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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 7, Issue 4 - 00 1994
Volume 7, Issue 3 - 00 1994
Volume 7, Issue 2 - 00 1994
Volume 7, Issue 1 - 00 1994
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Adsorptive Stripping Voltammetric Determination of Sex Hormones in Medicines
Kim, Il Kwang ; Chun, Hyun Ja ; Jang, Kyung Seon ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 133~140
The determination of sex hormones by adsorpive stripping voltammetry in
sodium hydroxide as supporting electrolyte has been investigated in the conditions as follows : 240sec. for deposition time, -0.80 volts deposition potential, medium size mercury drop, and 20mV/sec scan rate. Calibration curve has shown a linearlity in the range of
and the detection limits have been
for progesterone and
for testosterone propionate. This method has shown such a good sensitivity even in dilute solution that has been use full for analyzing sex hormones in medical supplies without interference of additives.
Adsorption Striping Voltammetric Analysis of Corticosteroid Hormones
Kim, Il Kwang ; Chun, Hyun Ja ; Jeong, Seung Il ; Park, Jung Hwan ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 141~147
The adsorptive stripping voltammetry of corticosterone was studied in
sodium hydroxide as supporting electrolyte. The analytical conditions were as follow : 360 sec. for deposition time, -8.0 volts deposition potential, medium size mercury drop, and 20mV/sec scan rate. Calibration curve has shown a linearlity in the range of
and the detection limits have been
for corticoterones. This method has shown such a high sensitivity even in dilute solution that has been useful for analyzing sex hormones in medical supplies without interference of additives.
Tissue-Based Amperometric Biosensor for Determination of L-Ascorbic Acid in Organic Media
Kwon, Hyo-Shik ; Lee, Cheal-Gyu ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 149~153
An amperometric sensor for L-ascorbic acid(AA) in methanol media has been made by immobilizing squash-tissues on a graphite rod disk. A detection limit of the electrode was
L-ascorbic acid. In comparison with an isolated enzyme based ascorbate oxidase(AO) electrode, the plant-tissue electrode offered high biocatalytic stability and activity and extremely low cost. The electrode has a useful lifetime of 1 week.
Characterization and Emission/Absorption Study of a Grimm-type Glow discharge source in the application of high frequency Glow Discharge
Suh, Jung-Gee ; Woo, Jin-Chun ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 155~164
A conventional Grimm-type glow discharge source was constructed and applied to radio-frequency(13.56MHz) discharge for metal and ceramic analysis. We investigated the emission spectrum for aluminium and aluminium oxide and the influence of discharge operating paramaters including argon pressure, rf-power and DC-bias voltages at the sample-side electrode. Scanning Electron Microscope(SEM) also was used to investigate the effect of rf-sputtering on the microstructure formation of the aluminium oxide. Linear analytical calibration curves were constructed for Manganese and zinc element in samples of low alloy steel(BAS 401-405) and brass(NIST 1108-1117).
Analysis of amino acids in the liver of Hamster treated with Dimethylnitrosamine
Kim, Soo Gyung ; Jung, Ha Seung ; Park, Taek Kyu ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 165~171
The effect of the chemical carcinogen dimetylnitrosamine(DMN) on the composition of amino acids of the liver in hamsters orally administered with DMN was studied by using the reversed phase high performance liquid chromatography technique. In the liver, the concentration of aspartic acid, glycine, glutamine, histidine, proline, tyrosine and leucine were increased ca. 2-fold of those observed in liver of control group, valine and tryptophan were increased ca. 3-fold, phenylalanine was markedly increased ca. 10-fold, whereas the concentration of threonine was decreased, serine, alanine, arginine, methionine, isoleucine and lysine were unchanged, respectively.
A Study on the Measurement of Dissociation Constant of Organic Acid with FIA
Rhee, Jae-Seong ; Park, Hyun-Mee ; Kim, Hee-Jin ; Lee, Kang-Bong ; Dasgupta, Purnendu K. ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 173~179
The point of present study was focused on developing the method for the determination of dissociation constant by means of FIA conjunction with Diode Array Spectrphotometry or spectrophotometry along with small amount of Bromocresol Green(mg order) within short time. On the calculation with computer, the indicator with pK=7 has been shown the most sensitive reaction when little amount of base or acid has been added. The pKa of Bromothymol Blue and Bromocresol Green were measured as 7.31 and 4.82 respectively with spectrophotometry after activity correction by Kielland method (Reported value by Bishop, 7.30 and 4.79). The pKa of Bromocresol Green by FIA was obtained as 4.78 and was comparable with other values determined by other methods.
A study on Stripping Voltammetric Determination of Ag(I) by Poly(3-methylthiophene) Conducting Polymer Film Electrode Containing 18-crown-6
Lee, Ihn Chong ; Sohn, Jeong-In ; Kim, Kuk Gin ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 181~186
Using poly(3-methylthiophene) conducting polymer film electrodes, feasiblity for Ag determination by stripping voltammetry has been studied. Ag ions accumulated by complexation with 18-crown-6, which are existing on the surface of the polymer film electrode, migrate inside of polymer film through potential scanning within limited potential range, and then are reduced and oxidized on the glassy carbon substrate. Therefore, the polymer film must have proper thickness and porosity for easy penetration of Ag ions. On the basis of these experimental results,
Ag(I) in aqueous solution could be determined.
