A Rapid Spectrofluorometric Method for the Determination of Aluminum at Nano-trace Levels in Some Real, Environmental, Biological, Hemodialysis, Food, Pharmaceutical, and Soil Samples Using 2',3,4',5,7-Pentahydroxyflavone.

A very simple and non-extractive spectrofluorometric method for the swift determination of aluminum at nano-trace levels using 2',3,4',5,7-pentahydroxyflavone (morin) has been developed. Morin reacts in a slightly acidic (0.005 - 0.025 M H2SO4) solution with aluminum in 20% ethanol to produce a highly fluorescent complex in aqueous solution, which has excitation and emission wavelengths of λex = 270 and λem = 565 nm, respectively. Linear calibration graphs were obtained for 0.01 - 800 µg L-1 of Al, providing a detection limit of 1 ng L-1. The limit of quantification of the reaction system was 10 ng L-1. The stoichiometric composition of chelate is 3:2 (Al:morin). The developed method was successfully used in the determination of aluminum in several Standard Reference Materials (SRM) as well as in some water, biological, hemodialysis solutions, food, pharmaceutical, soil sample, and complex synthetic mixtures. The results of the proposed method for biological and food analysis were found to be in excellent agreement with those obtained by AAS. The results of the proposed method for hemodialysis solutions were analogous with those obtained using the method described in British Pharmacopoeia within 95% confidence limits.

A highly sensitive and selective spectrofluorimetric method for the determination of cerium at pico-trace levels in some real, environmental, biological, soil, food and bone samples using 2-(α-pyridyl)-thioquinaldinamide.

A very simple, ultra-sensitive and highly selective non-extractive new spectrofluorimetric method is presented for the determination of cerium at pico-trace levels using 2-(α-pyridyl)-thioquinaldinamide (PTQA). PTQA has been proposed as a new analytical reagent for the direct non-extractive spectrofluorimetric determination of cerium(iv). This novel fluorimetric reagent, PTQA becomes oxidized in a slightly acidic (0.0005-0.0015 M H2SO4) solution with cerium(iv) in absolute ethanol to produce a highly fluorescent oxidized product (λ ex = 303 nm; λ em = 370 nm). Constant and maximum fluorescence intensities were observed over a wide range of acidity (0.0005-0.0015 M H2SO4) for the period between 5 min and 24 h. Linear calibration graphs were obtained for 0.001-600 µg L-1 of Ce, having a detection limit of 0.1 ng L-1; the quantification limit of the reaction system was found to be 1 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 cerium in several certified reference materials (alloys, steels, noodles, ores and sediments) as well as in some environmental waters (potable and polluted), biological fluids (human blood, urine and milk), soil samples, food samples (vegetable, rice, corn and wheat), bone samples (human, cow, bull, fish, hen, goat, sheep), solutions containing both cerium(iii) and cerium(iv) and complex. The results of the proposed method for assessing biological, food and vegetables samples were comparable with ICP-OES and were found to be in excellent agreement.

A highly sensitive and selective spectrofluorimetric method for the determination of manganese at nanotrace levels in some real, environmental, biological, soil, food and pharmaceutical samples using 2-(α-pyridyl)-thioquinaldinamide.

A very simple, ultra-sensitive and highly selective non-extractive spectrofluorimetric method is presented for the determination of manganese at nano-trace levels using 2-(α-pyridyl)-thioquinaldinamide (PTQA). PTQA has been proposed as a new analytical reagent for the direct non-extractive spectrofluorimetric determination of manganese(vii). This novel fluorimetric reagent, PTQA becomes oxidized in a slightly acidic (0.0125-0.05 M H2SO4) solution with manganese(vii) in absolute ethanol to produce a highly fluorescent oxidized product (λ ex = 319 nm; λ em = 373 nm). Constant and maximum fluorescence intensities were observed over a wide range of acidity (0.0125-0.05 M H2SO4) for the period between 5 min and 24 h. Linear calibration graphs were obtained for 0.01-800 µg L-1 of Mn, having a detection limit of 1 ng L-1; the quantification limit of the reaction system was found to be 10 ng L-1 and the RSD was 0-2%. A large excess of over 60 cations, anions and complexing agents do not interfere in the determination. The developed method was successfully used in the determination of manganese in several standard reference materials (alloys, steels, hair and sediments) as well as in some environmental waters (potable and polluted), biological samples (human blood, urine and hair), soil samples, food samples (vegetables, fruits, tea, rice, and wheat), fertilizer samples and pharmaceutical samples (multivitamin-mineral tablets and syrup), solutions containing both manganese(ii) and manganese(vii) speciation and complex synthetic mixtures. The results of the proposed method for assessing biological, food and vegetables samples were comparable with AAS and ICP-MS and were found to be in excellent agreement.

A simple and selective spectrophotometric method for the determination of trace gold in real, environmental, biological, geological and soil samples using bis (salicylaldehyde) orthophenylenediamine.

