Spectrophotometric determination of vanadium as vanadium(IV) pyridine thiocyanate

A spectrophotometric determination of vanadium as vanadium(IV) pyridine thiocyanate is described. The blue complex is formed in acidic aqueous solution and extracted into pyridine-chloroform. Absorbance is measured at 7.40 mμ. The range of best accuracy for 1-cm cells is from about 80 to 240 μg of vanadium per ml, and sensitivity is 0.4 μg of vanadium per cm² at 7.40 mμ. The vanadium may be present initially as vanadium(IV) or vanadium(V), which is reduced to vanadium(IV) by the large excess of thiocyanate ion added. Several elements interfere in the determination ; a separation procedure involving mercury cathode electrolysis is suggested.     

The spectrophotometric determination of aliphatic hydroxyl in esters with vanadium oxinate

A method is described for the precise determination of small amount of aliphatic alcohols in esters. The procedure is based on the formation of a red-coloured complex between the alcohol and a solution of vanadium oxinate in nitrobenzene. Studies have been made on the effect of solvent, reaction time and the stability of the complex on the accuracy of the determination.     

First-derivative spectrometric analysis of mixtures of peroxo complexes of titanium,vanadium, and molybdenum for respective metals

The application of first-derivative spectrometry to the simultaneous determination of titanium and vanadium; titanium and molybdenum; and vanadium and molybdenum in their mixtures with varying mass ratios has been described with hydrogen peroxide as color developing reagent. At a first-derivative isosbestic point for the peroxo complex of one constituent, the derivative absorbance of the other constituent is read and used for quantitation. The procedure does not require the solution of simultaneous equations. The first-derivative spectrometry is also feasible at 450.0 nm for the selective determination of titanium in the presence of vanadium, molybdenum, and tungsten.     

Separation and solvent extraction of vanadium and uranium with n-propyl 2,3,4-trihydroxybenzoate

A spectrophotometric method is described for the separation and determination of trace quantities of vanadium(IV) and (V) from uranium(VI). Vanadium is selectively separated from uranium by extraction at pH 6.5 into n-propyl 2,3,4-trihydroxybenzoate (PTB) dissolved in t-pentanol. Up to 120 microg of vanadium can be determined by measuring the absorbance of the blue complex in the organic phase at 585 nm. Uranium(VI) remains in the aqueous layer and can be determined spectrophotometrically by its reaction with PTB in aqueous acetone to produce a brown-red colour at pH 7.6-8.8. Solutions containing 25-275 microg of uranium absorb at 370-380 nm according to Beer's law. By modification, this procedure can be used for the determination of the two metals in native phosphate rocks. The effects of diverse ions on the determination of vanadium and uranium have also been examined.     

Bromometric determination of vanadium (V) by hydrazine

A method for the quantitative determination of vanadium(V), based on the reduction of vanadium(V) by hydrazine, has been described. The reduction is carried out in high concentration of hydrochloric acid and the excess hydrazine back-titrated against standard potassium bromate, using the dead-stop end-point procedure. Hydrazine is preferentially oxidized by bromate in presence of vanadium(IV). Accurate results have been obtained over a wide range of vanadium(V) concentration.     

Spectrophotometric determination of vanadium with 1,10-phenanthroline

A simple and sensitive spectrophotometric method for the determination of vanadium based upon the reaction of vanadate with 1,10-phenanthroline in the presence of sodium dithionite in ammoniacal solution is described. The absorbance of the complex measured at 645 nm follows Beer's law for solutions containing 30-400 microg of vanadium in 100 ml of solution. A 10-fold excess of molybdenum, tungsten, phosphorus or chromium does not interfere. The molar absorptivity is 8.0 x 10(3) 1 mole(-1) cm(-1). The complex is shown to be tris-1,10-phenanthroline vanadium(II). The method has been applied successfully to the determination of vanadium in bauxite.     

Spectrophotometric determination of vanadium(IV) with nitrilotriacetic acid

A new and convenient spectrophotometric method for the estimation of vanadium(IV) with NTA is described. The minimum ratio of metal ion to ligand, working pH, wavelength for maximum absorbance of the complex ion, and the effect of various cations and anions are described. The complex ion obeys Beer's law in the concentration range 1–32 mmol/liter of the vanadium(IV) ion. It is observed that iron(II), cobalt(II), nickel(II), copper(II), and oxidizing anions such as chromate and nitrite interfere in this determination, whereas managanese(II), chromium(III), iron(III), and anions like nitrate, chloride, bromide, iodide, thiocyanate, sulfate, and sulfite do not have any effect. Excessive amounts of acetate, phosphate, oxalate, tartrate and thiosulfate must also be avoided in this determination. Anions and cations which interfere in the determination of vanadium(IV) by NTA should not be present in the system.     

