• Title/Summary/Keyword: Ag(I) determination

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Determining Potassium Bromate in the Inhalable Aerosol Fraction in Workplace Air with Ion Chromatography

  • Kowalska, Joanna;Lis, Monika;Biesaga, Magdalena
    • Safety and Health at Work
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    • v.12 no.2
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    • pp.209-216
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    • 2021
  • Background: The article presents the results of studies performed in order to develop a new method of airborne potassium bromate(V) determination at workplaces. Methods: The method is based on a collection of the inhalable fraction of potassium bromate(V) using the IOM Sampler, then extraction of bromates with deionized water and chromatographic analysis of the obtained solution. The analysis was performed using ion chromatography with conductometric detection. The tests were performed on a Dionex IonPac®AS22 analytic column (250 × 4 mm, 6 ㎛) with AG22 precolumn (50 × 4 mm 11 ㎛). Results: The method provides for potassium bromate(V) determination within the concentration range of 0.043 ÷ 0.88 mg/m3 for an air sample of 0.72 m3 in volume, i.e., 0.1-2 times the exposure limit value as proposed in Poland. The method was validated in accordance with PN-EN 482. The obtained validation data are as follows: measuring range: 3.1-63.4 ㎍/mL, limit of detection (LOD) = 0.018 ㎍/mL and limit of quantification (LOQ) = 0.053 ㎍/mL. The developed method has been tested in the work environment, on laboratory employees having contact with potassium bromate(V). Conclusion: The analytical method allowed the determination of the inhalable fraction of airborne potassium bromate(V) at workplaces and can be used to assess occupational exposure.

Thallium(I)-Selective Electrodes Based on Calix[4]pyrroles

  • Park, Gyeong Sun;Jeong, Seong Uk;Lee, Sim Seong;Kim, Jae Sang
    • Bulletin of the Korean Chemical Society
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    • v.21 no.9
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    • pp.909-912
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    • 2000
  • Thallium(I) selective electrodes based on meso-alkyl substituted calix[4]pyrroles such as, meso-octamethyl-calix[4]pyrrole (L1), meso-octaethylcalix[4]pyrrole (L2) and meso-tetraspirocyclohexylcalix[4]pyrrole (L3) as sensor molecules have been pre pared and tested. The conditioned electrode (E4) incorporating L3gave best results with a wide working concentration range of 10-5.5 ~10-1 M near-Nernstian slope of 56.0 mV/decade of activity and detection limit of 10-6.0 M. This electrode exhibited a fast response time of 30 s and high selectivity over Na+ , K+ and other metal ions with only Ag+ interfering. The electrode works well in the pH range 2.0-11.0 and can be successfully employed for the determination of Tl+.This proposed electrode was also used as an indicator electrode in potentiometric titration of Tl+.

Quantitative Determination of $UO2^{2+}$ with Modified $[Ru(v-bpy)_3]^{2+}$ Polymer Film Electrode (수식된 $[Ru(v-bpy)_3]^{2+}$ 고분자 피막전극을 이용한 U(VI)의 정량)

  • Cha, Seong-Keuck
    • Journal of the Korean Chemical Society
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    • v.44 no.1
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    • pp.17-23
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    • 2000
  • Electrodes of the polycationic film with electropolymerized $[Ru(v-bpy)_3]^{2+}$ having about 1:1 ratio of $PF6^-/ClO_4^-$as the doped counter ions, were modified with xylenol orange and diethylditbiocarbamate by ion exchange which had stability constant as 38.6 and 17.5 respectively. These electrodes were employed in the quantitative multiple determination of U(W) in solution. The working electrode of electrochemical cell for the analytical signal was Pt/p-$[Ru(v-bpy)_3]^{2+}$, ligand, U(VI) with Ag/AgCl reference elecrode. In the stripping voltammetry. electrode process was electron transfer controlled one and calibration curves at the ranges of $1.0{\times}10^{-3}{\sim}1.0{\times}10^{-7}$ M had excellent relationship as 0.99 and relative standard deviation as 5${\sim}$8%.

