• Title/Summary/Keyword: 예비농축

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Preconcentration, Separation and Determination of lead(II) with Methyl Thymol Blue Adsorbed on Activated Carbon Using Flame Atomic Absorption Spectrometry (불꽃원자 흡수 분광법으로 활성탄소에 흡착된 메틸티몰 블루로 납(II)의 예비농축, 분리 및 측정)

  • Ensafi, Ali A.;Ghaderi , Ali R.
    • Journal of the Korean Chemical Society
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    • v.52 no.1
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    • pp.16-22
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    • 2008
  • on-line system for preconcentration and separation of lead(II) is presented. The method is based on the complex formation of Pb(II) with adsorbed Methyl thymol blue on activated carbon. The conditions of preparing the solid phase reagent and of quantitative recovery of Pb(II) from diluted solutions, such as acidity of aqueous phase, solid phase capacity, and flow variables were studied as well as effect of potential interfering ions. After preconcentration step, the metal ions are eluted automatically by 5 ml of 0.5 M HNO3 solution and the lead ions content was determined by flame atomic absorption spectrometry. Under the optimum conditions, the lead ions in aqueous samples were separated and preconcentrated about 1000-fold by the column. The detection limit was 0.001 g mL-1. Lead has been determined in river and tap water samples, with recovery of 98 to 102%.

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%.

Pre-concentration of Apple Juice with Different Reverse Osmosis Membranes (역삼투막을 이용한 사과쥬스의 예비농축)

  • Kim, Kil-Hwan;Park, Hyun-Jin;Kim, Dong-Man
    • Korean Journal of Food Science and Technology
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    • v.20 no.3
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    • pp.419-425
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    • 1988
  • The clarified apple juice was pre-concentrated by reverse osmosis system as a trial for reduction of heat treating time and quality drop in concentration of the juice. The permeate fluxes through CA 865 and CA 960 membranes were higher than those of HR 95 and HR 98 membranes even at the low operating pressure. In the concentration limit depended on the membranes used, HR membranes operated at 60 bar showed $29.0^{\circ}$Brix, and the time required to reach the limit was 86 min for HR 95 and 71 min for HR 98. In cases of CA membranes run at 30 bar, the juice concentration was linearly increased without the limit, and longer time to reach the same concentration was required in comparison with HR membranes. As the juice concentration was increased, the loss of soluble solids was increased, and the average contents of soluble solids in the permeate passed through HR 95, HR 98, CA 865 and CA 960 were 1.3, 0.5, 7.5 and $2.3^{\circ}$ Brix, respectively, in the juice concentration range of 20.0 -$25.0^{\circ}$ Brix. The lower amounts of sugars, total acid and flavor volatiles were involved in the permeate through HR membranes, especially HR 98 than in the permeate through CA membranes.

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Determination of Cd(II) after Preconcentration onto Microcrystalline p-Dichlorobenzene Loaded with 2-Mercaptobenzothiazole (2-Mercaptobenzothiazole이 내포된 p-Dichlorobenzene 미세결정으로 예비농축시킨 후 Cd(II) 정량)

  • Yoon, Ju-Im;Choi, Hee-Seon
    • Journal of the Korean Chemical Society
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    • v.53 no.1
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    • pp.27-33
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    • 2009
  • A sensitive technique for the determination of trace Cd(II) in various real samples after preconcentration onto microcrystalline p-dichlorobenzene loaded with 2-mercaptobenzothiazole was developed. Several experimental conditions such as the pH of the sample solution, the amount of chelating agent 2-mercaptobenzothiazole, the amount of adsorbent p-dichlorobenzene-2-MBT, and the flow rate of sample solution were optimized. The interfering effects of various concomitant ions were investigated. Cu(II) interfered with more seriously than any other ions. However, the interference by Cu(II) could be overcome sufficiently by adjusting tartrate ion concentration to be 0.01M or by controlling the amount of 2-mercaptobenzothiazole contained in 0.20 g p-dichlorobenzene to be 0.12 g. The dynamic range, the correlation coefficient ($R^2$) and the detection limit obtained by this proposed technique were $0.5{\sim}30$ ng $mL^{-1}$, 0.9962, and 0.39 ng $mL^{-1}$, respectively. Thus, good results were obtained by the use of p-dichlorobenze as adsorbent matrix. For validating this proposed technique, the aqueous samples(wastewater, stream water, and reservoir water) and the plastic sample were used. Recovery yields of $93{\sim}104$ % were obtained. By F test, these measured data were not different from ICP-MS data at 95 % confidence level. Based on the results from the experiment, it was found that this proposed technique could be applied to the preconcentration and determination of Cd(II) in various real samples.

