A Rapid,Simple, and Sensitive Spectrophotometric Determination of Traces of Vanadium (V) in Foodstuffs,Alloy Steels,and Pharmaceutical,Water, Soil,and Urine Samples

Abstract

A rapid, simple, sensitive, and selective spectrophotometric method is investigated for the determination of traces of vanadium (V) in foodstuffs, alloy steels, and pharmaceutical, water, soil, and urine samples in aqueous DMF medium. The metal ion forms a green colored complex with 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone (HMBATSC) in an acidic buffer of pH 6.0. The green colored solution, having an absorbance maximum at 380 nm, is stable for more than 72 hours. Beer's law is obeyed in the range of 0.051–2.037 µg ml^?1. The molar absorptivity and Sandell's sensitivity of the method are found as 2.75 × 10⁴ l mol^?1 cm^?1 and 0.0018 µg cm^?2, respectively. The green colored complex has 1:2 [V(V)-HMBATSC] stoichiometry. The stability constant of the complex is determined as 3.267 × 10¹¹ by Job's method. The optimum reaction conditions and other analytical parameters are studied. A sensitive and selective second-order derivative spectrophotometry has also been proposed for the determination of V(V). The interference of various cations and anions are studied. The present method is successfully applied to the determination of vanadium (V) in foodstuffs, alloy steels, and pharmaceutical, water, soil, and urine samples.     

Sensitive Spectrophotometric Determination of Vanadium in Environmental Samples at PPB Levels

Abstract

A new, sensitive and selective method for separation, and extraction - spectrophotometric determination of V (V) with pyrogallol {Ar (OH)₃} and hydroxyamidines (HOA) is described. The molar absorptivities of the colored species with six substituted HOA lie in the range of (0.52–1.5)x 10⁶ L mole^?1 cm^?1 at λ_max 430–440 nm. Of these, the simplest compound, N-hydroxy-N, N- diphenylbenz-amidine (HDPBA) gives the most sensitive color reaction and hence, it is used for detailed studies. No interference of almost all diverse ions tested is noticed. The method offers the determination of vanadium in different environmental samples.     

A New Spectrophotometric Method for the Determination of Maneb in Commercial Formulations

Abstract

A new rapid, selective and sensitive method has been developed for the determination of maneb using pyrocatechol-violet(PV) as chelating reagent in the pH range of 7.5–11.0 in the presence of CTAB producing a complex which shows maximum absorption at 640 nm. Working range of the method is 0.2–3.0 μg ml^?1 maneb (manganese ethylenebisdithiocarbamate). The molar absorptivity of the color system is 79600 1 mol^?1 cm^?1 and Sandell's sensitivity is 0.0033 μg cm^?2. The reproducibility of the method has been checked by the 10 replicate analysis of 15 μg of maneb in 10 ml of solution. The method is quite sensitive and has been applied for the determination of maneb in various commercial samples, crops, grains and synthetic samples.     

6-Phenyl -2,3-Dihydro-asym-trirzine-3-thione as a Selectiue Reagent for the Spectrophotometric Determination of Copper

Abstract

A sensitive and highly selective spectrophotometric method is described for the determination of 12-120 μg of copper using 6-phenyl-2,3-dihydro-asym-triazine-3-thione (PDTT) as a complexing agent. The red 1:4 water soluble complex was measured at 540nm, ε=1.26×10⁴ 1. mol^?1cm^?1.

The method was applled for the determination of copper in standard steels (B.C.S.) and estimation of the solubility product of copper (I) iodide. Comperison was also made with the 2-2 biquinoline method.     

Thiothenoyltrifluoroacetone as the Extracting and Colorimetric Reagent for Bismuth

Abstract

Thiothenoyltrifluoracetone (STTA) was used for the simultaneous extraction and direct spectrophotometric determination of bismuth at microgram concentration. About 98.5 μg of bismuth was extracted as the orange-red colored complex with 10 ml of 0.001 M STTA in carbontetrachloride. The extraction was quantitative at pH 6. The system conformed to Beer's Law in the concentration range of 2.5 to 30 μg/ml of bismuth at 460 nm. The method is both sensitive and selective.

The molar absorptivity was 5.6 × 10³ and sensitivity was 0.037 μg/cm². The method is selective as it is possible to accomplish extraction and colorimetrically determination of bismuth in the presence of 1:50 of several ions. Only ions such as cadmium, tin, iron, titanium and nickel interfere seriously. The overall process of extraction and determination takes hardly 30 minutes. The method is reproducible.     

