V. Krishna Reddy

Rapid, selective, direct and derivative spectrophotometric determination of titanium with 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone.

A simple and sensitive spectrophotometric method is developed for the determination of titanium in aqueous medium. The metal ion forms a reddish brown coloured complex with 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone (2,4-DHBINH) in the pH range 1-7. The complex shows two absorption maxima, one at 430 nm and the other at 500 nm. The reagent shows appreciable absorbance of 430 nm and negligible absorbance at 500 nm at pH 1.5. Beers law is obeyed in the range 0.09 to 2.15 mug ml(-1) of titanium(IV). The molar absorptivity and the Sandells sensitivity of the method are 1.35 x 10(4) 1 mol(-1) cm(-1) and 0.0049 mug cm(-2), respectively. A method for the determination of titanium by first-order derivative spectrophotometry is also proposed. The methods have been employed successfully for the determination of titanium in several alloy and steel samples.

Direct and Derivative Spectrophotometric Determination of Copper(II) with 5-Bromosalicylaldehyde Thiosemicarbazone

A rapid and sensitive spectrophotometric method is developed for the determination of Copper (II) in aqueous DMF medium. The metal ion forms a light greenish yellow coloured complex with 5-bromo salicylaldehyde thiosemicar- bazone (5-BSAT) in acidic medium. The complex shows absorption maximum at 390nm. Beers law is obeyed in the range 0.31 - 6.35 � gml -1 of Copper (II). The molar absorptivity (� ) and Sandells sensitivity are found to be 1.08 X 10 4 l mole -1 cm -1 and 0.062 � gcm -2 respectively. A method for the determination of copper by third derivative spectrophotome- try is also proposed. The methods have been employed successfully for the determination of copper in grape leaves and aluminum based alloy samples.

Simple and Simultaneous Method for Determination of Palladium(II) and Ruthenium(III) using Second-Order-Derivative Spectrophotometry

Abstract A simple, sensitive, and selective second-order-derivative spectrophotometric method has been developed for the simultaneous determination of palladium(II) and ruthenium(III) using 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone (HMBATSC) as a chromophoric reagent. The reagent (HMBATSC) reacts with Pd(II) and Ru(III) at pH 3.0, forming soluble yellowish green and dark brown species, respectively. Palladium and ruthenium present in the mixture were simultaneously determined without solving the simultaneous equations by measuring the second derivative amplitudes at 445 nm and 385 nm, respectively. Further, the Beers law was obeyed in the range 0.21–12.78 µg mL−1 and 0.25–13.42 µg mL−1 for Pd(II) and Ru(III), respectively. A large number of foreign ions did not interfere in the present method. The proposed method was successfully applied for the determination of palladium in hydrogenation catalysts and ruthenium in water samples.

Spectrophotometric Determination of Iron(II) and Cobalt(II) by Direct, Derivative, and Simultaneous Methods Using 2-Hydroxy-1-Naphthaldehyde-p-Hydroxybenzoichydrazone.

Optimized and validated spectrophotometric methods have been proposed for the determination of iron and cobalt individually and simultaneously. 2-hydroxy-1-naphthaldehyde-p-hydroxybenzoichydrazone (HNAHBH) reacts with iron(II) and cobalt(II) to form reddish-brown and yellow-coloured [Fe(II)-HNAHBH] and [Co(II)-HNAHBH] complexes, respectively. The maximum absorbance of these complexes was found at 405 nm and 425 nm, respectively. For [Fe(II)-HNAHBH], Beers law is obeyed over the concentration range of 0.055–1.373 μg mL−1 with a detection limit of 0.095 μg mL−1 and molar absorptivity ɛ, 5.6 × 104 L mol−1 cm−1. [Co(II)-HNAHBH] complex obeys Beers law in 0.118–3.534 μg mL−1 range with a detection limit of 0.04 μg mL−1 and molar absorptivity, ɛ of 2.3 × 104 L mol−1 cm−1. Highly sensitive and selective first-, second- and third-order derivative methods are described for the determination of iron and cobalt. A simultaneous second-order derivative spectrophotometric method is proposed for the determination of these metals. All the proposed methods are successfully employed in the analysis of various biological, water, and alloy samples for the determination of iron and cobalt content.