Spectrophotometric determination of vanadium(V) as a mixed thiocyanate-4-pyridone complex

The spectrophotometric determination of vanadium(V) as a mixed thiocyanate-3-hydroxy-2-methyl-1-phenyl-4-pyridone (HX) complex and as a mixed thiocyanate-3-hydroxy-2-methyl-1-(4-tolyl)-4-pyridone (HY) complex is described. The extracted complexes in chloroform have a maximum absorbance at 450 and 650 nm. The optimal conditions for the extraction and spectrophotometric determination of vanadium(V) are determined. The solutions of the V-SCN-HX and V-SCN-HY complexes in chloroform obey Beer's law in the range 1–10 ppm of vanadium, and are stable for at least 24 hr. The molar absorptivity of the method is 6.8 × 10³ liters mol^?1 cm^?1. The molar ratio V:SCN:HX (HY) of the extracted complex is 1:1:2.     

Spectrophotometric determination of vanadium(V) with oxine in isoamyl alcohol

A new method for the spectrophotometric determination of vanadium(V) with 8-hydroxyquinoline in isoamyl alcohol is described. The spectra show broad absorption maxima between 450 and 490 nm. The effects of amount of reagent, acidity, time, and temperature were also studied. The optimal interval of Beer's law application is 0.75–3.50 μg vanadium/ml. The nature of the complex in solutions, as well as the interference, reproducibility, and precision of the method, was investigated. The method has been applied to the determination of vanadium in foods.     

Determination of small amounts of titanium in pure molybdenum,tungsten, vanadium and their oxides after separation on silica gel

A new method for the separation of titanium from molybdenum, tungsten and vanadium is described, based on sorption of the titanium complex with hydrogen peroxide on silica gel under dynamic conditions. The eluted titanium is determined spectrophotometrically with diantipyrylmethane. The method can be applied to the determination of small amounts of titanium in tungsten, molybdenum and vanadium metals and in their oxides.     

The microchemical analysis of ferrous and non-ferrous alloys

Satisfactory methods are described for the determination of certain of the alloying constituents in small quantities of steels, aluminium alloys and white metals. In steels, lead is determined by using an extraction procedure with dithizone, whereas the stable colour produced by vanadium with 3 : 3' dimethylnaphthidine is used for determining this element. In aluminium alloys, absorptiometric procedures are recommended for determining copper, nickel, iron and manganese. The determination of silicon is advocated by the absorptiometric technique. For the determination of antimony, in white metals, a micro volumetric procedure with standard potassium bromate is recommended using α-naphthaflavone as indicator.     

Extraction--spectrophotometric determination of oxalate in urine and blood serum

An extraction--spectrophotometric method is described for the determination of oxalate, based on the formation of a mixed ligand vanadium (V)--mandelohydroxamic acid--oxalate complex. The complex was extracted into a solution of trioctylmethylammonium chloride (Adogen 446) in toluene and the absorbance measured at 535 nm. The experimental variables and interferences in this determination were studied. The detection limit is 0.5 microgram ml-1 and the range of application is between 2 and 8 micrograms ml-1. The method was applied to the determination of oxalate in urine and blood serum.     

Gravimetric Determination of Mercury(II) and Vanadium(IV) with Benzoylacetanilide

Abstract

Gravimetric methods for the determinations of mercury(II) and vanadium(IV) with benzoylacetanilide have been described. These metals have been separated from commonly associated ions and a procedure for the determination of vanadium content of steel has been developed. By these methods, 14 to 50 mg. of mercury and 5 to 20 mg. of vanadium have been estimated with relative standard deviations of 0.18% and 0.10%, respectively.     

N-m-Tolyl-o-Methoxybenzohydroxamic Acid (m-T-o-MBHA) as a Specific Reagent for Vanadium

Abstract

A high selective and sensitive spectrophotometric method is described for the determination of traces of vanadium(V) using N-m-tolyl-o-methoxybenzohydroxamic acid. The violet complex extracted into chloroform (λ_max = 545 nm) is stable for several days. As little as 0. 05 μg of vanadium is detectable.     

