A simple and sensitive kinetic spectrophotometric method for the determination of trace amounts of titanium(IV),based upon the catalytic effect of Ti(IV) on the oxidation of acid chrome blue K (ACBK) by hydrogen perox...A simple and sensitive kinetic spectrophotometric method for the determination of trace amounts of titanium(IV),based upon the catalytic effect of Ti(IV) on the oxidation of acid chrome blue K (ACBK) by hydrogen peroxide in 0.002 mol/L sulfuric acid,is described. The reaction rate is monitored spectrophotometrically by measuring the decrease in absorbance of ACBK at 524 nm. The detection limit of the method is 1.01×10?9 g/mL,and the linear range is 0-0.048 mg/L. The influence of acidity,concentration of reactants,reaction time,reaction temperature and for-eign ions is also discussed. The optimum reaction conditions were established and some kinetic parameters determined. The apparent activation energy of the catalytic reaction is 5.32 kJ/mol. The relative standard deviation for the determi-nation of titanium(IV) at the concentration of 0.048 mg/L is calculated to be 1.31% (n = 11). In combination with sol-vent extraction separation,the method has been successfully applied to the determination of trace titanium(IV) in human hair,plant matter,tea and rock samples. The results are in good agreement with the certified values with the relative standard deviations (RSD) of 1.4%-3.5%.展开更多
A simple and sensitive flow injection(FI) spectrophotometric method was reported for the determination of uric acid based on the reduction of Fe(III)/ferricyanide in the presence of uric acid. The in situ reduced ...A simple and sensitive flow injection(FI) spectrophotometric method was reported for the determination of uric acid based on the reduction of Fe(III)/ferricyanide in the presence of uric acid. The in situ reduced ions reacted with unreduced portion of ferricyanide/Fe(III) to form soluble Prussian blue, which was monitored at an absorption wavelength of 735 nm. The optimized conditions allow a linear calibration graph in a concentration range of 1―100 μmol/L. The relative standard deviation was in a range of 0.5%―2.5%, with a detection limit(3σ blank) of 0.3 μmol/L and a sampling frequency of 60 injection/h was obtained. The effect of common substances present in human physiological fluids on the determination of uric acid was examined. The method was applied to determining uric acid in human urine samples with the recoveries in a range of 96%―105%. The results agree well with those by spectrophotometric reference method at a confidence level of 95%. Spectrophotometric procedures for uric acid determination in clinical samples were reviewed briefly.展开更多
A novel sensitive and relatively selective kinetic method is presented for the determination of V(V) based on its catalytic effect on the oxidation reaction of Celestine blue by potassium bromate in the presence of ...A novel sensitive and relatively selective kinetic method is presented for the determination of V(V) based on its catalytic effect on the oxidation reaction of Celestine blue by potassium bromate in the presence of citric acid as an activator. The reaction was monitored spectropho- tometrically by measuring the decrease in absorbance of Celestine blue at a maximum absorption wavelength of 540 nm between 0.5 and 9 min (the fixed-time method) in an H3PO4 medium at 45℃. The effect of various parameters such as concentrations of H3PO4, citric acid, potassium bromate and Celestine blue, ionic strength, reaction temperature and time on the rate of V(V) catalyzed reaction was studied. The method is free from the most interferences, especially from large amounts of V(IV). The decrease in absorbance is proportional to the concentration of V(V) over the entire concentration range tested (0.025-1.25 lag.mL^-1) with a detection limit of 6.80 tag.L^-1 (according to statistical 3Sblank/k criterion) and a coefficient of variation (CV) of 1.78% (for ten replicate measurements at 95% confidence level). The proposed method suffers from a few interferences such as Cr(VI) and Hg(Ⅱ) ions. The method was successfully applied to the determination of V(V) in river water, lake water, tap water, natural drinking water samples and a certified standard reference material such as SRM-1640 with satis- factory results. The vanadium contents of natural water samples were detected by using both linear calibration curve and standard addition curve methods. The recoveries of spiked vanadium (V) into the certified standard water sample were found to be quantitative, and the reproducibility was satisfactory. It was observed that the results of the SRM 1640 were in good agreement with the certified value.展开更多
