A new method for the determination of cobalt was developed by dispersive liquid-liquid microextraction preconcentra-tion and flame atomic absorption spectrometry. In the proposed approach, 1,5-bis(di-2-pyridyl) methyl...A new method for the determination of cobalt was developed by dispersive liquid-liquid microextraction preconcentra-tion and flame atomic absorption spectrometry. In the proposed approach, 1,5-bis(di-2-pyridyl) methylene thiocarbohydrazide (DPTH) was used as a chelating agent, and chloroform and ethanol were selected as extraction and dispersive solvents. Some factors influencing the extraction efficiency of cobalt and its subsequent determination, including extraction and dispersive solvent type and volume, pH of sample solution, concentration of the chelating agent, and extraction time, were studied and optimized. Under the optimum conditions, a preconcentration factor of 8 was reached. The detection limit for cobalt was 12.4 ng?mL–1, and the relative standard deviation (RSD) was 3.42% (n = 7, c = 100 ng?mL–1). The method was successfully applied to the determination of cobalt in food, environmental and water samples.展开更多
A very simple, ultra-sensitive, highly selective and non-extractive new spectrofluorimetric method for the determination of arsenic at pico-trace levels using 2-(α-pyridyl)-thioquinaldinamide (PTQA) has been develope...A very simple, ultra-sensitive, highly selective and non-extractive new spectrofluorimetric method for the determination of arsenic at pico-trace levels using 2-(α-pyridyl)-thioquinaldinamide (PTQA) has been developed. PTQA has been proposed as a new analytical reagent for the direct non-extractive spectrofluorimetric determination of Arsenic (V). This novel fluorimetric reagent, PTQA becomes oxidized in a slightly acidic (0.025 - 0.1 M H2SO4) solution with Arsenic (V) in absolute ethanol to produce highly fluorescent oxidized product (λex = 303 nm;λem = 365 nm). Constant and maximum fluorescence intensities were observed over a wide range of acidity (0.025 - 0.1 M H2SO4) for the period between 2 min and 24 h. Linear calibration graphs were obtained for 0.001 - 800-μgL-1 of As, having a detection limit of 0.1-ngL-1;the quantification limit of the reaction system was found to be 1-ngL-1 and the RSD was 0% - 2%. A large excess of over 60 cations, anions and complexion agents (like, chloride, phosphate, azide, tartrate, oxalate, SCN, etc.) do not interfere in the determination. The developed method was successfully used in the determination of arsenic in several Certified Reference Materials (alloys, steels, ores, human urine, hair, nails, bovine liver and sediments) as well as in some biological fluids (human blood, urine, hair, nail and milk), soil samples, food samples (vegetables, fruits, rice, corn and wheat), solutions containing both arsenic (III) and arsenic (V) speciation and complex synthetic mixtures. The results of the proposed method for assessing biological, food and soil samples were comparable with both ICP-OES & AHG-AAS and were found to be in excellent agreement.展开更多
A new spectrofluorimetric reagent 2-(α-pyridyl)-thioquinaldinamide (PTQA) has been synthesized and characterized through novel reaction techniques. A very simple, ultra-sensitive and highly selective non-extractive n...A new spectrofluorimetric reagent 2-(α-pyridyl)-thioquinaldinamide (PTQA) has been synthesized and characterized through novel reaction techniques. A very simple, ultra-sensitive and highly selective non-extractive new spectrofluorimetric method for the determination of vanadium at Pico-trace levels using 2-(α-pyridyl)-thioquinaldinamide (PTQA) has been developed. PTQA has been proposed as a new analytical reagent for the direct non-extractive spectrofluorimetric determination of vanadium (V). This novel fluorimetric reagent, PTQA becomes oxidized in a slightly acidic (0.0035 - 0.0085 M H2SO4) solution within vanadium (V) in 20% ethanol to produce highly fluorescent oxidized product (λex = 319 nm;λem = 371 nm). Constant and maximum fluorescence intensities were observed over a wide range of acidity (0.0035 - 0.0085 M H2SO4) for the period between 5 min and 24 h. Linear calibration graphs were obtained for 0.001 - 600-μg·L-1 of V, having a detection limit of 0.3-ng·L-1;the quantification limit of the reaction system was found to be 3-ng·L-1 and the RSD was 0% - 2%. A large excess of over 60 cations, anions and complexing agents (like, chloride, phosphate, azide, tartrate, oxalate, SCN- etc.) do not interfere in the determination. The developed method was successfully used in the determination of vanadium in several Certified Reference Materials (alloys, steels, serum, bovine liver, drinking water, soil and sediments) as well as in some environmental waters (potable and polluted), biological fluids (human blood, urine, hair and milk), soil samples and food samples (vegetables, rice and wheat) solutions containing both vanadium (IV) and vanadium (V) speciation and complex synthetic mixtures. The results of the proposed method for assessing biological, food and vegetable samples were comparable with inductively coupled plasma optical emission spectroscopy (ICP-OES) and atomic-absorption spectrophotometer (AAS) was found to be in excellent agreement.展开更多
文摘A new method for the determination of cobalt was developed by dispersive liquid-liquid microextraction preconcentra-tion and flame atomic absorption spectrometry. In the proposed approach, 1,5-bis(di-2-pyridyl) methylene thiocarbohydrazide (DPTH) was used as a chelating agent, and chloroform and ethanol were selected as extraction and dispersive solvents. Some factors influencing the extraction efficiency of cobalt and its subsequent determination, including extraction and dispersive solvent type and volume, pH of sample solution, concentration of the chelating agent, and extraction time, were studied and optimized. Under the optimum conditions, a preconcentration factor of 8 was reached. The detection limit for cobalt was 12.4 ng?mL–1, and the relative standard deviation (RSD) was 3.42% (n = 7, c = 100 ng?mL–1). The method was successfully applied to the determination of cobalt in food, environmental and water samples.
