A sensitive and selective kinetic spectrophotometric method for the determination of V（V） was developed based on the catalytic oxidation of thionine by KBIO3 in 0.6 mol·L^-1 HaPO4 medium. The linear calibration...A sensitive and selective kinetic spectrophotometric method for the determination of V（V） was developed based on the catalytic oxidation of thionine by KBIO3 in 0.6 mol·L^-1 HaPO4 medium. The linear calibration range and detection limit at 25℃ were 0-0.5 μg·mL^-1 and 0.01 μg·mL^-1, respectively. In the presence of NaF and urea, most of the common ions did not interfere with the determination of V（V）. The proposed method was applied for the determination of vanadium in steels and satisfactory results were obtained.展开更多
A catalytic spectrophotometry for the determination of trace amount of vanadium was developed based on its catalytic effect on the oxidation of arsenazo by potassium bichromate in weak acidic medium. The optimized co...A catalytic spectrophotometry for the determination of trace amount of vanadium was developed based on its catalytic effect on the oxidation of arsenazo by potassium bichromate in weak acidic medium. The optimized conditions for determinations are: cK2Cr2O7=3.010-5 molL-1, carsenazo =3.010-5 molL-1, pH=4.0, t=90. The calibration graph is linear for 0.020.2 gml-1, and the detection limit is 0.02 gml-1 V. The apparent active energy of this catalytic reaction is 21.72 kJmol-1. Most foreign ions do not interfere with the determination of vadadium, except for Fe() and Co(), and their interferences could be eliminated by ion exchange. The present method has been used to make the determination of vanadium in human hair, tea, potato and wastewater, and the results were satisfactory.展开更多
A novel kinetic procedure for the determination of trace iron(Ⅲ) was proposed based on the aerial oxidation of Gallocyanine by oxygen dissolved in water at pH 7 0. The calibration graph is linear for 0 05—0.6 μg...A novel kinetic procedure for the determination of trace iron(Ⅲ) was proposed based on the aerial oxidation of Gallocyanine by oxygen dissolved in water at pH 7 0. The calibration graph is linear for 0 05—0.6 μg/ml, and the detection limit is 0 01μg/ml (Fe). The present procedure is selective for iron(Ⅲ) and very easy to control compared with kinetic procedures for iron. It had been used to the determination of trace iron in environmental samples, and the results were satisfactory.展开更多
A kinetic procedure for determination of trace silver was established based on the catalytic effect of Ag(Ⅰ) on the ligand substitution reaction between hexacyanoferrate (Ⅱ) and urea in acidic medium under the optim...A kinetic procedure for determination of trace silver was established based on the catalytic effect of Ag(Ⅰ) on the ligand substitution reaction between hexacyanoferrate (Ⅱ) and urea in acidic medium under the optimized conditions of [hexacyanoferrate]=8.0×10 -4 mol·L -1 , [CO(NH 2) 2]=6.0×10 -4 mol·L -1 , [CH 3COOH]=0.12 mol·L -1 , 80℃, 720 nm. The calibration curve is linear for 10～100 ng·ml -1 , and the detection limit is 0.4 ng·ml -1 Ag. The active energy of catalytic reaction is 18.12 kJ·mol -1 . The selectivity of this procedure is much better than that of other kinetic methods. Equal amount of mercury does not interfere with the determination of silver, and its sensitivity was also improved.展开更多
A novel kinetic procedure for determination of trace copper was proposed based on the catalytic effect of Cu 2+ on the aerial oxidation of gallocyanine (GC), by which GC was oxidized and a colourless product was ...A novel kinetic procedure for determination of trace copper was proposed based on the catalytic effect of Cu 2+ on the aerial oxidation of gallocyanine (GC), by which GC was oxidized and a colourless product was produced. The reaction was monitored spectrophotometrically in hexamethylene tetramine hydrochloric acid buffer solution. The calibration graph is linear for 0.05～0.5 μg/ml, and the detection limit is 0 02 μg/ml (Cu 2+ ). The selectivity for copper is satisfied as the interferences of Fe 3+ and Al 3+ could be easily and effectively eliminated by the addition of NH 4HF 2. The method was applied to the determination of copper in soil, tap water and simulated water samples, and the results were satisfactory.展开更多