A novel method for the determination of captopril by spectrophotometer is described in this paper. The experiment is based on the fact that Fe(Ⅲ) is reduced to Fe(Ⅱ) by captopril, then the in sire formed Fe(Ⅱ...A novel method for the determination of captopril by spectrophotometer is described in this paper. The experiment is based on the fact that Fe(Ⅲ) is reduced to Fe(Ⅱ) by captopril, then the in sire formed Fe(Ⅱ) reacts with potassium ferricyanide to give the soluble prussian blue at pH 4.00, and its maximal adsorption wavelength (λmax) is 735 nm. Good linear relationship is obtained between the absorbance and the concentration of captopril in the wide range of 0.05-20 μg/mL. The linear regression equation is A = -0.04314 + 0.11423C (μg/mL) with a correlation coefficient R = 0.9998. The detection limit (3σ/k) is 0.04 μg/mL, the molar absorption coefficient is 2.5×10^4 L/mol cm. By mensurating the absorbance of soluble prussian blue, the indirect determination of captopril can be obtained. This method has been successfully applied to determination of captopril in pharmaceutical samples. Analytical results obtained are satisfactory.展开更多
A simple and sensitive flow injection spectrophotometric method is reported for the determination of vitamin E using potassium ferricyanide-Fe(Ⅲ) detection system.In the presence of vitamin E,Fe(Ⅲ)/ferricyanide redu...A simple and sensitive flow injection spectrophotometric method is reported for the determination of vitamin E using potassium ferricyanide-Fe(Ⅲ) detection system.In the presence of vitamin E,Fe(Ⅲ)/ferricyanide reduces.The in situ reduced ions are then reacted with unreduced portion of ferricyanide/Fe(Ⅲ) to make soluble Prussian blue,which is monitored at absorption wavelength of 735 nm.Linear calibration graph was obtained in the concentration range of 0.1-40μg mL^(-1).The relative standard deviations (n=4) were in the range of 1.1-3.6%,with limits of detection(3 s blank) of 0.04μg mL^(-1).The proposed method allowed 12 injections h^(-1).The method is applied to determine vitamin E in pharmaceuticals,infant milk and blood serum samples using hexane extraction with the recoveries in the range of 93±3 to 97.5±4%.The method is validated using certified reference materials SRM 968c for blood serum samples.展开更多
A new kinetic spectrophotometric method has been developed for the determination of iron (Ⅲ). The method is based on the catalytic effect of iron (Ⅲ) on the oxidation of weak acid brilliant blue dye (RAWL) by ...A new kinetic spectrophotometric method has been developed for the determination of iron (Ⅲ). The method is based on the catalytic effect of iron (Ⅲ) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The advantages of the proposed method are that it is sensitive, accurate, rapid, inexpensive, can be operated under room temperature and has a large determination concentration range compared to other techniques. The obtained optimum conditions are: pH 3.15, RAWL (200 mgL^-1) 5.00mL, Potassium periodate solution (0.01 molL^-1) 0.30mL, phenanthroline (0.02 molL^-1) 1.00mL, reaction temperature 25℃ and reaction time 7 min. With this method iron could quantitively be determined in the range 0.00-0.02 mgL^-1, the detection limit being 4.10 × 10^10gmL^-1. The relative standard deviations (RSD) in five replicate determinations for 3 μgL^-1and 5 μgL^-1 iron (Ⅲ) are 3.1% and 1.9%, respectively. The method has been applied to the determination of iron (Ⅲ) in tap water samples and seawater samples (from the South China Sea), the recovery rates being 98.0% and 100.5%, respectively.展开更多
