• Title/Summary/Keyword: Liquid-coupled

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The separation of arsenic metabolites in urine by high performance liquid chromatography-inductively coupled plasma-mass spectrometry

  • Chung, Jin-Yong;Lim, Hyoun-Ju;Kim, Young-Jin;Song, Ki-Hoon;Kim, Byoung-Gwon;Hong, Young-Seoub
    • Environmental Analysis Health and Toxicology
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    • v.29
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    • pp.18.1-18.9
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    • 2014
  • Objectives The purpose of this study was to determine a separation method for each arsenic metabolite in urine by using a high performance liquid chromatography (HPLC)-inductively coupled plasma-mass spectrometer (ICP-MS). Methods Separation of the arsenic metabolites was conducted in urine by using a polymeric anion-exchange (Hamilton PRP X-100, $4.6mm{\times}150mm$, $5{\mu}m$) column on Agilent Technologies 1260 Infinity LC system coupled to Agilent Technologies 7700 series ICP/MS equipment using argon as the plasma gas. Results All five important arsenic metabolites in urine were separated within 16 minutes in the order of arsenobetaine, arsenite, dimethylarsinate, monomethylarsonate and arsenate with detection limits ranging from 0.15 to $0.27{\mu}g/L$ ($40{\mu}L$ injection). We used G-EQUAS No. 52, the German external quality assessment scheme and standard reference material 2669, National Institute of Standard and Technology, to validate our analyses. Conclusions The method for separation of arsenic metabolites in urine was established by using HPLC-ICP-MS. This method contributes to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies for arsenic exposure in South Korea.

Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

  • Yim, Yong-Hyeon;Park, Ji-Youn;Han, Myung-Sub;Park, Mi-Kyung;Kim, Byung-Joo;Lim, Young-Ran;Hwang, Eui-Jin;So, Hun-Young
    • Bulletin of the Korean Chemical Society
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    • v.26 no.3
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    • pp.440-446
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    • 2005
  • A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

Influence of Resin-Infiltrated Time on Wood Natural Materials Using Conventional/Air-Coupled Ultrasound Waves

  • Park, Je-Woong;Kim, Do-Jung;Kweon, Young-Sub;Im, Kwang-Hee;Hsu, David K.;Kim, Sun-Kyu;Yang, In-Young
    • Journal of the Korean Society for Nondestructive Testing
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    • v.29 no.3
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    • pp.235-241
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    • 2009
  • Composite wood materials are very sensitive to water and inspection without any coupling medium of a liquid is really needed to wood materials due to the permeation of coupling medium such as water. However, air-coupled ultrasound has obvious advantages over water-coupled experimentation compared with conventional C-scanner. In this work, it is desirable to perform contact-less nondestructive evaluation to assess wood material homogeneity. A wood material was nondestructively characterized with non-contact and contact modes to measure ultrasonic velocity using automated data acquisition software. We have utilized a proposed peak-delay measurement method. Also through transmission mode was performed because of the main limitation for air-coupled transducers, which is the acoustic impedance mismatch between most materials and air. The variation of ultrasonic velocity was found to be somewhat difference due to air-coupled limitations over conventional scan images. However, conventional C-scan images are well agreed with increasing the resin-infiltrated time as expected. Finally, we have developed a measurement system of an ultrasonic velocity based on data acquisition software for obtaining ultrasonic quantitative data for correlation with C-scan images.

Simultaneous Determination of Triterpenoid Saponins from Pulsatilla koreana using High Performance Liquid Chromatography Coupled with a Charged Aerosol Detector (HPLC-CAD)

  • Yeom, Hye-Sun;Suh, Joon-Hyuk;Youm, Jeong-Rok;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.31 no.5
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    • pp.1159-1164
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    • 2010
  • Several triterpenoid saponins from root of Pulsatilla koreana Nakai (Ranunculaceae) were studied and their biological activities were reported. It is difficult to analyze triterpenoid saponins using HPLC-UV due to the lack of chromophores. So, evaporative light scattering detection (ELSD) is used as a valuable alternative to UV detection. More recently, a charged aerosol detection (CAD) has been developed to improve the sensitivity and reproducibility of ELSD. In this study, we developed and validated a novel method of high performance liquid chromatography coupled with a charged aerosol detector for the simultaneous determination of four triterpenoid saponins: pulsatilloside E, pulsatilla saponin H, anemoside B4 and cussosaponin C. Analytes were separated by the Supelco Ascentis$^{(R)}$ Express C18 column (4.6 mm ${\times}$ 150 mm, 2.7 ${\mu}m$) with gradient elution of methanol and water at a flow rate of 0.8 mL/min at $30^{\circ}C$. We examined various factors that could affect the sensitivity of the detectors, including various concentrations of additives, the pH of the mobile phase, and the CAD range. Linear calibration curves were obtained within the concentration ranges of 2 - 200 ${\mu}g$/mL for pulsatilloside E, anemoside $B_4$ and cussosaponin C, and 5 - 500 ${\mu}g$/mL for pulsatilla saponin H with correlation coefficient ($R^2$) greater than 0.995. The limit of detection (LOD) and quantification (LOQ) were 0.04 - 0.2 and 2 - 5 ${\mu}g$/mL, respectively. The validity of the developed HPLC-CAD method was confirmed by satisfactory values of linearity, intra- and inter-day accuracy and precision. This method could be successfully applied to quality evaluation, quality control and monitoring of Pulsatilla koreana.