Spectrophotometric study was carried out, for the first time, to investigate the reaction between the vasodilator pentoxifylline hydrochloride (POX) and 1,2-naphthoquinone-4-sulphonate (NQS) reagent. The reaction occu...Spectrophotometric study was carried out, for the first time, to investigate the reaction between the vasodilator pentoxifylline hydrochloride (POX) and 1,2-naphthoquinone-4-sulphonate (NQS) reagent. The reaction occurs in alkaline medium to activate the nucleophilic substitution reaction producing an orange-colored product measured spectrophometrically at λ<sub>max</sub> 472 nm. The variables affecting the reaction were carefully studied and the conditions were optimized. The kinetics of the reaction was investigated and its activation energy was found to be 0.262 cal/mol. Owing to its low activation energy, the reaction proceeded easily and was successfully used for simple and rapid assay of POX. The stoichiometry of the reaction was determined (1:1), and the reaction mechanism was suggested. To develop a high-throughput methodology used in quality control laboratory, a comparative study of the reaction using the conventional spectrophotometric versus microwell assay was applied. Under the optimum reaction conditions, the initial rate and fixed time methods were utilized for constructing the calibration graphs for determination of POX concentrations. The linear range was 10 - 120 μg/ml with good correlation coefficients (0.9987 - 0.9998). The LOD was 2.5 and 3.4 μg/ml for initial rate and fixed time methods, respectively. The intra- and inter-day accuracy and precision of the developed methods were satisfactory, where RSD was ≤3.94%. The present methods have been successfully applied to the determination of POX in its pharmaceutical tablets, and the percentage recovery values were 97.9% - 101.9%. Therefore, we strongly recommend the proposed methods for determination of POX in quality control laboratories.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
A new procedure for the determination of cerium was established using the catalytic effect of Ce(IV) on the oxidation of tribromoarsenazo(TB-ASA) by potassium bromate.In 0.080 mol/L sulfuric acid medium,the maximum ab...A new procedure for the determination of cerium was established using the catalytic effect of Ce(IV) on the oxidation of tribromoarsenazo(TB-ASA) by potassium bromate.In 0.080 mol/L sulfuric acid medium,the maximum absorption peak of Ce(IV)-(TB-ASA)-KBrO3 system is at 510 nm.The amount of Ce(IV) and the difference of absorbance(△A) showed a good linear relationship over the range of 5.7×10-8-5.1×10-7 mol/L.The regression equation is △A=2.3×10-11 C(C:mol/L)+0.0196,with a regression coefficient of 0.9914 at t...展开更多
文摘A sensitive and selective kinetic spectrophotometric method for the determination of V（V） was developed based on the catalytic oxidation of thionine by KBIO3 in 0.6 mol·L^-1 HaPO4 medium. The linear calibration range and detection limit at 25℃ were 0-0.5 μg·mL^-1 and 0.01 μg·mL^-1, respectively. In the presence of NaF and urea, most of the common ions did not interfere with the determination of V（V）. The proposed method was applied for the determination of vanadium in steels and satisfactory results were obtained.
文摘A catalytic spectrophotometry for the determination of trace amount of vanadium was developed based on its catalytic effect on the oxidation of arsenazo by potassium bichromate in weak acidic medium. The optimized conditions for determinations are: cK2Cr2O7=3.010-5 molL-1, carsenazo =3.010-5 molL-1, pH=4.0, t=90. The calibration graph is linear for 0.020.2 gml-1, and the detection limit is 0.02 gml-1 V. The apparent active energy of this catalytic reaction is 21.72 kJmol-1. Most foreign ions do not interfere with the determination of vadadium, except for Fe() and Co(), and their interferences could be eliminated by ion exchange. The present method has been used to make the determination of vanadium in human hair, tea, potato and wastewater, and the results were satisfactory.