文摘A very simple, ultra-sensitive, highly selective and non-extractive new spectrofluorimetric method for the determination of arsenic at pico-trace levels using 2-(α-pyridyl)-thioquinaldinamide (PTQA) has been developed. PTQA has been proposed as a new analytical reagent for the direct non-extractive spectrofluorimetric determination of Arsenic (V). This novel fluorimetric reagent, PTQA becomes oxidized in a slightly acidic (0.025 - 0.1 M H2SO4) solution with Arsenic (V) in absolute ethanol to produce highly fluorescent oxidized product (λex = 303 nm;λem = 365 nm). Constant and maximum fluorescence intensities were observed over a wide range of acidity (0.025 - 0.1 M H2SO4) for the period between 2 min and 24 h. Linear calibration graphs were obtained for 0.001 - 800-μgL-1 of As, having a detection limit of 0.1-ngL-1;the quantification limit of the reaction system was found to be 1-ngL-1 and the RSD was 0% - 2%. A large excess of over 60 cations, anions and complexion agents (like, chloride, phosphate, azide, tartrate, oxalate, SCN, etc.) do not interfere in the determination. The developed method was successfully used in the determination of arsenic in several Certified Reference Materials (alloys, steels, ores, human urine, hair, nails, bovine liver and sediments) as well as in some biological fluids (human blood, urine, hair, nail and milk), soil samples, food samples (vegetables, fruits, rice, corn and wheat), solutions containing both arsenic (III) and arsenic (V) speciation and complex synthetic mixtures. The results of the proposed method for assessing biological, food and soil samples were comparable with both ICP-OES & AHG-AAS and were found to be in excellent agreement.
文摘A new spectrofluorimetric reagent 2-(α-pyridyl)-thioquinaldinamide (PTQA) has been synthesized and characterized through novel reaction techniques. A very simple, ultra-sensitive and highly selective non-extractive new spectrofluorimetric method for the determination of vanadium at Pico-trace levels using 2-(α-pyridyl)-thioquinaldinamide (PTQA) has been developed. PTQA has been proposed as a new analytical reagent for the direct non-extractive spectrofluorimetric determination of vanadium (V). This novel fluorimetric reagent, PTQA becomes oxidized in a slightly acidic (0.0035 - 0.0085 M H2SO4) solution within vanadium (V) in 20% ethanol to produce highly fluorescent oxidized product (λex = 319 nm;λem = 371 nm). Constant and maximum fluorescence intensities were observed over a wide range of acidity (0.0035 - 0.0085 M H2SO4) for the period between 5 min and 24 h. Linear calibration graphs were obtained for 0.001 - 600-μg·L-1 of V, having a detection limit of 0.3-ng·L-1;the quantification limit of the reaction system was found to be 3-ng·L-1 and the RSD was 0% - 2%. A large excess of over 60 cations, anions and complexing agents (like, chloride, phosphate, azide, tartrate, oxalate, SCN- etc.) do not interfere in the determination. The developed method was successfully used in the determination of vanadium in several Certified Reference Materials (alloys, steels, serum, bovine liver, drinking water, soil and sediments) as well as in some environmental waters (potable and polluted), biological fluids (human blood, urine, hair and milk), soil samples and food samples (vegetables, rice and wheat) solutions containing both vanadium (IV) and vanadium (V) speciation and complex synthetic mixtures. The results of the proposed method for assessing biological, food and vegetable samples were comparable with inductively coupled plasma optical emission spectroscopy (ICP-OES) and atomic-absorption spectrophotometer (AAS) was found to be in excellent agreement.
