• Title/Summary/Keyword: Chemical Determination

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Highly Selective Derivative Spectrophotometry for Determination of Nickel Using 1-(2-Pyridylazo)-2-naphthol in Tween 80 Micellar Solutions

  • Eskandari, Habibollah
    • Bulletin of the Korean Chemical Society
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    • v.25 no.8
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    • pp.1137-1142
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    • 2004
  • A spectrophotometric and first derivative spectrophotometric method was developed in aquatic Tween 80 micellar solutions for selective determination of nickel without using any pre-separation step. 1-(2-Pyridylazo)-2-naphthol (PAN), as a sensitive chromogenic complexing agent formed a red-colored Ni(II)-PAN complex in Tween 80 media with satisfactory solubility and stability. Conditions such as pH, PAN concentration, type and concentration of micellizing agent were optimized. Molar absorptivity of Ni-PAN complex was found $4.62\;{\times}\;10^4L\;cm^{?1}\;mol^{?1}$ at 569 nm, under the optimum condition. Calibration graphs were derived by zero, first and second derivative spectrophotometry at maximum wavelengths of 569, 578 and 571 nm with linear ranges of 30-1800, 20-2500 and 30-2000 ng $mL^{?1}$ , respectively. Precision as standard deviation as well as accuracy as recovery percent were in the range of 1-20 ng $mL^{?1}$, and 93.3-103.3%, respectively, for the entire of the linear ranges. Spectrophotometric detection limit was 3 ng $mL^{?1}$ and effects of diverse ions on the first derivative determination of nickel were studied to investigate selectivity of the method. Interferences of cobalt and copper on the nickel determination were prevented using o-phenanthroline as masking agent. The recommended procedures were applied to the various synthetic and stainless steel alloys, tea leaves and human hair, with satisfactory results.

Spectrophotometric and Derivative Spectrophotometric determination of Copper with N,N'-Oxalylbis(2-Pyridyl-3'-sulphobenzoylhydrazone) (N,N'-Oxalylbis(2-pyridyl-3'-sulphobenzoylhydrazone)을 이용한 구리의 분광광도법 및 미분 분광광도법 정량)

  • Kim Yong-Nam;Choi Kyu-Seong;Choi Seung-Choon;Chung Ryou-Jin
    • Journal of the Korean Chemical Society
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    • v.37 no.1
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    • pp.112-118
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    • 1993
  • A water-soluble chromogenic reagent, N,N'-oxalylbis(2-pyridyl-3'-sulphobenzoylhydrazone) has been synthesized. Spectrophotometric and first-and second-derivative spectrophotometric methods for the determination of copper with the reagent have been developed. Determination has been performed by measuring the absorbance and the first-and second-derivative values of the copper complexes in aqueous solutions (pH 1.89) at 379, 395, 363 and 421 nm, respectively. The method allows the determination of 0.12-1.20 ${\mu}g$ /ml of copper and has been applied to the analysis of aluminium alloy samples. The best results have been obtained from the measurements of the second-derivative values at 421 nm.

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Application of Organized Media for Rapid Spectrofluorimetric Determination of Trace Amounts of Cr(VI) in the Presence of Cr(III)

  • Madrakian, Tayyebeh;Afkhami, Abbas;Mohammadnejad, Masoumeh
    • Bulletin of the Korean Chemical Society
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    • v.30 no.6
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    • pp.1252-1256
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    • 2009
  • A simple, selective and sensitive fluorescence quenching method was developed to the determination Cr(VI). The method is based on the oxidation of $I^-\;to\;{{I_3}^-}$ by Cr(VI) in sulfuric acid solution followed by immediate formation of ion association compound between I3 − and rhodamine 6G in Tween-80 micellar media at room temperature. The influence of several surfactants on rhodamine 6G fluorescence signal was studied; particular attention was paid in the aggregation behavior of rhodamine 6G–Tween-80 system. The experimental parameters (e.g., type of surfactant, reagent concentration) were studied and the optimal conditions were established. The linear calibration graph was obtained in the range 2.0 - 100.0 ng m$L^{-1}$ Cr(VI). The detection limit of the method was 0.37 ng m$L^{-1}$. The relative standard deviation (R.S.D.) is less than 5% (n = 5). The efficiency of the method for the determination of Cr(VI) in the presence of Cr(III) in the sample was investigated. The method was applied successfully to the determination of Cr(VI) and total Cr in water, and liver tissue samples.

