Spectrophotometric determination of molybdenum with lobeline

Lobeline hydrochloride has been tested as a reagent for molybdenum(V). Molybdenum(VI) is reduced with hydrazine sulfate in hydrochloric acid solution to Mo(V) only and complexed with thiocyanate and lobeline which is extracted with chloroform. In the paper experimental conditions for the formation of the ion pair of lobeline with molybdenum thiocyanate are described and the composition of this complex is given.     

A solvent extraction study of molybdenum chloride and molybdenum thiocyanate complexes

The effect of reducing agents on molybdenum(VI) solutions in hydrochloric acid was studied by a solvent extraction technique to elucidate the composition of the colored molybdenum thiocyanate complex. Neither copper(I) chloride nor ascorbic acid have any effect on the extraction of MoO₂Cl₂; it is inferred that tin(II) chloride reduces Mo(VI) stepwise to a polynuclear Mo(V)·Mo(VI) complex and then to Mo(V). The colored thiocyanate complex produced by copper(I) and by ascorbic acid differs only slightly in extraction characteristics from the uncolored Mo(VI) complex. It is suggested that the color may be produced by an isomerization reaction of MoO₂(SCN)₂, and thus that the colored species may be a hexavalent rather than pentavalent molybdenum complex.     

Spectrophotometric determination of molybdenum in steel after extraction with thiocyanate and butyltriphenylphosphonium bromide into microcrystalline benzophenone

Molybdenum(VI) is reduced to molybdenum (V) with ascorbic acid, reacts with thiocyanate and the complex is extracted with butyltriphenylphosphonium by microcrystalline benzophenone and the solid phase is dissolved in chloroform and measured spectrophotometrically. The system is applied to the determination of molybdenum (0.53–4.92%) in high-speed tool steels without prior separation of iron.     

Acid decomposition method for visual colorimetric determination of molybdenum in geochemical exploration

A mixture of nitric and sulphuric acids is used for the decomposition of geochemical samples. Determination of molybdenum at the μg g^?1 level is effected by visually comparing the colour of the thiocyanate complex. The acid medium seems to be well suited for the colorimetric determination of molybdenum. The same solution can be used advantageously for atomic absorption measurements for larger amounts of molybdenum. The method is suitable for batch analysis and results in a high throughput.     

Bestimmung Von Molybdän Nach Extraction Mit O,O,S - Triäthyldithiophosphat

Abstract

The interaction of molybdenum(V) with potassium thiocyanate in a medium of O,O,S-triethyldithiophosphate [(C₂H₅O)₂P(S)SC₂H₅] and ethanol at a ratio 4:1 has been studied.

The stability constant of the molybdenum(V) thiocyanate complex was determined to be 7.6 × 10² with a molar ratio Mo(v) : SCN of 1:1. A new method based on the formation of the molybdenum-thiocyanate complex in the organic phase has been developed for the determination of molybdenum in steel.     

Molybdenum determination in iron matrices by ICP-AES after separation and preconcentration using polyurethane foam

A procedure is proposed for the separation and determination of molybdenum in iron matrices by a batch process. It is based on the solid-phase extraction of the molybdenum(V) ion as thiocyanate complex on polyurethane (PU) foam. The extraction parameters were optimized. Using 0.20 mol L-1 hydrochloric acid, a thiocyanate concentration of 0.10 mol L-1, 100 mg of polyurethane foam and shaking time of 10 min, molybdenum (5-400 micrograms) can be separated and preconcentrated from large amounts of iron (10 mg). Desorption was carried out instantaneously by conc. nitric acid or acetone. Distribution coefficients, sorption capacity of the PU foam and coefficients of variation were also evaluated. The effect of some ions on the separation procedure was assessed. Iron(III) should be reduced to iron(II). The proposed procedure was used to determine molybdenum in standard iron matrices such as steel and pure iron. The achieved results did not show significant differences with certified values.     

The extraction and determination of molybdenum as the thiocyanate complex

A method is presented for the determination of molybdenum by extraction of its thiocyanate complex with methyl isobutyl ketone. The method is accurate to ±4% or 3 μg of molybdenum, whichever is greater. The only elements which cause interference are rhenium (serious), platinum, palladium, rhodium, selenium and tellurium. The method has been applied to a number of standard samples with excellent results.     