Extraction and Spectrophotometric Determination of Zirconium(IV)

Abstract

A sensitive and selective method for the extraction and spectrophotometric determination of Zr(IV) with N-p-chlorophenyl-3,4-,5-trimethoxycinnamohydroxamic acid (PTCHA) has been developed. The binary complex of Zr(IV)-PTCHA is extracted from 2–6 M HCl into chloroform, having a maximum absorbance at 385 nm; molar absorptivity 2.1 × 10⁴ 1 mol^?1 cm^?1. A ternary complex with xylenol orange (Zr-PTCHA-XO) have been studied in chloroform-ethanol media, which absorbs at 540 nm; molar absorptivity 4.3 × 10⁴ 1 mol^?1 cm^?1. The present method is applied for the analysis of zirconium in standard samples.     

Diazotized reagent for spectrophotometric determination of glyphosate pesticide in environmental and agricultural samples

A new sensitive spectrophotometric method for the determination of glyphosate herbicide in environmental and agricultural samples is developed. The reaction is based on diazotization followed by coupling of glyphosate with p-dimethyl amino benzaldehyde. The resulted complex absorption spectra was observed at λ_max = 420 nm. The effects of other metal ions and pesticides were also tested for selective determination of glyphosate. The analytical parameters were optimized and have been successfully applied for determination of glyphosate in various environmental samples such as soil, water and vegetables. This method has a lower limit detection of 6 μg of glyphosate. Beer's law is obeyed over the concentration range of 6.0 μg–24.0 μg glyphosate in 25 mL of the final solution at 420 nm. The standard deviation and relative standard deviation calculated are 0.0055 and 1.023, respectively. The molar absorptivity of the colored system is 1.91 × 10¹⁰ L mol^?1cm^?1 and Sandell's sensitivity is found 0.408 × 10^?5 μg cm^?2. The proposed method is simple, sensitive, highly reproducible and time saving as compare to those complicated time consuming methods.     

Chemiluminescence Determination of Sulfite and Sulfur Dioxide Using Tris(1,10-Phenanthroline)Ruthenium-KMnO4 System

Abstract

The emission produced by sulfite after oxidation by potassium permanganate in acidic solution in the presence of Ru(phen)₃ ²⁺ is used to determine 1.0 × 10^?7 to 2.5 × 10^?5 mol/L sulfite. The limit of detection is 4.5 × 10^?9 mol/L and the relative standard deviation is 3.1% for a 1 × 10^?5 mol/L sulfite solution (n=8). The method was also applied satisfactorily to the determination of sulfur dioxide in air by using triethanolamine (TEA) as absorbent material.     

Extraction-Spectrophotometric or -Atomic Absorption Spectrophotometric Determination of Titanium Using Caffeic Acid and a Liquid Ion Exchanger

Abstract

A selective and sensitive method for the extraction followed by a spectrophotometric or atomic absorption spectrophotometric determination of titanium(IV) in trace amounts is described. The molar absorptivity of the caffeic acid-Aliquat 336 complex is 5.7 × 10⁴ l mol^?1 cm^?1 at 380 nm; the yellow coloured complex obeys Beer's law in the range 0.05–1.2 mg/l of titanium in the final extract. The method is applied to the preconcentration, separation and determination of titanium(IV) in steel, industrial effluents and environmental samples.     

Extraction,Spectrophotometric and Atomic Absorption Spectrophotometric Determination of Molybdenum with Caffeic Acid and Application in High Purity Grade Steel and Environmental Samples

Abstract

A new selective and sensitive method for extraction of yellow Mo (VI)-caffeic acid complex with a liquid ion exchanger, Aliquat 336 from 4.0 pH, and spectrophotometric determination of molybdenum in trace amounts is described. the molar absorptivity of the complex is 1.1 × 10⁵ 1 mol^?1 cm^?1 at 340 nm and the colour system obeys Beer's law in the range 0.04–0.99 ppm of Mo(VI). the molybdenum is also determined with AAS and the method is applied for its determination in steel and environmental samples.     

Synthesis of New Reagent 2,6‐Diacetylpyridine Bis‐4‐Phenyl‐3‐Thiosemicarbazone (2,6‐DAPBPTSC): Selective,Sensitive and Extractive Spectrophotometric Determination of Co(II) in Vegetable,Soil, Pharmaceutical and Alloy Samples

