• Title/Summary/Keyword: Extraction-Spectrophotometry

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Determination of Mefenamic Acid in Human Urine by Means of Two Spectroscopic Methods by Using Cloud Point Extraction Methodology as a Tool for Treatment of Samples

  • Tabrizi, Ahad Bavili
    • Bulletin of the Korean Chemical Society
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    • v.27 no.11
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    • pp.1780-1784
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    • 2006
  • Cloud point extraction was used to extract mefenamic acid (MF) from human urine, and spectrofluorimetry and spectrophotometry were used to analyze extracted MF. The variables affecting extraction and phase separation, i.e. HCl and Triton X-114 concentration, temperature and time of equilibration, were optimized. Under the experimental conditions used the limit of detection for extraction of 25 mL of sample was 0.006 and 0.045 mg $L^{-1}$, with relative standard deviations of 2.52 and 1.45% (n = 5) for spectrofluorimetric or spectrophotometric methods, respectively. Good recoveries in the range of 95-107% were obtained for spiked samples. The proposed methods were applied to the determination of MF in human urine.

Measurement conditions for cadmium in urine by flame atomic absorption spectrophotometry (불꽃원자 흡수광법에 의한요중 카드뮴 배설량 측정의 지적조건)

  • Choi, Ho-Chun;Chung, Kyou-Chull
    • Journal of Preventive Medicine and Public Health
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    • v.17 no.1
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    • pp.269-279
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    • 1984
  • The optimum conditions for measuring cadmium content of less than 0.2ppm by flame atomic absorption spectrophotometry were investigated. The cadmium in urine was extracted by APDC-MIBK for the analysis by atomic absorption spectrophotometry after ashing them by a wet method. 1. Optimum conditions by APDC-MIBK and DDTC-MIBK extractions. The acidic aqueous solution was prepared with appropriate amount of 0.IN nitric acid, 5ml of 25% (W/V) sodium potasstum tartarate, 10ml of saturated ammonium sulfate, and 2ml of 2% APDC(or 1 ml of 5% DDTC) chelating agent. The total volume of solution was adjusted to 55 ml and pH to $2{\sim}10$ (or$7{\sim}10$). The aqueous solution was extracted with 10ml MIBK. Concentration of Triton X-100 did not effect the absorbance for APDC-MIBK extraction of cadmium, but absorbance decreased as the concentration increased for DDTC-MIBK extraction. The sensitivity and detection limits for the cadmium determination from APDC-MIBK extraction were 0.0038ppm and 0.0102, 0.0022ppm and 0.0116 for DDTC-MIBK, and 0.0132ppm and 0.0034 for 0.1N nitric acid. APDC-MIBK and DDTC-MIBK extractions were 3 times higher than 0.1N nitric acid for the sensitivity. 2. Excretion of cadmium in 24-hour urine by APDC-MIBK extraction. Determination of cadmium in urine by atomic absorption spectrophotometry of A.A. (Cd=2 mA) mode and B.C. (Cd=4 mA) mode and B.C. (Cd=4mA, $D_2=20mA$) mode showed some difference (p<0.05). The difference of cadmium determination and recovery according to method of standard additions and standard calibration curve method in urine was not significant (p>0.05, $93.48{\pm}11.78%,\;94.83{\pm}22.00%$). Excretion of cadmium in 24-hour urine collection from normal person and variance analysis within measurement variation was not significant (p>0.05), but between interindividual was significant (0.05). Determination of cadmium content by two different methods of flame atomic absorption spectrophotometry and dithizone colorimetry showed that the results from the two methods can be described by a regression line with a good correlation (y=1.0153x-0.2927, x=Cd by D.C., y=Cd by A.A.S., $r=0.8651^*$, p<0.01).

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Determination of Gold by Flame Atomic Absorption Spectrophotometry using a New Chelating Agent (새로운 킬레이트 시약을 이용한 금의 원자흡수광도법 정량)

  • Lee, Jin-Sik;Uesugi, Katsuya;Thoru, Nagahiro;Choi, Won-Hyung;Kim, Kyung-Tae;Choi, Sung-Yung
    • Analytical Science and Technology
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    • v.8 no.3
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    • pp.391-396
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    • 1995
  • A rapid preconcentration method based on solvent extraction is described for the determination of gold by flame atomic absorption spectrophotometry. Trace amounts of gold was extracted as a new chelating agent, 3-thiophenaldehyde-4-phenyl-3-thiosemicarbazone from pH 4.0 in diisobutyl ketone. The method is simple, fast, free from the effect of many interfering ions and has a high sensitivity and a good precision. Gold is quantitatively separated and concentrated from the elements in standard sample, and the value of the recovery was 91.7 and 108.3% by the proposed method.

