• Title/Summary/Keyword: Ion chromatography system

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Determination of Halogen Elements in Volatile Organohalogen Compounds by the Wickbold Combustion Pretreatment Method and Ion Chromatography

  • Lee, Dong-Ho;Kwon, Soo-Han;Kim, Soo-Hwan;Lee, Sang-Hun;Min, Bum-Chan
    • Bulletin of the Korean Chemical Society
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    • v.28 no.1
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    • pp.59-62
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    • 2007
  • A quantitative analysis method of halogen elements in volatile organohalogen compounds was established by the Wickbold combustion pretreatment in an enclosed system and ion chromatography. The sample pretreatment parameters of Wickbold combustion were experimentally optimized, and using the determined optimal pretreatment parameters, the reproducibility was estimated by ion chromatography. As a comparison for real samples, NIST certified reference materials (CRMs) were analyzed for the recovery efficiency and reproducibility.

Qualitative Analysis of the Major Constituents in Traditional Oriental Prescription Bang-poong-tong-sung-san by Liquid Chromatography/Ultraviolet Detector/Ion-Trap Time-of-Flight Mass Spectrometry

  • Eom, Han Young;Kim, Hyung-Seung;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.24-29
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    • 2014
  • An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

Ion-Pair Chromatography of Aromatic Carboxylic Acids on the Reversed-phase System (역상계에서 방향족 카르복시산류의 이온-쌍 크로마토그래피)

  • Hae-Beom Oh;Sam-Woo Kang;Seung-Seok Lee
    • Journal of the Korean Chemical Society
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    • v.30 no.3
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    • pp.312-319
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    • 1986
  • Dodecyltrimethylammonium bromide (DTAB) was examined as a counter-ion in the investigation of capacity factor and separation of aromatic carboxylic acids on alkyl-modified silica (ODS) column as a stationary phase by ion-pair chromatography on reversed-phase system. The capacity factor of samples was influenced by the several factors such as a concentration of counter-ion as well as kinds and concentration of electrolyte, concentration of methanol in mobile phase and kinds and position of functional group in sample molecule. Some mixtures of samples were able to be separated under optimum condition.

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Direct Determination of Total Arsenic and Arsenic Species by Ion Chromatography Coupled with Inductively Coupled Plasma Mass Spectrometry

  • Nam, Sang-Ho;Kim, Jae-Jin;Han, Soung-Sim
    • Bulletin of the Korean Chemical Society
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    • v.24 no.12
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    • pp.1805-1808
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    • 2003
  • The simultaneous determination of As(III), As(V), and DMA has been performed by ion chromatography (IC) coupled with inductively coupled plasma-mass spectrometry (ICP-MS). The separation of the three arsenic species was achieved by an anionic separator column (AS 7) with an isocratic elution system. The separated species were directly detected by ICP-MS as an element-selective detection method. The IC-ICP-MS technique was applied for the determination of arsenic species in a NIST SRM 1643d water sample. An As(III) only was detected in the sample. The detection limits of As(III), As(V) and DMA were 0.31, 0.45, and 2.09 ng/mL, respectively. It was also applied for the determination of arsenic species in a human urine obtained by a volunteer, and three arsenic species were identified. The determination of total As in human urines that were obtained from 25 volunteers at the different age was also carried out by ICP-MS.

Simultaneous Determination of Anions and Cations in Natural Water by Ion-exclusion/Cation-exchange Chromatography with a Weakly Acidic Cation-exchange Resin Column

  • Lee, Kwang-Pill;Choi, Seong-Ho;Park, Yu-Chul;Bae, Zun-Ung;Lee, Mu-Sang;Lee, Sang-Hak;Chang, Hye-Yong;Kwon, Se-Mok;Kazuhiko Tanaka
    • Bulletin of the Korean Chemical Society
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    • v.24 no.9
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    • pp.1324-1328
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    • 2003
  • The simultaneous determination of anions ($SO_4 ^{2-},\;Cl^-,\;and\;NO_3^-$) and cations ($Na^+,\;NH^{4+},\;K^+,\;Mg^{2+},\;and\;Ca^{2+}$) in natural water obtained by Nakdong River waters system in Korea were performed by ion-exclusion/cationexchange chromatography with conductimetric detection. The stationary phase was a polymethacrylate-based weakly acidic cation-exchange resin column in the $H^+$-form and a weak-acid eluent. When using only a 1.4 mM sulfosalicylic acid/6 mM 18-crown-6 ether as an eluent, good resolution of both anions and cations, minimum time required for the separation, and satisfactory detection sensitivity were obtained in a reasonable time. The method was successfully applied to the simultaneous determination of anions and cations in natural waters.