Reaction of lithiated pyridine with
and its identification with NMR spectroscopic methods(R=Me,
Kim, Duk-Mook ; Son, Byung-Yung ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 187~191
A reactive intermediate 1,2-dihydropyridine derivative 2 has been prepared and isolated from the reaction of pyridine with
and trimethylchlorosilane in nonpolar condition at low temperature 2 has characterized by
fine structure analysis with SPINX3. The mechanistic information of formation of 2 was obtained from synthesized 2,5-disubstituted pyridine derivatives 3 and 4.
The Study on the Intercalation-Deintercalation of Potassium-Carbon Fiber Intercalation Compounds
Oh, Won-Chun ; Cho, Sung-Jun ; Choi, Young-Jai ; Ko, Young-Shin ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 193~199
We have synthesized K-CFICs by the modified two-bulb method. These synthesized compound were analysed with X-ray diffractometer and UV/VIS spectrophotometer. According to X-ray diffraction analysis, the intercalation of potassium between the carbon layers of carbon fiber was better then other intercalants. From obtained data for this deintercalation process, we can see that a number of potassiums were presented as a residue between the carbon layers and this residue compounds had a stability for a long term. Therefore, it is appear that these compounds have a capability as new useful material. From UV/VIS spectrometry data, we can suppose that spectrum of K-CFICs synthesized at
had only a
, and spectra of any other compounds were not appeared charecteristic peaks because potassium ions were little affect the energy levels of original carbon fiber.
Enrichment of Lithium Isotopes by Cation Exchange Chromatography
Kim, Dong Won ; Kim, Chang Suck ; Choi, Ki Young ; Jeon, Young Shin ; Jeong, Young Kyu ; Park, Sung Up ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 201~204
Cation exchange column chromatography of lithium was carried out to investigate the lithium isotope separation in aqueous ion exchange system. A Pyrex glass column of
inner radius with a water jacket was used as the separation column in experiment. Upon column chromatography using hydrochloric and succinic acid mixtures as an elunent, single separation factor,
, 1.0068 was obtained. From the experiment, it was found that
was enriched in the resin phase and
in the solution phase.
Separation of Chromium(III) and Chromium(VI) by Carboxymethylated Polyamine-Polyurea Resin Column
Chung, Yong Soon ; Lee, Kang Woo ; Hwang, Jong Youn ; Lee, Yong Moon ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 205~211
Acetic acid and succinic acid bonded polyamine-polyurea(CPPI and SAPPI) resins were synthesized from the reaction of polyethylenimine-polymethylenepolyphenylene isocyanate(PPI) resin as matrix polymer and chloroacetic acid and chlorosuccinic acid respectively. These resins were confirmed with infrared spectrometry and elemental analysis. The adsorption characteristics of the chromium(III) and dichromate(or chromate) ions on the resins were studied by measuring distribution coefficients(
) with changing pH of the solution. It was thought that these ions were adsorbed by ion exchange mechanism. Chromium(III) and dichromate ion could be separated with stepwise elution method by changing pH of the eluent using SAPPI resin packed column(
). Also, dichromate ion could be preconecntrated with CPPI resin column by a concentration factor of 50.
INTRINSIC NMR ISOTOPE SHIFTS OF CYCLOOCTANONE AT LOW TEMPERATURE
Jung, Miewon ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 213~224
Several isotopomers of cyclooctanone were prepared by selective deuterium substitution. Intrinsic isotope effects on
NMR chemical shifts of these isotopomers were investigated systematically at low temperature. These istope effects were discussed in relation to the preferred boat-chair conformation of cyclooctanone. Deuterium isotope effects on NMR chemical shifts have been known for a long time. Especially in a conformationally mobile molecule, isotope perturbation could affect NMR signals through a combination of isotope effects on equilibria and intrinsic effects. The distinction between intrinsic and nonintrinsic effects is quite difficult at ambient temperature due to involvement of both equilibrium and intrinsic isotope effects. However if equilibria between possible conformers of cyclooctanone are slowed down enough on the NMR time scale by lowering temperature, it should be possible to measure intrinsic isotope shifts from the separated signals at low temperature.