Extractive-spectrophotometric determination of molybdenum as an ion-association complex with thiocyanate and adogen

A selective and sensitive method is described for the determination of trace amounts of molybdenum, based on its reaction with thiocyanate and its extraction (into toluene) as an ion-association complex formed with adogen (methyltrioctylammonium chloride). The molar absorptivity is 2.13 x 10(4) l.mole(-1).cm(-1) at lambda(max) 467 nm. The method has been applied to molybdenum determination in steels.     

Separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quaternary ammonium salt

Methods were developed for the separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quaternary ammonium salt, Zephiramine. Tungsten was extracted into chloroform as an ion associate of tungsten(V)-thiocyanate complex and Zephiramine cation was retained on a column of Teflon powder coated with Zephiramine, but molybdenum(III) was neither extracted nor retained. The extraction chromatographic method was successfully applied to the determination of trace amounts of tungsten in molybdenum by neutron activation analysis.     

Sequential Injection Photometric Determination of Molybdenum Using Organic Wetting Film Extraction

Wetting film extraction was combined with colorimetry to determine nanogram amounts of molybdenum(VI). The simple extraction procedure enhanced sensitivity and selectivity while maintaining a high sample throughput. Extraction and back extraction steps were exploited to exclude interference from the 31 metal species and 11 anions tested. In the first step, molybdenum(VI) was extracted into a toluene film as an ion paired complex. Molybdenum(VI) reacted with thiocyanate to form anionic molybdenum(V) and/or molybdenum(VI) thiocyanate complexes. The complexes were extracted into a toluene film containing tetraheptylammonium bromide as ion pairing reagent. The thiocyanate ligands were displaced by 1,5-diphenylcarbazone (DPC) to form a more intensely colored complex (λ_max= 540 nm). DPC was introduced in the back extraction solvent, methanol. The relative standard deviation was 2.5% for 50 ng ml⁻¹of molybdenum(VI) (n= 10) at a rate of 25 samples h⁻¹. The detection limit (3 × baseline noise) was 2.5 × 10⁻⁸M.     

Spectrophotometric determination of molybdenum in rocks with thiocyanate

A rapid procedure for the determination of microgram amounts of molybdenum in rocks is described. After acid decomposition, molybdenum is extracted from a hydrochloric acid solution into xylene with tributyl phosphate. After back-extraction with water, molybdenum is extracted as the α-benzoinoximate into chloroform, stripped into hydrochloric acid extracted as the thiocyanate into amyl alcohol, and determined spectrophotometrically. The molybdenum thiocyanate color produced is stable, sensitive, and reproducible. Results of analyses of several of the U.S. Geological Survey standard rocks are given.     

Spectral and electrochemical studies on oxoisothiocyanatobis(pyrrolidinyldithiocarbamato)molybdenum(V)

The complex, oxoisothiocyanatobis(pyrrolidinyldithiocarbamato)molybdenum(V), MoO(NCS) (pyrroldtc)₂ was prepared. The IR spectra of the complex suggest that the thiocyanate group is attached through nitrogen and the presence of MoO³⁺ moiety. The voltammograms of the complex in acetonitrile exhibited a pronounced cathodic wave at ?0.23 V vs S.C.E. which was attributed to Mo(V)/Mo(IV) couple. The magnetic, epr and electrochemical studies indicate that the compound is mononuclear and molybdenum is in +5 oxidation state.     

Molybdenum determination in iron matrices by ICP-AES after separation and preconcentration using polyurethane foam

A procedure is proposed for the separation and determination of molybdenum in iron matrices by a batch process. It is based on the solid-phase extraction of the molybdenum(V) ion as thiocyanate complex on polyurethane (PU) foam. The extraction parameters were optimized. Using 0.20 mol L^–1 hydrochloric acid, a thiocyanate concentration of 0.10 mol L^–1, 100 mg of polyurethane foam and shaking time of 10 min, molybdenum (5–400 μg) can be separated and preconcentrated from large amounts of iron (10 mg). Desorption was carried out instantaneously by conc. nitric acid or acetone. Distribution coefficients, sorption capacity of the PU foam and coefficients of variation were also evaluated. The effect of some ions on the separation procedure was assessed. Iron(III) should be reduced to iron(II). The proposed procedure was used to determine molybdenum in standard iron matrices such as steel and pure iron. The achieved results did not show significant differences with certified values.     

