• Journal of the Korean Chemical Society
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• v.38 no.2
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• pp.146-150
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• 1994

The simultaneous determination of Zn, Cd, Pb and Cu in 1.000%(w/v) tungsten matrix by differential pulse anodic stripping voltammetry at a hanging mercury drop electrode has been studied. Tartaric acid(pH=5.00) was used as a supporting electrolyte. Optimum analytical conditions were found that the deposition potential was -1.2 volt(vs. Ag/AgCl), the deposition time was 3 minutes. The linear concentration range of all trace metal ions in 1.000%(w/v) tungsten matrix were 10 to 50 ppb. And the detection limit(3${\sigma}$) of zinc, cadmium, lead and copper were 1.25, 1.02, 1.69, and 1.02 ppb respectively. This method was superior to the ICP-AES method which detection limits(3${\sigma}$) in 1.000%(w/v) tungsten matrix were 8.0, 5.0, 120 and 5 ppb respectively.

• Korean Journal of Materials Research
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• v.15 no.8
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• pp.528-535
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• 2005

It is inclined to increase that use of hazardous substances such as lead(Pb), mercury (Hg), cadmium(Cd) etc. are prohibited in the electronics according to environmental friendly policies of an advanced nation for protecting environment of earth. As this reasons, many researches for ensuring the reliability were proceeding in Pb free soldering process. n the flux remains on the PCB(printed circuit board) in the soldering process or the electronics exposed to corrosive environment, it becomes the reasons of breakdown or malfunction of the electronics caused by corrosion. Therefore in this studies we researched the polarization and Tafel properties of Sn40Pb and SnCu system solders based on the electrochemical theory. The experimental polarization curves were measured in distilled ionized water and 1 mole $3.5 wt\%$ NaCl electrolyte of $40^{\circ}C$, pH 7.5. Ag/AgCl and graphite were utilized by reference and counter electrodes, respectively. To observe the electrochemical reaction, polarization test was conducted from -250mV to +250mV. From the polarization curves composed of anodic and cathodic curves, we obtained Tafel slop, reversible electrode potential(Ecorr) and exchange current density((cow). In these results, we compared the corrosion rate of SnPb and SnCu solders.

• Journal of the Korean Chemical Society
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• v.28 no.5
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• pp.315-322
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• 1984

The dependence of polarographic parameters on the pressure for the reduction of In(III), Cr(III), Cd(II), Pb(II), Mn(II), Co(II), Tl(I) in 0.1M KCl aqueous solution at the dropping mercury electrode have been discussed. In this experiment the temperature varied from $25^{\circ}C\;to\;35^{\circ}C$ and the pressure ranges from 1 atmosphere to 1,800 atmospheres. By increasing the pressure the reduction half-wave potentials of all metal ions are shifted markedly to more negative values and the diffusion currents of all metal ions become considerably larger. The slope of the linear relationship of E vs. log[$\frac{id-i)}{i}$] become much larger with increase in pressure, which indicates more irreversible reduction. The temperature coefficient observed over the range of the temperature from $25^{\circ}C\;to\;35^{\circ}C$ are not sensitive with increase in pressure.

• The Korean Journal of Nuclear Medicine
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• v.34 no.4
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• pp.336-343
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• 2000

Purpose: Thallous-201 chloride produced at Korea Cancer Center Hospital(KCCH) is used in detecting cardiovascular disease and cancer. Thallium impurity can cause emesis, catharsis and nausea, so the presence of thallium and other metal impurities should be determined. According to USP and KP, their amounts must be less than 2 ppm in thallium and 5 ppm in total. In this study, the detection method of trace amounts of metal impurities in $[^{201}Tl]$TICI injection with polarography was optimized without environmental contamination. Materials and Methods: For the detection of metal impurities, Osteryoung Square Wave Stripping Voltammetry method was used in Bio-Analytical System (BAS) 50W polarograph. The voltammetry was composed of Dropping Mercury Electrode (DME) as a working electrode, Ag/AgCl as a reference electrode and Pt wire as a counter electrode. Square wave stripping method, which makes use of formation and deformation of amalgam, was adopted to determine the metal impurities, and pH 7 phosphate buffer was used as supporting electrolyte. Results: Tl, Cu and Pb in thallous-201 chloride solution were detected by scanning from 300 mV to -800 mV Calibration curves were made by using $TINO_3,\;CuSO_4\;and\;Pb(NO_3){_2}$ as standard solutions. Tl was confirmed at -450 mV peak potential and Cu at -50 mV Less than 2 ppm of Tl and Cu was detected and Pb was not detected in KCCH-produced thallous-201 chloride injection. Conclusion: Detection limit of thallium and copper is approximately 50 ppb with this method. As a result of this experiment, thallium and other metal impurities in thallous-201 chloride injection, produced at Korea Cancer Center Hospital, are in the regulation of USP and KP Polarograph could be applied for the determination of metal impurities in the quality control of radiopharmaceuticals conveniently without environmental contamination.

