Determination Of Vanadium In Steels Research Articles

Direct and selective spectrophotometric method for the determination of vanadium in steel, environmental and biological samples

A simple, direct and selective spectrophotometric method for determination of vanadium is described. The present methodology is based on the strong oxidizing power of vanadium (V). Vanadium (V) selectively oxidizes leucocrystal violet (LCV) to crystal violet in the presence of phosphoric acid. The violet colored dye obtained shows maximum absorbance at 590 nm. Beer's law is obeyed in the concentration range 0.06–0.6 μg ml −1. The molar absorptivity and Sandell's sensitivity are found to be 6.78 × 10 4 l mol −1 cm −1 and 0.0044 μg cm −2, respectively. The proposed method is simple, direct, and sensitive. It has been successfully applied for the determination of vanadium in various environmental, biological and steel samples.

Extraction Spectrophotometric Determination of Vanadium in Steels with Thiosalicylic Acid (TSA)

In this paper thiosalicylic acid (TSA) is proposed for a simple, rapid and selective method for the spectrophotometric determination of vanadium based upon the formation of the TSA-vanadium complex and its extraction into Adogen 464-toluene solution. Under optimum operating conditions, a green colour is formed when the complex is extracted, from weak acidic 40% ethanolic solution, In the organic solvent (apparent molar absorptivity 1,700 L.mol−1·cm−1 at wavelength of 600 nm). The relative error is 2.3%, in the determination of 16 μg.mL−1 of vanadium, and its limit of detection is 3 μg·mL−1. The method has been applied to the determination of vanadium in steels.

Highly Selective Derivative Spectrophotometric Determination of Vanadium(V) in Steels, Minerals and Soil Samples

A simple, selective and sensitive spectrophotometric method has been developed for the determination of trace amounts of Vanadium(V) in acetic acid medium using a newly synthesized reagent acetoacetanilide salicyloylhydrazone (AASH). The molar absorptivity and Sandell's sensitivity of the coloured species were found to be 1.20 x 104 L mol-1cm-1 and 4.2 ng cm-2 respectively. Beer's law is obeyed in the range 0.3 -3.0μ.g mL-1 of vanadium (V) at 405 nm. The stochiometry of the complex was found to be 1:1 (V (V): AASH). A highly selective first order derivative spectrophotometric method for the determination of vanadium is also reported. A calibration graph was derived by measuring first derivative amplitudes at 430 nm (trough depth). The metal ions which are normally associated with vanadium in minerals and alloys do not interfere. The developed procedure has been successfully applied for the trace level determination of vanadium in steels, minerals and soil samples.

Kinetic spectrophotometric determination of vanadium in steels based on the catalytic oxidation of thionine by potassium bromate

Abstract A sensitive and selective kinetic spectrophotometric method for the determination of V(V) was developed based on the catalytic oxidation of thionine by KBrO 3 in 0.6 mol·L −1 H 3PO 4 medium. The linear calibration range and detection limit at 25°C were 0-0.5 μg·mL −1 and 0.01 μg·mL −1, respectively. In the presence of NaF and urea, most of the common ions did not interfere with the determination of V(V). The proposed method was applied for the determination of vanadium in steels and satisfactory results were obtained.

Extraction-spectrophotometric study on the vanadium(V)-2,3-dihydroxynaphthalene — iodonitrotetrazolium chloride — water — chloroform system and its analytical application

Abstract The formation of a new ternary ion-associate complex of vanadium(V) with 2,3-dihydroxynaphthalene and iodonitrotetrazolium chloride with a composition ratio of 1:2:1 is reported. The complex is quantitatively extracted from water into chloroform. The molar absorptivity (ɛ) of the extract at λ max=340 nm is 2.5 × 104 dm3/mol cm, and Beer’s law is obeyed for concentrations ranging from 0.1 to 0.9 µg/cm3 V(V). The following constants are determined: the extraction constant, the association constant, the distribution constant, and the recovery factor. The effects of foreign ions and reagents are studied. A selective and sensitive method is developed for determination of vanadium in steels.