文摘A novel kinetic procedure for the determination of trace iron(Ⅲ) was proposed based on the aerial oxidation of Gallocyanine by oxygen dissolved in water at pH 7 0. The calibration graph is linear for 0 05—0.6 μg/ml, and the detection limit is 0 01μg/ml (Fe). The present procedure is selective for iron(Ⅲ) and very easy to control compared with kinetic procedures for iron. It had been used to the determination of trace iron in environmental samples, and the results were satisfactory.
文摘A kinetic procedure for determination of trace silver was established based on the catalytic effect of Ag(Ⅰ) on the ligand substitution reaction between hexacyanoferrate (Ⅱ) and urea in acidic medium under the optimized conditions of [hexacyanoferrate]=8.0×10 -4 mol·L -1 , [CO(NH 2) 2]=6.0×10 -4 mol·L -1 , [CH 3COOH]=0.12 mol·L -1 , 80℃, 720 nm. The calibration curve is linear for 10～100 ng·ml -1 , and the detection limit is 0.4 ng·ml -1 Ag. The active energy of catalytic reaction is 18.12 kJ·mol -1 . The selectivity of this procedure is much better than that of other kinetic methods. Equal amount of mercury does not interfere with the determination of silver, and its sensitivity was also improved.
文摘A novel kinetic procedure for determination of trace copper was proposed based on the catalytic effect of Cu 2+ on the aerial oxidation of gallocyanine (GC), by which GC was oxidized and a colourless product was produced. The reaction was monitored spectrophotometrically in hexamethylene tetramine hydrochloric acid buffer solution. The calibration graph is linear for 0.05～0.5 μg/ml, and the detection limit is 0 02 μg/ml (Cu 2+ ). The selectivity for copper is satisfied as the interferences of Fe 3+ and Al 3+ could be easily and effectively eliminated by the addition of NH 4HF 2. The method was applied to the determination of copper in soil, tap water and simulated water samples, and the results were satisfactory.
文摘Spectrophotometric study was carried out, for the first time, to investigate the reaction between the vasodilator pentoxifylline hydrochloride (POX) and 1,2-naphthoquinone-4-sulphonate (NQS) reagent. The reaction occurs in alkaline medium to activate the nucleophilic substitution reaction producing an orange-colored product measured spectrophometrically at λ<sub>max</sub> 472 nm. The variables affecting the reaction were carefully studied and the conditions were optimized. The kinetics of the reaction was investigated and its activation energy was found to be 0.262 cal/mol. Owing to its low activation energy, the reaction proceeded easily and was successfully used for simple and rapid assay of POX. The stoichiometry of the reaction was determined (1:1), and the reaction mechanism was suggested. To develop a high-throughput methodology used in quality control laboratory, a comparative study of the reaction using the conventional spectrophotometric versus microwell assay was applied. Under the optimum reaction conditions, the initial rate and fixed time methods were utilized for constructing the calibration graphs for determination of POX concentrations. The linear range was 10 - 120 μg/ml with good correlation coefficients (0.9987 - 0.9998). The LOD was 2.5 and 3.4 μg/ml for initial rate and fixed time methods, respectively. The intra- and inter-day accuracy and precision of the developed methods were satisfactory, where RSD was ≤3.94%. The present methods have been successfully applied to the determination of POX in its pharmaceutical tablets, and the percentage recovery values were 97.9% - 101.9%. Therefore, we strongly recommend the proposed methods for determination of POX in quality control laboratories.
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）.
文摘A new procedure for the determination of cerium was established using the catalytic effect of Ce(IV) on the oxidation of tribromoarsenazo(TB-ASA) by potassium bromate.In 0.080 mol/L sulfuric acid medium,the maximum absorption peak of Ce(IV)-(TB-ASA)-KBrO3 system is at 510 nm.The amount of Ce(IV) and the difference of absorbance(△A) showed a good linear relationship over the range of 5.7×10-8-5.1×10-7 mol/L.The regression equation is △A=2.3×10-11 C(C:mol/L)+0.0196,with a regression coefficient of 0.9914 at t...