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Determination of Hg22+ Ions Using a Modified Glassy Carbon Electrode with 2,2':6':2''-Terpyridine

  • Kong, Young-Tae;Bae, Yun-Jung;Shim, Yoon-Bo
    • Bulletin of the Korean Chemical Society
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    • v.23 no.2
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    • pp.346-350
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    • 2002
  • A glassy carbon electrode (GCE) modified with 2,2':6':2”-terpyridine (2,2':6':2”-TPR) using a spin coating method was applied for the highly selective and sensitive analysis of a trace amount of $Hg_2^{2+}$ ions. Various experimental parameters, which influenced the response of the 2,2':6':2”-TPR modified electrode to $Hg_2^{2+}$ ions, were optimized. The linear sweep and differential pulse voltammograms for the 2,2':6':2”-TPR modified electrode deposited with Hg show a well-defined anodic peak at +0.65 V (vs. Ag|AgCl). After a 25 min preconcentration time in an $Hg_2^{2+}$ ion solution (0.1 M acetate buffer, pH 5.0), differential pulse voltammetry(DPV) with 2,2':6':2”-TPR modified electrode shows a linear response between $1.0\;{\times}\;10^{-6}M\;and\;2.0\;{\times}\;10^{-7}M$. The least-square treatment of these data produce an equation of I[${\mu}A$] = 0.031 + 0.005C with r = 0.980(n = 5). The detection limit of this electrode with linear sweep voltammetry and differential pulse anodic voltammetry were $2.0\;{\times}\;10^{-6}M\;and\;8.0\;{\times}\;10^{-8}M$, respectively. The presence of Pb, Fe, Cd, Ti, Ni, Co, Mg, Al, Mn, and Zn did not interfere in the analysis of the $Hg_2^{2+}$ ion. The 2,2':6':2”-TPR modified GCE has been successfully applied in determination trace amounts of Hg in a human urine sample.

Electrochemical Behavior of Mordant Red 19 and its Complexes with Light Lanthanides

  • Sang Kwon Lee;Taek Dong Chung;Song-Ju Lee;Ki-Hyung Chjo;Young Gu Ha;Ki-Won Cha;Hasuck Kim
    • Bulletin of the Korean Chemical Society
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    • v.14 no.5
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    • pp.567-574
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    • 1993
  • Mordant Red 19(MR19) is reduced at mercury electrode at -0.67 V vs. Ag/AgCl with two electrons per molecule in pH 9.2 buffer by differential pulse polarography and linear sweep voltammetry. The peak potential is dependent on the pH of solution. The exhaustive electrolysis, however, gives 4 electrons per molecule because of the disproportionation of the unstable hydrazo intermediate. The electrochemical reduction of lanthanide-MR19 complexes is observed at more cathodic potential than that of free ligand. The difference in peak potentials between complex and free ligand varies from 75 mV for $La^{3+}$ to 165 mV for $Tb^{3+}$ and increases with increasing the atomic number of lanthanide. The electrochemical reduction of lanthanide complexes with MR19 is due to the reduction of ligand itself, and it can be potentially useful as an indirect method for the determination of lanthanides. The shape of i-E curves and the scan rate dependence indicates the presence of adsorption and the adsorption was confirmed by potential double-step chronocoulometry and the effect of standing time. Also the surface excess of the adsorbed species and diffusion coefficients are determined. The composition of the complex is determined to be 1 : 2 by spectrophotometric and electrochemical methods.

