• Title/Summary/Keyword: liquid-solid phase separation

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A Study on the Densifcation of Stellite Fine Powder for Iniection Molding (사출성형용 Stellite미분말의 소결 치밀화에 관한 연구)

  • 임태환
    • Journal of Powder Materials
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    • v.4 no.2
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    • pp.113-121
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    • 1997
  • The densification of the compacts of Co+32%Cr+20%W+l.5%C, Co+32%Cr+20%W+3.0%C and Co+32%Cr+20%W+4.5%C sintered under $H_2$ gas or vacuum was investigated. The effect of V and B addition on the densification was also investigated. The densification of these compacts were always incomplete regardless of sintering atmosphere, temperature and time. The amounts of oxygen and carbon in compacts sintered in $H_2$ for 3.6ks at 1523K were 0.105~0.160 mass% and 0.33~0.89 mass%, respectively. And those in vacuum were 0.028~0.032% and 0.957~4.08%, respectively. Relative density(Ds) of Co+29%Cr+17%W+3.0%C compact containing 6%V and Co+32%Cr+20%W+2.97%C compact containing 0.03%B were 99 and 100%, respectively, indicating complete densification by solid phase sintering. Victors hardness of sintered compacts containing 6%V or 0.03%B were 632 and 568, showing 50~60% increase in comparison to those without V or B. These results can be explained in terms of oxidation/reduction of oxides and equilibrium pressure of CO in isolated pore, instead of presence of liquid formation and grain boundary separation from pores due to large grain growth.

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Solid Phase Extraction(SPE) of Curcuminoids from Turmeric by Optimization Analytical Condition (최적 분석조건에 의한 강황으로부터 Curcuminoids의 고체상추출(SPE))

  • Lee, Kwang Jin;Ma, Jin Yeul;Kim, Young Jun;Kim, Young Sik
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.13 no.10
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    • pp.4927-4935
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    • 2012
  • Turmeric is a medicinal herb with various pharmacological activities. Curcumin, demethoxycurcumin(DMC) and bisdemethoxycurcumin(BDMC) were extracted from turmeric by dipping and ultrasonic wave method. And extraction efficiency was identified using solid phase extraction(SPE). The extracted sample were simultaneously separated and analyzed from three kinds of commercial $C_{18}$ reversed-phase high performance liquid chromatography using water and acetonitrile as mobile phase with isocratic elution mode. Flow rate 1.0mL/min, injection volume $10{\mu}L$ and column oven temperature $40^{\circ}C$ at 425nm wavelength has been conducted. From the experimental results, the optimum mobile phase composition of water/acetonitrile 50/50vol% using RS tech column. It is evident that the amount of curcuminoids extracted(extraction time 4h) by 100% MeOH was higher than any aqueous MeOH composition. Finally, in 100% water extraction, the amount(mAU${\times}$mim) of curcuminoids extracted by SPE was 14.3 and 24.5 times respectively higher than ultrasonic wave and dipping method. The shown results can be applied as sources for pharmaceuticals and functional material.

Separation and recovery of semi-volatile substances of Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus by reduced pressure collections and GC-MS

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
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    • v.33 no.1
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    • pp.11-22
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    • 2020
  • When extracting semi-volatile components of herbal medicines using hot water vapor, some substances may react with water vapor or oxygen, and some volatile substances may be lost, when using an organic solvent extraction method has the disadvantage that it may contain a non-volatile material and residual organic solvent. In addition, it is inefficient to separate semi-volatile substances from herbal medicines into each single component and conduct biological activity research for each component to determine the effective ingredient, and some components may be lost in the separation process. In this study, semi-volatile substances evaporated under two pressure-reduced conditions in Chinese herbal medicines such as Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were separated by cooling with liquid nitrogen. Those were analyzed by gas chromatography-mass spectrometry (GC-MS) to identify the components, and this method may be used to study biological activities at the cellular level. The substances separated under reduced pressure, essential oil obtained by simultaneous distillation extraction (SDE) method and substances by using solid phase micro-extraction (SPME) from Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were analyzed by GC-MS. In the case of Cnidii Rhizoma and Aucklandiae Radix, there were some differences among the essential oil components obtained by SDE and those identified by low temperature capture (CT) and SPME method, these were believed to be produced by some volatiles reacting with water or oxygen at the boiling point temperature of water.