Investigations of Thiocyanate Complexes of Rhenium,Molybdenum, Vanadium and Tungsten by Ion-Exchange Chromatography Method

Abstract

The main purpose of this paper is examination of complexe formation between thiocyanate ions and rhenium, molybdenum, vanadiun and tungsten under identical detailed analysis of the chromatographic conditions of complex separation, definition of relative stability of the complexes, in order to determine the separation method of complex mixture of these ions.     

Extractive spectrophotometry of the molybdenum (III) 1,10-phenanthroline thiocyanate and 2,2'-bipyridyl thiocyanate complexes

New extraction spectrophotometric methods for the determination of small amounts of molybdenum have been developed, using thiocyanate and 1,10-phenanthroline or 2,2'-bipyridyl as reagents in the presence of chlorostannous acid. Extracts of the ternary complexes of tervalent molybdenum in 1,2-dichloroethane obey Beer's law in the range 1-10 mug/ml at 525 nm. A 10-fold excess of iron and vanadium and 100-fold excess of tungsten, phosphorus and silicate do not interfere.     

The chemical analysis of ternary alloys of plutonium with Molybdenum and Uranium

It is shown that the absorptiometric determination of molybdenum as thiocyanate may be used in the presence of plutonium. Molybdenum interferes with previously published methods for determining uranium and plutonium but conditions have been established for its complete removal by solvent extraction of the compound with a-benzoin oxime. The previous methods for uranium and plutonium are satisfactory when applied to the residual aqueous phase following this solvent extraction.     

Carminic acid as a reagent for the spectrofluorimetric determination of molybdenum and tungsten-II Determination of molybdenum in mild steel

A method is described for the spectrofluorimetric determination of molybdenum in mild steel down to 0.01 %. After dissolution of the sample, molybdenum is separated from the bulk of iron by extraction of molybdenum(V) thiocyanate with isoamyl acetate. It is then determined with carminic acid as described in Part I.     

The separation and estimation of hexa-and pentavalent molybdenum by paper chromatography

Preliminary investigations were made upon the chromatographie separation of hexa- and pentavalent molybdenum by organic solvent systems which contained potassium thiocyanate. A method for the quantitative separation of these valency states by paper chromatography in a water-acetic acid-potassium thiocyanate eluant is described. The estimations were performed colorimetrically as molybdenum pentathiocyanate which was extracted into ethyl acetate. As little as 10 μg Mo can be detected in the respective valency states. The probable error of the quantitative estimation is of the order of ± 3% for 50–100 μg Mo.     

Spectrophotometric determination of some histamine H1-antagonists drugs in their pharmaceutical preparations

Two rapid, simple and sensitive extractive specrophotometric methods has been developed for the determination of three histamine H1-antagonists drugs, e.g., chlorphenoxamine hydrochloride (CPX), diphenhydramine hydrochloride (DPH) and clemastine (CMT) in bulk and in their pharmaceutical formulations. The first method depend upon the reaction of molybdenum(V) thiocyanate ions (Method A) with the cited drugs to form stable ion-pair complexes which extractable with methylene chloride, the orange red color complex was determined colorimetrically at lambda(max) 470nm. The second method is based on the formation of an ion-association complex with alizarin red S as chromogenic reagents in acidic medium (Method B), which is extracted into chloroform. The complexes have a maximum absorbance at 425 and 426nm for (DPH or CMT) and CPX, respectively. Regression analysis of Beer-Lambert plots showed a good correlation in the concentration ranges of 5.0-40 and 5-70microgmL(-1) for molybdenum(V) thiocyanate (Method A) and alizarin red S (Method B), respectively. For more accurate analysis, Ringbom optimum concentration ranges were calculated. The molar absorptivity, Sandell sensitivity, detection and quantification limits were calculated. Applications of the procedure to the analysis of various pharmaceutical preparations gave reproducible and accurate results. Further, the validity of the procedure was confirmed by applying the standard addition technique and the results obtained in good agreement well with those obtained by the official method.     

Inorganic polarography in organic solvents-II: polarographic examination of the molybdenum(V) thiocyanate complex in diethyl ether

A procedure involving the solvent extraction of molybdenum(V) thiocyanate into diethyl ether followed by a direct polarographic examination of the organic phase offers a selective method for the determination of molybdenum down to 0.5 ppm. Only molybdenum, amongst 21 elements examined, is observed to give a reduction wave under the recommended conditions. The method is evaluated with respect to various experimental factors and is applied to the determination of molybdenum in mild and alloy steels.