The Effects of Sloshing on the Responses of an LNG Carrier Moored in a Side-by-side Configuration with an Offshore Plant (해양플랜트에 병렬 계류된 LNG 운반선의 거동에 슬로싱이 미치는 영향)

  • Lee, Seung-Jae
    • Journal of Ocean Engineering and Technology
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    • v.24 no.5
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    • pp.16-21
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    • 2010
  • During the loading/offloading operation of a liquefied natural gas carrier (LNGC) that is moored in a side-by-side configuration with an offshore plant, sloshing that occurs due to the partially filled LNG tank and the interactive effect between the two floating bodies are important factors that affect safety and operability. Therefore, a time-domain software program, called CHARM3D, was developed to consider the interactions between sloshing and the motion of a floating body, as well as the interactions between multiple bodies using the potential-viscous hybrid method. For the simulation of a floating body in the time domain, hydrodynamic coefficients and wave forces were calculated in the frequency domain using the 3D radiation/diffraction panel program based on potential theory. The calculated values were used for the simulation of a floating body in the time domain by convolution integrals. The liquid sloshing in the inner tanks is solved by the 3D-FDM Navier-Stokes solver that includes the consideration of free-surface non-linearity through the SURF scheme. The computed sloshing forces and moments were fed into the time integration of the ship's motion, and the updated motion was, in turn, used as the excitation force for liquid sloshing, which is repeated for the ensuing time steps. For comparison, a sloshing motion coupled analysis program based on linear potential theory in the frequency domain was developed. The computer programs that were developed were applied to the side-by-side offloading operation between the offshore plant and the LNGC. The frequency-domain results reproduced the coupling effects qualitatively, but, in general, the peaks were over-predicted compared to experimental and time-domain results. The interactive effects between the sloshing liquid and the motion of the vessel can be intensified further in the case of multiple floating bodies.

A Study of Analytical Method for Trace Metal Ions in Whole Blood and Urine by Inductively Coupled Plasma-Mass Spectrometry using Solid-Liquid Extraction Technique (유도결합 플라스마-질량분석법과 고체-액체 추출법을 이용한 혈액 및 소변중 미량금속의 분석에 관한 연구)

  • Lee, Won;Hur, Young-Hoe;Park, Kyung-Su
    • Analytical Science and Technology
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    • v.11 no.4
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    • pp.281-291
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    • 1998
  • An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in blood and urine has been investigated by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Microwave oven was used for the pretreatment of blood samples using nitric acid and hydrogen peroxide in a closedvessel digestion system with 1 mL whole blood for 8 minutes. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Detection limits for Cu, Sn, and Bi by this method were 0.000375 ng/mL, 0.000297 ng/mL, and 0.000174 ng/mL, respectively. Recoveries of 99.1% for Cu, 102.5% for Sn, and 98.4% for Bi were obtained for the standard spiked NIST SRM 955a blood sample. The developed method was applied for whole real blood and urine samples.

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Rapid separation and identification of 31 major saponins in Shizhu ginseng by ultra-high performance liquid chromatography-electron spray ionization-MS/MS

  • Sun, Ting-Ting;Liang, Xin-Lei;Zhu, He-Yun;Peng, Xu-Ling;Guo, Xing-Jie;Zhao, Long-Shan
    • Journal of Ginseng Research
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    • v.40 no.3
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    • pp.220-228
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    • 2016
  • Background: Among the various ginseng strains, Shizhu ginseng is endemic to China, mainly distributed in Kuandian Manchu Autonomous County (Liaoning Province, China); however, not much is known about the compounds (especially saponins) in Shizhu ginseng. Methods: A rapid, sensitive, and reliable ultra-high performance liquid chromatography coupled with MS/MS (UHPLC-MS/MS) method was developed to separate and identify saponins in Shizhu ginseng. Results: The separation was carried out on a Waters ACQUITY UPLC BEH $C_{18}$ column ($100mm{\times}2.1mm$, $1.7{\mu}m$) with acetonitrile and 0.1% formic acid aqueous solution as the mobile phase under a gradient elution at $40^{\circ}C$. The detection was performed on a Micromass Quattro Micro API mass spectrometer equipped with electrospray ionization source in both positive and negative modes. Under the optimized conditions, a total of 31 saponins were identified or tentatively characterized by comparing retention time and MS data with related literatures and reference substances. Conclusion: The developed UHPLC-MS/MS method was suitable for identifying and characterizing the chemical constituents in Shizhu ginseng, which provided a helpful chemical basis for further research on Shizhu ginseng.