Determination of Trace Vanadium by Adsorptive Stripping Voltammetry at a Carbon Paste Electrode

A method for the voltammetric determination of vanadium using a carbon paste electrode (CPE) was described. The new procedure is based on the adsorptive accumulation of the V(V)‐alizarin red S(ARS) complex onto the surface of the CPE, followed by the electrochemical reduction of adsorbed species. The optimal experimental conditions include the use of 0.10 mol/L acetate buffer (pH 5.1), 1.0×10^?5 mol/L ARS, an accumulation potential of ?0.10 V (versus SCE), an accumulation time of 2 min, a scan rate of 200 mV/s and a second‐order derivative linear scan mode. The reduction peak for the complex appears at ?0.52 V. The peak current is proportional to the concentration of V(V) over the range of 0.10–15.0 μg/L, and the detection limit is 0.04 μg/L for a 2 min adsorption time. The relative standard deviations(n=8) for 2.0 and 0.50 μg/L V(V) are 3.1 and 4.7%, respectively. The proposed method was applied to the determination of vanadium in water samples.     

Determination of submicrogram amounts of vanadium in biological materials by extraction with N-cinnamoyl-N-2,3-xylylhydroxylamine and flameless atomic-absorption spectrometry with an atomizer coated with pyrolytic graphite

A highly sensitive and simple method for determination of vanadium in plants and biological samples by solvent extraction and flameless atomic-absorption spectrometry with a carbon tube coated with pyrolytic graphite is described. After digestion of the sample, vanadium is separated by extraction of its N-cinnamoyl-N-2,3-xylylhydroxylamine complex into carbon tetrachloride from 6M hydrochloric acid medium. The method can be used to determine vanadium in plants and biological samples with average recovery of 94% and coefficient of variation of 14%. The sensitivity (1% absorption) is estimated to be 4 x 10(-11) g.     

Determination of trace amounts of vanadium with a new reagent [1-(3-methoxysalicylidene-amino)-8-hydroxy-3,6-naphthalene disulfonic acid, disodium salt] by fluorescence quenching method

A fluorescence quenching method is described for the determination of trace amounts of vanadium(V) based on the formation of a complex in acidic medium with a new reagent [1(3-methoxysalicylideneamino)-8-hydroxy-3,6-naphthalene disulfonic acid, disodium salt]. The fluorescence emission is measured at 415 nm (wavelength of excitation 360 nm), and the experimental variables and interferences in this determination have been studied. The detection limit is 12.5 ng/ml and linear range is between 50 and 600 ng/ml. The method has been applied to determine trace vanadium(V) in steel and cast iron.     

Determination of trace vanadium in natural waters by a combined ion exchange—catalytic photometric method

A sensitive, selective and simple method is described for the determination of trace vanadium in natural waters. Vanadium is separated and concentrated by a combined cation- and anion-exchange procedure in 0.05 M HCl—0.1 % H₂O₂ media, and determined by the catalytic method based on the oxidation of gallic acid by bromate. The proposed method is applied to the analysis of natural waters. The relative standard deviations are 3.9 % for 0.8 p.p.b. of vanadium in river water and 3.2 % for 1.9 p.p.b. of vanadium in lake water (surface). As little as 0.03 p.p.b. of vanadium can be determined in samples of 100 ml or less.     

The separation of titanium from vanadium and molybdenum by cupferron solvent extraction

The isolation of small amounts of titanium from vanadium and molybdenum before the spectrophotometric determination of titanium as the “pertitanate” complex has been achieved by a. solvent extraction procedure using cupferron and chloroform at pH 6 in the presence of EDTA.     

Determination of vanadium by solid-phase spectrophotometry after its preconcentration as an Eriochrome Cyanine R complex on a dextran-type exchanger

A method is described for the determination by solid phase spectrophotometry (SPS) of trace amounts of vanadium in natural water and crude petroleum samples. The procedure is based on fixation on a dextran-type anion exchanger of the complex V(IV)-Eriochrome Cyanine R. The absorbance of the gel, at 563 and 750 nm, packed in a 1 mm cell, is measured directly. Vanadium can be determined in the 0.6-25.0 mug l(-1) range with a relative standard deviation of 2.2%. The comparison of the SPS method and the gallic acid persulphate method shows that the linearity, analytical sensitivity and precision were better for the SPS method, and that the latter method has lower detection and quantification limits than the gallic acid persulphate method.