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.

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 and Extraction of Copper on Activated Carbon Using 4-Amino-2, 3-dimethyl-1-phenyl-3-pyrazoline or 4-(4-methoxybenzylidenimin) thiophenole (4-Amino-2,3-dimethyl-1-phenyl-3-pyrazoline 또는 4-(4-Methoxybenzylidenimin)thiophenole을 이용한 활성탄에서의 구리의 예비 농축 및 추출)

  • Ghaedi, Mehrorang;Ahmadi, Farshid;Karimi, Hajir;Gharaghani, Shiva
    • Journal of the Korean Chemical Society
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    • v.50 no.1
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    • pp.23-31
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    • 2006
  • carbon modified methods were used for the preconcentration and determination of copper in some real samples using the flame atomic absorption spectrometry. The copper ions was adsorbed quantitatively on the activated carbon due to their complexation with 4- amino-2, 3-dimethyl-1-phenyl-3-pyrazoline (ADMPP) or 4-(4- methoxybenzylidenimin) thiophenole (MBITP). The adsorbed copper on solid phase was eluted quantitatively using small amount of nitric acid. The influence of important parameters including pH, amount of carrier, flow rate, amount of activated carbon and type and concentration of eluting agent for obtaining maximum recovery were investigated. The methods based on ADMPP and MBITP at optimum conditions is linear over concentration range of 0.05-1.5 g mL-1 and 0.05-1.2 g mL-1 of copper with correlation coefficient of 0.9997 and 0.9994 and both detection limit of 1.4 ng mL-1, respectively. The preconcentration leads to enrichment factor of 310 and break through volume of 1550 mL for both ligands. The method has a good tolerance limit of interfering ion and a selectivity that has been successfully applied for the determination of copper content in real sample such as tap, spring, river and waste water.

Determination and preconcentration of Cu(II) using microcrystalline p-Dichlorobenzene loaded with salicylaldoxime (Salicylaldoxime이 내포된 p-Dichlorobenzene 미세결정을 이용한 Cu(II)의 예비농축 및 정량)

  • Lee, Ha-Na;Choi, Hee-Seon
    • Analytical Science and Technology
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    • v.23 no.3
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    • pp.240-246
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    • 2010
  • A technique for the determination of trace Cu(II) in various real samples by FAAS after the column preconcentration onto p-dichlorobenzene-SA adsorbent, which is microcrystalline p-dichlorobenzene loaded with salicylaldoxime (SA) has been developed. Several experimental conditions such as pH of the sample solution, the amount of chelating agent salicylaldoxime, the amount of adsorbent p-dichlorobenzene-SA, and flow rate of sample solution were optimized. The interfering effects of various concomitant ions were investigated. $CN^-$ interfered more seriously than any other ions. However, the interference by $1\;{\mu}g\;mL^{-1}\;CN^-$ could be overcome completely by controlling the concentration of Ni(II) to $20\;{\mu}g\;mL^{-1}$. The linear range, correlation coefficient ($R^2$) and detection limit obtained by this technique were $3.0\sim100\;ng\;mL^{-1}$, 0.9901, and $3.1\;ng\;mL^{-1}$, respectively. For validating this technique, the aqueous samples (wastewater, reservoir water and stream water) and the food samples (orange juice, fresh egg and skim milk) were used. Recovery yields of 93~104% were obtained. These measured mean values were not differents from ICP-MS data at 95% confidence level. The good results were obtained from the experiments using the rice flour certified reference material (CRM) sample. Based on the experimental results, it was found that this technique could be applied to the preconcentration and determination of Cu(II) for various real samples.