Prochlorperazine bismethanesulfonate: Sensitive and selective reagent for the spectrophotometric determination of microgram amounts of osmium

Prochlorperazine bismethanesulfonate (PCPMS) is proposed as a new sensitive and selective reagent for the spectrophotometric determination of microgram amounts of osmium. PCPMS forms a red-colored species with osmium(VIII) or osmium(VI) instantaneously at room temperature in 5 M phosphoric acid medium. The red species exhibits maximum absorbance at 529 nm. Beer's law is valid over the concentration range 0.05–3.6 ppm for osmium(VIII) and 0.15–6.4 ppm for osmium(VI). Sandell's sensitivity of the reaction is 2.89 nm cm^?2 for osmium(VIII) and 4.24 ng cm^?2 for osmium(VI). The effects of time, temperature, acidity, order of addition of reagents, reagent concentration, and diverse ions are investigated. The application of the proposed method in the determination of osmium content in synthetic ores has been explored.     

1,3-Cyclopentanedione bis(4-methylthiosemicarbazone) monohydrochloride as a spectrophotometric reagent for the determination of lodate in acetic and perchloric acid media

1,3-Cyclopentanedione bis(4-methylthiosemicarbazone) monohydrochloride produces colored solutions with iodate ions in acid medium. The yellow color obtained has been used to proposed Spectrophotometric methods for determination of IO₃^? in the concentration range 1.0–11.0 ppm in acetic acid medium (molar absorptivity 1.08 × 10⁴ liters mol^?1 cm^?1 at a wavelength of 415 nm) and 0.5–8.0 ppm in perchloric acid medium (molar absorptivity 2.05 × 10⁴ liters mol^?1 cm^?1 at a wavelength of 400 nm).     

Extractive spectrophotometric determination of molybdenum as a thiocyanate-2-acetylpyridinethiosemicarbazone complex

A new spectrophotometric method for the determination of molybdenum is based on the extraction of the orange red molybdenum thiocyanate-2-acetylpyridinethiosemicarbazone complex into chloroform from hydrochloric acid. The complex has an absorption maximum at 470 nm with a molar absorptivity of 1.7 × 10⁴ liters mol^?1 cm^?1. Beer's law is valid from 0.1 to 6.5 ppm of molybdenum. The equilibrium shift method indicated a 1:4:2 complex. The method has been used successfully for the determination of molybdenum in molybdenum steels.     

Nonpyridinic derivatives in C-5 of 2-thiohydantoin for spectrophotometric determination of palladium

The reactions between Pd(II) and four nonpyridinic derivatives of 2-thiohydantoin (5-benzal-2-thiohydantoin, 5-(o-hydroxy)benzal-2-thiohydantoin, 5-(m-hydroxy)benzal-2-thiohydantoin, and 5-anisal-2-thiohydantoin) have been considered. The influence of the different experimental parameters on the formation of the complexes was studied, and the optimum conditions for the determination of palladium were established. The anisal derivative was selected among these four reagents and the spectrophotometric determination of palladium described in detail. The precision of the procedure, expressed in terms of relative standard deviation was 0.9%, and numerous ions that usually interfere in palladium determination, such as Os(VIII), Rh(III), and Ru(IV) (of the platinum group) and Pb(II), Cd(II), Ni(II), Co(II), Zn(II), and others of the transition series, were tolerated.     

Electrothermal atomic-absorption spectrophotometric determination of molybdenum

The sensitivity for determining Mo by ETA-AA is dependent on the heating programme employed when the peak-height method is used, but not when the peak area is used for evaluation of the AA signals. The linear range is greater at lower heating rate. Molybdenum can be directly determined in up to 8% NaCl solution without chemical pretreatment or background correction by making use of the high ashing temperature allowed, at which the matrix NaCl can be totally removed. The minimum recovery is 94.5%. Amounts of alkaline earth metals greater than 4000 times the amount of Mo give scatter signals, but these are time-resolved from the Mo signal. Any small effect on the peak height or area can be compensated for by background correction. The interference of tungsten is significant even at low concentrations (2-5 mug/ml) owing to the formation of stable compounds. Mo is determined in brines and acid digests of phosphate rocks after preconcentration and separation with the APDC-MIBK system, by ETA-AA of the organic extracts with or without mineralization.     

Studies on pollutants: A new reagent for the detection of fluoride

A new solid analytical reagent is reported for the detection and semiquantitative determination of traces of fluoride. A blue (λ_max 590 nm) trypan blue dye is liberated from an insoluble zirconium-trypan blue complex by the action of fluoride in dilute acetic acid medium. The detection limit is 0.8 ppm and the range of semiquantitative determination is 0.8 to 8 ppm. The method is simple and can be conveniently used for field detection of fluoride in polluted waters.     

