• Title/Summary/Keyword: Preconcentration and separation

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Determination of Copper Ion with 2-Mercaptobenzimidazol Immobilized on Surfactant-Coated Alumina (계면활성제를 코팅한 알루미나에 부동화한 2-Mercaptobenzimidazol을 이용한 구리이온의 정량)

  • Absalan, G.;Goudi, A.Aghaei
    • Journal of the Korean Chemical Society
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    • v.51 no.2
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    • pp.141-146
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    • 2007
  • The present paper describes a procedure for separation, preconcentration and determination of trace amount of copper in natural water samples by using 2-mercaptobenzimidazol as the complexing agent. The proposed method is based on the surfactant aggregation formed on γ-alumina by mixing sodium dodecyl sulfate and γ-alumina in water; 2-mercaptobenzimidazol was incorporated into inner hydrophobic part of produced ad-micelles in acidic media to produce an assemble suitable for preconcentration and determination of copper ion. Optimum experimental conditions for adsorption of μg/ml levels of copper ions from aqueous solution by the adsorbent have been reported. The copper ions were quantitively adsorbed by the sorbent over the pH range of 7.1-8.0 and were quantitatively desorbed afterward by using sulfosalycilic acid as the eluent. The determination of copper was not interfered in the presence of common metal ions. The procedure was applied for analysis of river water sample. Relative standard deviation was found to be 4.91%.

Determination of copper(II) in various samples by flame atomic absorption spectrophotometry after column separation by adsorption of its N-benzoylphenylhydroxylamine complex on benzophenone

  • Park, Moon-Hee;Choi, Hee-Seon
    • Analytical Science and Technology
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    • v.20 no.1
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    • pp.55-60
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    • 2007
  • A sensitive technique for the determination of trace Cu(II) in various samples after the column preconcentration by adsorbing its N-benzoylphenylhydroxylamine (BPHA) onto benzophenone was developed. Several experimental conditions such as the pH of the sample solution, the amount of chelating agent, the amount of benzophenone, and the flowrate of sample solution and so forth were optimized. The interfering effects of diverse concomitant ions were investigated. Fe(III) and $CN^-$ interfered with more seriously than any other ions. However, the interference by these ions could be overcome sufficiently by adjusting the added volume of 0.01M BPHA to 10 mL. The dynamic range, the correlation coefficient ($r^2$) and the detection limit obtained by this proposed technique were 5.0~120 ng/mL, 0.9974, and 2.1 ng/mL, respectively. For validating this proposed technique, the aqueous samples (stream water, reservoir water, and wastewater), the plastic sample and the diluted brass sample were used. Recovery yields of 93~102% were obtained. These measured data were not different from ICP-MS data at 95% confidence level. This method was also validated by the rice flour CRM (normal, fortified) samples. Based on the results from the experiment, it was found that this proposed technique could be applied to the determination of Cu(II) in various real samples.

Preconcentration of Copper(II) Using Mesoporous Organo-Silicas and Determination by Flame Atomic Absorption Spectrometry (메조다공성 유기-실리카를 이용한 구리(II)의 예비농축과 불꽃원자 흡수분광법으로의 정량)

  • Moghimi, Ali
    • Journal of the Korean Chemical Society
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    • v.52 no.2
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    • pp.155-163
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    • 2008
  • .A simple and reproducible method for the rapid extraction and determination of trace amounts of copper(II) ions using mesoporous organo-silicas mesoporous silica and atomic absorption spectrometry is presented. Common coexisting ions did not interfere with the separation and determination. The preconcentration factor was 100 (1 ml elution volume) for a 100 ml sample volume. The limit of detection of the proposed method is 1.0 ng ml-1. The maximum sorption capacity of sorbent under optimum conditions has been found to be 5mg of copper per gram of sorbent. The relative standard deviation under optimum conditions was 2.8% (n=10). Accuracy and application of the method was estimated by using test samples of natural and synthetic water spiked with different amounts of copper(II) ion.