Stability indicating ion chromatography method for the simultaneous determination of ibandronate sodium drug substance and its impurities.

A simple and sensitive ion chromatography method has been developed for the simultaneous assay of ibandronate sodium drug substance and the determination of its impurities. The separation was achieved on Allsep™ anion column 150 mm × 4.6 mm, 7 μm particle diameter. The mobile phase consisted of 1% (v/v) aqueous formic acid and acetone 98:2% (v/v); flow rate 1.0 ml min(-1) at ambient temperature. The analytes were monitored by conductometric detector. The drug substance was subjected to stress conditions of hydrolysis, oxidation, photolytic, thermal and humidity degradation. Considerable degradation was achieved only under oxidative conditions. Mass balance was demonstrated in all stress conditions. The method was validated for specificity, precision, linearity, solution stability and accuracy. The limits of detection (LOD) and limits of quantification (LOQ) for impurities were in the range of 0.36-0.80 μg ml(-1) and 1.00-2.40 μg ml(-1), respectively. For ibandronate LOD was 38 μg ml(-1) and LOQ was 113 μg ml(-1). The average recoveries for impurities and ibandronate were in the range of 99.0-103.1% and the method can be successfully applied for the routine analysis of ibandronate sodium drug substance.

First Order Derivative Spectrophotometric Determination of Vanadium(V) and Iron(III) Individually and Simultaneously

A novel, sensitive and highly selective first derivative spectrophotometric method is proposed for the determination of vanadium(V) and iron(III) metal ions separately and simultaneously in a mixture. 2-Hydroxy-1-naphthaldehyde benzoylhydrazone (OHNABH) reacts with vanadium(V) and iron(III) in sodium acetate–acetic acid buffer medium (pH 5.0) forming yellow and yellowish brown colored soluble complexes, respectively. The first derivative curves of these colored solutions show maximum derivative amplitudes at 465 nm (V(V)) and 540 nm (Fe(III)) obeying Beers law in the range 0.12–2.50 μg ml–1 and 0.14–4.20 μg ml–1, respectively. Large number of foreign ions do not interfere in the present method. A very simple and accurate simultaneous first derivative method is also reported for the determination of V(V) and Fe(III) in mixtures without solving simultaneous equations. The method is applied for the analysis of various natural samples, food and biological materials.

DIRECT AND SECOND DERIVATIVE SPECTROPHOTOMETRIC DETERMINATION OF MOLYBDENUM (VI) IN FOOD STUFFS AND IN ALLOY STEELS USING 2- HYDROXY-3-METHOXY BENZALDEHYDE THIOSEMICARBAZONE (HMBATSC)

A rapid, simple, sensitive and selective spectrophotometric method is developed for the determination of molybdenum (VI) in aqueous dimethyl formamide (DMF). Molybdenum (VI) forms a yellow coloured complex with 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone in the pH range 1.0-6.0. The complex shows maximum absorbance at 375nm and in the pH range 1.0-2.0. However, at this wave length, the reagent shows considerable absorbance. At 385nm, the complex shows large absorbance while the reagent blank shows negligible absorbance. Hence, analytical studies are carried out at 385nm and at pH 1.5 against reagent blank. Beers law is obeyed in the range 0.24-4.32 µg ml-1. The molar absorptivity and Sandells sensitivity forthe coloured solution are found to be 2.3 x 10-4 1 mol-1 cm-1 and 0.0042 µg cm-2 respectively. The interference effect of various diverse ions has been studied. The complex shows 1:1 [Mo (VI): HMBATSC] stoichiometry with a stability constant 2.35 x 106. The standard deviation of the method in the determination of 2.396 µg ml-1 of Mo(VI) is calculated as ± 0.0012. A second order derivative spectroscopic method is developed for the determination of molybdenum(VI), which is more sensitive than the zero order method.. The developed method has been employed for the determination of molybdenum (VI) in food stuffs and in alloy steels. The results are in excellent agreement with the certified values

