• Title/Summary/Keyword: ion pair extraction

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Studies on Atomic Absorption Spectrophotometric Analysis of Hexavalent Chromium in Waste Water by Solvent Extraction (용매 추출법에 의한 폐수중 6가크롬의 원자흡수 분광분석에 관한 연구)

  • Eung-Pyo Kim;Young-Sang Kim
    • Journal of the Korean Chemical Society
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    • v.30 no.5
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    • pp.423-432
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    • 1986
  • Atomic absorption spectrophotometric (AAS) determination of hexavalent chromium [Cr(VI)] in a waste water was studied. Cr(VI) was extracted with p-xylene from the wastewater, in the way of ion pair formation with anion exchanger aliquat-336(tri-caprylmethyl ammonium chloride). 100ml waste water, after organic materials were extracted out with toluene, was acidified with conc. HCl adjusting the medium to pH 0.5 and 20ml of p-xylene containing 0.01M aliguat-336 was used to extract Cr(VI) from the acidified solution. The absorbance of chromium was measured with air-acetylene flame at 357.9nm. Standard addition method was used in the determining concentration of Cr(VI) extracted. No interference has been found in the extraction of Cr(VI) by the Al(III), Fe(III) and Cr(III) ion presented. However, Fe(II) decreased the absorbance of Cr(VI), due to the fact Fe(II) reduces Cr(VI) to Cr(III). The contained organic material was removed prior to extracting process, since it may reduced the absorbance of Cr(VI). The recovery of added Cr(VI) was over 96%, which seems to be promising and the relative standard deviation was 3.95%

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Studies on Atomic Absorption Spectrophotometric Analysis of Chromium in Urine by Trioctylamine (Trioctylamine을 이용한 뇨중 크롬의 원자흡수 분광분석에 관한 연구)

  • Kim, Suk Won
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.1 no.2
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    • pp.214-220
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    • 1991
  • As chromium in urine remains as oxychromic acid ions, chromium was extracted by using ion pair formed by anion exchanger trioctylamine. then after it is noted whether this TOA-MIBK method is effective or not for the chromium analysis by using flame method of Atomic absorption Spectrophotometric Analysis. The result is as following. 1. Effects of various acids on the extraction of Cr with MIBK including TOA are good in order $NHO_3$, $H_2SO_4$, HCl in distilled water sample and its proper concentration of HCl is 0.2 N. 2. For the analysis of urine sample, the best result can be achieved by following condition. After finished pretreatment adjusted to pH 6.5-7.5 by NaOH and again controlled pH 0.5-0.6 by HCl. 3. Though TOA concentration slightly affects the analytic value, best result is noted in 1-3% concentration. 4. Recovery rates of urine samples made by $0.3mg/l{\cdot}urine$, $0.6mg/l{\cdot}urine$, $0.9mg/l{\cdot}urine$ are shown from 96.7% to 104.8%. 5. Recovery rates of urine samples made by $0.01mg/l{\cdot}urine$, $10.03mg/{\cdot}urine$, $0.05mg/l{\cdot}urine$ are shown from 89.3% to 98.6%.

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Spectrophotometric Determination of Trace Amount of Sulfide by Formation of Iodide and Its Solvent Extraction with Mehtylene Green (요오드이온 생성 및 Methylene Green과의 용매추출에 의한 미량 황이온의 분광광도법 정량)

  • Kam, Sang-Kyu;Kim, Kyung-Youn
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.261-269
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    • 1994
  • The iodide formed stoichiometrically for sulfide by its oxidation with iodate was extracted as an ion-pair with methylene green into 1,2-dichloroethane and the extract was measured spectrophotometrically at 656nm for the determination of sulfide. Hydrogen sulfide separated from the sample matrix was introduced into a solution containing pH 3.5 acetate buffer and iodate, in which the hydrogen sulfide was completely converted into iodide. A linear calibration graph was obtained over the range $3{\times}10^{-7}{\sim}1.2{\times}10^{-5}M$ sulfide($0.0096{\sim}0.384{\mu}g$ of $S^{2-}/ml$) and the detection limit was $0.0032{\mu}g/ml$. The apparent molar absorptivity and a correlation coefficient(r) were $6.7{\times}10^4L\;mole^{-1}\;cm^{-1}$ and 0.999, respectively. When applied to the stream water samples, the proposed method gave a relative standard deviation of 1.59% at $5{\times}10^{-6}M$ sulfide level.

