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REFERENCE LINKING PLATFORM OF KOREA S&T JOURNALS
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Analytical Science and Technology
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Journal DOI :
The Korean Society of Analytical Science
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Volume & Issues
Volume 6, Issue 5 - 00 1993
Volume 6, Issue 4 - 00 1993
Volume 6, Issue 3 - 00 1993
Volume 6, Issue 2 - 00 1993
Volume 6, Issue 1 - 00 1993
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A Study on the Development of Analytical Methods and Behaviors of Environmental Pollutants ( I ) : Elution Behavior of Monosubstituted Phenols and Benzenes by Micellar Reversed-Phase Liquid Chromatography
Lee, Dai Woon ; Bang, Eun Jung ; Cho, Byung Yun ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 1~8
The purpose of this study is to investigate the elution behavior of monosubstituted phenols and benzenes in micellar liquid chromatographic system,
column-anionic surfactant, sodium dodecyl sulfate(SDS). The partition coefficients between the micellar pseudophase-water and modified stationary phase-water are calculated by the relationship between solute retention and micellar mobile phase(SDS) composition. The free energy of transfer of solute from water to micelle is also calculated from these values. There is a direct correlation between the hydrophobicity parameters in MLC and corresponding partition data for 1-octanol-water, which indicates that the hydrophobicity of molecules plays an important role in the partition for both systems and that quantitative structure activity relationships(QSAR) are available from studies on micellar partition. The other purpose of this study is to investigate methylene selectivity of alkyl homologous series through correlation between retention and the number of carbons. The correlation between hydrophobicity parameters in MLC and 1-octanol-water partition data was also observed when n-propanol was as a modifier in the mobile phase.
An analytical method of soap biodegradability with fatty acid p-BPB derivatives
Oh, Se-Woong ; Lee, Ja-Kyoung ; Chung, Yong ; Chang, Sug-Youn ; Kim, Yeo-Kyung ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 9~19
Fatty acid salts derived from soap can be transferred into a typical derivative with p-bromophenacyl bromide using crown ether, a catalizer by the solid-liquid phase transfer reaction in nonpolar, aprotic solvents and separated by the reverse phase high performance liquid Chromatography (RP-HPLC) and determined using UV detector. The minimal limit of detection was defined at approximately 10~50ng in accordance with the chain length. The derivatization reaction in the presence of EDTA can be applied mot only to the calcium salts but also to the other various metal salts. The recoveries of fatty acid derivatizations in the absence and presence of the midium containing the yeast extract were obtained
respectively. The analytical method would be applicable to determine the biodegradation of fatty acid salts in nature as well as in artificial condition such as shaker flask-medium method.
A Study on the Separation of n-Hexane by Molecular Sieve 5A and the Purification for HPLC use
Choi, Beom Suk ; Kim, Young Man ; Kim, Sun Tae ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 21~27
Technical grade n-hexane whose purity is 54% has been purified for HPLC use. Methylcyclopentane, 2-methylpentane, and 3-methylpentane which are hardly isolated by fractional distillation were separated by the liquid-solid chromatography using molecular sieve 5A. UV and fluorescence impurities whose contents are critically regulated for HPLC solvent were removed by the adsorptive separation with alumina and silica gel. The present method also reduced the impurities of color(APHA), acidity, water, residue after evaporation, sulfur, and thiophene content, and the impurity contents were well within the specifications of HPLC solvent.
The Solvent Extraction of Univalent Cation Picrates by New Podands
Jung, Jong Hwa ; Cho, Sung Bae ; Kim, Jineun ; Kim, Jae Sang ; Lee, Shim Sung ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 29~37
Some new podands containing phenyl(B), benzyl(Bz), pyridine(Py), quinoline(Q) and naphthalene(Np) as end-groups, and oxygen(O) and sulfur(S) in ether chains as donor atoms have been synthesized. The univalent cation binding characteristics of these podands have been studied by NMR titration and solvent extraction. By NMR titration we have found that the most of podands form 1:1 complexes with
ion. Especially, the substituted sulfur atoms in ether chains show the effects to enhance the stabilities. We also carried out the extractions of univalent cation picrates including alkaline metal,
ions from aqueous to chloroform layer by using these podands. We found that the extractabilities of
ion with the quinoline-containing podands such as,
were 86.8, 86.6 and 48.0% respectively, but the naphthalene-containing podands such as,
extracted quite small amount. Otherwise, in cases of
which have sulfur atoms and benzyl groups showed the highest extraction selectivity for
ion. This result seems due to not only the strong interaction of
ion with sulfur donors according to the HSAB theory, but also the effective
stacking interaction between two aromatic end-groups which is enhanced by the flexible methylene spacing group in benzyl groups instead of phenyl groups. The extraction coefficients gave the similar tendency as the extractabilities and the stabilities. From these results, it could be concluded that the predominant factor affected to extraction coefficients is the stabilities, which are strongly influenced by the structures of podands.