Simultaneous Determination of Cobalt(II) and Nickel(II) by Fourth-Order Derivative Spectrophotometric Method Using 2-Hydroxy-3-Methoxy Benzaldehyde Thiosemicarbazone.

A simple and new simultaneous fourth derivative spectrophotometric method is proposed for the analysis of a two-component system containing cobalt(II) and nickel(II) without separation using 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone (HMBATSC) as a chromophoric reagent. The reagent reacts with cobalt(II) and nickel(II) at pH 6.0, forming soluble brown and yellow colored species, respectively. Cobalt(II) and nickel(II) present in themixture are simultaneously determined without solving the simultaneous equations bymeasuring the fourth derivative amplitudes at 468.5 nm and 474.5 nm, respectively. The derivative amplitudes obey Beers law at 468.5 nm and 474.5 nm for Co(II) and Ni(II) in the range 0.059–3.299 μg mL−1 and 0.058–3.285 μg mL−1 respectively. A large number of foreign ions do not interfere in the present method. The present simultaneous method is used for the determination of micro amounts of cobalt in biological samples, nickel in plant samples, and in some alloy steels and soil sample.

2-Hydroxy-1-naphthaldehyde-P-hydroxybenzoichydrazone: A New Chromogenic Reagent for the Determination of Thorium(IV) and Uranium(VI)

Simple, sensitive, selective, direct, derivative, and simultaneous spectrophotometric methods are developed for the determination of uranium and thorium individually and simultaneously. The methods are based on the reaction of 2-hydroxy-1-naphthaldehyde-p-hydroxybenzoichydrazone (HNAHBH) with thorium(IV) and uranium(VI). HNAHBH reacts with thorium and uranium at pH 6.0 forming stable yellow and reddish brown coloured complexes, respectively. [Th(IV)-HNAHBH] complex shows maximum absorbance at 415 nm. Beer’s law is obeyed over the concentration range 0.464–6.961 μg mL−1 with a detection limit of 0.01 μg mL−1 and molar absorptivity, e, 3.5 × 104 L mol−1 cm−1. Maximum absorbance shown by [U(VI)-HNAHBH] complex is at 410 nm with Beer’s law range 0.476–7.140 μg mL−1, detection limit 0.139 μg mL−1 and molar absorptivity, e, 1.78 × 104 L mol−1 cm−1. Highly sensitive and selective second-order derivative methods are reported for the direct and simultaneous determination of Th(IV) and U(VI) using HNAHBH. The applicability of the developed methods is tested by analyzing water, ore, fertilizer, and gas mantle samples for thorium and uranium content.

Erratum to: Direct and derivative spectrophotometric determination of thorium with 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone

A simple and sensitive spectrophotometric method is developed for the determination of throium in aqueous medium. The metal ion forms yellow coloured complex with 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone (2,4-DHBINH) in the pH range 2.0–8.0. The complex shows an absorption maximum at 390 nm. The absorbance of the complex is maximum at pH 5.5 Beers law is obeyed in the range 0.30–7.00 μg/ml of thorium(IV). The molar absorptivity and the Sandells sensitivity of the method are 2.20· 104 l·mol−1·cm−1 and 0.0106 μg/cm−2, respectively. The interference of various ions was studied. The composition of the complex is 1:1 {Th(IV) : 2,4-DHBINH}. The first derivative spectrum of the complex shows a zero cross at 391.2 nm and maximum amplitude at 415 nm. Thus a sensitive derivative spectrophotometric method for the determination of Th(IV) is proposed.