Determination of Heparin Using Norfloxacin-cerium Complex as a Fluorescence Probe by Spectrofluorimetry

  • Patil, Shailaja R.;Mote, Umesh S.;Patil, Shivajirao R.;Kolekar, Govind B.
    • Bulletin of the Korean Chemical Society
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    • v.30 no.12
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    • pp.3034-3038
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    • 2009
  • A simple, rapid, practical and sensitive spectofluorimetric method was developed for the determination of trace amount of heparin (Hep). Under the Optimum conditions, we studied the interaction between NFLX-Ce$^{3+}$-Hep complex by using absorption and fluorescence spectra. It was observed that Hep remarkably enhance the fluorescence intensity of the NFLX-Ce$^{3+}$ complex at ${\lambda}$= 356 nm in the buffer solution of pH = 7.60 and the enhancement effect is shown to relate with the concentration of Hep. The linear range and detection limit for the determination of Hep was obtained. By the Rosenthal graphic method, the association constant (K) and binding numbers (N) of Hep with probe were investigated. This method is relatively free of interference from coexisting substances and successfully applied for the determination of heparin in heparin sodium injection samples. A suitable mechanism of fluorescence enhancement between NFLX-Ce$^{3+}$ and the NFLX-Ce$^{3+}$-Hep systems were proposed and discussed.

Integrated Microdisk Gold Electrode Modified with Metal-porphyrin and Metal-phthalocyanines for Nitric Oxide Determination in Biological Media

  • Kim, Il-Kwang;Bae, Hyun-Ok;Oh, Gi-Soo;Chung, Hun-Taeg;Kim, Young-Jin;Chun, Hyun-Ja
    • Bulletin of the Korean Chemical Society
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    • v.24 no.11
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    • pp.1579-1584
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    • 2003
  • An integrated gold microdisk electrode was constructed and modified with metal-porphyrin or metal-phthalocyanines for NO determination in biological media. Microanalysis of NO using square wave anodic stripping voltammetry in $1\;{\times}\;10^{-2}$ M $HClO_4$ was optimal when the accumulation potential was 0.1 V, frequency 100 Hz, and the scan rate was 200 mV/s. When the electrode was modified with metal-porphyrin or metal-phthalocyanines, the anodic peak currents of NO increased due to the catalytic oxidation of NO. In case of Fe(II)-phthalocyanine modified electrode, the peak currents remarkably increased and the sensitivity was high. The calibration curve had good linearity in the range from $3.6\;{\times}\;10^{-5}$ M to $7.2\;{\times}\;10^{-7}$ M, and the detection limit was $5.7\;{\times}\;10^{-7}$ M. For the structural stability and increased sensitivity, Fe(II)-phthalocyanine modified gold microdisk electrode coated with Nafion was applied to determination of NO released from cultured macrophase.

Voltammetric Determination of Cobalt(Ⅱ) Using Carbon Paste Electrodes Modified with 1-(2-Pyridylazo)-2-naphthol

