• Title/Summary/Keyword: Eluent Concentration

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Determination of Trace Aldehydes in Ambient Air by Liquid Chromatography (액체 크로마토그래프법에 의한 대기시료중 미량 알데히드류의 정량)

  • 이용근;정태우
    • Journal of Korean Society for Atmospheric Environment
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    • v.11 no.4
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    • pp.339-349
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    • 1995
  • The purpose on this study is to optimize the chromatographic determination method of trace aldehydes in ambient air. Carbonyl compounds in urban air were trapped at $C_{18}$ DNPH-coated cartridges, and generated hydrazone derivatives were separated by HPLC and detected by UV-vis spectroscopic detector at 360nm. Formaldehyde and acetaldehyde compounds could be isolated from urban(Seoul) air with more than 95% collection efficiency. The analytical detection limits for formaldehyde and acetaldehyde are 0.06pp $b_{v}$, 0.08pp $b_{v}$ for 108 L air samples, respectively. The precision of this method are 3 .sim. 4%(RSD) for mutiple injection of hydrazone standards. Separation of seven dinitrophenylhydrazones could be achieved in appoximately 20 minutes operation time using $C_{18}$ column with apprepriate eluent. The method was applied to the analysis of aldehydes and ketone in Seoul ambient air. The 24-h ambient levels of formaldehyde, acetaldehyde reached up to 6 .sim. 14 and 3 .sim. 8ppbv, respectively. The daily average concentration ratio were 0.60 for acetaldehyde/formaldehyde.yde.

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Rapid Gas Chromatographic Screening of Saliva Samples for Organic Acids (기체크로마토그래피법에 의한 타액내 유기산의 신속한 스크리닝)

  • 김경례;김정한;박영준;김정옥
    • YAKHAK HOEJI
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    • v.39 no.3
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    • pp.283-288
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    • 1995
  • Rapid gas chromatographic profiling method was applied to saliva from healthy subjects for the analysis of free organic acids. Saliva samples were first saturated with NaHCO$_{3}$ and extracted with diethyl ether. The aqueous phase was solid-phase extracted using Chromosorb P as the adsorbent and diethyl ether as the eluent after the acidification and NaCl saturation, followed by triethylamine treatment. The resulting tiiethylammonium salts of acids were directly converted into stable tert.-butyl-dimethylsflyl derivatives, with subsequent analysis by dual-capiuary column gas chromatography and gas chromatograpy -mass spectrometry. From the ten saliva samples studied, twenty eight free organic acids including various fatty acids, hydroxy acids, dicarboxylic acids, md aromatic acids were tentatively identified. Among the acids identified , the concentration of lactic acid was highest for five saliva samples while $\alpha$-hydroxyisocaproic acid was most abundant for me sample, and succinic acid and glycolic acid for two samples. respectively. When the GC profiles were simplified to the corresponding acid retention index spectra of bar graphical form, they presented characteristic patterns for each individual.

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DETERMINATION OF TRIETHANOLAMINE BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH POST COLUMN REACTION

  • Kim, Jin-Woo;Kim, Seung-Jung;Lee, Bo-Seaub
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.14 no.1
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    • pp.1-15
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    • 1988
  • A new method for liquid chromatography with post column reaction is suggested for the separation and quantification of tertiary amines. A mixture of triethanolamine and N-ethyl diethanolamine was separated by a strong cation exchange column, followed by spectrophtometric detection of the blue colors generated from the reaction of each amine with the Folin-Ciocalteau reagent. The tertiary amines were properly separated when an eluent of pH 9.5 containing 0.5M sodium nitrate was used. Under this condition, calibration curve of triethanolamine in 2-10mg/100ml concentration range was attained. Good results were obtained when cream and shampoo preparations containing known amount of triethanolamine were analysed according to this method. In case the sample did not contain any other interfering reducing substances, the amine was quantitatively determined by the simple reaction of the samples with Folin-Ciocalteau reagent, and the subsequent spectrophotometric measurement.

