• Title/Summary/Keyword: Phase Calibration

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Analysis of Cationic Surfactants in Cosmetics By Reverse phase Ion-Pair Chromatigraphy with Suressed Conductivity Detector and UV Detector

  • Jong-Keun Choi;Jae
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.23 no.3
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    • pp.161-167
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    • 1997
  • Determination of several cationic surfactants in cosmetics has been investigated. Reverse phase ion pair chromatography was used to identify and quantitate cationic surfactants. Cationic surfactants analyzed in this experiment were cetylpyridium chloride, stearyltrimetylammonium chloride, bezalkonium chloride, benzyldicethylcetylammonium chloride, and bihenyltrimethyl ammonium chloride. The separation was achieved on a reverse phase coumn with 10mM HCl-acetonitrile eluent. In this condition, the most of cationic surfactants with exception of CPC and CTAC respectively with suppressed conductivity detector and UV detector connected in series. The calibration curves obtained by plotting the peak areas of the cationic surfactants were linear at levels ranging from 0.005 to 0.1% correlation coefficient, r=0.9988. The detection limits were 1 to 5ppm in sample solution. The average recoveries of cationic surfactants added to hair treatment cream and hair rinse in three to five experiments were 96.7 105.2% and relative standard deviations were 1.1-3.8%. The case that there were CPC and CTAC in same solution was also tested. CPC and CTAC which couldn't be separated on reverse phase column were quantitated with suppressed conductivity detector and UV detector connected in series. Recovery of CPC and CTAC were 101.6 and 89.2% respectively. The proposed method was applied to the determination of cationic surfactants in commercial hair treatment cream.

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Reversed-Phase Liquid Chromatographic Separation of Metal Ions by Chelate Formation with 1-(2-Pyridylazo)-2-Naphthol (역상 액체크로마토그래피에 의한 1-(2-Pyridylazo)-2-Naphthol과 킬레이트를 형성하는 금속이온의 분리)

  • Kang, Sam Woo;Park, Sun Ja
    • Journal of the Korean Chemical Society
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    • v.42 no.2
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    • pp.197-202
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    • 1998
  • 1-(2-Pyridylazo)-2-Naphthol (PAN) has been widely used as a spectrophotometric reagent and metallochromic indicator for many metal ions. In this work, the chelate reagent of PAN was used as mobile phase additive for the separation of metal ions by reversed phase chromatography. Metal ions could be detected by monitoring the effluent at 570 nm with spectrophotometric detector. In order to investigate retention behaviors of the metal ions, the chromatograms and capacity factors were obtained as the variation of pH, ionic strength and composition of organic modifier in mobile phase. Under the obtained optimum conditions, the mixtures of Fe(III), Ni(II), Cu(II), Zn(II) and Co(II) could be separated successfully and the calibration curves under the recommended conditions showed an excellent linearity. The detection limits(S/N) were feasible at the nanogram level.

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Determination of Total Phenols in Environmental Waters by Capillary-HPLC with U.S.E.P.A. Classified Eleven Priority Pollutant Phenols after Nitrosation and Their Visible Spectrophotometric Detection

  • Chung, Yong-Soon
    • Bulletin of the Korean Chemical Society
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    • v.26 no.2
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    • pp.297-302
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    • 2005
  • The determination of total phenols was accomplished by capillary-high performance liquid chromatography (capillary-HPLC) after nitrosation of the U.S.E.P.A. classified 11 priority pollutant phenols, using the nitrosated parent phenol (POHNO) as a reference for calibration. The optimum mobile phase composition for this analysis was found by examining the effect of changing the percentage of acetonitrile (MeCN) in the mobile phase on retention factors (k values) and peak intensities. As MeCN percentage was increased, k values were reduced and peak intensities were generally increased. From the results obtained, it was found that the optimum mobile phase was 90%(v/v) MeCN solution at pH 8.0, the detection wavelength of 400 nm, and a detection limit (D.L., concentration at signal to noise ratio (S/N) of 3.0) of 4.5 ${\times}$ $10^{-7}$ M. In addition, 10 of the 11 phenols present in mineral or waste water were separated after the nitrosation by capillary-HPLC. The optimum mobile phase for separation was a 40%(v/v) MeCN solution at pH 5.0.