  • 배준웅;박유철;이상학;전우성;장혜영
    • Bulletin of the Korean Chemical Society
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    • v.17 no.11
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    • pp.995-999
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    • 1996
  • A method for the determination of cobalt(Ⅱ) by differential pulse voltammetry using a carbon paste electrode constructed by incorporating 1-(2-pyridylazo)-2-naphthol(PAN) into a conventional carbon paste mixture composed of graphite powder and Nujol oil has been developed. Several influencing factors for the determination of cobalt(Ⅱ) were studied in detail and the optimum analytical conditions were found to be as follows: pH, 4.6; composition of electrode, 20%; temperature of deposition, 43 ℃; time of preconcentration, 15 min. Regeneration of the electrode surface for the continuous uses of the electrode was achieved by exposing the carbon paste electrode to an acidic solution. Response of the electrode was reproducible for the uses of five times and the relative standard deviations were 6.7 and 4.6% for 2.0×10-5 M and 4.0×10-6 M cobalt(Ⅱ), respectively. The calibration curve for cobalt(Ⅱ) obtained by differential pulse voltammetry was divided into two linear ranges of 1.7× 10-6-1.3×10-4 M and 2.0×10-7-8.0×10-7 M. The detection limit was estimated to be 1.3×10-7 M. The effects of coexisting ions were also investigated to test the applicability of the proposed method to the determination of cobalt(Ⅱ) in real samples.

Highly Sensitive Luminescence Assessment of Bile Acid Using a Balofloxacin-Europium(III) Probe in Micellar Medium

  • Cai, Huan;Zhao, Fang;Si, Hailin;Zhang, Shuaishuai;Wang, Chunchun;Qi, Peirong
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.4145-4149
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    • 2012
  • A novel and simple method of luminescence enhancement effect for the determination of trace amounts of bile acid was proposed. The procedure was based on the luminescence intensity of the balofloxacin-europium(III) complex that could be strongly enhanced by bile acid in the presence of sodium dodecyl benzene sulfonate (SDBS). Under the optimum conditions, the enhanced luminescence intensity of the system exhibited a good linear relationship with the bile acid concentration in the range $5.0{\times}10^{-9}-7.0{\times}10^{-7}\;mol\;L^{-1}$ with a detection limit of $1.3{\times}10^{-9}\;mol\;L^{-1}$ ($3{\sigma}$). The relative standard deviation (RSD) was 1.7% (n = 11) for $5.0{\times}10^{-8}\;mol\;L^{-1}$ bile acid. The applicability of the method to the determination of bile acid was demonstrated by investigating the effect of potential interferences and by analyzing human serum and urine samples. The possible enhancement mechanism of luminescence intensity in balofloxacin-europium(III)-bile acid-SDBS system was also discussed briefly.

On-line Trace Enrichment in High Performance Liquid Chromatography Using XAD-2 Precolumn for the Determination of Lonazolac in Human Plasma

  • Lee, Hye-Suk;Kim, Eun-Joo;Zee, Ok-Pyo;Lee, Yoon-Joong
    • Archives of Pharmacal Research
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    • v.12 no.2
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    • pp.108-113
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    • 1989
  • A new column-switching high performance liquid chromatographic method was developed for the determination of lonazolac in plasma. This method was based on the on-line trace enrichment of lonazolac using a precolumn packed with Amberlite XAD-2. The analysis was complete in 20 min. between injections and the limit of detection was $0.1{\mu}g/ml$ using $100{\mu}l$ of plasma. The method was linear in range of $0.1-10{\mu}g/ml$ with a correlation coefficient of 0.9991. Absolute recovery of lonazolac from the spiked plasma samples ranged from 95.6% to 97.1%. The method was shown to be reproducible over the concentration range studied.

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Simplistic Determination of Operation Parameters for Simulated Moving Bed (SMB) Chromatography for the Separation of Ketoprofen Enantiomer

  • Park, Tae-Hyun;Yoon, Tae-Ho;Kim, In-Ho
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.10 no.4
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    • pp.341-345
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    • 2005
  • Since it is troublesome to estimate adequate flow rates in four sections of SMB chromatography, a systematic determination of the flow rates has been suggested by using ketoprofen as a model chiral enantiomer. S-ketoprofen. less retained species, was separated from raffinate stream and the variation in its purity was dependent on the changes of the flow rate of section 4 ($Q_4$), the raffinate flow rate ($Q_{raf}$), and the feed flow rate ($Q_{feed}$) under a fixed switch­ing time t$^{\ast}$. When one parameter was changed at the given experimental condition, purities of product were changed and these phenomena has be well explained by the triangle theory.