A simple high sensitive, selective, and rapid spectrophotometric method for the determination of trace gold based on the rapid reaction of gold(III) with bis(salicylaldehyde)orthophenylenediamine (BSOPD) in aqueous and micellar media has been developed. BSOPD reacts with gold(III) in slightly acidic solution to form a 1:1 brownish-yellow complex, which has an maximum absorption peak at 490 nm in both aqueous and micellar media. The most remarkable point of this method is that the molar absorptivities of the gold-BSOPD complex form in the presence of the nonionic TritonX-100 surfactant are almost a 10 times higher than the value observed in the aqueous solution, resulting in an increase in the sensitivity and selectivity of the method. The apparent molar absorptivities were found to be 2.3 x 10(4) L mol(-1) cm(-1) and 2.5 x 10(5) L mol(-1) cm(-1) in aqueous and micellar media, respectively. The reaction is instantaneous and the maximum absorbance was obtained after 10 min at 490 nm and remains constant for over 24 h at room temperature. The linear calibration graphs were obtained for 0.1-30 mg L(-1) and 0.01-30 mg L(-1) of gold(III) in aqueous and surfactant media, respectively. The interference from over 50 cations, anions and complexing agents has been studied at 1 mg L(-1) of Au(III); most metal ions can be tolerated in considerable amounts in aqueous micellar solutions. The Sandell's sensitivity, the limit of detection and relative standard deviation (n = 9) were found to be 5 ng cm(-2), 1 ng mL(-1) and 2%, respectively in aqueous micellar solutions. Its sensitivity and selectivity are remarkably higher than that of other reagents in the literature. The proposed method was successfully used in the determination of gold in several standard reference materials (alloys and steels), environmental water samples (potable and polluted), and biological samples (blood and urine), geological, soil and complex synthetic mixtures. The results obtained agree well with those samples analyzed by atomic absorption spectrophotometry (AAS).

A rapid spectrophotometric method for the determination of trace level lead using 1,5-diphenylthiocarbazone in aqueous micellar solutions.

A very simple, ultra-sensitive and fairly selective direct spectrophotmetric method is presented for the rapid determination of lead(II) at ultra-trace level using 1,5-diphenylthiocarbazone (dithizone) in micellar media. The presence of the micellar system avoids the previous steps of solvent extraction and reduces the cost and toxicity while enhancing the sensitivity, selectivity and the molar absorptivity. The molar absorptivities of the lead-dithizone complex formed in the presence of the cationic cetyltrimethylammonium bromide (CTAB) surfactants are almost ten times the value observed in the standard method, resulting in an increase in the sensitivity of the method. The reaction is instantaneous and the absorbance remains stable for over 24 h. The average molar absorption coefficient was found to be 3.99 x 10(5) L mol(-1) cm(-1) and Sandell's sensitivity was 30 ng cm(-2) of Pb. Linear calibration graphs were obtained for 0.06-60 mg L(-1) of Pb(II); the stoichiometric composition of the chelate is 1:2 (Pb:dithizone). The interference from over 50 cations, anions and complexing agents has been studied at 1 mg L(-1) of Pb(II). The method was successfully used in the determination of lead in several standard reference materials (alloys and steels), environmental water samples (potable and polluted), biological samples (human blood and urine), soil samples and solutions containing both lead(II) and lead(IV) and complex synthetic mixtures. The method has high precision and accuracy (sigma = +/-0.01 for 0.5 mg L(-1)).

A simple spectrophotometric method for the determination of cobalt in industrial, environmental, biological and soil samples using bis(salicylaldehyde)orthophenylenediamine.

Bis(salicylaldehyde)orthophenylenediamine (BSOPD) has been proposed as new analytical reagent for the direct non-extractive spectrophotometric determination of cobalt. It reacts with cobalt in slightly acidic (0.0002-0.001 M H(2)SO(4)) 50% 1,4-dioxanic medium to form a red-orange chelate with a molar ratio 1:1. The reaction is instantaneous and the maximum absorbance was obtained at 458 nm and remains constant for over 24h. The average molar absorption coefficient and Sandell's sensitivity were found to be 1.109 x 10(4)l mol(-1)cm(-1) and 20 ng cm(-2) of Co(II), respectively. Linear calibration graph was obtained for 0.1-15 mg l(-1) of Co(II) with a correlation coefficient value of 0.995 for Co-BSOPD complex. Large excess of 44 cations, anions and complexing agents do not interfere in the determination. The method was successfully used in the determination of cobalt(II) from synthetic mixture and certified reference materials for the purpose of validating the method and the results of analyses were found to be excellent agreement with those of actual values. This developed method was also used for determination of cobalt in some environmental waters (potable and polluted), biological (blood and urine) and soil samples and solution containing both cobalt(II) and cobalt(III). The results of the proposed method for biological samples were comparable with AAS and were found to be in good agreement. The method has high precision and accuracy (s=+/-0.01 for 0.5 mg l(-1)).

A simple spectrophotometric determination of trace level mercury using 1,5-diphenylthiocarbazone solubilized in micelle.