New synthesized reagent 2,6‐diacetylpyridine bis‐4‐phenyl‐3‐thiosemicarbazone (2,6‐DAPBPTSC) is proposed as a sensitive and selective analytical reagent for the extractive spectrophotometric determination of cobalt(II). Cobalt(II) forms a reddish brown colored complex with 2,6‐DAPBPTSC, which is extracted into isoamylalcohol, under optimum conditions. The maximum absorption of the isoamylalcohol extract is measured at 400 nm. Beer's law is applied in the range 0.6‐6.0 ppm of cobalt(II). The molar absorptivity and Sandell's sensitivity of the complex is calculated as 2.2 × 10⁴ L mol^?1 cm^?1 and 2.68 × 10^?3 μg cm^?2, respectively. An adequate linearity with a correlation coefficient value of 0.969 is obtained for the Co(II)‐2,6‐DAPBPTSC complex. The instability constant of the complex, calculated from Asmus' method is 3.75 × 10^?4 The precision and accuracy of the method is checked with calculation of relative standard deviation (n = 5), 0.388 and the detection limit a value is 0.0028 μg mL^?1. The method is successfully employed for the determination of cobalt(II) in real samples, such as vegetables, soil, water samples, standard alloy samples, and the performance of the present method was evaluated in terms of Student ‘t’ test and Variance ‘f’ test, which indicates the significance of the present method is an inter comparison of the experimental values, using atomic absorption spectrometer (AAS).     

A new voltammetric sensor for the determination of sulfite in water and wastewater using modified-multiwall carbon nanotubes paste electrode

The electrochemical response of a modified-carbon nanotubes paste electrode with p-aminophenol was investigated as an electrochemical sensor for sulfite determination. The electrochemical behaviour of sulfite was studied at the surface of the modified electrode in aqueous media using cyclic voltammetry and square wave voltammetry. It has been found that under the optimum condition (pH 7.0) in cyclic voltammetry, the oxidation of sulfite occurs at a potential about 680?mV less positive than that of an unmodified-carbon nanotubes paste electrode. Under the optimized conditions, the electrocatalytic peak current showed linear relationship with sulfite concentration in the range of 2.0?×?10^?7–2.8?×?10^?4?mol?L^?1 with a detection limit of 9.0?×?10^?8?mol?L^?1 sulfite. The relative standard deviations for ten successive assays of 1.0 and 50.0?µmol?L^?1 sulfite were 2.5% and 2.1%, respectively. Finally, the modified electrode was examined as a selective, simple and precise new electrochemical sensor for the determination of sulfite in water and wastewater samples.     

Photochemical Fluorescence Enhancement of Terbuium-Fleroxacin System and Determination of Fleroxacin

ABSTRACT

The sensitized fluorescence of the terbium ion (Tb³⁺) can be observed when excited in the presence of fleroxacin (FLRX) in the aqueous solution because a Tb³⁺ -FLRX complex was formed. The sensitised fluorescence was greatly enhanced after the complex system was irradiated by 365nm ultraviolet light. The irradiation makes the complex system undergo photochemical reactions and a new terbium complex which is more favourable to the intramolecular energy transfer is formed. On this basis a new sensitive and selective photochemical fluorimetric method for the determination of FLRX was developed. Under the optimum experimental conditions, the linear range of the determination is 1.0—200×10^?7 mol 1^?1 for FLRX, and the detection limit is 1.2×10^?8mol 1^?1. Without any pre-treatment the recoveries of FLRX in human urine samples were determined with satisfaction.     

Spectrophotometric Determination of Sulphathiazole

Abstract

A new, rapid, simple, selective and sensitive method for the spectrophotometric determination of sulphathiazole is described. The drug forms a yellow coloured complex with Pd(II) in alkaline medium (1 M NaOH). The drug complex exhibits maximum absorbance at 410 nm, with a molar absorptivity of 1.9 × 10³ 1 mol^?1 cm^?1. Effects of molarity of NaOH, reagent concentration on the proper complex formation are discussed. The system obeys Beer's law in the concentration range of 10-160 ppm of sulphathiazole.     

Extractive Separation and Spectrophotometric Determination of Traces of Ruthenium from Mixtures Containing Excess Platinum Group Metals

Abstract

A highly selective, sensitive, and rapid method has been developed for the spectrophotometric determination of ruthenium with 5-chloro-2-hydroxythiobenzhydrazide after extraction into molten naphthalene. Ruthenium was determined in the range 1.2–4.5 ppm. The complex was stable for more than 12 h with molar absorptivity of 1.516 × 10⁴ L mol^?1 cm^?1 and detection limit of 0.0066 ppm. The method was found to be selective for ruthenium in the presence of a large number of diverse ions. Ruthenium was determined in various synthetic mixtures. The method permits the sequential separation and determination of ruthenium, osmium, and platinum from their mixtures.     

Selective solid phase extraction and preconcentration of ultra-trace inorganic mercury in water samples using 2,6-dimethyl-morpholine dithiocarbamate

A sensitive and selective solid-phase spectrophotometric method for the determination of trace amounts of Hg(II) cation in water is described. A complex was created with Hg(II) using 2,6-dimethyl-morpholine dithiocarbamate (DMMDTC) to form Hg(II)–(DMMDTC) and this complex was adsorbed onto microcrystalline naphthalene (MN) and then eluted with 5% acetic acid (in ethanol) solution. A preconcentration factor of 187 and a recovery of 95% were observed at pH of 5.0 and for 10 min. of extraction. The separated Hg(II) ions were quantified by using ultraviolet-visible spectrophotometer at 490.0 nm by creating a colored complex with dithizone in Triton X-100 surfactant media. Molar absorptivity and sandell’s sensitivity for the Hg(II)-dithizone were determined as 4.96 × 10⁵ Lmol^?1cm^?1 and 0.4032 µg cm^?2, respectively. The detection limit (LOD) was 1.7 μg L^?1 under the optimized conditions of the analytical method.     