Preconcentration of Ultra Trace Amounts Bismuth in Water Samples Using Cloud Point Extraction with Na-DDTC and Determination by Electrothermal Atomic Absorption Spectrometry (ET-AAS) (Na-DDTC로 흐림점 추출을 사용한 물시료에서 초미량 비스머스의 예비농축)

  • Moghimi, Ali
    • Journal of the Korean Chemical Society
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    • v.52 no.2
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    • pp.140-147
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    • 2008
  • .A new approach for a cloud point extraction-electrothermal atomic absorption spectrometric method was used for determining bismuth. The aqueous analyte was acidified with sulfuric acid (pH 3.0-3.5). Triton X-114 was added as a surfactant and natriumdiethyldithiocarbaminat (Na-DDTC) was used as a complexing agent. After phase separation at 50oC based on the cloud point separation of the mixture, the surfactant-rich phasen was diluted using tetrahydrofuran (THF). Twenty microliters (20 L) of the enriched solution and 10 l of 0.1% (w/v) Pd(NO3)2 as chemical modifier were dispersed into the graphite tube and the analyte determined by electrothermal atomic absorption spectrometry. After optimizing extraction conditions and instrumental parameters, a preconcentration factor of 195 was obtained for a sample of only 10 mL. The detection limit was 0.04 ng ml-1 and the analytical curve was linear for the concentration range of 0.04-0.70 ng mL-1. Relative standard deviations were <5%. The method was successfully applied for the extraction and determination of bismuth in water samples.

Chromatographic Behavior of Cryptand[2,2] Modified Resin on Metal Cations

  • Suh, Moo-Yul;Eom, Tae-Yoon;Suh, In-Suk;Kim, Si-Joong
    • Bulletin of the Korean Chemical Society
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    • v.8 no.5
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    • pp.366-372
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    • 1987
  • Cryptand[2,2] was grafted to low crosslinked styrene-divinylbenzene copolymer by substitution reaction with chloromethylated styrene-divinylbenzene copolymer. This resin was stable in concentrated acid and base, and showed a good resistance to heat. The pH, time, and concentration dependence of the adsorption of metal ions by this resin were studied. Studies on the chromatographic separation of lanthanides, $Cu^{2+}$ and $UO_2^{2+_2}$ were also carried out with various eluents. These studies demonstrate that this resin has the applicability to the preconcentration and separation of metal ions.

Separation of Fe(Ⅱ) from Co(Ⅱ), Ni(Ⅱ), Pb(Ⅱ) Using Amberlite IRA 400 Loaded with Alizarin Red S (Alizarin Red S가 결합된 Amberlite IRA 400 에 의한 Co(Ⅱ), Ni(Ⅱ), Pb(Ⅱ) 중 Fe(Ⅱ)의 분리)

  • Cha, Ki Won;Park, Chan Il;Kang, Ji Soo
    • Journal of the Korean Chemical Society
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    • v.42 no.2
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    • pp.172-176
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    • 1998
  • An anion exchange resin which has Alizarin Red S (ARS) as functional group was prepared by batch method. The resin is stable in acidic solutions below 0.5 M hydrochloric acid, nitric acid and sulfuric acid and adsorption capacity of Fe(Ⅱ) ion on the resin was larger than other metal ions. The preconcentration and the separation of Fe(Ⅱ) ion from the mixture solution were carried out with the pH 4.5 buffer solution and 0.1 M $HNO_{3}$ as eluents.