Quantitative Analysis and Enantiomeric Separation of Ephedra Alkaloids in Ma Huang Related Products by HPLC-DAD and UPLC-MS/MS

  • Kyoung-Moon Han;Jinwoo Hwang;Sun Hee Lee;Boreum Park;Hyungil Kim;Sun Young Baek
    • Natural Product Sciences
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    • v.28 no.4
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    • pp.168-180
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    • 2022
  • Ephedra is a genus of the Ephedraceae family and is found in temperate regions, such as Central Asia and Europe. Among the various ephedra species, Ma Huang (Ephedra herb) is derived from the aerial parts of Ephedra sinica S tapf, Ephedra equisetina Bunge, and Ephedra intermedia Schrenk & C.A. Mey. Ma Huang contains various ephedra alkaloids, including (-)-ephedrine, (+)-pseudoephedrine, (-)-norephedrine, (+)-norpseudoephedrine, (-)-methylephedrine, and (+)-methylpseudoephedrine, which are found naturally as single enantiomers, although they can be prepared as racemates. Although the use of Ma Huang in foods is prohibited in Korea, products containing Ma Huang can be imported, and so it is necessary to develop a suitable analytical technique for the detection of Ma Huang in foods. Herein, we report the development of analytical methods for the detection of ephedra alkaloids in products containing Ma Huang. Following sample purification by solid phase extraction, quantitative analysis was performed using ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). Additionally, the enantiomers were successfully separated using HPLC-DAD. We successfully analyzed various food samples, where the ephedra alkaloids were qualitatively and quantitatively determined, and the enantiomers were separated. It is expected that these methods may contribute toward preventing the distribution of illegal products containing Ma Huang.

Optimization of solid-phase extraction for the liquid chromatography-tandem mass spectrometry analysis of basic drugs in equine urine (액체크로마토그래피-텐덤질량분석법을 위한 경주마 소변 중 염기성 약물의 고체상 추출법 최적화)

  • Shin, Hyun Du;Yang, Ji Suk;Jung, Mihye;Kim, Hyung-Seung;Youm, Jeong-Rok;Hu, Man Bae;Kim, Sung Jean;Han, Sang Beom
    • Analytical Science and Technology
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    • v.21 no.5
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    • pp.412-423
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    • 2008
  • A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.

An Investigation of Interfacial Strength in Epoxy-based Solid Polymer Electrolytes for Structural Composite Batteries

  • Mohamad A. Raja;Su Hyun Lim;Doyun Jeon;Hyunsoo Hong;Inyeong Yang;Sanha Kim;Seong Su Kim
    • Composites Research
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    • v.36 no.6
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    • pp.416-421
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    • 2023
  • Multifunctional composite materials capable of both load-carrying and energy functions are promising innovative candidates for the advancement of contemporary technologies owing to their relative feasibility, cost-effectiveness, and optimized performance. Carbon fiber (CF)-based structural batteries utilize the graphitic inherent structure to enable the employment of carbon fibers as electrodes, current collectors, and reinforcement, while the matrix system is an ion-conduction and load transfer medium. Although it is possible to enhance performance through the modification of constituents, there remains a need for a systematic design methodology scheme to streamline the commercialization of structural batteries. In this work, a bi-phasic epoxy-based ionic liquid (IL) modified structural battery electrolyte (SBE) was developed via thermally initiated phase separation. The polymer's morphological, mechanical, and electrochemical characteristics were studied. In addition, the interfacial shear strength (IFSS) between CF/SBE was investigated via microdroplet tests. The results accentuated the significance of considering IFSS and matrix plasticity in designing composite structural batteries. This approach is expected to lay the foundation for realizing smart structures with optimized performance while minimizing the need for extensive trial and error, by paving the way for a streamlined computational design scheme in the future.

Examining the Effect of L/W Ratio on the Hydro-dynamic Behavior in DAF System Using CFD & ADV Technique (전산유체역학과 ADV기술을 이용한 장폭비의 DAF조내 수리흐름에 미치는 영향 연구)

  • Park, No-Suk;Kwon, Soon-Bum;Lee, Sun-Ju;Bae, Chul-Ho;Kim, Jeong-Hyun;Ahn, Hyo-Won
    • Journal of Korean Society of Water and Wastewater
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    • v.19 no.4
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    • pp.421-428
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    • 2005
  • Dissolved air flotation (OAF) is a solid-liquid separation system that uses fine bubbles rising from bottom to remove particles in water. In this study, we investigated the effect of L/W (L; Length, W; Width) on the hydro-dynamic behavior in DAF system using CFD (Computational Fluid Dynamics) and ADV (Acoustic Doppler Velocimetry) technique. The factual full-scale DAF system, L/W ratio of 1:1, was selected and various L/W ratio (2:1, 3:1, 4:1 and 5:1) conditions were simulated with CFD. For modelling, 2-phase (gas-liquid) flow equations for the conservation of mass, momentum and turbulence quantities were solved using an Eulerian-Eulerian approach based on the assumption that very small particle is applied in the DAF system. Also, for verification of CFD simulation results, we measured the factual velocity at some points in the full-scale DAF system with ADV technique. Both the simulation and the measurement results were in good accordance with each other. As the results of this study, we concluded that L/W ratio and outlet geometry play important role for flow pattern and fine bubble distribution in the flotation zone. In the ratio of 1:1, the dead zone is less than those in other cases. On the other hands, in the ration of 3:1, the fine bubbles were more evenly distributed.