Uncertainties of ionic species in snowpit samples determined with ion chromatography system (이온크로마토그래피 시스템을 이용한 눈 시료의 이온성분 측정자료의 불확도 산출)

  • Hong, Sang-Bum;Hur, Soon-Do;Kim, Sun-Mee;Hong, Sungmin;Chung, Ji-Woong;Kang, Namgoo;Kang, Chang-Hee
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.350-363
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    • 2012
  • To determine ionic species in snowpit samples using ion chromatography system, we described the performance of ion chromatography(IC) system, cleaning method of bottle, and interference by filtering procedure. The limit of detection, reproducibilities, and accuracies determined with BCR$^{(R)}$-408 were 0.01-0.26 ${\mu}g$/L, 0.4-17.4%, 4.5-12.0% for cations and 0.02-0.26 ${\mu}g/L$, 0.1-27.6%, 1.3-5.6% for anions, respectively. Lab blank test for sample bottle indicated that $CH_3CO_2{^-}$, $HCO_2{^-}$, and $NH_4{^+}$ can be easily contaminated in the lab environment. The positive interferences of $NO_3{^-}$ were partly attributed to the cleaning method of bottle. The filtering of melted snow sample should be carefully applied because it can positively affect the concentration levels of some ionic species. Finally, this method was applied to measure ionic species in snowpit samples from the upward area near NEEM camp and the uncertainties of measurement data of $F^-$ were also estimated.

Ion-Pair Chromatography of Organic and Inorganic Anions (유기 및 무기음이온에 대한 이온쌍크로마토그래피)

  • Sam Woo Kang
    • Journal of the Korean Chemical Society
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    • v.29 no.4
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    • pp.365-371
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    • 1985
  • A cationic dye, methylene blue $(MTB^+)$ was examined as a counter ion in the separation of organic and inorganic anions by ion-pair chromatography. Nonabsorbing anions could be indirectly detected by photometric detector with the assistance of MTB^+ in visible range (665nm). A mixture of anions was able to be separated with good base line resolution and high sensitivity. The capacity factors were also determined in various experimental conditions to study retention mechanism. The retention followed the ion-interaction model where the $MTB^+$ occupies a primary layer at the stationary phase while the analyte anion and other anions in the system compete for forming the secondary layer.

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Development of Continuous Flow Microwave Digestion Procedures for Analysis of Trace Metal in Water Using Ion Chromatography

  • Youn Doo Kim;Gae Ho Lee;Hyung Seung Kim;Dong Soo Kim;Kwang Kyu Park
    • Bulletin of the Korean Chemical Society
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    • v.15 no.9
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    • pp.786-791
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    • 1994
  • A simple and rapid sample pretreatment process necessary for determination of metal oxides in water was proposed. Samples were injected into the continuous-flow tube installed inside the microwave oven and the treated samples were cooled before entered to the Ion Chromatography (IC) or Inductively Coupled Plasma (ICP). By coupling this microwave digestion system with IC or ICP, a fully automatic analytical procedures may be easily established. In this study, two different types of digestion methods were considered; the open tubing method (OTM) and the restraint tubing method (RTM). The RTM was proved to be 3 times faster in digestion period and 10 times higher in detection range than the OTM. Validation of proposed sample digestion system was carried out by using an ICP. The results showed that both of continuous-flow methods, the OTM and the RTM were comparable in accuracies with the conventional batch-type vessel digestion method.

Development of the Purification Method of Ovotransferrin in Egg White (난백 내 Ovotransferrin의 분리방법에 관한 연구)

  • Jang, A.;Jo, Y.J.;Lee, M.;Kim, J.C.
    • Journal of Animal Science and Technology
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    • v.47 no.6
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    • pp.1025-1032
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    • 2005
  • This study was carried out to separate ovotransferrin in chicken egg white by gel chromatography and heparin affinity chromatography. In gel filtration which was performed with 50mM Phosphate buffer (pH 7.2, 0.15M salt) at a flow rate of 2.0 ml/min, ovotransferrin and ovalbumin were eluted together in fraction number 11-16. In order to separate pure ovotransferrin, fraction No. 12-14 of them which have high concentration of ovotransferrin were concentrated and rechromatographed. However, the ovotransferrin did not separated clearly. In heparin affinity chromatography, the separation was performed with 50mM ethylaminetetraacetic acid (EDTA, pH7.2) and 50mM Phosphate buffer (pH 7.2, 0.15M salt contained) on ferrous and ferric ion saturated column at as same flow rate as gel filtration system's. Ovotransferrin and albumin were eluted together at 10-15min (fraction No.3) and 15-20min (fraction No.4), respectively. However, purified ovotransferrin was eluted at 156-165min and 165-175min (tube No.32-33) with 50 mM phosphate buffer (pH 7.2, 0.15M salt free), respectively. Heparin affinity chromatography with ferric ion saturated column was resulted in the best separation of ovotransferrin rather than separation by gel chromatography and ferrous ion saturated heparin affinity chromatography.

Detectio of Malonaldehyde-thiobarbituric Acid (MA-TBA) Complex by High Performance Liquid Chromatography(HPLC) in a Model System

  • Whang, Key
    • Preventive Nutrition and Food Science
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    • v.4 no.3
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    • pp.167-170
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    • 1999
  • Various concentrations of malonaldehyde (MA) produced upon hydrolysis of 1, 1, 3,3-tetraethoxypropane (TEP) were reacted with 2-thiobarbituric acid (TBA)and th e contents of MA-TBA complex were measured both with spectrophotometer and high performance liquid chromatography (HPLC). As the concentrations of MA-TBA increased, their absorbances and the corresponding HPLC peak areas increased. The correlation coefficient between absorbances and HPLC peak areas of MA-TBA peaks from the other compounds and butanol extraction of the complex increased its recovery its recovery by 29.4% . Measurement of the content of MA-TBA complex for monitoring the development of lipid oxidation was proven to be successful with the use of high performance liquid chromatography.

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