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Ion-exchange Separation and Spectrophotometric Determination of Trace Amount of Aluminium with Thorinin the Presence of Triton X-100 (Triton X-100 존재하에 Thorin에 의한 미량의 알루미늄 이온의 분광학적 정량 및 이온-교환 분리)

  • Park, Chan-Il;Cha, Ki-Won;Jung, Duck-Chae
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.515-520
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    • 1999
  • The spectrophotometric determination of Al(III) with thorin have been investigated. The optimum condition of pH, concentration of ligand and surfactant, and stability were evaluated. The thorin ligand offers selective separation of Al(III) from sample solution containing Fe(III), Ni(II), Cu(II), Pb(II) and Cu(II). Various surfactants were tested and Triton X-100 showed the best stability and the maximum absorbance in an aqueous solution of Al(III)-Thorin-Triton X-100 complex appears about 526 nm. The method was applied for the determination of Al(III) in mixed sample solution. Separation and preconcentration was performed with a short column filled with resorcinol-formaldehyde resin. Control of the pH during the column operation is essential because the adsorption capacities are very sensitive to change in pH. Their separation was carried out in 0.2 M acetic acid-sodium acetate buffer solution (pH 4.5) and 1.0 M $HNO_3$media.

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Separation of Fe(III) and Concentration of Metal Ions Using Cation Exchange Resin Bonded with Xylenol Orange (Xylenol Orange가 결합된 양이온 교환체에 의한 금속이온의 농축 및 Fe(III)의 분리)

  • Park, Chan Il;Kim, Hyun Soo;Cha, Ki Won
    • Journal of the Korean Chemical Society
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    • v.43 no.6
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    • pp.651-655
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    • 1999
  • Xylenol Orange was bonded on an anion-exchange resin (Amberlite lRA 400, in $Cl^-$form) by batch equilibration. The resin was proved to be stable in acidic solutions of about 0.1 M HCl, $HNO_3$ or $H_2SO_4$. Sorption capacities for the metal ions on the Amberlite IRA 400 bonded with xylenol orange have been measured by batch method. The result showed that Fe(III) is higher than any other metals for sorption capacity. The preconcentration and the separation of Fe(lll) from the mixture soIution, therefore, were carried out with the 0.1 M sulfosalicylic acid as an eluent.

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Continuous Coprecipitantion Preconcentration-Hydride Generation for Arsenic in Inductively Coupled Plasma-Atomic Emission Spectrometry (연속적 공침 선농축-수소화물 발생법을 이용한 ICP-AES에서의 비소의 감도 개선)

  • Kim, Chang-Gyu;Pak, Yong-Nam
    • Journal of the Korean Chemical Society
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    • v.48 no.6
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    • pp.583-589
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    • 2004
  • In a stream of aqueous sample, trace arsenic ions were quantitatively coprecipitated and detected in ICP-AES through hydride generation. In was used as a coprecipitating reagent. The precipitate was collected on a filter and dissolved by HCl. The eluted As was sent into the reaction coil to generate hydrides and analyzed by ICP. With optimal conditions, and with a sample of 0.3 mL, an enrichment of 70 was obtained with the sampling speed of 10/hr. When compared with coprecipitation and hydride generation technique, the sensitivity was increased by 7 and 10 times, respectively. The limit of detection limit$(3{\sigma})$ was 0.020 ${\mu}g\;L^{-1}$ and the precision was 7-10%. Separation of $As^{3+}\;and\;As^{5+}$ were possible using citric acid in hydride generation.

The Determination of Dissolved Total Fe by Flow Injection Analysis in Environmental Samples

  • Kim, Do Hoon;Takeda, Kazuhiko;Sakugawa, Hiroshi;Lee, Jin Sik
    • Analytical Science and Technology
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    • v.14 no.6
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    • pp.510-515
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    • 2001
  • There has been an increasing need for analytical methods of dissolved total iron (tFe) that are highly sensitive, rapid, inexpensive and simple for environmental samples. A sensitive flow injection analysis (FIA) method for determining the concentration of tFe in environmental samples was developed. The proposed method required 10 minutes and only $500{\mu}L$ of sample for and analysis. The standard deviation was 5.0% at $0.5{\mu}gL^{-1}$ (n=6), and the detection limit was $0.075{\mu}gL^{-1}$. The developed method was applied to environmental samples such as tap water, mineral water, rain, snow and cloud water. Since this FIA system was free form interferences of coexisting ions commonly found in samples, sub-${\mu}gL^{-1}$ level of tFe could be easily determined without further preconcentration and separation.

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