• Title, Summary, Keyword: dithizone

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Studies on the Micro-determination of Metals by Spetrophotometry (II) Micro-determination of pb by Dithizone Method (Spectrophotometer에 의한 금속의 최상정량법에 관한 연구 (제 2 보) Dithizone에 의한 Pb의 미량정량법)

  • 노일협
    • YAKHAK HOEJI
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    • v.5 no.1
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    • pp.24-26
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    • 1960
  • Micro-determination of Lead by Dithizone Method was studied as follows: 1) Max. absorption wave length of Dithizone-pb complex in CC $l_{4}$ soln. is 510m.mu., 2) at the range of 5.gamma.-120.gamma. pb content, Bourguer-Beer's law hold good, 3) co-existence of F $e^{++}$ Z $n^{++}$, and C $u^{++}$ interfere.rfere.

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Extraction Equilibria and Analytical Application of Metal-Dithizone Complexes(II) Partition and Extraction Equilibria into Chloroform (디티존 금속착물의 용매추출평형과 분석적 응용(제2보) 클로로포름 용매에 대한 분배 및 추출평형)

  • Choi, Yoon-Seok;Choi, Hee-Seon;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.370-377
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    • 1997
  • The several fundamental parameters on the solvent extraction of Co(II), Cu(II) and Zn(II) with dithizone were investigated. The value of $K_{a1}/K_p$ of dithizone(at $25^{\circ}C$) between an aqueous phase and a chloroform was found to be $4.72{\times}10^{-11}$. And the mole ratios of metal ion to dithizone in its metal complexes were determined by mole ratio method. The extractibilities(%) for metal-dithizone chelates were obtained from the extraction equilibria of metal-dithizone complexes between an aqueous phase and a chloroform as follows. Co(II) : 92.3% at pH 8.0 : Cu(II) : 97.1% at pH 4.0 and Zn(II) : 99.0% at pH 7.0. And also, in optimum experimental conditions the extraction constants of Co(II), Cu(II) and Zn(II) were examined.

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Analytic study on lead and cadmium in copper contained carbon materials (구리를 함유한 탄소소재의 납 및 카드뮴 분석에 관한 연구)

  • Choi, Zel-Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.6
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    • pp.307-313
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    • 2010
  • Quantitative analytical condition for lead and cadmium in copper contained carbon materials using solvent extraction followed by inductively coupled plasma-atomic emission spectrometry was studied. Copper contained carbon samples were dissolved by nitric acid-perchloric acid digestion. Lead and cadmium were determined after separation with KCN masked copper by an dithizone-chloroform solvent extraction. Recovery efficiency of analyte elements was satisfactory, and most of matrix elements causing interference could be effectively eliminated by the separation. Lead and cadmium were quantitatively determined without influence of sample matrix, by applying it procedure to artifact sample.

Determination of Methylmercury in Biological Samples Using Dithizone Extraction Method Followed by Purge & Trap GC-MS

  • Lee, Jung-Sub;Ryu, Yoon-Jung;Park, Jae-Sung;Jeon, Sung-Hwan;Kim, Sam-Cwan;Kim, Young-Hee
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2293-2298
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    • 2007
  • In this study, a dithizone extraction technique involving purge & trap GC-MS was developed for the determination of methylmercury in biological samples, especially blood and fish. After alkaline digestion, methylmercury in biological samples was extracted into dithizone and back-extracted into aqueous sulfide solution. The extracted methylmercury was converted to the volatile ethyl derivative, purged and trapped onto a solid-phase collection medium, and then introduced into the GC-MS system. The determined MDLs of the established method were 0.9 ng·g?1 for biological samples and its accuracy and precision were found to be 93% and 3.8%, respectively. The method was validated by analysis of CRMs such as SRM 966, BCR 463 and IAEA 407 and all analytical results were within certified ranges with average RSDs of less than 6%. The analytical results of field-sampled fish also showed that the method can be successfully used as an alternative for commonly used distillation method followed by GC-CVAFS detection.

Studies on Solvent Extraction and Analytical Application of Metal-dithizone Complexes(I). Separation and Determination of Trace Heavy Metals in Urine (Dithizone 금속착물의 용매추출 및 분석적 응용(제1보). 뇨중 흔적량 중금속 원소의 분리 정량)

  • Jeon, Moon-Kyo;Choi, Jong-Moon;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.9 no.4
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    • pp.336-344
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    • 1996
  • The extraction of trace cobalt, copper, nickel, cadmium, lead and zinc in urine samples of organic and alkali metal matrix into chloroform by the complex with a dithizone was studied for graphite furnace AAS determination. Various experimental conditions such as the pretreatment of urine, the pH of sample solution, and dithizone concentration in a solvent were optimized for the effective extraction, and some essential conditions were also studied for the back-extraction and digestion as well. All organic materials in 100 mL urine were destructed by the digestion with conc. $HNO_3$ 30 mL and 30% $H_2O_2$ 50 mL. Here, $H_2O_2$ was added dropwise with each 5.0 mL, serially. Analytes were extracted into 15.0 mL chloroform of 0.1% dithizone from the digested urine at pH 8.0 by shaking for 90 minutes. The pH was adjusted with a commercial buffer solution. Among analytes, cadmium, lead and zinc were back-extracted to 10.00 mL of 0.2 M $HNO_3$ from the solvent for the determination, and after the organic solvent was evaporated, others were dissolved with $HNO_3-H_2O_2$ and diluted to 10.00 mL with a deionized water. Synthetic digested urines were used to obtain optimum conditions and to plot calibration-eurves. Average recoveries of 77 to 109% for each element were obtained in sample solutions in which given amounts of analytes were added, and detection limits were Cd 0.09, Pb 0.59, Zn 0.18, Co 0.24, Cu 1.3 and Ni 1.7 ng/mL, respectively. It was concluded that this method could be applied for the determination of heavy elements in urine samples without any interferences of organic materials and major alkaline elements.

