• Title/Summary/Keyword: reversed phase

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Quantitative analysis of selenium species in sea food using solid phase extraction and HPLC-ICP/MS (해산물 시료에서 solid-phase extraction 및 HPLC-ICP/MS를 이용한 셀레늄 화학종의 정량분석)

  • Kim, Eunju;Joo, Minkyu;Kwon, Hyosik;Pak, Yongnam
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.307-314
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    • 2013
  • Selenium exists in various forms of chemical species. The activity and bioavailability is strongly dependent on its chemical form and concentration. Consequently the information on each selenium species and its concentration must be exactly determined for the food we take in. In this study, selenium species in seafood were separated and quantified by RP (reversed phase) HPLC (high performance liquid chromatography) coupled with ICP-MS (inductively coupled plasma mass spectrometry) using post-column isotope dilution. $^{79}Br$, which interferes on $^{80}Se$, has mostly been removed by solid phase extraction and then mathematical correction has been applied for the more accurate correction. The experimental result for CRM (certified reference material) DOLT-4 agreed well with the certified value but each selenium species could not be compared. SeCys (selenocysteine) and SeMet (selenomethionine) were the major species detected in seafood such as belt fish, spanish mackerel, and squid that have been serving as Korean diet. The concentrations found in Korean sea food for SeCys and SeMet were in the range of 0-661.6 mg/kg and 137.3-462.7 mg/kg, respectively.

Influence of Variation of Aging Heat Treatment Condition on Phase Transformation and Mechanical Properties of 15-5PH Stainless Steel (15-5PH 스테인리스강의 시효열처리 조건변화가 상변태 및 기계적 성질에 미치는 영향)

  • Kim, T.S.;Lee, Jewon;Roh, Y.S.;Sung, J.H.;Lim, S.G.
    • Journal of the Korean Society for Heat Treatment
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    • v.32 no.5
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    • pp.212-223
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    • 2019
  • This study is to investigate the relationship between microstructural factors and tensile properties after aging heat treatment of the 15-5PH stainless steel at the temperature range of $450^{\circ}C$, $500^{\circ}C$ and $550^{\circ}C$ for various time. For the aging time of 2 hours, hardness showed maximum at $450^{\circ}C$ and then decreased with increasing aging temperature. While, hardness decreased gradually during aging $450^{\circ}C$, $500^{\circ}C$ and $550^{\circ}C$ from 1 hour to 5 hours but the hardness nearly unchanged until the 100 hours after 5 hours aging. When aging at $450^{\circ}C$, Cu atoms preferentially aggregated at the prior austenite grain boundaries and martensite lath boundaries, and Cu concentration at those boundaries was nearly unchanged even after aging for 100 hours. Therefore it was suggested that the coherency is still maintained after 100 hours aging at $450^{\circ}C$. Aging at $500^{\circ}C$ and $550^{\circ}C$ results in an increase in the concentration of Ni at the martensite lath boundaries and prior austenite grain boundaries, resulting in the formation of reversed austenite. Especially, when aged at $550^{\circ}C$ for 100 hours, the concentration of Ni remarkably increased at those boundaries, and thus the microstructure of herring bone shape was appeared. Considering the migration of Ni atom to the lath boundaries and prior austenite grain boundaries, Ni atoms contributed greatly to the formation of reversed austenite. On the other hand, it was found that Cu atoms hardly moving to those boundaries may not be contributed to the formation of reversed austenite. When aging at $450^{\circ}C$, the coarsening of the precipitated Cu atoms proceeded very slowly with increasing aging time, therefore the decrease in strengths were small but the reduction area was considerably increased due to the softening of the matrix. At the aging temperature of $500^{\circ}C$ and $550^{\circ}C$, the strengths decreased and the elongation and reduction area increased due to the appearance of the reversed austenite. Especially, the increase of reduction area was remarkable.

Emulsion Inversion and Emulsion Transition (에멀젼 변환과 에멀젼 전이)

  • Lim, Kyung-Hee
    • Journal of the Korean Applied Science and Technology
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    • v.21 no.4
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    • pp.267-273
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    • 2004
  • It has been 40 years since emulsion inversion was observed. Emulsion inversion is a phenomenon in which O/W emulsion inverts to W/O emulsion or vice versa. In other words, the dispersed and continuous phase of an emulsion is reversed after emulsion inversion takes place. For three-phase emulsions, not only emulsion inversion but also emulsion transition has been observed. In emulsion transition the continuous phase of an emulsion remains unchanged, but the dispersed emulsion drops, which is basically a two-phase emulsion, experience emulsion inversion at a certain temperature. Such temperature is called the emulsion transition temperature. Emulsion transition was a product of theoretical speculation and was experimentally observed for a couple of ternary amphiphile/oil/water systems. This phenomenon is a novel one, which has been unreported to date. In this article emulsion inversion and emulsion transition are compared and discussed.