Solvent extraction and spectrophotometric determination of palladium(II) with some nitrogen-containing heterocyclic hydrazones in the presence of chloride ions

Three terdentate hydrazones, all containing the 1-phthalazino grouping in the hydrazine moiety but differing in the heterocyclic substituent in the aldehyde moiety, have been used as analytical reagents for palladium(II), the optimal conditions for the extractive spectrophotometric determination of palladium(II) in the presence of chloride ions being deduced. These compounds are highly selective and sensitive reagents for palladium(II), since they are not extracted into chloroform from sulfuric acid solutions and do not react with other platinum group metals. The desirable spectral properties of the palladium(II) complex of benzothiazole-2-aldehyde-1-phthalazinohydrazone (BAPhH) have also been discussed with respect to preference of the C  N structural form in the heterocyclic ring on the aldehyde moiety of the ligand.     

Girard-P derivative of 2-pyridinecarboxaldehyde as analytical reagent. Spectrophotometric determination of copper

The synthesis, characteristics, properties, and reactions with metallic ions of pycolinaldehyde derivatives of Girard-P reagent have been studied. The reagents form complexes with Cu(II), Ni(II), Co(II), Hg(II) and (I), Zn(II), Cd(II), and Fe(III), and (II), which exhibit a good sensibility but whose spectra have the absorption maxima located in the ultraviolet zone. The spectrum of copper complex in the presence of ascorbic acid shows another absorption band at the visible region and this makes the spectrophotometric determination of copper very selective. The influence of the different experimental parameters on the formation of copper complex without ascorbic acid and with this compound was studied, and the optimum conditions for the determination of copper were established. The precision of the procedure, expressed in terms of relative standard deviation, was 1.1%. The method has been tested on “white metal E-8” samples.     

Indole as a reagent for nitrite in aqueous solution

A fairly selective and sensitive spectrophotometric method for the trace determination of nitrite in aqueous solution is described. The titled ion reacts with indole in acidic medium to form a soluble pink-red product, which is measured at 530 nm. Maximum absorbance is achieved in 10 min and remains constant for about 45 min. This method is applicable to water samples containing 0–2 μg/ml with a relative error of 0.0 to–0.8%, and relative standard deviation of 0.3–0.8%, depending on the concentration level. The optimum reaction conditions affecting and related to the color reaction and interferences due to foreign ions have been studied.     

Ethylisobutrazine hydrochloride as a selective and sensitive reagent for the spectrophotometric determination of vanadium(V) and its application to vanadium-bearing minerals and alloys

Ethylisobutrazine hydrochloride is proposed as a selective and sensitive reagent for the spectrophotometric determination of vanadium(V). It forms a red-colored species with vanadium(V) in 3.5–6.5 M phosphoric acid medium. An eight-fold molar excess of reagent is necessary for the full development of the color. The red species exhibits an absorption maximum at 518 nm with a molar absorptivity of 9.75 × 10³ liters mol⁻¹ cm⁻¹. Sandell's sensitivity is 5.2 ng cm⁻². Beer's law is obeyed over the range 0.1–6.2 ppm of vanadium(V) with an optimum concentration range of 0.4–6.0 ppm. The effects of acidity, time, temperature, order of addition of reagents, reagent concentration, and the interferences from various ions, are reported. The method has been used successfully for the determination of vanadium in ilmenite and vanadium steels that contain chromium, molybdenum, manganese, nickel, copper, tungsten, and titanium.     

Extractive spectrophotometric determination of molybdenum(V) in molybdenum steels

An extraction spectrophotometric method has been developed for the determination of traces of molybdenum present in molybdenum steels which is based on the extraction of the orange-red molybdenum-thiocyanate-acetonethiosemicarbazone complex into chloroform from hydrochloric acid medium. The complex has an absorption maximum at 472 nm with a molar absorptivity of 1.9 × 10⁴ liters mol⁻¹ cm⁻¹. Beer's law is valid over the concentration range 0.1–9.5 ppm of molybdenum with an optimum concentration range of 0.4–9 ppm. The equilibrium shift method indicates 1:4:2 composition for molybdenumthiocyanate-acetonethiosemicarbazone complex. The effect of acidity, reagent concentrations, temperature, and interferences from various ions are reported.     

Spectrophotometric determination of BrO3− using the 1,2,4-trihydroxyanthraquinone-3-carboxylic acid as reagent

The reaction between the 1,2,4-trihydroxyanthraquinone-3-carboxylic acid and BrO₃^? in hydrochloric acid medium has been studied spectrophotometrically. The red color of the oxidation product serves as basis for a new method for determination of traces of BrO₃^?, measuring the absorbance at 520 nm. The influence of foreign ions on the determination, the stoichiometry of the reaction, and the nature of the oxidation product, have been reported.     