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Determination of Copper, Lead, Cadmium and Zinc in Water by Square Wave Polarography with Dithizone-Chloroform Extraction Method (디티존-클로로포름 抽出, 短形波폴라로그래피에 의한 물중의 구리, 납, 카드뮴 및 아연의 定量)

  • Su-Chan Moon
    • Journal of the Korean Chemical Society
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    • v.19 no.6
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    • pp.428-433
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    • 1975
  • 500 ml of a sample water was extracted with 10 ml of 0.01 % dithizone-$CHCl_3$three times. When $CHCl_3$ layer was back extracted with 10 ml of 0.1 N HCl containing mercuric ion, the free metal ions come into aqueous layer. The aqueous layer was added with 2 ml of 2 N KCl and was washed with 10 ㎖ of $CHCl_3$two times in order to remove the trace dithizone, and then was recorded square wave polarogram. The concentration of copper, lead and cadmium can be determined up to 3 ppb and that of zinc up to 14 ppb with an error of 10 %.

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Studies on Solvent Extraction and Flotation Technique Using Metal-Dithizone Complexes(II). Determination of Trace Elements in Water Samples by Solvent Sublation

  • 김영상;최윤석;최희선
    • Bulletin of the Korean Chemical Society
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    • v.19 no.10
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    • pp.1036-1042
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    • 1998
  • The preconcentration and determination of trace elements in water samples were studied by a solvent sublation utilizing dithizonate complexation. After metal dithizonates were formed, trace amounts of cadmium, cobalt, copper and lead were floated and extracted into small volume of a water-immiscible organic solvent on the surface of sample solution and determined in the solvent directly by GF-AAS. Several experimental conditions as formation condition of metal-dithizonate complexes, pH of solution, amount of dithizone, stirring time, the type and amount of surfactants, N2 bubbling rate and so on were optimized for the complete formation and effective flotation of the complexes. And also four kinds of light solvents were compared each other to extract the floated complexes, effectively. After the pH was adjusted to 4.0 with 5 M HNO3, 8.0 mL of 0.05% acetone solution of dithizone was added to 1.00 L water sample. The dithizonate complexes were flotated and extracted into the upper methyl isobutylketone (MIBK) layer by the addition of 2.0 mL 0.2% ethanolic sodium lauryl sulfate solution and with the aid of small nitrogen gas bubbles. And this solvent sublation method was applied to the analysis of real water samples and good results of more than 85% recoveries were obtained in spiked samples.

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Comparative Studies on the Analysis of Pesticide Residues. in Rice, Barley and Wheat (주곡중의 잔류농약분석에 관한 연구)

  • Park Seung Heui
    • Korean journal of applied entomology
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    • v.13 no.4
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    • pp.235-243
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    • 1974
  • Recenty, the pesticides Pollutions in connection with the maintenance of dietary life are poised as serious sanitary problems. Author have established an appropriate analysis method in this connection and, at the same time, analysed the levels of pesticides residues, such as organochloride pesticides and organic mercurials, contained in main cereals (rice, barley, and wheat) collected throughout the country. Using gas liquid chromatography method, comparative analyses were made of organochloride Pesticides with electron capture detector, and organic mercurials with electron capture detector and the Dithizone Method. As a result, the organic mercurials analysis using gas liquid chromatography is believed to hold out an especially good method for both in terms of its sensitivity and its Practical applications. The summary obtained from these results is as follows; The detectable limit of organochloride pesticides is $5\times10^{-10}$ grams and that of organic mecurials is $5\times10^{-9}$ grams. The detections using the Dithizone Method are difficult. The gas liquid chromatographic analysis of organic mercurials is very simple in its operation and high in its sensitivity, compare with the analysis using the Dithizone Method. Therefore, this analysis is expected to be a good method applicable to the pesticide residues analysis. The levels of pesticide residues contained in samples are very little for tolerance and, therefore, no problem i.: foreseen for eating. The appropriate conditions of gas liquid chromatographic analysis obtained from these results are expected very useful for the date establishing an officially authorized analysis method.

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Determination of Lead in Different Samples by Atomic Absorption Spectrometry after Preconcentration with Dithizone Immobilized on Surfactant-Coated Alumina

  • Dadfarnia, S.;Haji Shabani, A.M.;Dehgan Shirie, H.
    • Bulletin of the Korean Chemical Society
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    • v.23 no.4
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    • pp.545-549
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    • 2002
  • A simple and rapid technique for the separation and preconcentration of lead in water and biological samples has been devised. Preconcentrationis based on the depositionof analyte onto a column packed with dithizone immobilized on sodium dodecyl sulfate coated alumina at pH $\geq$ 3. The trapped lead is eluted with 5 mL of 4 M nitric acid and determined by flame atomic absorption spectroscopy. A sample of 1 L, results in a preconcentration factor of 200 and the precision at 20${\mu}g$ $L^{-1}$ is 1.3%(n=8). The procedure is applied to tap water, well water, river water, vegetable extract and milk samples, and accuracy is assessed through recovery experiments and by independent analysis by furnace atomic absorption.