Variable Optical Attenuator using Optical Coupling between a Side Polished Fiber and Refractive Index Matching Liquid (측면 연마된 광섬유와 굴절률 정합액사이의 광결합을 이용한 가변 광 감쇠기)

  • Kim, Kwang-Taek;Song, Jae-Won
    • Journal of the Korean Institute of Telematics and Electronics D
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    • v.36D no.9
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    • pp.50-55
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    • 1999
  • In this paper we proposed a variable optical attenuator using the side polished fiber coupled with a refractive index matching liquid. Small variation of refractive index of matching liquid can induce very large change of optical loss due to the coupling between the fiber mode and radiation mode. The thermo-optic effect of matching liquid was used to ontrol the optical attenuation. The side polished fiber block was fabricated using the silicon V gloove. Experimental results showed that $5^{\circ}C$ temperature variation was enough to adjust full range attenuation. The polarization dependent loss and insertion loss of the fabricated devices were 0.5dB and 0.2dB respectively.

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Holographic Polymer-Dispersed Liquid Crystals and Polymeric Photonic Crystals Formed by Holographic Photolithography

  • Kyu Thein;Meng Scott;Duran Hatice;Nanjundiah Kumar;Yandek Gregory R.
    • Macromolecular Research
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    • v.14 no.2
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    • pp.155-165
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    • 2006
  • The present article describes the experimental and theoretical observations on the formation of holographic, polymer-dispersed, liquid crystals and electrically switchable, photonic crystals. A phase diagram of the starting mixture of nematic liquid crystal and photo-reactive triacrylate monomer was established by means of differential scanning calorimetry (DSC) and cloud point measurement. Photolithographic patterns were imprinted on the starting mixture of LC/triacrylate via multi-beam interference. A similar study was extended to a dendrimer/photocurative mixture as well as to a single component system (tetra-acrylate). Theoretical modeling and numerical simulation were carried out based on the combination of Flory-Huggins free energy of mixing and Maier-Saupe free energy of nematic ordering. The combined free energy densities were incorporated into the time-dependent Ginzburg-Landau (Model C) equations coupled with the photopolymerization rate equation to elucidate the spatio-temporal structure growth. The 2-D photonic structures thus simulated were consistent with the experimental observations. Furthermore, 3-D simulation was performed to guide the fabrication of assorted photonic crystals under various beam-geometries. Electro-optical performance such as diffraction efficiency was evaluated during the pattern photopolymerization process and also as a function of driving voltage.

High-Performance Liquid Chromatographic Determination of Cyclosulfamuron Residues in Soil, Water, Rice Grain and Straw

  • Lee, Young-Deuk;Kwon, Chan-Hyeok
    • Korean Journal of Environmental Agriculture
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    • v.23 no.4
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    • pp.251-257
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    • 2004
  • Analytical methods were developed to determine cyclosulfamuron residues in soil, water, rice grain and straw using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. In these methods, cyclosulfamuron was extracted with aqueous $Na_2HPO_4$/acetone and acetone/methanol mixture from soil and rice samples respectively. Liquid-liquid partition coupled with ion-associated technique, Florisil column chromatography, and solid-phase extraction (SPE) were used to separate cyclosulfamuron from interfering co-extractives prior to HPLC analysis. For water sample, the residue was enriched in $C_{18}$-SPE cartridge, cleaned up in situ, and directly subjected to HPLC. Reverse-phase HPLC under ion-suppression was successfully applied to determine cyclo-sulfamuron in sample extracts with the detection at its ${\lambda}_{max}$ (254 nm). Recoveries from fortified samples averaged $87.8{\pm}7.1%$ (n=12), $97.3{\pm}7.2%$ (n=12), $90.8{\pm}6.6%$ (n=6), and $78.5{\pm}6.7%$ (n=6) for soil, water, rice grain and straw, respectively. Detection limits of the methods were 0.004 mg/kg, 0.001 mg/L, 0.01 mg/kg and 0.02 mg/kg for soil, water, rice grain and straw samples, respectively.