A simple flow injection spectrophotometric method is reported for the determination of cysteine,N-acetyl cysteine and glutathione based on the reduction of Fe(Ⅲ)/ferricyanide,the in situ reduced ions are reacted wi...A simple flow injection spectrophotometric method is reported for the determination of cysteine,N-acetyl cysteine and glutathione based on the reduction of Fe(Ⅲ)/ferricyanide,the in situ reduced ions are reacted with unreduced portion of ferricyanide/Fe(Ⅲ) to form soluble Prussian blue,which is monitored at 735 nm.The calibration graphs are linear in the concentration ranges of(1―100)×10-6 mol/L for cysteine and N-acetyl cysteine,and(1―50)×10-6 mol/L for glutathione.The relative standard deviations of 1.8%,2.5% and 1.9% were found for eleven replicate analyses of 5×10-6 mol/L cysteine,N-acetyl cysteine and glutathione.The limits of detection(3σ blank) at 5×10-7 mol/L for cysteine,and 3×10-7 mol/L for N-acetyl cysteine and glutathione were obtained.The proposed method allowed 60 injections/h.The effects of common substances present in pharmaceuticals and human physiological fluids were examined.The method was applied to determining cysteine in pharmaceutical formulations with the recoveries in a range of 97% to 106% and the results obtained are agreed well with labeled values.展开更多
A novel catalytic kinetic method is proposed for the determination of Se(Ⅳ), Se(Ⅵ), and total inorganic selenium in water based on the catalytic effect of Se(Ⅳ) on the reduction of Celestine blue by sodium su...A novel catalytic kinetic method is proposed for the determination of Se(Ⅳ), Se(Ⅵ), and total inorganic selenium in water based on the catalytic effect of Se(Ⅳ) on the reduction of Celestine blue by sodium sulfide at pH 7.0 phosphate buffer. The fixed-time method was adopted for the determination and speciation of inorganic selenium. Under the optimum conditions, the two calibration graphs are linear with a good correlation coefficient in the range 2-20 and 20-200 μg·L-1 of Se(Ⅳ) for the fixed-time method at 30℃. The experimental and theo- retical detection limits of the developed kinetic method were found to be 0.21 and 2.50 μg·L-1 for the fixed-time method (3 min). All of the variables that affect the sensitivity at 645 nm were investigated, and the optimum conditions were established. The interference effect of various cations and anions on the Se(Ⅳ) determination was also studied. The selectivity of the selenium determination was greatly improved with the use of the strongly cation exchange resin such as Amberlite IR120 plus as long as chelating agents of thiourea and thiosulphate. The proposed kinetic method was validated statistically and through recovery studies in natural water samples. The relative standard deviations (RSDs) for ten replicate measurements of 2, 10, and 20 μg·L-1 of Se(Ⅳ) change between 0.35% and 5.58%, while the RSDs for ten replicate measurements of 3, 6, and 12 μg·L-1 of Se(Ⅵ) change between 0.49% and 1.61%. Analyses of a certified standard reference material (NIST SRM 1643e) for selenium using the fixed-time method showed that the proposed kinetic method has good accuracy. The Se(Ⅳ), Se(Ⅵ), and total inorganic selenium in lake and river water samples have been successfully determined by this method after selective reduction of Se(Ⅵ) to Se(Ⅳ).展开更多
基金Project 0520002 supported by the Natural Science Foundation of Jiangxi Province
文摘A simple and sensitive kinetic spectrophotometric method for the determination of trace amounts of titanium(IV),based upon the catalytic effect of Ti(IV) on the oxidation of acid chrome blue K (ACBK) by hydrogen peroxide in 0.002 mol/L sulfuric acid,is described. The reaction rate is monitored spectrophotometrically by measuring the decrease in absorbance of ACBK at 524 nm. The detection limit of the method is 1.01×10?9 g/mL,and the linear range is 0-0.048 mg/L. The influence of acidity,concentration of reactants,reaction time,reaction temperature and for-eign ions is also discussed. The optimum reaction conditions were established and some kinetic parameters determined. The apparent activation energy of the catalytic reaction is 5.32 kJ/mol. The relative standard deviation for the determi-nation of titanium(IV) at the concentration of 0.048 mg/L is calculated to be 1.31% (n = 11). In combination with sol-vent extraction separation,the method has been successfully applied to the determination of trace titanium(IV) in human hair,plant matter,tea and rock samples. The results are in good agreement with the certified values with the relative standard deviations (RSD) of 1.4%-3.5%.
