\pi$gas flow counter, respectively. The cross sections of $^{93}Nb(n,\alpha)^{90}Y$, $^{90}Zr(n,p)^{90}Y$,$^{93}Nb(n,\alpha)^{90m}Y$and $^{90}Zr(n,p)^{90m}Y$ reactions were found to be$0.14\pm0.01mb$, $0.83\pm0.02mb$, $0.018\pm0.02mb$ and $0.33\pm0.02mb$, respectively. The possible use of $^{90m}Y$ instead of $^{90}Y$ was discussed as a better means for the determination of niobium.

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Simultaneous determination of preservatives in sausages using liquid chromatography with electrospray ionization tandem mass spectrometry (LC-MS/MS를 이용한 소시지 중 보존료 동시분석)

  • Koh, Ba-Ra-Da;Kim, Ji-Yeon;Jang, Mi-Sun;Seo, Doo-Ri;Jung, Bo-Ram;Shin, Ji-Hyun;Lim, Jin-Taek;Kim, Yong-Hwan;Kim, Eun-Sun
    • Korean Journal of Veterinary Service
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    • v.38 no.2
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    • pp.127-136
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    • 2015
  • A simultaneous determination method was developed for nine preservatives (benzoic acid, sorbic acid, dehydroacetic acid, methyl-, ethyl-, isopropyl-, propyl-, isobutyl- and butyl-parabens) in sausage by liquid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). Each parameter was established by multiple reaction monitoring in negative mode. Separation was achieved on a phenyl-hexyl ($2.5{\mu}m$, $2.1{\times}150mm$, Waters) with A-20 mM ammonium acetate containing 0.1% acetic acid in water, B-Acetonitrile as mobile phase with gradient mode at a flow rate of 0.3 mL/min. The developed method was validated for specificity, linearity, accuracy and precision in sausages samples. Linearity was over 0.998 with calibration curve of the mixed standards. The mean recoveries from sausages fortified at the level of 2.0~10.0 mg/L were in range of 98.60~109.16% with RSDs lower than 8.93%. The limits of detection (LOD) and the limits of quantification (LOQ) were in the range between 0.0003~0.085 mg/L and 0.01~0.257 mg/L, respectively. Intra-day precision and inter-day precision were 0.45~6.16% and 2.81~13.33%, respectively. Using presently developed determination method, 33 field sausage samples from Gwangju city in Korea were screened over nine preservatives. As a result, no preservatives were detected in all samples.