Cytogenetic Analysis of Korean Shinner, Coreoleuciscus splendidus (Cyprinidae) (쉬리, Coreoleuciscus splendidus (Cyprinidae)의 세포유전학적 연구)

  • Kim, Dong-Soo;Song, Ha-Yeun;Bang, In-Chul;Nam, Yoon-Kwon
    • Journal of Aquaculture
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    • v.20 no.2
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    • pp.140-143
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    • 2007
  • Cytogenetic analyses of an endemic species, Coreoleuciscus splendidus (Cyprinidae) was performed including erythrocyte measurement, chromosome count and karyotyping, nucleolar organizing region (NOR) banding and flow cytometric analysis of genome size. C. splendidus had the same modal chromosome number of 2n = 48 between sexes, however, displayed a sex-related dimorphism in their chromosome karyotypes. Males represented a pair of heteromorphic chromosomes which couldn‘t be seen in any female individuals, indicating that the sex determination mechanism of this species should be a typical XX-XY based male heterogamety (female=10M+6SM+8A+XX vs male=10M+6SM+8A+XY). Other cytogenetic features such as Ag-NORs located in a pair of acrocentric chromosomes, estimated nuclear volume ($28{\mu}m^3$) and cellular DNA content (2.4 pg/cell) suggest that genetic recombination might be the main driving force responsible for the evolution of this species rather than the polyploidy-based evolutionary process as in many other Cyprinidae species.

Separation and Recovery for the Analysis of Radioiodine in RI Wastes (RI 폐기물 내 방사성요오드 분석을 위한 분리 및 회수)

  • Kang, Sang-Hoon;Han, Sun-Ho;Lee, Heung-N.;Jee, Kwang-Yong;Lee, In-Koo
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.5 no.4
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    • pp.267-272
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    • 2007
  • Various kinds of RI wastes are discharged from licensed organizations of radioisotopes les such as hospitals and clinic organizations, educational organizations, research institutions, and public organizations. Radioiodines such as $^{125}I\;and\;^{131}I$ are radioisotopes mainly used in nuclear medicine and industry. A method for the determination of radioiodines in RI wastes has been applied to measure low level activity using acid decomposition method and HPGe gamma ray spectrometer. Prior to analysis of real samples, $^{131}I$ reference solution and 10 g of yellow tissue paper was added to flask in mantle and was heated in 100 mL of 0.4 N $K_2Cr_2O_7$ and 100 mL of 9 M $H_2SO_4$, and then distilled after adding 10 mL of 30% $H_2PO_3$ and 1 mL of 30% $H_2O_2$. The condensed iodine by circulator was extracted into $CCl_4$, then back-extracted into the aqueous phase with 10 mL of 5% $K_2SO_2$ solution. Finally, $^{131}I$ was measured at 364.48 keV using HPGe gamma ray spectrometer after precipitation and filtration. Chemical yield of three steps such as acid decomposition process, chemical separation process, and precipitation and filtration process was more han 94% respectively, MDA(Minimum Detectable Activity) of $^{131}I$ at this analytical condition was 0.6 Bq/g.

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Separation and Concentration of Trace Mercury [Hg(II)] in Water Sample by Coprecipitation Flotation Technique (공침-부선기술에 의한 수용액 시료 중 흔적량 수은 [Hg(II)]의 분리 및 농축)

  • Lee Kang-Seok;Choi Hee-Seon;Kim Seon-Tae;Kim Young-Sang
    • Journal of the Korean Chemical Society
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    • v.35 no.4
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    • pp.355-361
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    • 1991
  • The separative preconcentration of trace mercury[Hg(II)] in a water sample was studied by a coprecipitation flotation technique. The trace Hg(II) was precipitated together with Ce(OH)$_3$ by adding 3.0 ml of 0.1M Ce$^{3+}$ solution to 1,000 ml of water sample and adjusting pH to 11.0 with 1.0M NaOH solution. The hydrophobic precipitate[Ce(OH)$_3$-Hg(OH)$_2$], which was formed by adding 2.0 ml of 0.1${\%}$ ethanolic sodium oleate solution, were floated on the surface with an aid of tiny nitrogen gas bubbles. The floated materials were quatitatively collected in a suction flask and dissolved with 5.0 ml of 2.0M HNO$_3$. The solution was marked to 25.00 ml with a deionized water. The content of Hg(II) was determined by cold vapor atomic absorption spectrophotometry. Any interferences of concomitants such as Ag$^+$, Br$^-$, I$^- $, etc. were not observed on the whole procedure. The analytical result showed that Hg(II) found in the wastewater of Seochang Campus, Korea University was 1.98 ng/ml with the relative standard deviation of 3.6${\%}$. And recoveries of Hg(II) in the wastewater into which 1.0 ng/ml and 2.0 ng/ml were added were 95${\%}$ and 91${\%}$, respectively. From such results, this procedure could be concluded to be tolerably accurate and reproducible for the determination of trace mercury in a water sample.