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DETERMINATION OF CADMIUM, COPPER, LEAD, ZINC AND MERCURY IN SEA WATER BY ATOMIC ABSORPTION SPECTROPHOTOMETRY (해수중 카드뮴, 구리, 납, 아연 및 수은의 원자흡광정량법)

  • WON Jong Hun;PARK Chung Kil;YANG Han Serb
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.9 no.3
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    • pp.169-175
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    • 1976
  • A solvent extraction-atomic absorption spectrophotometry for determination of trace amount of cadmium, copper, lead and zinc and a flameless atomic absorption spectrophotometry for mercury in sea water were studied. The optimum pH range for solvent extraction was pH 4-7. A better solvent extraction efficiency was obtained with MIBK solvent than nitrobenzene, benzene, isoamylalcohol, n-buthylacetate. DDTC was more advantageous than APDC as chelating agent. The metals, chelated with DDTC and concentrated into MIBK by solvent extraction with a volume of $1\iota$ of sea water for cadmium, copper and lead, and 200m1 for zinc, were determined simultaneously by atomic absorption spectrophotometry. For mercury determination, 500ml of sea water was digested with permanganate-sulfuric acid and mercury( II ) was reduced by stannous chloride and aerated the solution with air pump until the absorbance reached a constant value. The precisions, in standard deviation, of these methods were 0.058ppb for cadmium, 0.084 ppb for copper, 0.44ppb for lead, 2.49ppb for zinc and 0.08 ppb for mercury. The sensitivities, expressed in $ppb/1\%$ absorption, were 0.058 ppb cadmium, 0. 15 ppb copper, 0.6 ppb lead, 1.2 ppb zinc and 0.01 ppb mercury respectively. No significant adsorption on the wall of polyethylene sample bottle occurred during 30 days of storing by acidification to pH 1.5 with nitric acid except zinc. Poor reproducibility was found for zinc with this method.

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Nickel(II) Determination by Spectrophotometry Coupled with Preconcentration Technique in Water and Alloy Samples

  • Rekha, Dasari;Kumar, Jengiti. Dilip;Jayaraj, Bellum;Lingappa, Y.;Chiranjeevi, Pattium
    • Bulletin of the Korean Chemical Society
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    • v.28 no.3
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    • pp.373-378
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    • 2007
  • A micro organism Agrobacterium tumifacient as an immobilized cell on a solid support was presented as a new biosorbent in a simple and sensitive spectrophotometry determination of Ni(II) in various samples using 4-hydroxy benzaldehyde-4-bromophenyl hydrazone as a color developing agent (λmax 497 nm) at pH 4.0 ± 0.2. Beer's law was obeyed over the range of 0.01-0.1 μg L-1. The molar absorptivity and Sandell's sensitivity were 1.285 × 105 L mol-1cm-1 and 0.007245 μg cm-2 respectively. Under these conditions, the preconcentration factor obtained was 82, and the detection limit achieved was 0.05 μg L-1. The detailed study of various interfering ions made the method more sensitive and selective. The recovery of Ni(II) from various samples range from 97.75 to 99.35%. The present method was successfully applied for the determination of Ni(II) in spiked, natural water and alloy samples. The proposed method was compared with reported methods in terms of Student's ‘t'-test and Variance ratio ‘f'-test which indicates that there is no significant difference between proposed and literature method at 95% confidence level.

he Study of Nucleic Acid Extraction Method from Archival Paraffin Blocks (보존된 파라핀 블록에서 핵산 추출기법에 관한 연구)

  • Joo, Kyung-Woong
    • Korean Journal of Clinical Laboratory Science
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    • v.40 no.2
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    • pp.113-117
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    • 2008
  • It designed a study to examine the efficiency of DNA and RNA extraction from archival formalin-fixed, paraffin-embedded tissues using an non-heating and heating method. Archival paraffin blocks of liver, kidney, colon were randomly selected. Each paraffin block was prepared in 20 microtubes. For each paraffin blocks were tested non-heating DNA extraction to 10 microtubes and heating protocol under pH 7.0 and $100^{\circ}C$ to 10 microtubes. Evaluation of the results of DNA extraction was carried out by measuring concentration by UV spectrophotometry and then PCR amplification. DNA extraction content that non-heating method was liver $5{\pm}0.7{\mu}g/mL$, kidney $2{\pm}0.3{\mu}g/mL$, colon $6{\pm}0.4{\mu}g/mL$ and heating method was liver $12{\pm}0.6{\mu}g/mL$, kidney $7{\pm}0.5{\mu}g/mL$, colon $10.{\pm}0.3{\mu}g/mL$. Successful RNA extraction was observed, by ${\beta}$-actin amplification, in 46.7% sections for samples treated by the heating method versus 30.0% using non-heating DNA extraction. The extracted nucleic acid showed better values for samples heated at $100^{\circ}C$. Therefore heating extraction of nucleic acid is reliable, quick and efficiency.