基金Supported by the CIIT-Project Funded by COMSATS Institute of Information Technology,Pakistan
文摘A simple and sensitive flow injection(FI) spectrophotometric method was reported for the determination of uric acid based on the reduction of Fe(III)/ferricyanide in the presence of uric acid. The in situ reduced ions reacted with unreduced portion of ferricyanide/Fe(III) to form soluble Prussian blue, which was monitored at an absorption wavelength of 735 nm. The optimized conditions allow a linear calibration graph in a concentration range of 1―100 μmol/L. The relative standard deviation was in a range of 0.5%―2.5%, with a detection limit(3σ blank) of 0.3 μmol/L and a sampling frequency of 60 injection/h was obtained. The effect of common substances present in human physiological fluids on the determination of uric acid was examined. The method was applied to determining uric acid in human urine samples with the recoveries in a range of 96%―105%. The results agree well with those by spectrophotometric reference method at a confidence level of 95%. Spectrophotometric procedures for uric acid determination in clinical samples were reviewed briefly.
文摘A novel sensitive and relatively selective kinetic method is presented for the determination of V(V) based on its catalytic effect on the oxidation reaction of Celestine blue by potassium bromate in the presence of citric acid as an activator. The reaction was monitored spectropho- tometrically by measuring the decrease in absorbance of Celestine blue at a maximum absorption wavelength of 540 nm between 0.5 and 9 min (the fixed-time method) in an H3PO4 medium at 45℃. The effect of various parameters such as concentrations of H3PO4, citric acid, potassium bromate and Celestine blue, ionic strength, reaction temperature and time on the rate of V(V) catalyzed reaction was studied. The method is free from the most interferences, especially from large amounts of V(IV). The decrease in absorbance is proportional to the concentration of V(V) over the entire concentration range tested (0.025-1.25 lag.mL^-1) with a detection limit of 6.80 tag.L^-1 (according to statistical 3Sblank/k criterion) and a coefficient of variation (CV) of 1.78% (for ten replicate measurements at 95% confidence level). The proposed method suffers from a few interferences such as Cr(VI) and Hg(Ⅱ) ions. The method was successfully applied to the determination of V(V) in river water, lake water, tap water, natural drinking water samples and a certified standard reference material such as SRM-1640 with satis- factory results. The vanadium contents of natural water samples were detected by using both linear calibration curve and standard addition curve methods. The recoveries of spiked vanadium (V) into the certified standard water sample were found to be quantitative, and the reproducibility was satisfactory. It was observed that the results of the SRM 1640 were in good agreement with the certified value.
文摘A novel method for the determination of captopril by spectrophotometer is described in this paper. The experiment is based on the fact that Fe(Ⅲ) is reduced to Fe(Ⅱ) by captopril, then the in sire formed Fe(Ⅱ) reacts with potassium ferricyanide to give the soluble prussian blue at pH 4.00, and its maximal adsorption wavelength (λmax) is 735 nm. Good linear relationship is obtained between the absorbance and the concentration of captopril in the wide range of 0.05-20 μg/mL. The linear regression equation is A = -0.04314 + 0.11423C (μg/mL) with a correlation coefficient R = 0.9998. The detection limit (3σ/k) is 0.04 μg/mL, the molar absorption coefficient is 2.5×10^4 L/mol cm. By mensurating the absorbance of soluble prussian blue, the indirect determination of captopril can be obtained. This method has been successfully applied to determination of captopril in pharmaceutical samples. Analytical results obtained are satisfactory.
文摘A simple and sensitive flow injection spectrophotometric method is reported for the determination of vitamin E using potassium ferricyanide-Fe(Ⅲ) detection system.In the presence of vitamin E,Fe(Ⅲ)/ferricyanide reduces.The in situ reduced ions are then reacted with unreduced portion of ferricyanide/Fe(Ⅲ) to make soluble Prussian blue,which is monitored at absorption wavelength of 735 nm.Linear calibration graph was obtained in the concentration range of 0.1-40μg mL^(-1).The relative standard deviations (n=4) were in the range of 1.1-3.6%,with limits of detection(3 s blank) of 0.04μg mL^(-1).The proposed method allowed 12 injections h^(-1).The method is applied to determine vitamin E in pharmaceuticals,infant milk and blood serum samples using hexane extraction with the recoveries in the range of 93±3 to 97.5±4%.The method is validated using certified reference materials SRM 968c for blood serum samples.