HPLC Study for Egg White Analysis (달걀 단백질 분석을 위한 HPLC 연구)

  • Jeon, Young-Ju;Lee, Eun;Kim, In-Ho
    • KSBB Journal
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    • v.22 no.2
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    • pp.119-122
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    • 2007
  • Since egg white contains various protein, it is important to research the protein distribution of egg white. Specially, lysozyme and ovalbumin important proteins, are used in medicine and food industry. Reversed phase high performance liquid chromatography has been used for separation of egg white, and column of RP-HPLC is available in variety. We have used C4, C8 and C18 columns to obtain chromatograms by varying carbon chain length of stationary phase. Long carbon chain length of stationary phase has good separation of egg white. Also, we have changed the composition of mobile phase (acetonitrile, water, and trifluoroacetic acid) to find optimum chromatograms. Acetonitrile and water composition of 50 : 50 show many peaks from egg white. Isocartic and gradient elution in RP-HPLC were used to compare the chromatography of egg white.

A Study on the Elution Mechanism of Ni(II)-Isonitrosoethylacetoacetate Imine Chelates by Reversed Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 Ni(II)-Isonitrosoethylacetoacetate Imine 유도체 킬레이트의 용리 메카니즘에 관한 연구)

  • Kim In-Whan;Choi Gang-Yeol;Lee Man-Ho;Kang Chang-Hee;Lee, Won
    • Journal of the Korean Chemical Society
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    • v.36 no.5
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    • pp.697-708
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    • 1992
  • Liquid Chromatographic behavior of Ni(II) in Isonitrosoethylacetoacetate Imine(IEAA-NR), Ni(IEAA-NH)(IEAA-NR)(R = H, CH_3, C-2H_5, n-C_4H_9, C_6H_5-CH_2) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of Ni(IEAA-NH)(IEAA-NR) chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It was fo$und that metal chelates were properly eluted in an acceptable range of capacity factor value(0{\le}logk'{\le}1). The dependence of the logarithm of capacity factor (k') on the volume fraction of water in the binary mobile phase as well as on the liquid-liquid extraction distribution ratio (Dc) in methanol-water/n-alkane extraction system showed the good linearties, and the dependence of the logarithm of capacity factor (k') on the column temperature and on the enthalpy exhibited the good linearties, and the compensation temperature ({\beta}) from the slope was 773.47{\circ}K. It was suggested that the retention of metal chelates was largely affected by the hydrophobic effect.

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Development of Separation and Trace Analysis Methods for Platinum Group Elements-Separation and Retention Behavior of Platinoid Metal Acetylacetonates in Reversed-Phase Liquid Chromatography (백금족 원소의 분리 및 미량분석법 개발에 관한 연구: 역상 액체 크로마토그래피에 의한 백금족 금속-아세틸아세톤 킬레이트들의 분리 및 머무름 거동)

  • Lee, Dai Woon;Kim, Kyung Soo;Park, Young Hun;Czea, Myoung Zoon;Chung, Koo Soon
    • Analytical Science and Technology
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    • v.6 no.1
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    • pp.107-119
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    • 1993
  • The purpose of this study is to investigated the elution behavior of platinoid metal acetylacetonates, which is the key to elucidate their retention mechanism and optimize their RPLC separation conditions. The retention data of four platinoid metal acetylacetonates have been measured on four different columns in methanol-water and acetonitrile-water systems. The retention of uncharged platinoid metal acetylacetonates is interpreted by solvophobic effect. The retention of platinoid metal acetylacetonates is also greatly influenced by the geometric structure of the complexes. The square planar chelates, $Pd(acac)_2$, $Pt(acac)_2$, are retained longer than the octahedral chelates, $Rh(acac)_3$, $Ir(acac)_3$. It is likely due to that square planar chelates show greater interaction with nonpolar stationary phase than octahedral chelates. The results of van't Hoff plots have shown that platinoid metal acetylacetonates is operated on the same retention mechanism in the temperature range of $25{\sim}45^{\circ}C$. The study of the retention mechanism by the enthalpy-entropy compensation phenomenon has indicated that the retention mechanism of octahedral chelates and square planar chelates do not vary with the composition change of methanol-water mobile phase, respectively. In acetonitrile-water mobile phase, however, the retention mechanism is observed to be more complicated. Optimum condition for the separation of four platinoid metal acetylacetonates is found to be 40% methanol, polymeric C18 column, and $45^{\circ}C$.