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Comparison of Analytical Methods for DEHP Migration from PVC Bags for Blood Storage and Infusion; By Gas Chromatography and UV-vis Spectrophotometry (혈액·수액용 PVC 백에서 용출된 DEHP의 검출 분석 방법 비교; 기체 크로마토그래프와 분광 광도계)

  • Kim, Jung Hwan;Kim, Seong Hun;Choi, Hyeong Ki;Lee, Chang Hyung
    • Analytical Science and Technology
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    • v.15 no.1
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    • pp.72-79
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    • 2002
  • Di-(2-ethylhexyl)phthalate (DEHP) may be released from plasticized poly(vinyl chloride) (PVC) articles. In the cases of various methods for the quantitative analysis of migrating DEHP, there are much differences in migrating quantity according to the experimental methods. It is therefore important to make the comparison and analysis between these two results. A study of DEHP migration from blood and infusion bags has been carried out in different methods to evaluate the amount of DEHP migration using gas chromatograph and UV-vis spectrophotometry. Five PVC bags were cut into plane sheets in size of $40{\times}10{\times}0.4mm$, then were immersed in extraction solvent for an hour to release DEHP. It was determined by a gas chromatograph that $23.2{\sim}70.9{\mu}g/mL$ of DEHP was extracted. While extraction solvent was injected into PVC bags which were then placed for an hour to leach DEHP out. It was checked by a UV-vis spectrophotometer that the concentration of DEHP in extraction solvent was $24.8{\sim}41.3{\mu}g/mL$. Two results show different values according to the extraction conditions and experimental methods and the gas chromatographic results were converted into UV-vis spectroscopic results on condition that DEHP would be extracted equally per unit time and unit contact area. It was concluded that DEHP migrating amounts are approximately equal in two analytical methods.

A Study on Enhancement of Np Extraction by TBP Through the Electrochemical Adjustment of Np Oxidation State by Using a Glassy Carbon Fiber Column Electrode

  • Kim, Kwang-Wook;Song, Kee-Chan;Lee, Eil-Hee;Park, In-Kyu;Yoo, Jae-Hyung
    • Nuclear Engineering and Technology
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    • v.32 no.4
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    • pp.309-315
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    • 2000
  • The changes of Np oxidation state in nitric acid and the effect of nitrous acid on the oxidation state were analyzed by spectrophotometry, solvent extraction, and electrochemical methods. An enhancement of Np extraction to 30 vol.% TBP was carried out through adjustment of Np oxidation state by using a glassy carbon fiber column electrode system. The information of electrolytic behavior of nitric acid was important because the nitrous acid affecting the Np redox reaction was generated during the electrolytic adjustment of the Np oxidation state. The Np solution used in this work consisted of Np(V) and Np(Ⅵ)without (IV). The composition of Np(V) in the range of 0.5M -5.5 M nitric acid was 32% ~ 19%. The electrolytic oxidation of Np(V) to Np(Ⅵ)in the solution enhanced Np extraction efficiency about five times higher than the case without the electrolytic oxidation. It was confirmed that the nitrous acid of less than about 10-5 M acted as a catalyst to accelerate the chemical oxidation reaction of Np(V) to Np(Ⅵ).

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Studies on the Formation of Copper Complexes of Sulfa-Drug II.Study on Chemical Constisuent of Copper Sulfa-Drug Complex by Continuous Variation Method. (Sulfa제-Cu착화합물의 형성에 관하여 II Spectrophotometry 에 의한 Copper Sulfa-Drug Complex 의 화학조성결정)

  • 이왕규
    • YAKHAK HOEJI
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    • v.8 no.4
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    • pp.96-99
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    • 1964
  • In the previous study, the composition ratios of the Cu-sulfa drugs complexes determined by gravimetric and solvent extraction method reported. In this paper, the continuous variations method has been used to know whether the complexes are simple complexes or chelates, and to recertify the composition ratios of the complexes at pH 7-8. It has been certified that the ratio of $Cu^{+2}$ ion to sulfa drugs in 1:2 from the result of this experiment.

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Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

  • Hu, Qiu-Fen;Yang, Guan-Gyu;Huang, Zhang-Jie;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • v.25 no.4
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    • pp.545-548
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    • 2004
  • A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with $C_{18}$ membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with $C_{18}$ membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was $1.32{\times}10^5L\;mol^{-1}cm^{- 1}$ at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 ${\mu}$g/mL. This method was applied to the determination of nickel in water and biological samples with good results.