Simultaneous Determination of the Water Soluble Vitamins in Multi-Nutrient Tablets by Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Hyung-Soo;Jang, Duck-Kyu;Woo, Dong-Kyun;Woo, Kang-Lyung
    • Preventive Nutrition and Food Science
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    • v.7 no.1
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    • pp.12-17
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    • 2002
  • Simultaneous determination of nine water-soluble vitamins contained in multi-nutrient tablets was carried out by reversed phase high-performance liquid chromatography (RP-HPLC) equipped with analytical $C_{18}$ column and UV (270 nm) detector. Those standard vitamins were successfully separated within 23 minutes by gradient elution with solvent A (0.5 M potassium phosphate monobasic) and solvent B (0.25 M potassium phosphate monobasic-methanol, 1:1). Calibration curves showed good linealities with correlation coefficients (> 0.92) in tested ranged respectively. The detection limits were considered to be 2.1 ng for ascorbic acids 60 ng for Vit B$_{6}$ 3 ng for p-aminobenzoic acid, 9 ng for niacinamide, 9 ng for thiamin, 5.0 ng for folic acid and 1.5 ng for riboflavin at 0.05 a.u.f.s. Solid phase extraction through Sep-Pak (C$_{18}$ ) cartridge was successfully applied for purification of water soluble vitamins in commercial multi-nutrient tablets.ts.

Pressure-load Calibration of Multi-anvil Press and the Thermal Gradient within the Sample Chamber (멀티 앤빌 프레스의 압력-부하 보정 작업과 시료 내의 온도구배 연구)

  • Kim, Eun Jeong;Lee, Sung Keun
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.3
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    • pp.161-172
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    • 2018
  • Multi-anvil press (MAP) is one of the high pressure apparatuses and often generates the pressure-conditions ranging from 5 to 25 GPa and temperature-conditions up to $2,300^{\circ}C$. The MAP is, therefore, suitable to explore the pressure-induced structural changes in diverse earth materials from Earth's mantle and the bottom of the mantle transition zone (~660 km). In this study, we present the experimental results for pressure-load calibration of the 1,100-ton multi-anvil press equipped in the authors' laboratory. The pressure-load calibration experiments were performed for the 14/8 step, 14/8 G2, 14/8 HT, and 18/12 assembly sets. The high pressure experiments using ${\alpha}$-quartz, wollastonitestructure of $CaGeO_3$, and forsterite as starting materials were analyzed by powder X-ray diffraction spectroscopy. The phase transition of each mineral indicates the specific pressure that is loaded to a sample at $1,200^{\circ}C$: a transition of ${\alpha}$-quartz to coesite at 3.1 GPa, that of garnet-structure of $CaGeO_3$ to perovskite-structure at 5.9 GPa, that of coesite to stishovite at 9.2 GPa, and that of forsterite to wadsleyite at 13.6 GPa. While the estimated pressure-load calibration curve is generally consistent with those obtained in other laboratories, the deviation up to 50 tons is observed at high pressure above 10 GPa. This is partly because of the loss of oil pressure at high pressure resulting from the differences in a sample chamber, and the frictional force between pressure medium and second anvil. We also report the ${\sim}200^{\circ}C/mm$ of thermal gradient in the vertical direction of the sample chamber of 14/8 HT assembly. The pressure-load calibration curve and the observed thermal gradient within the sample chamber can be applied to explain the structural changes and the relevant macroscopic properties of diverse crystalline and amorphous earth materials in the mantle.

Pressure-load Calibration of Multi-anvil Press at Ambient Temperature through Structural Change in Cold Compressed Amorphous Pyrope (비정질 파이로프의 저온 압축에 따른 구조 변화를 이용한 멀티 앤빌 프레스의 상온 압력-부하 보정)

  • Lhee, Juho;Kim, Yong-Hyun;Lee, A Chim;Kim, Eun Jeong;Lee, Seoyoung;Lee, Sung Keun
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.1
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    • pp.65-73
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    • 2022
  • The proper estimation of physical and chemical properties of Earth materials and their structures at high pressure and high temperature conditions is key to the full understanding of diverse geological processes in Earth and planetary interiors. Multi-anvil press - high-pressure generating device - provides unique information of Earth materials under compression, mainly relevant to Earth's upper mantle. The quantitative estimation of the relationship between the oil load within press and the actual pressure conditions within the sample needs to be established to infer the planetary processes. Such pressure-load calibration has often been based on the phase transitions of crystalline earth materials with known pressure conditions; however, unlike at high temperature conditions, phase transitions at low (or room) temperatures can be sluggish, making the calibration at such conditions challenging. In this study, we explored the changes in Al coordination environments of permanently densified pyrope glasses upon the cold compression using the high-resolution 27Al MAS and 3QMAS NMR. The fractions of highly coordinated Al in the cold compressed pyrope glasses increase with increasing oil load and thus, the peak pressure condition. Based on known relationship between the peak pressure and the Al coordination environment in the compressed pyrope glasses at room temperature, we established a room temperature pressure-load calibration of the 14/8 HT assembly in 1,100-ton multi-anvil press. The current results highlight the first pressure-load calibration of any high pressure device using high-resolution NMR. Irreversible structural densification upon cold compression observed for the pyrope glasses provides insights into the deformation and densification mechanisms of amorphous earth materials at low temperature and high pressure conditions within the subducting slabs.