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Determination of Ultimate Biodegradability and Multiple Decay Rate Coefficients in Anaerobic Batch Degradation of Organic Wastes (유기성폐기물의 회분식 혐기성 최종생분해도와 다중분해속도 해석)

  • Kang, Ho;Shin, Kyung-Suk;Richards, Brian
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.5
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    • pp.555-561
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    • 2005
  • A new graphical method was developed to separate two distinctive decay rate coefficients($k_1$ and $k_2$) at their respective degradable substrate fractions($S_1 and $S_2$). The mesophilic batch reactor showed $k_1$ of $0.151\;day^{-1}$ for wasted activated sludge(WAS), $0.123\;day^{-1}$ for thickened sludge(T-S), $0.248{\sim}0.358\;day^{-1}$ at S/I ratio of $1{\sim}3$ for sorghum and $0.155{\sim}0.209\;day^{-1}$ at S/I ratio $0.2{\sim}1.0$ for swine waste, whereas their long term batch decay rate coefficients($k_2$) were $0.021\;day^{-1}$, $0.001\;day^{-1}$, $0.03\;day^{-1}$ and $0.04\;day^{-1}$ respectively. At least an order of magnitude difference between $k_1$ and $k_2$ was routinely observed in the batch tests. The portion of $S_1$, which degrades with each $k_1$ appeared 71% for WAS, 39% for T-S, 90% for sorghum, and $84{\sim}91%$ at S/I ratio of $0.2{\sim}1.0$ for swine waste. Ultimate biodegradabilities of 50% for WAS, 40% of T-S, $82{\sim}92%$ for sorghum, and $81{\sim}89%$ for swine waste were observed.

Determination of Tritium in Spent Pressurized Water Reactor (PWR) Fuels (가압 경수로 사용후핵연료 중 삼중수소 분석)

  • Lee, Chang Heon;Suh, Moo Yul;Choi, Kwang Soon;Jee, Kwang Yong;Kim, Won Ho
    • Analytical Science and Technology
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    • v.17 no.5
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    • pp.381-387
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    • 2004
  • To characterize chemically a spent pressurized water reactor (PWR) fuel, an analytical method for trace amounts of tritium ($^3H$) in it has been established. Considering the effective management of radioactive wastes generated through the whole experimental process and the radiological safety for analysts, a separation condition under which $^{14}C$ and $^3H$ can be sequentially recovered from a single fuel sample was optimized using simulated spent PWR fuel dissolved solutions. $^{14}CO_2$ evolved during dissolution of the spent PWR fuels with nitric acid was trapped in an aliquot of 1.5 M NaOH. $^{129}I_2$ which was volatilized along with $^{14}CO_2$ was removed using a silver nitrate-impregnated silica gel absorbent. $^3H$ remaining in the fuel dissolved solution as $^3H_2O$ was selectively recovered by distillation. Its recovery yield was 97.9% with a relative standard deviation of 0.9% (n=3). $^3H$ in a spent PWR fuel with burnup value of 37,000 MWd/MtU was analyzed, reliability of this analytical method being evaluated by standard addition method.