• Title/Summary/Keyword: Atomic absorption spectrophotometry

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Determination of Metoclopramide by Flameless Atomic Absorption and Spectrophotometry (무염 원자흡광도법과 흡광광도법에 의한 제제중의 Metoclopramide의 정량)

  • 박만기;임병연;유경수;용군호
    • YAKHAK HOEJI
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    • v.22 no.1
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    • pp.27-32
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    • 1978
  • Metoclopramide reacts with ammonium cobaltothiocyanate to form a stable ion pair which has an absorption maximum of 625mm. The reaction product was insoluble in water but soluble in most organic solvents. 1,2-Dichlorethane was the best extracting solvent among the several organic solvents tested. Metoclopramide can be determinded not only by visible light spectrophotometry but also indirectly by estimation of cobalt in the organic phase by flameless atomic absorption spectrophotometry. Linear relationship was found between absorbance and concentration in the range of 10$^{-4/}$-10$^{-3}$M by spectrophotometry and 10$^{-5}$-10$^{-4}$M by flameless atomic absorption spectrophotometry. The coefficient of variation by spectrophotometry was 0.9% and that of flameless atomic absorption was 1.8%. There was no interference with excipients, pH, temperature and reaction time. With this method, it is possible to determine accurately metoclopramide and tertiary amines in pharmaceutical preparations.

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Determination of Pipethanate$\cdot$HCl by Spectrophotometry and Atomic Absorption Spectrophotometry (흡광광도법 및 원자흡광광도법에 의한 Pipethanate$\cdot$HCl의 정량)

  • 이왕규;박만기;김박광;손채연
    • YAKHAK HOEJI
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    • v.27 no.4
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    • pp.303-307
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    • 1983
  • Pipethanate*HCl reacts with ammonium cobaltothiocyanate to form a stable ion pair which has an absorption maximum at 626nm. The reaction product was insoluble in water but freely soluble in most organic solvents. 1, 2-Dichloroethane was the best extracting solvent among the several organic solvents. Pipethanate*HCl can be determined not only by the spectrophotometry but also inderectly by estimation of cobalt in the organic phase by atomic absorption spectrophotometry. Linear relationship was found between absorbance and concentration in the range of $1.0{\times}10^{-3}~4.0{\times}10^{-3}M$ by spectrophotometry and $1.5{\times}10^{-4}~4.0{\times}10^{-4}M$ by atomic absorption spectrophotometry. With this method it was possible to determine pipethanate$\cdot$HCl in the pharmaceutical preparations.

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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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Studies on the Determination of Rifampicin by Atomic Absorption Spectrophotometry (원자흡광광도법에 의한 리팜피신의 정량에 관한 연구)

  • 이왕규;김박광;유병기
    • YAKHAK HOEJI
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    • v.29 no.4
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    • pp.220-222
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    • 1985
  • Rifampicin reacts with cupric ion to produce rifampicin-Cu(II) chelate (2:1) at pH 6.5, which can be extracted with methylisobutylketone (MIBK). Therefore, rifampicin can be quantitatively, determined by measuring the quantity of Cu(II) in the organic phase by atomic absorption spectrophotometry. Because higher absorbance ratio was obtained in pH 6.0~7.0, buffer solution at pH 6.5 was used in this measurement. Linear relationship was found between absorbance and concentration in the range of 1.0~4.0${\times}10^{-4}M$. This method might be applicable to the determination of rifampicin in the preparations.

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Determination of Inorganic Elements in Paddy Soils by Atomic Absorption Spectrophotometry (원자흡광법(原子吸光法)에 의(依)한 답토괴(沓土壞)의 미량원소(微量元素) 정량(定量))

  • Hwang, Jae-Soon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.10 no.1
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    • pp.107-116
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    • 1981
  • This experiment was attempted to establish the optimal condition, e.g., the effects of pH, interferences of other elements, for the determination of the inorganic elements in the paddy soils by atomic absorption spectrophotometry. Inorganic elements of 100 paddy soils which were sampled in Jeon bug provincial farm land were determined by atomic absorption spectrophotometer in that condition. The results obtained in this experiment are summarized as follows: 1) The optimal pH for determination of inorganic elements in paddy soils is about 7.0. 2) It was investigated that the absorbance of potassium was increased, and that of calcium, magnesium and zinc was decreased by adding of $Fe^{++}$ and $Cu^{++}$ in the sample. 3) It was shown that paddy soils in Jeonbug provincial farm land contain the normal amounts of inorganic elements (K, Ca, Mg, Zn,). But comparing to the results of 1976 year, it was known that the contents of inorganic elements in paddy soils considerably was changed.