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Separation of Optical Isomers of Amino Acids with Addition of Benzyl-L-proline Copper (II) Chelate by Reversed Phase Liquid Chromatography

  • Lee, Sun-Haing;Oh, Dae-Sub;Kim, Byoung-Eog
    • Bulletin of the Korean Chemical Society
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    • v.9 no.6
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    • pp.341-345
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    • 1988
  • Separation of optical isomers of dansyl amino acids by a reversed phase liquid chromatography has been accomplished by adding a copper (II) chelate of N-benzyl-L-proline to the mobile phase. The pH, the eluent composition and the concentration of copper (II) chelate all affect the optical separations. The elution orders between D and L DNS-amino acids were consistant except dansyl phenylalanine showing that D forms of DNS-amino acids elute earlier than L forms. These behaviors are different from the results obtained by the use of copper (II) proline. The retention mechanism for the optical separation of the dansyl amino acids can be explained by the equilibrium of liqand exchange and by hydrophobic interaction.

Elution Behavior of Copper(II) and Iron(II) Ions by Phenol Sulfonic Acid on Chelating Resin (킬레이트 수지에서 Phenol Sulfonic Acid에 의한 구리(Ⅱ)와 철(Ⅱ) 이온의 용리현상)

  • Cha, Ki Won;Hong, Jang Wook;Choi, Bae Du
    • Journal of the Korean Chemical Society
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    • v.42 no.3
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    • pp.292-296
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    • 1998
  • The elution behavior of copper(Ⅱ) and iron(Ⅱ) ions by phenol sulfonic acid(PSA) as an eluent on chelating resin, Amberlite IRC-718 have been investigated. When copper(Ⅱ) and iron(Ⅱ) solutions were adsorbed on the resin and eluted with various concentration of PSA, two peaks of each ion were appeared in the elution curve. These two peak areas were changed according to the PSA concentration. Using these phenomena, the stability constants of complex formation between the two ions and PSA were calculated. The values are 7.0 for copper(II) and $4.5{\times}10^4$ for iron(II), respectively.

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Sorption and Separation of Thiocyanate Gold and Silver Complexes and Determination of Gold by Diffuse Reflectance Spectroscopy

  • Danilenko, N.V.;Kononova, O.N.;Kachin, S.V.;Kholmogorov, A.G.;Dmitrieva, Zh.V.;Plotnikova, E.A.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.7
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    • pp.1019-1024
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    • 2004
  • The present paper is focused on simultaneous sorption concentration of gold (III) and silver (I) from thiocyanate solutions using high-selective anion exchanger AN-25 and subsequent separation of these ions at various concentrations of thiocarbamide (eluent). As a result, silver (I) ions are completely eluted from AN-25 and gold (III) ions remain in the resin phase and can be determined directly in the solid phase by diffuse reflection spectroscopy. It is proposed to use the sorption-spectroscopic method for Au(III) determination in aqueous solutions. The calibration curve is linear in the concentration range of 1-19 mg/L (sample volume is 10.0 mL) and the detection limit is 0.05 ${\mu}g/mL$. The presence of Cu(II), Co(II), Fe(II) do not hinder this determination. Au(III) was determined in industrial solutions.

Endophytic Diaporthe sp. ED2 Produces a Novel Anti-Candidal Ketone Derivative

  • Yenn, Tong Woei;Ring, Leong Chean;Nee, Tan Wen;Khairuddean, Melati;Zakaria, Latiffah;Ibrahim, Darah
    • Journal of Microbiology and Biotechnology
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    • v.27 no.6
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    • pp.1065-1070
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    • 2017
  • This study aimed to examine the anti-candidal efficacy of a novel ketone derivative isolated from Diaporthe sp. ED2, an endophytic fungus residing in medicinal herb Orthosiphon stamieus Benth. The ethyl acetate extract of the fungal culture was separated by open column and reverse phase high-performance liquid chromatography (HPLC). The eluent at retention time 5.64 min in the HPLC system was the only compound that exhibited anti-candidal activity on Kirby-Bauer assay. The structure of the compound was also elucidated by nuclear magnetic resonance and spectroscopy techniques. The purified anti-candidal compound was obtained as a colorless solid and characterized as 3-hydroxy-5-methoxyhex-5-ene-2,4-dione. On broth microdilution assay, the compound also exhibited fungicidal activity on a clinical strain of Candida albicans at a minimal inhibitory concentration of $3.1{\mu}g/ml$. The killing kinetic analysis also revealed that the compound was fungicidal against C. albicans in a concentration- and time-dependent manner. The compound was heat-stable up to $70^{\circ}C$, but its anti-candidal activity was affected at pH 2.

