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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 10, Issue 6 - 00 1997
Volume 10, Issue 5 - 00 1997
Volume 10, Issue 4 - 00 1997
Volume 10, Issue 3 - 00 1997
Volume 10, Issue 2 - 00 1997
Volume 10, Issue 1 - 00 1997
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Analysis of Tertiary Amines and Quaternary Ammonium Salts in Electrolyte Solutions of Electrolytic Capacitors by Ion-Pair Liquid Chromatography
Chung, Yongsoon ; Chang, Cheolkyu ; Lee, Jeongmi ; Lee, Younghoon ; Kim, Seong Ho ;
Analytical Science and Technology, volume 10, issue 4, 1997, Pages 231~239
We developed a procedure that can effectively separate and determine tertiary amines and quaternary ammonium salts in some samples with reverse phase ion-pair high performance chromatography, employing indirect spectrophotometric detection method. Detection and ion-pairing reagents used in this study were benzyl trimethylammonium chloride (BTMACl) and sodium dodecyl sulfate(DDSANa), respectively. Eluting the electrolyte solutions of some commercial electrolytic capacitors with a MeOH(40):water(60) eluent (pH 8.5 adjusted with NH4Cl-NH3 buffer) containing 0.010M DDSANa and 0.004 M BTMACl through Supelco LC-18 or
-Bondapak phenyl column, amines and ammonium salts contained in the sample were successfully separated and determined. Varying the composition, especially the content of quaternary ammonium salts, of electrolyte solutions based on this analysis. we could prepare the low impedance(0.08~0.13) electrolytic capacitors with excellent electrical properties and it was a confirmation that the analysis is favorable.
A study on the determination of lead in whole blood by ICP/MS
Park, Kyung Su ; Kim, Sun Tae ;
Analytical Science and Technology, volume 10, issue 4, 1997, Pages 240~245
An accurate analysis method for the determination of lead in whole blood by ICP/MS was developed. Whole blood samples were decomposed in microwave digestion system without any contamination and loss of lead. The 96 samples were analyzed by ICP/MS using mass
isotope of lead. Lead concentrations of human whole blood were ranged of
. The accuracy of this analysis method was verified by analyzing of NIST SRM 955a series(lead in blood).
Electrochemical Properties of Nickel(II) Complexes with Multidentate N, O-Schiff Base Ligands
Kim, Sun-Deuk ; Kim, Jun-Kwang ; Roh, Soo-Gyun ;
Analytical Science and Technology, volume 10, issue 4, 1997, Pages 246~255
A series of Ni(II) complexes with multidentate N, O-Schiff base ligands: ie [bis-(salicylaldehyde) ethylenediamine(SED), bis-(salicylaldehyde) propylenediamine(SPD), bis-(salicylaldehyde) dietrylenetriamine(SDT), and bis-(salicylaldehyde) triethylenetetraamine(STT)] and Ni(II) complexes were synthesized. The Ni(II) complexes were characterized by elemental analysis, IR, UV-Vis and mass spectrometry. The stability constants of each nickel (II) complexes were determined by potentiometry in 70% dioxane-30%
and ethanol. The stability constants of Nickel(II) complexs increased in the order of Ni(II)-SPD
Synthesis of Naphthol-Containing Polyamines and Determination of Stability Constants of Their Metal Complexes by Potentiometric Titration
Kim, Sun-Deuk ; Kim, Jun-Kwang ;
Analytical Science and Technology, volume 10, issue 4, 1997, Pages 256~263
The new naphthol-containing hexadentate ligands, 1,12-bis (2-naphthol)- 2,5,8,11-tetraazadodecane 4HCl (nptr) and 1,14-bis(2-naphthol)- 2,6,9,13- tetraazatetradodecane .4HCl (npptr) were synthesized and characterized by elemental analysis, IR, NMR, and mass spectrometry. Acid dissociation constants and stability constants of Co(II), Ni(II). Cu(II), and Zn(II) complexes were determined at
and ionic strength (
) by potentiometry. The relationship between basicity and stability constants of ligands containing aliphatic amines and 2-naphthol were studied.
Studies on the anodic oxidation of some volatile organic halogen compounds(THM)
Yoo, K.S. ; Park, S.Y. ; Yang, S.B. ; Woo, S.B. ;
Analytical Science and Technology, volume 10, issue 4, 1997, Pages 264~273
Anodic oxidation reaction was applied to remove trihalomethanes in an aqueous solution. Each component was determined by using solid phase microextraction(SPME) fiber and GC-ECD. Anodic and cathodic compartments were separated in order to protect contaminants and connected by
-agar bridge. The calibration graphs of the 6 THM components were shown good linearlity from a few ppb up to a few hundreds ppb concentration level. Anodes such as platinum(Pt), titanium(Ti). zircornium(Zr), titanium metal coated with iridium(Ti-Ir), and glassy carbon coated with mixed valence ruthenium(mv Ru) were tried to remove the THMs at different potentials. The best result was obtained on the Ti-Ir anode applied 9 volts DC. The electrode could effectively remove almost all the THM components from the stirring solution within about 1.5 hours. The glassy carbon electrode coated with mixed valence ruthenium showed excellent removing effect at the begining, but the maximum removing level was remained at 60% probably due to the destruction of the electrode surface. The concentration of chloroform, however, tends to be increased due to the electrode reaction producing the component at the condition.