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Determination of Trace Elements in Urine Samples by Graphite Furnace Atomic Absorption Spectrophotometry (흑연로 원자흡수분광광도법에 의한 뇨시료 중 흔적량 원소의 정량)

  • Choi, Chong-Moon;Choi, Hee-Seon;Park, Chang Joon;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.7 no.4
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    • pp.555-561
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    • 1994
  • A method was described for the graphite furnace atomic absorption spectrophotometric determination of trace cadmium, copper, chromium and lead in urine samples. The elements were directly determined without any other treatments. The ash temperature was intensively optimized to improve the large background by the removal of organic materials and alkali and alkali earth metals in urine samples. Two kinds of standard solutions were used to plot calibration curves. From the recovery data, it could be confirmed that the analytical results with the synthetic urine matrix similar to real urine were more accurate than with a deionized water matrix.

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Graphite Furnace Atomic Absorption Spectrophotometric Determination of Trace Horseradish Peroxidase Using Nanosilver

  • Jiang, Zhi-Liang;Tang, Ya-Fang;Wei, Lin;Liang, Ai-Hui
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2732-2736
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    • 2011
  • In pH 4.2 HAc-NaAc buffer solution, horseradish peroxidase (HRP) catalyzed $H_2O_2$ oxidation of nanosilver to form $Ag^+$. After centrifugation, $Ag^+$ in the supernatant can be measured by graphite furnace atomic absorption spectrophotometry (GFAAS) at the silver absorption wavelength of 328.1 nm. When HRP concentration increased, the $Ag^+$ concentration in the supernatant increased, and the absorption value enhanced. The HRP concentration in the range of 0.84-50 $ng{\cdot}mL^{-1}$ was linear to the enhanced absorption value (${\Delta}A$), with a regression equation of ${\Delta}A$=0.012C+0.11, correlation coefficient of 0.9988, and detection limit of 0.41 $ng{\cdot}mL^{-1}$ HRP. The proposed GFAAS method was used to detect HRP in waste water samples, with satisfactory results.

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 Lead in Urine by Atomic Absorption Spectrophotometry (원자흡광법을 이용한 요중 연 배설량의 정량)

  • Paik, Nam-Won;Yoon, Bock-Sang;Chung, Kyou-Chull
    • Journal of Preventive Medicine and Public Health
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    • v.7 no.2
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    • pp.377-381
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    • 1974
  • Determination of lead in urine is important in industrial hygiene and toxicology. Dithizone method has been principally used for the determination of lead in urine, which gives accurate results in skilful hands but is usually complex and time-consuming. Atomic absorption spectrophotometry is a new simple method and several procedures have been described. However, the influences of pH and the presence of chelating agents during treatment of lead poisoning are not clear. The purpose of this study was to find out the effect of pH and chelating agents on the determination of lead using Shimadzu atomic absorption/flame spectrophotometer, model AA-610. The results obtained were as follows: 1. The atomic absorption spectrophotometry(AAS) could be applied without prior acid digestion to specimens in the absence of chelating agents. The absorbance at $2,170\;{\AA}$, though more sensitive, was more noisy electronically. Therefore, we selected the wavelength of $2,833\;{\AA}$ plus scale expansion. 2. The optimal pH was in the range from 2 to 3. 3. The sensitivity was $0.075{\mu}g/ml/%$ and detection limit was about $0.2{\mu}g/ml$. 4. In the presence of EDTA, lead could not be completely determined without prior acid digestion. 5. On specimens from patients receiving penicillamine therapy, a comparison was made between the values obtained with dithizone method and AAS method with prior acid digestion. The results of comparison showed a very good agreement.

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Matrix Modification for Graphite Furnace Atomic Absorption Spectrophotometric Determination of Volatile Elements(III) Trace Bismuth

  • Kim, Young-Sang;Choi, Jong-Moon;Kim, Young-Man
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.435-442
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    • 1995
  • A matrix modification was studied for the determination of trace bismuth in water samples by graphite furnace atomic absorption spectrophotometry. The type and quantity of modifiers as well as the use of auxiliary modifiers were investigated to realize the efficient modification. Palladium was chosen as a single modifier. By the addition of palladium($5{\mu}g/mL$) to 100 ng/mL bismuth solution, the temperatures could be raised from $500^{\circ}C$ to $1,300^{\circ}C$ for the charring and from $2,000^{\circ}C$ to $2,200^{\circ}C$ for the atomization as well as the sensitivity and reproducibility were improved. The absorbance of bismuth was maximum and not changed in the range of Pd $3-25{\mu}g/mL$. And several materials were examined as an auxiliary modifier. The mixed solution of $1{\mu}g/mL$ palladium and $200{\mu}g/mL$ nickel have raised the temperatures as with $5{\mu}g/mL$ palladium only. The maximum absorbance of bismuth was shown in the nickel concentration range of $100-300{\mu}g/mL$ in $1{\mu}g/mL$ palladium modified system. With such optimum conditions, the trace amount of bismuth in several water samples could be determined by a calibration curve method, and good recoveries were also obtained.

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