Spectrophotometric determination of vanadium using variamine blue and its application to synthetic, environmental and biological samples

A simple, rapid and accurate spectrophotometric method is described for the determination of trace amounts of vanadium using variamine blue (VB) as a chromogenic reagent. The method is based on the oxidation of variamine blue to form a violetcolored species on reaction with vanadium(V), having an absorption maximum at 570 nm. Beer’s law is obeyed in the range of 0.1–2.0 μg ml−1. The molar absorptivity and Sandell’s sensitivity were found to be 1.65 × 104 l mol−1 cm−1 and 0.003 μg cm−2, respectively. Optimum reaction conditions were evaluated in order to delimit the linear range. The effect of interfering ions on the determination is described. The proposed method has been successfully applied to the determination of vanadium in steel, pharmaceutical, environmental, and biological samples.

Selective and sensitive spectrophotometric determination of total vanadium with hydrogen peroxide and 4-(2-pyridylazo)-resorcinol

A selective and sensitive method for the spectrophotometric determination of the total amount of vanadium based on the reaction with 4-(2-pyridylazo)-resorcinol, PAR, and hydrogen peroxide is proposed. The formed complex shows maximum absorbance at 542 nm with molar absorptivity=1.85×10 4 l mol −1 cm −1 in the range from 0.01 to 0.5 mol l −1 of sulfuric acid and obeys the Beer's law up to 3.0 μg ml −1 of vanadium. The limit of detection of the method is 0.0028 μg ml −1 (3 σ). The analytical method can be directly applied for the determination of vanadium in steels providing good results. Prior separation of some interfering elements is not necessary. The characteristics of the method, i.e. simplicity, selectivity, sensitivity and rapid calibration, make it specially suitable for routine analysis.

A Highly Sensitive and Selective Spectrophotometric Determination of Vanadium(V) Using 6-Chloro-3-hydroxy-7-methyl-2-(2-thienyl)-4H-chromen-4-one.

A simple, rapid, highly sensitive and selective method for the extractive spectrophotometric determination of micro amounts of vanadium(V) has been worked out using 6-chloro-3-hydroxy-7-methyl-2-(2-thienyl)-4H-chromen-4-one (CHMTC) as a complexing agent in a weakly acidified (HCl, pH 0.84–1.09) medium. The greenish-yellow complex is quantitatively extractable into carbon tetrachloride, and shows maximum absorbance at 417–425 nm. The method obeys Beer’s law up to 0.9 m g V ml–1, having molar absorptivity and Sandell’s sensitivity of 8.26×104 dm3 mol–1 cm–1 and 0.0006 m g V cm–2, respectively. As many as 39 cations and 14 anions and/or complexing agents do not interfere. The method has good reproducibility and can be satisfactorily applied to the determination of vanadium in steels, reverberato-ry flue dust and water samples.

RP-HPLC study of redox equilibria in vanadium-PAR binary and ternary systems: Direct determination of vanadium in steel

The reversed-phase high-performance liquid Chromatographic (RP-HPLC) behaviour of the binary chelates of V(V) and V(IV) with 4-(2-pyridylazo) resorcinol (PAR) and ternary chelates of vanadium with PAR and auxiliary ligands: hydrogen peroxide, hydroxylamine, tartrate and citrate were studied using a C18 column. The complex double-peak chromatograms of V(IV)/V(V)-PAR systems were studied and the origin of each peak was proved. Vanadium in ternary systems with PAR and hydrogen peroxide was found exclusively in V(V)-H2O2-PAR complex (single peak on the chromatogram) despite its initial oxidation state. The double role of hydroxylamine (complex agent and reductor) in vanadium systems with PAR was confirmed: in the V(V) system three species were identified (V(V)-PAR, V(V)-NH2OH-PAR and V(IV)-PAR), but in the V(IV) system only two: V(IV)-PAR and V(V)-NH2OH-PAR. Citrate and tartrate giving single peak were found as auxiliary ligands in ternary V(V) systems of analytical importance. Due to its masking potential towards iron (III) ions, citrate was chosen as the most suitable third component of a ternary vanadium system with PAR, to form the basis of an RP-HPLC method for direct determination of V in steel.