Determination of Tb(III) in aqueous solution by fluorescence spectrometry
Lee, Sang Hak ; Bae, Zun Ung ; Chung, Hae Young ; Choi, Sang Seob ;
Analytical Science and Technology, volume 10, issue 4, 1997, Pages 274~281
Methods to determine terbium(III) ion in aqueous solution by measuring the enhanced fluorescence intensity of terbium(III)-terephthalic acid(TPA) complex ion have been studied. The optimum analytical conditions for pH, excitation wavelength and concentration of TPA were found to be 6.0, 260nm and
, respectively. The fluorescence intensity of the terbium(III) complex ion was further increased with addition of trioctylphosphine oxide (TOPO). In this case Triton X-100 was used to dissolve TOPO in aqueous solution. When TOPO was used, the optimum analytical conditions for pH, excitation wavelength, and concentrations of TPA, TOPO and Triton X-100 were found to be 4.5, 285nm.
, and 0.05%, respectively. Under the optimum experimental conditions, calibration curve for Tb(III) was linear over the range from
and the detection limit was
. When TOPO was used, the concentration range of linear response, and the detection limit were
, respectively. Effects of interferences from various cations for the determination of terbium(III) ion were also investigated.
Studies on the Separation and Preconcentration of Metal Ions by XAD-16-[4-(2-thiazolylazo)] orcinol Chelating Resin
Lee, Won ; Seol, Kyung-Mi ; An, Hye-Sook ; Lee, Chang-Heon ; Lim, Jae-Hee ;
Analytical Science and Technology, volume 10, issue 4, 1997, Pages 282~290
The sorption and desorption properties of U(VI), Th(IV), Zr(IV), Cu(II), Pb(II), Ni(II), Zn(II), Cd(II) and Mn(II) ions on XAD-16-[4-(2-thiazolylazo)orcinol] (TAO) chelating resin were studied by elution method. The effect was examined with respect to overall capacity of each metal ion, separation of mixed metal ions, flow rate and concentration of buffer solution for optimum condition of sorption. The overall capacities of some metal ions on this chelating resin were 0.35nmol U(VI)/g resin, 0.49nmol Th(IV)/g resin, 0.41nmol Cu(II)/g resin, and 0.31nmol Zr(IV)/g resin, respectively. The elution order of metal ions obtained from breakthrough capacity and overall capacity at pH 5.0 was Th(IV)>Cu(II)>U(VI)>Zr(IV)>Pb(II)>Ni(II)>Zn(II)>Mn(II)>Cd(II). The group separation of mixed metal ions was possible by increasing pH in pH range 2~5 at a flow rate of 0.28mL/min. Characteristics of desorption were investigated with desorption agents such as
. It was found that 2M
showed high desorption efficiency to most of metal ions except Zr(IV) ion. Also, desorption and recovery of Zr(IV) ion were successfully performed with 1M
. Recovery of trace amount of U(VI) ion from artificial sea water was over 94%. The chelating resin, XAD-16-TAO was successfully applied to group separation of rare earth metal ions from U(VI) by using 2M
as an eluent.
Synthesis of 2,2'-Iminodibenzoic Acid-Cellulose Adsorbent and Its Adsorptivity of Cu(II) and Pb(II)
Shim, Sang-Kyun ; Min, Byoung-Do ;
Analytical Science and Technology, volume 10, issue 4, 1997, Pages 291~299
2,2'-iminodibenzoic acid-cellulose was prepared by reacting 2,2'-iminodibenzoic acid salt with cellulose-Cl obtained by chlorination of cellulose-OH which is the major component of sawdust. The adsorptivity of Pb(II) and Cu(II) was studied using the synthetic chelating adsorbent. The adsorption amounts of those ions increased with increasing pH and the optimum adsorption time of metal ion was about 1hr. The adsorptivity of Pb(II) was larger than that of Cu(II).
Studies on effects of calibration methods and current lead position on the direct current potential drop method for crack length measurement
Cho, C.C. ; Kim, I.S. ; Kim, S.S. ; Choe, S.J. ; Hur, B.Y. ;
Analytical Science and Technology, volume 10, issue 4, 1997, Pages 300~306
The effective resolution of the direct current potential drop (DCPD) method for crack length determination is strongly affected by a number of factors including wire locations and calibration method. In the present study, the effects of wire locations, thermal EMF and reference probe locations on the accuracy of calibration methods, including Hicks-Pickard equation and Johnson's equation, were examined with the CT specimens which were nine times larger than the standard specimen. In light of experimental results, it was found that Hicks-Pickard equation can accurately represent the a/W-V/Vo relationship when current input wire is located at the load line. It was also found that the accuracy of DCPD method can be greatly improved with the thermal EMF calibration and the use of Vo value at a/W = 0.241. The use of reference potential was found to be impractical when current input wire is located at the load line.