Direct and Derivative Spectrophotometric Determination of Zinc with 2,4-Dihydroxybenzaldehyde Isonicotinoyl Hydrazone in Potable Water and Pharmaceutical Samples

A simple and sensitive spectrophotometric method is developed for the determination of zinc in aqueous solutions. The metal ion forms a greenish-yellow colored complex with 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone (2,4-DHBINH) in the pH range of 4–10. The complex shows maximum absorbance at 390 nm and in the pH range of 6–8. Beer's law is obeyed in the range 0.10–1.50 μg/mL of Zn(II). The molar absorptivity and Sandell's sensitivity are 3.55 × 10⁴ mol⁻¹ cm⁻¹ and 0.0016 μg/cm², respectively. The composition of the complex is 1 : 1. The effect of interfering ions has been studied, and the method was applied to the determination of zinc(II) in potable water and pharmaceutical samples. A fast derivative spectrophotometry method is also proposed for the determination of zinc in the range 0.06–1.60 μg/mL, which is more sensitive than the zero order method. __________ Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 9, 2005, pp. 933–937. Original Russian Text Copyright ? 2005 by Sivaramaiah, Raveendra Reddy. The text was submitted by the authors in English.     

Electrocatalytic oxidation of sulfite by acetylferrocene at glassy carbon electrode

The electrochemical oxidation of sulfite catalyzed by acetylferrocene (AFc) at a glassy carbon electrode (GCE) in 0.2 M NaClO₄ aqueous solution has been studied by cyclic voltammetry. Although sulfite itself showed a sluggish electrochemical response at the GCE, the response could be enhanced greatly by using AFc as a mediator, which enables a sensitive determination of the substrate (sulfite). The reaction rate constant for catalytic oxidation was evaluated as (7.02 ± 0.05) × 10⁴ M ^?1 s^?1 by chronoamperometry. Experimental conditions that maximize the current efficiency of the electrocatalytic oxidation, such as the pH and both the catalyst (AFc) and substrate (sulfite) concentrations, were also investigated. The electrochemical kinetics of electrocatalytic oxidation of sulfite by AFc has been studied by cyclic voltammetry. In the presence of 5 × 10^?4 M AFc, the oxidation current is proportional to the sulfite concentration and the calibration plot was linear over the concentration range 2 × 10^?4–2.4 × 10^?3 M . This result can be applied in the determination of real samples. Copyright © 2005 John Wiley & Sons, Ltd.     

Spectrophotometric Determination of Iron In Wines,Vegetables, Pharmaceutical Compounds and Minerals With Mandelohydroxamic Acid (Mha)

Abstract

A new reagent, mandelohydroxamic acid (MHA), which has an easy synthesis and an high water solubility (64.48 gL^?1) is proposed for a simple, rapid, selective and sensitive method for the spectrophotometric determination of iron based upon the formation of the MHA-Fe(III) complex and its extraction into n-butanol under optimum operating conditions. A yellow color is formed when the complex is extracted from acidic aqueous medium (Vw/Vo[dbnd]5) in the organic solvent (apparent molar absortivity 1.15 10⁴ L mol^?1 cm^?1 at a wavenlength of 430 nm). the relative error is 0.5% (2 ppm of iron) and the detection limit is 0.05 g mL^?1 of Fe(III). the method has been applied to the determination of iron in wines, vegetables, pharmaceutical compounds and minerals.     

Determination of Vanadium with Chlorosubstituted Hydroxamic Acids for Photometric and Atomic Absorption Spectrophotometric Determination

Abstract

The eight newly synthesized chlorosubstituted hydroxamic acids are described for the extraction and spectrophotometric determination of vanadium. The sensitive and selective reagent, N-m-Chlorophenylpalmito hydroxamic acid, (m-CPPHA), which gives violet coloured vanadium complex was extracted with chloroform from 6M HCl. The violet coloured complex thus obtained has a maximum absorbance at 520 nm and molar absorptivity 4.9 ± 10³1mol^?1cm^?1. The Beer's law obeyed in the region 0.50-12.0ppm. Effects of acidity, reagent concentration, diverse ions have also been investigated. A comparison has been made with atomic absorption spectrophotometric method. Vanadium has been determined in the environment, e.g. plant, soil, rock, etc.