Chemiluminescent determination of vanadium in steel

A chemiluminescent method for the determination of vanadium in steel with cinchomeronic hydrazide as analytical reagent is proposed. The optimum conditions are pH 11.75 (phosphate buffer), 1.0×10−3 mol/l cinchomeronic hydrazide, 6.6×10−3 mol/l hydrogen peroxide and 2.8×10−3 mol/l V(IV). The maximum chemiluminescent emission is obtained at 420 nm. A linear relationship exists in the range of 0.04–1.00 μg/ml of V(IV) with a 3.6% variation coefficient at 0.50 μg/ml of V(IV) level for ten replicates. Cobalt(II), copper(II) and chromium(VI) show strong interference and a chloroform extraction procedure with α-benzo-inoxime is recommended to avoid these interferences. This method has been applied to determine vanadium in a certified steel with excellent results.

Liquid anion-exchange separation of vanadium from malonate media

Vanadium(IV) and (V) can be quantitatively extracted with 0.2 mol/l Amberlite LA-2 in xylene at pH 3.0 from 0.02 mol/l malonic acid, stripped with 0.5 mol/l hydrochloric acid, and determined spectrophotometrically. Five other liquid anion exchangers (Amberlite LA-1, Primene JM-T, Aliquat 336S, TOA and TIOA) were examined as possible extractants. The extraction of vanadium(IV) was found to be quantitative only with Amberlite LA-2, while that of vanadium(V) was quantitative with Amberlite LA-1 and LA-2, Primene JM-T and Aliquat 336S. Eight common solvents were tested as diluents; of these hexane, cyclohexane, benzene, and xylene were found to be satisfactory. Vanadium was separated from elements that do not form anionic complexes with malonic acid by selective extraction, from those that form weak complexes by washing the organic extract with water, and from metals that form strong malonato complexes by selective stripping with hydrochloric, nitric, or sulphuric acid. The method has been applied to the determination of vanadium in steel, coal fly ash and fuel oil. The precision of measurement is within ±5% and the detection limit of the method for vanadium is 0.5 mg/kg.

Determination of vanadium in steels and geological materials by liquid-liquid extraction and graphite furnace atomic absorption spectrometry

A procedure for determining vanadium in steels and geological materials involves dissolving the samples in concentrated HNO 3 for steels and iron-rich meteorites or in HClO 4-HF-HNO 3 (1:1:1) for siliceous materials. The solutions are evaporated to dryness and the residue is dissolved in 6 M HCl. The solutions are oxidized with K 2S 2O 8 and KMnO 4 at 70°C prior to separation of iron, chromium and molybdenum by extraction into isobutyl methyl ketone. After separation, the aqueous solution is reoxidized with KMnO 4 at 70°C. The residual solution containing vanadium and nickel is evaporated to dryness, the residue dissolved in 6 M HNO 3 and the vanadium extracted into tributyl phosphate, leaving the nickel behind. This purified extract is back-extracted into 2% H 2O 2 in 6 M HNO 3. The aqueous back-extract is analysed for vanadium by graphite furnace atomic absorption spectrometry. The limit of detection is about 0.3 μg V g −1 in the original sample. The relative standard deviation of the method was 3.7% for seventeen replicates of the NBS SRM 361 standard steel, with a relative error of 4.5%. Replicate analyses of standard silicate rocks (CAAS SY-1 anal SU-1) gave similar good precision and accuracy. Vanadium was determined in several iron meteorites and in the carbonaceous chondrite Allende.

Ion-exchange separation and spectrophotometric determination of vanadium in environmental samples

A selective and sensitive method for the extraction and spectrophotometric determination of vanadium(V) in microgram quantities is described. The molar absorptivity of the yellow vanadium(V)—caffeic acid—Aliquat 336 extract is 1.3 × 10 4 1.mole −1.cm −1 at 370nm. The method is compared with the atomic-absorption spectrometric method and applied to the trace determination of vanadium in steel, alloys, a rock and environmental samples.

Determination of vanadium in steels using phenylfluorone and cetylpyridinium bromide

AbstractVanadium(V) was determined spectrophotometrically by reaction with phenylfluorone (I) at pH 8.8 in the presence of cetylpyridinium bromide to form a 1:2 vanadium‐I chelate. The molar absorptivity of the sensitised chelate was 7.0 × 104 dm3 mol−1 cm−1 at 550 nm and the sensitivity index was 0.7 ng cm−2. Beer's law was followed up to 0.37 ppm of vanadium. The interference of other metal ions was eliminated by electrolytic separation using a mercury cathode. The developed method was successfully applied for the determination of vanadium in steels.