• Journal of the Korean Chemical Society
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• v.33 no.1
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• pp.55-64
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• 1989

Reduction and equilibrium of vanadium-DTPA (DTPA = diethylenetriaminepentaacetic acid, $H_5A$) complexes at mercury electrodes are studied in 0.5M $NaClO_4$ aqueous solution at 3.2 < pH < 10.5 and 25$^{\circ}$C. At 3.2 < pH < 5.9, the reduction reaction is $V{\cdot}A^{2-}+H^-+e^-=V{\cdot}HA^{2-}$, while at 5.9 < pH < 10.5 it is $V{\cdot}A^{2-}+H^-+e^-=V{\cdot}A^{3-}$. The stability constants of $V{\cdot}HA^{2-}$ and $V{\cdot}A^{3-}$ are found to be $6.46{\times}10^{9}$ and $3.09{\times}10^{14}$, respectively. V(IV)-DTPA undergoes stepwise complexation as $VO^{2+}+H_2A^{3-}=VO{\cdot}HA^{2+}H^{+}$ and $VO{\cdot}HA^{2-}=VO{\cdot}A^{3+}+H$, where acidity constant of $VO{\cdot}HA^{2-}$- is pKa = 7.15. Stability constants of $VO{\cdot}HA^{2-}$ and $VO{\cdot}A^{3-}$ are found to be $1.41{\times}10^{14}$ and $3.80{\times}10^{17}$, respectively. It is detected that $VO^{2+}-DATA$ is reduced irreversibly to $VO^{2-}$ with the transfer coefficient of $\alpha$ = 0.43. At more cathodic overpotential, the reduction is stepwise as V(IV)${\to}$V(III)${\to}$V(II). The first one corresponds to $VO{\cdot}HA^{2-}+e^{-}{\to}VO{\cdot}HA{3+}$ at 3.2 < pH < 7.2 and $VO{\cdot}A^{3-}+e^{-}{\to}VO{\cdot}A^{4-}$ at 7.2 < pH < 10.5. The second is identical to that of V(III). Diffusion coefficients of $VO{\cdot}HA^{2-}$ and $VO{\cdot}A^{3-}$ are found to be $(9.0{\pm}0.3){\times}10^{-6}cm^2/s$ and $(5.9{\pm}0.4){\times}10^{-6}cm^2/ses$, respectively.

• Analytical Science and Technology
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• v.5 no.3
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• pp.249-261
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• 1992

Electrochemical behavior of the heavy lanthanide complexes of alizarin red S(ARS) has been investigated by d. c. polarography, differential pulse polarography and cyclic voltammetry. The reduction mechanism at a mercury electrode of alizarin red S as a complexing ligand showed a one step of two-electron transfer and the electron process is found to be reversible. Alizarin red S forms a 3:1 adsorptive complexes with lanthanides and the complexes are reduced via one step of two-elctron. The reduction potential of complex wave($P_2$) shifted more negatively than the ligand wave($P_1$). The linear calibration curves of the decreacing $P_1$ and increasing $P_2$ is obtained when the lanthanide concentration varies from $2.0{\times}10^{-6}M$ to $6.4{\times}10^{-5}M$ under the condition of pH 9.5, 0.1M LiCl and $1{\times}10^{-3}M$ ARS.

• Analytical Science and Technology
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• v.5 no.3
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• pp.239-247
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• 1992

The complexations and selectivities of the 10 species of mono- and dimethylsubstituted anilinium ions with 18-crown-6 in methanol are examined at dropping mercury electrode. The stability constants of these complexes varies drastically due to the steric hindrance by the positions and numbers of methyl groups. And the analyses of the isomeric mixtures of methylanilinium, which are impossible to detect due to the overlapped peaks in normal conditions, were also accomplished by the additions of 18-crown-6 as the supporting complexing agent using the selective complexations by the steric hindrance effects. As results in case of the difference of stability, ${\Delta}log\;K$ were about 0.7~1.3, it was possible to confirm the existence of two species qualitatively. Otherwise when ${\Delta}log\;K$ were large than 1.6, the quantitative determinations of each species could be accomplished sucessfully. From these results it is deduced that the selective recongnition of the positions and numbers of methyl groups as the steric hindrance in anililniums by 18-crown-6 cause the large variation of the magnitudes of negative shift of reduction waves for guest ions in mixtures.

• Journal of the Korean Chemical Society
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• v.29 no.3
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• pp.197-204
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• 1985

The dependence of polarographic parameters on pressure and temperature for the reduction of 2.0 ${\times}\;10^{-4}$M 1-(2-pyridylazo)-2-naphthol (PAN) and 5.0 ${\times}\;10^{-4}$M 4-(2-pyridylazo)-resorcinol(PAR) in buffered methanol-water mixed solution at the dropping mercury electrode, has been discussed. In this experiment the temperature is varied from 25$^{\circ}C$ to 35$^{\circ}C$ and the pressure is ranging from 1 atmosphere to 1,800 atmospheres. The reduction half-wave potentials are shifted to the more positive potentials with increase in pressure. The diffusion currents of two depolarizers become considerably larger with increase in pressure from 1 atmosphere to about 1,000 atmospheres but are getting smaller above 1,000 atmospheres. The slopes of log plot become much larger with increase in pressure, which indicates the more irreversible reduction. The reduction currents of two depolarizers are found to be diffusion controlled over all pressure ranges. The linear relationships between diffusion current and the concentration of two depolarizers are good agreement over all pressure ranges (1 atm∼1,800atm.).