UV Resonance Raman Studies of Cis-Peptide, Diketopiperazine
Song, Sunho ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 39~45
We have examined Raman spectra of cis-peptide model complex, diketopiperazine in water and
with 320 nm through 218 nm excitation. Our study examines assignment of the resonance enhanced amide vibrations and characterizes their enhancement mechanism. Three resonance enhaned cis-peptide marker bands were observed in aqueous solution at 1676, 1533 and
, which were assigned to the cis-amide I, II and S band, respectively. The
amide II band, which is almost pure C-N stretching, was most dominant in water and shifted to
upon N-deuteration. This band will be probably a potential probe band for cis-peptide moieties in proteins. The excitation profile data and an Albrecht A-term fit indicated that the cis-peptide vibrations derive their intensities from the 188 nm cis-peptide
electronic transition. We Propose that the geometry of cis-peptide
excited state is C-N bond displacement relative to that of electronic ground state.
Determination of Cyanide Ion in the Presence of Sulfide Ion by Differential Pulse Cathodic Stripping Voltammetry
Park, Se Yeon ; Kwon, Young Soon ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 47~55
The quantitative determination of trace cyanide ion in the presence of sulfide ion has been studied by addition of cupric ion using differential pulse Cathodic Stripping Voltammetry. The detection limit of cyanide ion in the presence of
sulfide ion and
cupric ion was
in KCI-Phosphate buffer(pH=7.0) at accumulation potential -0.30V and accumulation time 3.0 min.
Flow Injection Spectrophotometric Determination of Cobalt with 2-(5-Bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino)aniline
Kang, Sam Woo ; Kim, In Yong ; Han, Hong Seok ; Lee, Seung Seok ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 57~63
Spectrophotometric determination of cobalt by flow injection method is described. 2-(5-Bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino) aniline rapidly forms a water-soluble complex with cobalt in
buffer solution at pH 10.5. The absorption maxima of this complex is at 545 nm with molar absorptivity of
. The calibration curve of cobalt is linear over the range of 0.1 to 0.6ppm and the detection limit is 25ppb. The relative standard deviation is
for 0.5ppm and the sampling rate is
. The interfering effect of some cations and anions was investigated. Ni(II), Cu(II), Fe(III) and
interfered severely. The interfering effect of these matallic ions could be decreased by adding
EDTA solution to the carrier stream.
Comparison of Physical Properties of CFC Alternative Cleaning Solvents
Row, Kyung Ho ; Lee, Youn Yong ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 65~75
A number of alternative cleaning solvents to CFC 113 which was identified as a ozone-depleting meterial were collected to measure their experimental physecal properties of density, surface tension, Refractive Index, boiling point, pH, viscosity, flash point, and soltbility. They might be classified as aqueous, simi-aqeous, alcohol ketone, and halogen cleaning solvents. The solubilities of abietic acid, a major component of flux used in PCB (Printed Circuit Board) of the electronic indystry, into the cleaning solvents including CFC 113 were determined for comparison. The assorted cleaning solvents have their own advantages and disadvantages. Therefore a end-user carefully needs to choose the best-fit cleaning solvent after the safety, stability, and economics as well as the effectiveness by physical properties of the alternative cleaning solvents are integratedly considered.
Application of Negative Ion Mass Spectrometry in Amino Acid Analysis
Pyo, Dongjin ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 77~82
Negative chemical ionization mass spectrometry(NCI-MS) can provide the enhancement in sensitivity in the analysis of amino acids. For molecules which are strongly electron-capturing, NCI-MS has been of amino to have detection limits in the femtomole to attomole(
) range. Because of the selectivity of the ionization process, background noise is diminished, further enhancing signal to noise ratio. In this paper, we explored a dinitro-phenyl derivatives of amino acids by NCI-MS and compared it with eletron ionization method. The results demonstrated NCI-MS produces very clean spectra with a very little noise.
Synthesis and Electrochemical Characteristics of Lantanium and Neodynium Metal Complexes
Oh, Je Jik ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 83~92
The electrochemical behaviors of lanthanide ion(La and Nd) and lanthanide complexes with 2, 2, 6, 6-tetramethyl-3, 5-heptanedione(THD), sym-hydroxydibenzo-16-crown-5(HD16C5) and sym-dibenzo-16-crown-5-oxyacetic acid(D16C5A) ligands in acton solution have been investigated by the use of cyclic voltammetry and direct current polarography. The peak potential and peak current, their dependency on the concentration, temperature, the reversibility of the eleotrode reactions are described. The reduction of the lanthanide ions and complexes in 0.05 M TEAP proceeded one-electron step in first step and one two-electron step in second step. These reduction step was irreversible and the reduction current was diffusion controlled. Macrovcyclic crown ethers, sym-hydroxydibenzo-16-crown-5(HD16C5) and sym-dibenzo-16-crown-5-oxyacetic acid(D16C5A), were prepared from 1, 5-bis-(2-hydroxyphenoxy)-3-oxapentane with epichlorohydrin. The voltammetric behaviors of Ln(III)-HD16C5 and Ln-D16C5A complexes in aceton solution have been investigated by the voltammetric method. The composition and stability constants of lanthanide complexes were determined.