Selective and sensitive extraction spectrophotometric method for the determination of vanadium (V) as a mixed ligand complex withN-phenyl benzohydroxamic acid and 4-(2-pyridylazo)resorcinol in non-aqueous media

A selective, sensitive and direct method for the spectrophotometric determination of vanadium in steels is developed in which vanadium is extracted withN-phenyl benzohydroxamic acid (PBHA) into chloroform from 5M hydrochloric acid medium followed by colour development by addition of 4-(2-pyridylazo)resorcinol (PAR) inN,N-dimethyl formamide (DMF). The vanadium(V)-PBHA-PAR mixed ligand complex shows maximum absorbance at 560 nm with a molar absorptivity 3.6 × 104 l mol−1 cm−1 and obeys Beer's law up to 2.0 μg/ml of vanadium. The composition of the mixed ligand complex is determined by Job's method of continuous variations which revealed a 1 ∶ 1 ∶ 1 ratio for V(V) ∶ PBHA ∶ PAR. This method can be directly applied for the determination of vanadium in steels, while in the case of titanium base alloys, after separation of titanium matrix it gives good results even at 50–200 μg of vanadium per gram level.

Extraction-spectrophotometric determination of vanadium with 5,5′-dithiodisalicylhydroxamic acid (DTDSHA)

A new method for the extraction-spectrophotometric determination of V(V) is proposed. The violet complex V(V)-5,5′-dithiodisalicylhydroxamic acid formed in aqueous medium (pH 5.0) is extracted into a solution of trioctylmethylammonium chloride (Adogen 464) in toluene, and its spectrophotometric characteristics are studied. The stoichiometry of the complexes formed is 1:1 and 2:1 (reagent:vanadium), and 1:3 for the ionic association complex (2:1):trioctylmethylammonium ion. The system follows Beer's law at pH 5.0 (λ = 550 nm) over the concentration range 0.4 to 2.0 ppm (ϵ = 7.34 × 10 3 liter · mol −1 · cm −1). The method is applied for the determination of vanadium in steel.

Spectrophotometric determination of vanadium in steel and alloys with 2-(5-chloro-2-pyridylazo)-5-dimethylaminophenol

Using spectrophotometric methods, the protopysis constant of the 5.ClDMPAP reagent (p K a1 = −0.19; p K a2 = 1.97; p K a3 = 11.98) and the stability constant of its vanadic complex (6.0 ± 0.11) × 10 14 were determined. A high-sensitivity spectrophotometric method was developed to determine V(V) using 0.1–1.2 ppm and pH = 3.8. ϵ 586 = 55,300 ± 400 liters · mol −1 · cm −1. A study on the most important interferences and the way to eliminate them was carried out. The method can be applied to the determination of the element in steels and ferrovanadiums.

Use of N-benzyl-2-naphthohydroxamic acid as a highly selective reagent for solvent extraction and spectrophotometric determination of vanadium(V)

N-Benzyl-2-naphthohydroxamic acid extracts vanadium(V) selectively and quantitatively into chloroform from 2–8.5 M hydrochloric acid in the presence of Mo(VI), Zr(IV) and Ce(IV). The extraction takes place quickly and gives a stable reddish-violet extract which shows an absorption maximum at 505 nm with molar absorptivity of (5.34 ± 0.05) × 10 3 1.mole −1.cm −1. The optimum range for the determination is 2.2–7.4 ppm of vanadium(V) in the final solution. The method has been used for the determination of vanadium in steels.

2-Hydroxy-l-naphthaldehyde guanylhydrazone as analytical reagent for spectrophotometric estimation of vanadium

A spectrophotometric determination of V(V) with 2-hydroxy-1-naphthaldehy-de guanylhydrazone can be performed in a concentration range varying from 0.70–8.70 ppm of vanadium; the molar absorptivity is 7.7 ×l03 litres mol−1 cm−1 at 405 nm and the relative error is ±0.60. The stoichiometry (1: 1) of the complex was established by different methods. This method of spectrophotometric determination has been applied satisfactorily to the determination of vanadium in steel.

Spectrophotometric Determination of Vanadium in Steel using 4(2-Thiazolylazo)-Resorcinol and Hydroxylamine

Spectrophotometric Determination of Vanadium in Steel using 4(2-Thiazolylazo)-Resorcinol and Hydroxylamine