NMR has been successfully utilized in the study on molecular conformation in solution when one deals with stable conformers or molecules were rapid interconversion occurs at ambient temperature. The study of dynamic processes in general requires analysis of spectra at several temperature. Anet et al. did
NMR study of cyclooctanone at low temperature to freeze out a stable conformation, but were not able initially to deduce which conformation was stable because of the complexity of alkyl region in the
NMR spectrum. They also reported the
NMR spectra of the
cycloalkanones with changing temperature from
, but they did not report a variable temperature
NMR study of cyclooctanone. For the analysis of the intrinsic isotope effect with relation to cylooctanone conformation,
NMR spectra are obtained in the present work at low temperatures (up to
) in order to find the chemical shifts at the temperature at which the dynamic process can be "frozen-out" on the NMR time scale and cyclooctanone can be observed as a stable conformation. Both the ring inversion and pseudorotational processes must be "frozen-out" in order to see separate resonances for all eight carbons in cyclooctanone. In contrast to
spectra, slowing down just the ring inversion process has no apparent effects on the
spectra because exchange of environments within the pairs of methylene carbons can still occur by the pseudorotational process. Several isotopomers of cyclooctanone were prepared by selective deuterium substitution (fig. 1) : complete deuterium labeling at C-2 and C-8 positions gave cyclooctanone-2, 2, 8,
: complete labeling at C-2 and C-7 positions afforded the 2, 2, 7,
isotopomer : di-deuteration at C-3 gave the 3,
isotopomer : mono-deuteration provided cyclooctanone-2-D, 4-D and 5-D isotopomers : and partial deuteration on the C-2 and C-8 position, with a chiral and difunctional case catalyst, gave the trans-2,
isotopomer. These isotopomer were investigated systematically in relation with cyclooctanone conformation and intrinsic isotope effects on
NMR chemical shifts at low temperature. The determination of the intrinsic effects could help in the analysis of the more complex effects at higher temperature. For quantitative analysis of intrinsic isotope effects, the
NMR spectrum has been obtained for a mixture of the labeled and unlabeled compounds because the signal separations are very small.
The Solvent Extraction of Silver Ion by Novel Sulfur-Containing Podans
Jung, Jong Hwa ; Park, Jung Min ; Kim, Dae Yeon ; Lee, Shim Sung ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 225~232
The podands I-VII, acyclic polyethers, expected high extractability for
were designed and synthesized with high yields. Using podands I-VII as extractants, the %extraction(%Ex) of
as picrates were determined in water/chloroform systems. The stability constants(log K) for the complexation of
with podands I-VII were also determined by potentiometry. %Ex(
) were proportional to the numbers of substituted sulfur donor atoms. Podand VI(log K : 7.65) having 3 substituted sulfur and podand VII(log K : 9.15) having 4 substituted sulfur, however, exhibited almost 100% of extractability, respectively. In %Ex(
, oxygen-sulfur mixed donor podands(IV-VII) showed the higher values. Otherwise, the values of log K and %Ex(
) largely depended on the variation of donor-site of sulfur. From the results of NMR experiments, it seems that it is due to the
stacking interaction between the aromatic end-groups.
Determination of Emulsion Stability Index in W/O Emulsion
Chang, Pahn Shick ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 233~236
To evaluate the emulsion stability indices of W/O emulsion system, we developed the simple and sensitive "VOLUMETRIC METHOD". This technique involved the first step of homogenizing the milk fat-water system with Ultra-turrax T25, then the volume of the added water phase was measured immediately. After quiescent incubation in test tubes at room temperature for a desired storage time, the bottom volume of the separated water layer was measured. And then "emulsion stability index(ESI)" was calculated by the following equation :
means the volume of the added water in the W/O emulsion and
represents the volume of the separated water in the W/O emulsion for a desired storage time. The emulsion stability indices of W/O emulsion system at sorbitan trioleate, span 60, and tween 20 were
respectively. Furthermore, the differences between "VOLUMETRIC METHOD" and "Titus et al method" were less than 5.0 of ESI Value.
Relationship between Emulsion Stability Index and HLB Value of Emulsifier in the Analysis of W/O Emulsion Stability
Chang, Pahn Shick ; Shin, Myung Gon ; Lee, Won Myo ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 237~243
The stability of W/O emulsions (milk fat : water=4 : 1, w/w) containing various emulsifiers was compared to determine the effect of different chemical types of emulsifiers in relation to the change of HLB value caused by emulsifier type and the influence of single vs. binary emulsifier systems. These variables were compared at emulsifier HLB values of 0.5~16.7 and at emulsifier concentrations of 1.0~3.0%(w/w). Eleven emulsifiers used as 11 different single mixtures and 16 different binary mixtures were evaluated in W/O type emulsion systems containing 20.0%(w/w) of water in milk fat. This W/O emulsion was stable (more than 90.0 of ESI value) in the range of low value of emulsifier HLB (less than 4.7 of HLB value). All the ESI values of binary emulsifier systems were higher than those of single emulsifier systems. But, the influence pattern of emulsifier HLB on this emulsion stability in single emulsifier systems was very similar to the trend in binary emulsifier systems.
Determination of Sodium Chondroitin Sulfate by Enzymatic Digestion and HPLC
Kang, Seong-Ho ; Shin, Hoon ; Chang, Sun-Ki ; Yoon, Hyung-Jung ;
Analytical Science and Technology, volume 7, issue 2, 1994, Pages 245~251
In order to determine sodium chondroitin sulfate in the mixture, chondroitinase ABC was used for enzymatic reaction. The procedure was rapid, simple, quantitative and the HPLC analysis of
-D-gluco-4-enepyranosyluronic acid)-6-0-sulfo-D-galactose) in the sodium chondroitin sulfate was obtained. The absorbance was measured at 230nm and detection limit was
. When we applied this method to the drugs(capsule, opthalmic solution), it gave the mean contents of