In Situ Observation of Solidification Behavior in Undercooled $Pd_{40}Cu_{30}Ni_{10}P_{20}$ Alloy Melts during Linear Cooling (연속냉각 중 과냉 된 $Pd_{40}Cu_{30}Ni_{10}P_{20}$ 합금 용탕의 실시간 응고거동 관찰)

  • Kim, Ji-Hun
    • Journal of Korea Foundry Society
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    • v.23 no.5
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    • pp.276-285
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    • 2003
  • In the undercooled melt of $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy, the solidification behavior including nucleation and growth of crystals at the micrometer level has been observed in-situ by use of a confocal scanning laser microscope combined with an infrared image furnace. The $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy specimens were cooled from the liquid state to glass transition temperature. 575 K, at various cooling late under a helium gas flow. According to the cooling rate, the morphologies of the solidification front are changed among various types, irregular jog like front, columnar dendritic front, cellular grain, star like shape jog and fine grain, etc. The velocities of the solid-liquid interface are measured to be $10^{-5}{\sim}10^{-8}$ m/s which are at least two orders higher than the theoretical crystal growth rates. Combining the morphologies observed in terms of cooling rates and their solidification behaviors, we conclude that phase separation takes place in the undercooled molten $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy. The continuous cooling transformation (CCT) diagram was constructed from solidification onset time at various linear cooling conditions with different rate. The CCT diagram suggests that the critical cooling rate for glassy solidification is about 1.5 K/s, which is in agreement with the previous calorimetric findings.

Validation of Analytical Method for Male Sex Hormone Monitoring in Urine due to the Chemical Castration (성충동약물치료 시행에 따른 소변 중 남성호르몬의 분석법 확립)

  • Jeong, Sujin;Baeck, Seungkyung;Park, Sunhye;Son, Kkonnip;Park, Yonghoon;Lee, Sangki
    • YAKHAK HOEJI
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    • v.57 no.5
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    • pp.330-336
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    • 2013
  • "The Act on Medication Treatment of Sexual Impulse of Sex Offenders" known as chemical castration has been effective since July 2011 in Korea. According to the law, monitoring of male sex hormone in urine is enforced to request National Forensic Service more than once a month after injection of medicine designed to reduce sex impulse. We established a rapid and sensitive method for the monitoring of testosterone (T) and epitestosterone (E) in human urine by liquid chromatography with tandem mass spectrometry (LC-MS/MS). Three mL of urine was pretreated by solid-phase extraction for purification and performed enzymatic hydrolysis. The pretreated samples were extracted twice with 2 ml of ethyl acetate and n-hexane (2 : 3). The separation was applied on Thermo Hypersil GOLD C18 column ($1.9{\mu}m$, $100{\times}2.1mm$). A gradient elution of methanol and water of 0.1% formic acid were used as mobile phase and the retention time was less than 10 min. LC-MS/MS system coupled with an electrospray ionization source was performed in multiple reaction monitoring mode. The transitions of the analytes executed as following: m/z $289{\rightarrow}97$, 109 for T and E, m/z $292{\rightarrow}109$ for $T-d_3$ and $E-d_3$ as internal standards. The validation results of the method were satisfactory. The limits of detection were 0.05 ng/ml and the limits of quantification were 0.1 ng/ml. This method was successfully applied to real human urine sample. The developed method will be useful for monitoring T/E ratio in urine of sex offenders.

Concentration and Environmental Loading of Veterinary Antibiotics in Agricultural Irrigation Ditches

  • Kim, Sung-Chul;Chung, Doug Young;Kim, Kye Hoon;Lee, Ja Hyun;Kim, Hyo Kyung;Yang, Jae E.;Ok, Yong Sik;Almarwei, Yaser A.O.
    • Korean Journal of Soil Science and Fertilizer
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    • v.45 no.6
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    • pp.867-876
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    • 2012
  • The concentration of veterinary antibiotics in aqueous and sediment matrices was measured in agricultural irrigation ditches bordering several animal-feeding operations (AFOs) and then compared to its concentration in the watershed. Analytical determination in aqueous samples was based on solid phase extraction (SPE) and appropriate buffer solutions were used to extract residuals in sediment samples. Separation and detection of extracted veterinary antibiotics were performed with high performance liquid chromatograph tandem mass spectrometry (HPLC/MS/MS). In general, higher concentrations of antibiotic were observed in the aqueous phase of irrigation ditches, with the highest concentration of erythromycin hydrochloride (ETM-$H_2O$) of $0.53{\mu}g\;L^{-1}$, than in aqueous watershed samples. In contrast, higher concentrations were measured in river sediment than in irrigation ditch sediment with the highest concentration of oxytetracycline of $110.9{\mu}g\;kg^{-1}$. There was a high calculated correlation ( > 0.95) between precipitation and measured concentration in aqueous samples from the irrigation ditches for five of the ten targeted veterinary antibiotics, indicating that surface runoff could be an important transport mechanism of veterinary antibiotics from field to environment. Further, environmental loading calculation based on measured concentrations in aqueous samples and flow information clearly showed that irrigation ditches were 18 times greater than river. This result suggests the likelihood that veterinary antibiotics can be transported via irrigation ditches to the watershed. The transport via surface runoff and likely environmental loading via irrigation ditches examined in this study helps identify the pathway of veterinary antibiotics residuals in the environment.