Mass Spectra of Chlorinated Organophosphorus Pesticides
Hong, Jongki ; Eo, Yunwoo ; Rhee, Jaeseong ; Kim, Taekjae ; Kim, Kangjin ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 93~106
Fragmentation patterns on electron impact of 8 chlorinated organophosphorus pesticides were investigated. In most cases, characteristic ions could e identified and the peak clusters due to the
isotopes in the fragment ions were found to be highly characteristic. The fragmentation patterns of phosphorus moiety were coincident with previous report in the aspect of mechanism.
Development of Separation and Trace Analysis Methods for Platinum Group Elements-Separation and Retention Behavior of Platinoid Metal Acetylacetonates in Reversed-Phase Liquid Chromatography
Lee, Dai Woon ; Kim, Kyung Soo ; Park, Young Hun ; Czea, Myoung Zoon ; Chung, Koo Soon ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 107~119
The purpose of this study is to investigated the elution behavior of platinoid metal acetylacetonates, which is the key to elucidate their retention mechanism and optimize their RPLC separation conditions. The retention data of four platinoid metal acetylacetonates have been measured on four different columns in methanol-water and acetonitrile-water systems. The retention of uncharged platinoid metal acetylacetonates is interpreted by solvophobic effect. The retention of platinoid metal acetylacetonates is also greatly influenced by the geometric structure of the complexes. The square planar chelates,
, are retained longer than the octahedral chelates,
. It is likely due to that square planar chelates show greater interaction with nonpolar stationary phase than octahedral chelates. The results of van't Hoff plots have shown that platinoid metal acetylacetonates is operated on the same retention mechanism in the temperature range of
. The study of the retention mechanism by the enthalpy-entropy compensation phenomenon has indicated that the retention mechanism of octahedral chelates and square planar chelates do not vary with the composition change of methanol-water mobile phase, respectively. In acetonitrile-water mobile phase, however, the retention mechanism is observed to be more complicated. Optimum condition for the separation of four platinoid metal acetylacetonates is found to be 40% methanol, polymeric C18 column, and
pH Effect for the Separation of Lanthanides with Pyromellitic Acid and Oxalic Acid
Lee, Kyung-Ae ; Kim, Chae-Kyun ; Sung, Hak-Je ; Chang, Choo-Wan ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 121~129
UV/VIS spectrophotometer interfaced with HPIC(High Performance Ion Chromatography) has been applied to the determination of lanthanide elements. The separation of lanthanide elements with HPIC helped to avoid erroneous analytical results due to interferences. Individual lanthanide elements at ppm level were separated on a HPIC CS5 column using pyromellitic acid and oxalic acid. The individual lanthanide elements were detected at 520nm following post-column reaction with PAR. Sm, Eu, Gd, Y, Tb, Dy, Ho, Er, Tm, Tb, and Lu were separated by pyromellitic acid. La, Ce, Pr and Nd were separated by oxalic acid. Appropriate pH of pyromellitic acid for separation was at pH 2.99.
Studies on Analysis of Gallium and Indium in Zinc Ores by Inductively Coupled Plasma Atomic Emission Spectrometry
Hwang, Youn-Ok ; Sim, Sang-Kwon ; Sung, Hack-Je ; Yang, Myung-Kwon ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 131~139
The separation of gallium and indium from the matrix elements such as zinc and other ions, especially form Fe(III) ion was studied for the determination of trace level of them in zinc ores and zinc blendes by inductively coupled plasma atomic emission spectrometry(ICP-AES). Gallium and indium were extracted from the sample solution with a solvent of tributyl phosphate(TBP). The type and concentration of acid, interferences of other ions, the ratio of aqueous phase to organic phase, TBP concentration, sripping efficiency were optimized for the effective extraction. Gallium and indium were separated from other ions in the 5N hydrochloric acid solution of the samples by the extraction with 100% TBP. In this time, Fe(III) was reduced to Fe(II) with hydroxylamine hydrochloride to prevent its coextraction prior to the main extraxtion. After stripped from organic phase by the back-extraction with 0.02N HCl, they were determined in the aqueous phase by ICP-AES. This method was known to be quantitative from the overall extraction of more than 95%.
Behavior of Reverted Austenite in Fe-Ni-Mn-(Ti) Maraging Steels
Kim, Sung-Joon ;
Analytical Science and Technology, volume 6, issue 1, 1993, Pages 141~147
The behavior of reverted austenite in Fe-Ni-Mn(Ti) maraging steels has been investigated in the temperature range from
using TEM equipped with EDX. Four kinds of reverted austenite appeared depending on the aging temperatures and time : Widmanstatten, granular, lath-like and recrystallized austenite. The reverted austenites are enriched in Ni and Mn due to the dissolution of precipitates and redistribution of alloying elements. Widmanstatten austenite appears unformly in the lath martensite having the K-S orientation relationship with the martensite lath, while lath-like martensites showed K-S and N relations depending on the chemistry and heat treating condition. The recrystallized austenite forms at
after long aging times : some becomes unstable and transforms to lath martensite on cooling.