文摘A new kinetic spectrophotometric method has been developed for the determination of iron (Ⅲ). The method is based on the catalytic effect of iron (Ⅲ) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The advantages of the proposed method are that it is sensitive, accurate, rapid, inexpensive, can be operated under room temperature and has a large determination concentration range compared to other techniques. The obtained optimum conditions are: pH 3.15, RAWL (200 mgL^-1) 5.00mL, Potassium periodate solution (0.01 molL^-1) 0.30mL, phenanthroline (0.02 molL^-1) 1.00mL, reaction temperature 25℃ and reaction time 7 min. With this method iron could quantitively be determined in the range 0.00-0.02 mgL^-1, the detection limit being 4.10 × 10^10gmL^-1. The relative standard deviations (RSD) in five replicate determinations for 3 μgL^-1and 5 μgL^-1 iron (Ⅲ) are 3.1% and 1.9%, respectively. The method has been applied to the determination of iron (Ⅲ) in tap water samples and seawater samples (from the South China Sea), the recovery rates being 98.0% and 100.5%, respectively.
文摘A simple flow injection spectrophotometric method is reported for the determination of cysteine,N-acetyl cysteine and glutathione based on the reduction of Fe(Ⅲ)/ferricyanide,the in situ reduced ions are reacted with unreduced portion of ferricyanide/Fe(Ⅲ) to form soluble Prussian blue,which is monitored at 735 nm.The calibration graphs are linear in the concentration ranges of(1―100)×10-6 mol/L for cysteine and N-acetyl cysteine,and(1―50)×10-6 mol/L for glutathione.The relative standard deviations of 1.8%,2.5% and 1.9% were found for eleven replicate analyses of 5×10-6 mol/L cysteine,N-acetyl cysteine and glutathione.The limits of detection(3σ blank) at 5×10-7 mol/L for cysteine,and 3×10-7 mol/L for N-acetyl cysteine and glutathione were obtained.The proposed method allowed 60 injections/h.The effects of common substances present in pharmaceuticals and human physiological fluids were examined.The method was applied to determining cysteine in pharmaceutical formulations with the recoveries in a range of 97% to 106% and the results obtained are agreed well with labeled values.
基金Cumhuriyet University Scientific Research Council (with F-225 code) for financial support of the present work
文摘A novel catalytic kinetic method is proposed for the determination of Se(Ⅳ), Se(Ⅵ), and total inorganic selenium in water based on the catalytic effect of Se(Ⅳ) on the reduction of Celestine blue by sodium sulfide at pH 7.0 phosphate buffer. The fixed-time method was adopted for the determination and speciation of inorganic selenium. Under the optimum conditions, the two calibration graphs are linear with a good correlation coefficient in the range 2-20 and 20-200 μg·L-1 of Se(Ⅳ) for the fixed-time method at 30℃. The experimental and theo- retical detection limits of the developed kinetic method were found to be 0.21 and 2.50 μg·L-1 for the fixed-time method (3 min). All of the variables that affect the sensitivity at 645 nm were investigated, and the optimum conditions were established. The interference effect of various cations and anions on the Se(Ⅳ) determination was also studied. The selectivity of the selenium determination was greatly improved with the use of the strongly cation exchange resin such as Amberlite IR120 plus as long as chelating agents of thiourea and thiosulphate. The proposed kinetic method was validated statistically and through recovery studies in natural water samples. The relative standard deviations (RSDs) for ten replicate measurements of 2, 10, and 20 μg·L-1 of Se(Ⅳ) change between 0.35% and 5.58%, while the RSDs for ten replicate measurements of 3, 6, and 12 μg·L-1 of Se(Ⅵ) change between 0.49% and 1.61%. Analyses of a certified standard reference material (NIST SRM 1643e) for selenium using the fixed-time method showed that the proposed kinetic method has good accuracy. The Se(Ⅳ), Se(Ⅵ), and total inorganic selenium in lake and river water samples have been successfully determined by this method after selective reduction of Se(Ⅵ) to Se(Ⅳ).