3D simulation of Heat transfer in MEMS-based microchannel (MEMS 로 제작된 마이크로 채널에서의 3 차원 열전달 해석)

  • Choi, Chi-Woong;Huh, Cheol;Kim, Dong-Eok;Kim, Moo-Hwan
    • Proceedings of the KSME Conference
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    • 2007.05b
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    • pp.1870-1875
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    • 2007
  • The microchannel heat sink is promising heat dissipation method for high heat flux source. Contrary to conventional circular channel, MEMS based microchannel had rectangular or trapezoidal cross-sectional shape. In our study, we conducted three dimensional conjugate heat transfer calculation for rectangular shape microchannel. First, we simulated that channel was completely drained with known heating power. As a result we obtained calibration line, which indicates heat loss was function of temperature. Second, we simulated single phase heat transfer with various mass flux, 100-400 $kg/m^2s$. In conclusion, the single phase test verified that the present heat loss evaluation method is applicable to micro scale heat transfer devices. Heat fluxes from each side wall shows difference due to non-uniform heating. However those ratios were correlated with supplied total heat. Finally, we proposed effective area correction factor to evaluate appropriate heat flux.

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Quantitative Determination of Flavonoids from Stems of Spatholobus suberectus

  • Park, Jinseon;Park, So Yeon;Shim, Sang Hee
    • Natural Product Sciences
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    • v.19 no.2
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    • pp.145-149
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    • 2013
  • A simple reversed phase HPLC method was established for quantitative determination of liquiritigenin (1), genistein (2), isoliquiritigenin (3), and 7-hydroxyflavanone (4) from stems of Spatholobus suberectus Dunn (Leguminosae) using a binary gradient of $H_2O$ and MeOH as a mobile phase with UV detection at 280 nm. All calibration curves showed good linear regression ($r^2$ > 0.998) within test ranges. The detection limits of the four compounds were $0.43{\sim}1.63{\mu}g/mL$. The contents of four flavonoids (1 - 4) from the stem of S. suberectus were 6.54 mg/g, 1.66 mg/g, 6.65 mg/g, and 1.93 mg/g, respectively.

A Study on the Calibration of Shape Measurement System Using Digital moire (Digital moire 형상측정 시스템의 보정에 관한 연구)

  • 유원재;김도훈;안재웅;강영준;노형민
    • Proceedings of the Korean Society of Precision Engineering Conference
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    • 2002.05a
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    • pp.199-202
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    • 2002
  • Moire topography method is a well-known non-contacting 3-D measurement method. Recently, the automatic 3-D measurement by moire topography has been required since the method was frequently applied to the engineering and medical fields. 3-D measurement using digital projection moire topography is very attractive because of its high measuring speed and high sensitivity. In this paper, using different N-bucket algorithm method of digital projection moire topography is tested to measuring object with the 2$\pi$-ambiguity problem. Experimental results prove that the proposed scheme is capable of finding measurement errors that decreased more by using the flour-three step algorithm method than the same step in the phase shifting of different pitchs.

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Electrical Power and Energy Reference Measurement System with Asynchronous Sampling (비동기 샘플링에 의한 전력과 에너지 측정 기준시스템)

  • Wijesinghe, W.M.S.;Park, Young-Tae
    • Proceedings of the KIEE Conference
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    • 2009.07a
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    • pp.684_685
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    • 2009
  • A digital sampling algorithm that uses a two high resolution integrating Voltmeters which are synchronized by Phase Lock Loop (PLL) time clock for accurately measuring the parameters, active and reactive power, for sinusoidal power measurements is presented. The PLL technique provides high precision measurements, root mean square (rms), phase and complex voltage ratio, of the AC signal. The system has been designed to be used at the Korean Research Institute of Standards and Science (KRISS) as a reference power standard for electrical power calibrations. The test results have shown that the accuracy of the measurements is better than $10 {\mu}W/VA$ and the level of uncertainty is valid for the power factor range zero to 1 for both lead and lag conditions. The system is fully automated and allows power measurements and calibration of high precision wattmeters and power calibrators at the main power frequencies 50 and 60 Hz.

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