Effect of Concentration of Ionic Liquids on Resolution of Nucleotides in Reversed-phase Liquid Chromatography

  • Hua, Jin Chun;Polyakova, Yulia;Row, Kyung-Ho
    • Bulletin of the Korean Chemical Society
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    • v.28 no.4
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    • pp.601-606
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    • 2007
  • The chromatographic behaviors of nucleotides (inosine 5'-monophosphate, uridine 5'-monophosphate, guanosine 5'-monophosphate, and thymine monophosphate disodium salts) on a C18 column were studied with different types of ionic liquids (ILs) as additives for the mobile phase in reversed-phase liquid chromatography (RPLC). Three ILs, 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF4]), 1-ethyl-3-methylimidazolium tetrafluoroborate ([EMIm][BF4]), and 1-ethyl-3-methylimidazolium methylsulfate ([EMIm][MS]), were used. Eluents were composed of water and methanol (90/10%, vol) with the addition of 0.5-13.0 mM of ILs. The effects of the concentration of ILs on retention and separation were investigated and discussed. The results showed that the addition of ILs affects the retention and resolution of the tested compounds. Use of 13.0 mM of [BMIm][BF4] as the eluent modifier resulted in a baseline separation of nucleotides without requiring gradient elution. This study demonstrates that ILs can be potentially applied as a mobile phase modifier in RPLC.

Determination of La in $U_3Si/Al$ Spent Nuclear Fuel by Ion Chromatography-Inductively Coupled Plasma-Mass Spectrometry (Ion Chromatography-Inductively Coupled Plasma-Mass Spectrometry에 의한 $U_3Si/Al$ 사용후핵연료 중 La의 분리 및 정량)

  • Han, Sun Ho;Choi, Kwang Soon;Kim, Jung Suk;Jeon, Young Shin;Park, Yang Soon;Jee, Kwang Yong;Kim, Won Ho
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.601-607
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    • 2000
  • Lanthanum has been used as one of the burnup monitor in spent nuclear fuel. $U_3Si/Al$ spent nuclear fuel contains small amount of La in high concentration of U and Al. Therefore, chemical separation of La is required to remove matrix elements. At first, ion chromatography (IC) and inductively coupled plasma systems were installed in radiation shielded glove box to handle the radioactive samples. Retention behavior of uranium, aluminum, lanthanum and some interesting fission products (Sr, Zr, Y, Mo, Ru, Pd, Rh, Cs, Ba, Ce, Pr, Nd, Sm, Eu and Cd) was investigated using the CG10 column and ${\alpha}$-HiBA eluent. As all elements were eluted earlier than lanthanum in 0.2 M ${\alpha}$-HiBA eluent, a portion of U and Al was directly passed to waste using a three way valve between the column and the nebulizer. Thus it was possible to determine the lanthanum in a high concentration of U and Al matrix. Retention time of La was about 12 minutes in this separation condition. Optimum range for the determination of La in $U_3Si/Al$ spent nuclear fuel was $1-10{\mu}g/L$ (ppb) with this system and detection limit was $0.25{\mu}g/L$ in case of $200{\mu}L$ of sample volume.

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Separation of Alkali and Alkaline Earth Metal Ions using Novel HDBPDA Ion Exchanger and Its Ion Exchange Characteristics (새로운 HDBPDA 이온교환체를 사용한 알칼리 및 알칼리토금속 이온들의 분리와 그의 이온교환특성)

  • Kim, Dong-Won;Kim, Chang-Suk;Choi, Ki-Young;Jeon, Young-Shin;Yoon, Yeo-Hag
    • Journal of the Korean Chemical Society
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    • v.37 no.9
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    • pp.820-825
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    • 1993
  • The ion exchange capacity of HDBPDA ion exchanger, {(4,5) : (13,14)-dibenzo-6,9,12-trioxa-3,15,21-triazabicyclo[15.3.l]heneicosa-(1,17,19)(18,20,21) triene ion exchanger: HDBPDA ion exchanger} was 3.8 meq/g. The distribution coefficients of alkali and alkaline earth metal ions in water and the various concentration of hydrochloric acid were determined. Concentration of hydrochloric acid have almost not influenced on the distribution coefficients of alkali and alkaline earth metal ions, but generally, the distribution coefficient was slightly increased with decrease of concentration of hydrochloric acid. The distribution coefficients of metal ions in water are larger than those of various hydrochloric acid concentrations. Also, alkali and alkaline earth metal ions are separated by column ion exchange chromatography using HDBPDA ion exchange with water as eluent. The distribution coefficents of alkali and alkaline earth metal ions were increased with increase of ionic radii of metal ions.

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