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Spectrophotometric Determination of Some Fluoroquinolone Antibacterials through Charge-transfer and Ion-pair Complexation Reactions

  • El-Brashy, Amina Mohamed;Metwally, Mohamed El-Sayed;El-Sepai, Fawzi Abdallah
    • Bulletin of the Korean Chemical Society
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    • v.25 no.3
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    • pp.365-372
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    • 2004
  • Two simple, rapid and sensitive spectrophotometric methods for the determination of three fluoroquinolones, namely levofloxacin, norfloxacin and ciprofloxacin have been performed either in pure form or in their tablets. In the first method, levofloxacin and norfloxacin are directly treated with bromocresol green (BCG) in dichloromethane while ciprofloxacin is allowed to react with the same dye in aqueous acidic buffer. Highly yellow colored complex species were formed instantaneously in case of levofloxacin and norfloxacin or after extraction into dichloromethane for ciprofloxacin. The formed complexes are quantified spectrophotometrically at their absorption maxima at 411 nm for levofloxacin and 412 nm for norfloxacin and ciprofloxacin. The second method involves the reaction of levofloxacin with ${\rho}$-chloranilic acid ( ${\rho}$-CA) and norfloxacin with tetracyanoethylene (TCNE) in acetonitrile to give complexes with maximum absorbance at 521 and 333 nm for the two drugs, respectively. Adopting the first procedure, calibration graphs were linear over the range 1- 20 ${\mu}g\;mL^{-1}$ with mean percentage recoveries of 100.41 ${\pm}$ 0.72, 99.99 ${\pm}$ 0.54 and 100.23 ${\pm}$ 0.91 for the theree drugs, respectively. For the second procedure, the concentration ranges were 15-250 ${\mu}g\;mL^{-1}$ for levofloxacin using ${\rho}$-CA and 0.8-16 ${\mu}g\;mL^{-1}$ for norfloxacin using TCNE with mean percentage recoveries of 99.88 ${\pm}$ 0.45 and 100.26 ${\pm}$ 0.68 for the two drugs, respectively. The proposed methods were successfully applied to determine these drugs in their tablet formulations and the results compared favorably to that of reference methods. The proposed methods are recommended for quality control and routine analysis.

Determination of Pantothenic acid in Fortified Foods by HPLC (시판 영양강화식품중 판토텐산의 분석)

  • 최윤주;장재희;박혜경;박건상;구용의;황인경;김대병
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.33 no.2
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    • pp.381-385
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    • 2004
  • This study was conducted to develop an HPLC method for determining pantothenic acid in fortified foods which has typically been determined by microbiological assay (MBA) according to AOAC and Korean Food Code approved methods. Pantothenic acid was determined by reversed-phase ion-pair HPLC using UV absorption (200 nm) after extraction with 20 mM potassium phosphate solution by sonication. The recovery of spiked samples and detection limit (LOD) by HPLC were 83.5∼109.6% and 0.5 ppm (mg/kg), respectively. The LOD of the microbiological assay (MBA) was much lower than that of HPLC. The concentrations of pantothenic acid analyzed in all tested samples (n=13) confirmed compliance with declared label claims. The range of recovery ratio by the HPLC method when compared to the microbiological assay was 91.9∼117.6%. There was not significant difference (p<0.01) between the HPLC and MBA methods and the equation of the regression curve was y=1.1428x-0.2269 (r=0.9842). This proposed HPLC method for determining pantothenic acid appears to be suitable for determining pantothenic acid concentrations above 0.25 mg/100 g in fortified foods.