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Separation of Egg White Using HPLC with Change of Mobile Phase and Temperature (HPLC에서 이동상 변화와 온도에 따른 난백의 분리)

  • Do, Jin-Sun;Song, Shin-Young;Cho, Ki-Jung;Kim, In-Ho
    • Korean Chemical Engineering Research
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    • v.49 no.6
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    • pp.829-834
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    • 2011
  • Lysozyme in egg white functions as bacteriolysis agent and ovalbumin plays a role as antigen in immune system. Egg white analysis methods usually include electrophoresis, gel permeation chromatography and reversed-phase HPLC(RP-HPLC). Among them, RP-HPLC was selected for rapid analysis and C18 column(Agilent, USA) was used as HPLC column. Optimum conditions were searched by changing mobile phase and temperature. Capacity factor and resolution were calculated and compared for various elution conditions. In the isocratic elution, mobile phase volume ratio was changed from 30/70/0.1 to 60/40/0.1(Acetonitrile(ACN)/Distilled water(DW)/Trifluoroacetic acid(TFA)). ACN composition was increased by 10% and temperature was set as $20^{\circ}C$. In the gradient elution, ACN/DW ratio was changed from 10/90 to 60/40 during 20 minute and temperature was varied as 20, 30 and $40^{\circ}C$. In the isocratic elution, three peaks were separated at 50/50/0.1. Lysozyme and ovalbumin were confirmed as first and third peak in three peaks respectively. In the gradient elution, four peaks were separated at $30^{\circ}C$. Lysozyme and ovalbumin were confirmed as first peak and third peak in four peaks respectively.

A Study on the Elution Behavior of Pd-Isonitroso ethylacetoacetate imine Chelates by Reversed-phase High Performance Liquid Chromatography (역상 고성능 액체 크로마토 그래피에 의한 Pd(II) - isonitrosoethylacetoacetate imine 유도체 킬레이트의 용리거동에 관한 연구)

  • Kim, Hyun
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.19 no.1
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    • pp.20-30
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    • 1993
  • Liquid Chromatographic behavior of Pd(II) in Isonitosoethylacetoacetate imine IEAA-NR: R=H, CH3, C2H5, n-C3H7, n-C4H9, C6H5-CH2) Chelates were investigated by reversed phase high performance 1iquid chromatography on Micropak MCH-5 Column using Methanol /water as mobile phase. The optimum condition for the separation of Pd-Isonitrosoethylacetoacetate imine chelates were examined with respect to the flow rate, mobile phase strength. It was found that Pd(IEAA-NR)2 chelates were eluted in an acceptable range of the capacity factor value (0 $\leq$ log k' $\leq$ 1), The dependence of the logarithm of capacity factor(k') on the volume fraction of water in mixture with in the binary mobile phase was examined. Also, the dependence of k'on the liquid-liquid extraction distribution constant in methanol-water / n-alkane extraction system was on system was invert tigated for Pd(IEAA-NR)2. Both kinds of dependence are linear, which suggests that the retention of the electroneutral metal chelates be largely due to the solvophobic effect.

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Implementation and Design of Wideband IFIU using Aperture Open Loop Resonator and Reversed Phase Technique (역 위상 기법과 Aperture를 갖는 개방형 루프 공진기를 사용한 광대역 IF 모듈 설계 및 제작)

  • 김영완
    • Journal of the Institute of Electronics Engineers of Korea TC
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    • v.41 no.11
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    • pp.17-23
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    • 2004
  • The implementation and design of the wideband IFIU using aperture open loop resonator and reversed phase technique to reduce the local oscillator leakage signal was represented in this paper. The local oscillator leakage signal is generated in stage of frequency conversion, especially in frequency conversion of fully digital modulation signal close to DC signal. The leakage signal and spurious signals, which have effects on adjacent channel or in-band channel as interference signals, were reduced below -60 dBc for 45 Mbps and 155 Mbps IF interface units. The group delay for both IFIUs shows low ripple characteristics of 15 ns and 8 ns, respectively. Also, the amplitude ripple characteristic in 150 MHz bandwidth with L-band center frequency satisfies the required specification of 2 dB. The implemented IFIU provides the required specifications for wideband satellite communication system.

Isolation of Iron and Calcium-Binding Peptides from Cottonseed Meal Protein Hydrolysates (면실박 단백질로부터 가수분해물 제조 및 철분, 칼슘 결합 펩타이드의 분리)

  • Choi, Dong-Won;Kim, Nam-Ho;Song, Kyung Bin
    • Journal of Applied Biological Chemistry
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    • v.55 no.4
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    • pp.263-266
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    • 2012
  • Isolation of iron and calcium-binding peptides derived from cottonseed meal protein (CMP) hydrolysates was investigated. The degree of hydrolysis of CMP by Flavourzyme was monitored using trinitrobenzenesulfonic acid method and sodium dodecyl sulfate-polyacrylamide gel electrophoresis. Enzymatic hydrolysis of CMP for 12 h was sufficient for the preparation of CMP hydrolysates, and the hydrolysates were membrane-filtered under 3 kDa as a molecular weight. The filtered solution was fractionated using Q-Sepharose fast flow, Sephadex G-15, and reversed phase-high performance liquid chromatography for iron and calcium-binding peptides. As a result, F51 fraction was obtained as the best candidate for calcium and iron chelation, and the isolated iron and calcium-binding peptides can be used as functional food additives, similar to iron and calcium supplements.