Spectrophotometric and analogue derivative spectrophotometric determination of ultramicro amounts of cadmium with cationic porphyrins

alpha,beta,gamma,delta-Tetrakis(1-methylpyridinium-3-yl)porphine [T(3-MPy)P] and alpha,beta,gamma,delta-tetrakis(1-methylpyridinium-4-yl)porphine [T(4-MPy)P] have been found to react rapidly with cadmium to give coloured complexes in weakly alkaline media at room temperature. Simple and practical methods for the determination of cadmium at ng/ml levels by conventional and analogue derivative spectrophotometry have been proposed. The analogue method gives higher sensitivity. T(3-MPy)P gives higher sensitivity than T(4-MPy)P. The interference of various foreign cations and anions has also been examined and in many cases eliminated or reduced. Adsorption of the porphyrins and their cadmium complexes onto the glassware, which is usually observed under the conditions of reaction and causes significant errors in the determination, can be suppressed almost completely by addition of fairly large amounts of a salt such as sodium chloride.     

Rapid spectrophotometric determination of cerium(IV), arsenic(III), and nitrite with perphenazine

Perphenazine dihydrochloride, PPN, is proposed as a new reagent for the spectrophotometric determination of cerium(IV), arsenic(III), and nitrite. The reagent forms a red-colored species with cerium(IV) instantaneously in 3.5–5.5 M phosphoric acid medium. The red species exhibits maximum absorbance at 516 nm. A 15-fold molar excess of PPN is necessary for the full development of the color intensity. Beer's law is obeyed over the cerium concentration range 0.4–20 ppm and Sandell's sensitivity is found to be 0.016 μg/ cm². The effects of acidity, time, order of addition of reagents, temperature, reagent concentration, and diverse ions are reported. The proposed method offers the advantages of good sensitivity, simplicity, rapidity, selectivity, and a wider range of determination without the need for heating or extraction. Arsenic(III) and nitrite are also indirectly determined. The method is extended to the determination of cerium content in synthetic mixture corresponding to misch metal.     

Oxidative addition of aryl halides to iridium(I) complexes. A new arylation reagent

Oxidative addition of aryl halides, ArX, to chlorocarbonylbis(triphenylphos-phine)iridium(I) yields iridium(III) aryl complexes, IrCl(X)(Ar)(CO)(PPh₃)₂. The reactivity of the aryl halide decreases in the order I > Br > C1, and electron-withdrawing substituents in the aryl ring accelerate the reaction. The Ir^III compounds may be utilised as arylating agents.     

Determination of cyanide by a highly sensitive indirect spectrophotometric method

Complexation of Pd(2+) with cyanide inhibits the extraction of the palladium complex of 5-phenylazo-8-aminoquinoline. This effect is used for the indirect spectrophotometric determination of cyanide at the mug level. Cyanide in industrial waste water and in sea-water is determined after distillation as HCN from the sample and collection in sodium hydroxide solution.     

Sensitive spectrophotometric determination of La(III) with 1-(2-pyridylazo)-2-naphthol

A simple and sensitive method for spectrophotometric determination of lanthanum has been developed. At pH 9.6, in presence of 50% ethanol, lanthanum reacts with 1-(-2-pyridylazo)-2-naphthol (PAN) to form a red complex which has two absorption maxima, at 545 and 510 nm. The molar absorptivity at 545 nm is 0.55 × 10⁴ liters · mol^?1 cm^?1. On the other hand, lanthanum reacts with PAN in pure ethanol to form a red complex at 530 nm, with high molar absorptivity (8 × 10⁴ liters · mol^?1 cm^?1).     

Solvent extraction and spectrophotometric determination of titanium(IV) with 3-phenyl-3-methyl-2-mercaptopropenoic acid

The distribution equilibria of 3-phenyl-3-methyl-2-mercaptopropenoic acid (PhMMP) and the titanium(IV)-PhMMP complex have been studied. An extraction-photometric method for the determination of microamounts of titanium has been developed. We have investigated the influence of pH, the reagent, and the presence of electrolytes and masking agents in the aqueous phase on the equilibrium. From the slope analysis of the distribution curves the composition of the extracted species has been found to be Ti(OH)₂(HR)₂. The complex is extracted quantitatively. Beer's Law is followed over the range 0.09–3.74 μg ml^?1 of titanium(IV), the molar absorptivity is 1.65 × 10⁴ liters mol^?1 cm^?1, and the Sandell sensitivity is 2.8 ng cm^?2 at 439 nm. This method has been applied to the determination of titanium in a bauxite.