A very simple, ultra-sensitive and fairly selective non-extractive spectrophotmetric method is presented for the rapid determination of mercury(II) at ultra-trace level using 1,5-diphenylthiocarbazone (dithizone) as a new micellar spectrophotometric reagent (lambdamax = 490 nm) in a slightly acidic (0.07 - 0.17 M H2SO4) aqueous solution. The presence of a micellar system avoids the previous steps of solvent extraction and reduces the cost, toxicity while enhancing the sensitivity, selectivity and the molar absorptivity. The reaction is instantaneous and the absorbance remains stable for over 24 h. The average molar absorption coefficient and Sandell's sensitivity were found to be 5.02 x 10(4) L mol(-1) cm(-1) and 10 ng cm(-2) of Hg, respectively. Linear calibration graphs were obtained for 0.05 - 10 mg L(-1) of Hg; the stoichiometric composition of the chelate is 1:2 (Hg:dithizone). The method is characterized by a detection limit of 1 microg L(-1) of Hg. Large excesses of over 60 cations, anions and complexing agents (e.g. EDTA, tartrate, oxalate, citrate, phosphate, thiourea, azide, SCN-) do not interfere in the determination. The method was successfully applied to a number of environmental water samples (potable and polluted), biological samples (human blood and urine; milk and fish) and soils; solutions contained both mercury(I) and mercury(II) as well as complex synthetic mixtures. The method has high precision and accuracy (s = +/-0.01 for 0.1 mg L(-1)).

A simple spectrophotometric method for the determination of cadmium in industrial, environmental, biological and soil samples using 5,7-dibromo-8-hydroxyquinoline.

A very simple, ultra-sensitive and highly selective non-extractive spectrophotometric method for the determination of trace amount of cadmium using 5,7-dibromo-8-hydroxyquinoline (DBHQ) has been developed. DBHQ reacts in a slightly acidic solution with cadmium to give a deep greenish-yellow chelate, which has an absorption maximum at 396 nm. The average molar absorption co-efficient and Sandell's sensitivity were found to be 5.3 x 10(3) L mol(-1) cm(-2) and 20 ng cm(-2) of Cd, respectively. Linear calibration graphs were obtained for 0.1-30 microg mL(-1) of Cd. A large excess of over 50 cations, anions and some common complexing agents do not interfere with the determination. The method was successfully used in the determination of cadmium in several Standard Reference Materials as well as in some environmental waters, biological and soil samples.

A simple spectrophotometric method for the determination of copper in industrial, environmental, biological and soil samples using 2,5-dimercapto-1,3,4-thiadiazole.

A simple spectrophotometric method is presented for the rapid determination of copper at a trace level using 2,5-dimercapto-1,3,4-thiadiazole (DMTD) as a new spectrophotometric reagent. The method is based on the reaction of non-absorbent DMTD in a slightly acidic (0.002-0.014 mol dm(-3) sulfuric acid) aqueous solution with copper(II) to produce a highly absorbent greenish-yellow chelate product that has an absorption maximum at 390 nm. The reaction is instantaneous and the absorbance remains stable for 24 h. The average molar absorption coefficient and Sandell's sensitivity were found to be 5.65 x 10(4) dm3 mol(-1) cm(-1) and 10 ng cm(-2) of CuII, respectively. Linear calibration graphs were obtained for 0.1-20 microg cm(-3) of CuII; the stoichiometric composition of the chelate is 1:2 (Cu:DMTD). A large excess of over 50 cations, anions and complexing agents (e.g. tartrate, oxalate, citrate, phosphate, thiourea, SCN-) do not interfere in the determination. The method was successfully used for the determination of copper in several Standard Reference Materials as well as in some environmental water samples, biological samples, soil samples and solutions containing both copper(I) and copper(II) and complex synthetic mixtures. The method has high precision and accuracy (s = +/-0.01 for 0.5 microg cm(-1)).

A rapid spectrophotometric method for the determination of molybdenum in industrial, environmental, biological and soil samples using 5,7-dibromo-8-hydroxyquinoline.

A very simple, ultra-sensitive and highly selective non-extractive spectrophotometric method for the determination of trace amount of molybdenum(VI) using 5,7-dibromo-8-hydroxyquinoline (DBHQ) has been developed. 5,7-Dibromo-8-hydroxyquinoline reacts in a slightly acidic solution (0.05 - 1.0 M H2SO4) with molybdenum(VI) to give a deep greenish-yellow chelate which has an absorption maximum at 401 nm. The reaction is instantaneous and the absorbance remains stable for over 24 h. The average molar absorption coefficient and Sandell's sensitivity were found to be 4.13 x 10(3) L mol(-1) cm(-1) and 7 ng cm(-2) of molybdenum(VI), respectively. Linear calibration graphs were obtained for 0.1 - 50 microg mL(-1) of molybdenum(VI). The stoichiometric composition of the chelate is 1:3 (Mo:DBHQ). A large excess of over 50 cations, anions and some common complexing agents (e.g. EDTA, oxalate, citrate, phosphate, thiourea, SCN-) do not interfere with the determination. The method was successfully used in the determination of molybdenum in several Standard Reference Materials (alloys, steels and waters) as well as in some environmental waters (inland and surface), biological samples (human blood and urine), soil samples, solution containing both molybdenum(V) and molybdenum(VI) and complex synthetic mixtures. The method has high precision and accuracy (S = +/-0.01 for 0.5 microg mL(-1)).