Rapid spectrophotometric determination of ruthenium(III) with prochlorperazine maleate

A rapid, simple spectrophotometric method for the determination of μg amounts of ruthenium, based on the formation of a pink complex between the metal and prochlorperazine maleate (PCPM) in sulphuric or hydrochloric acid solution, is described. The complex has an absorption maximum at 530 nm and its molar absorptivity is 6.733·10³ l mol^?1 cm^?1. The sensitivity is 0.0151 μg Ru cm^?2 for log I_o/I = 0.001. Beer's law is valid over the range 0.2–10 μg Ru ml^?1 ; the optimal range for spectrophotometric determination is 0.8–8.0 μg Ru ml^?1. Job's method of continuous variation, the mole ratio method and the slope ratio method indicate a 1:1 composition for the complex. The effects of acidity, time, temperature, order of addition of reagents, reagent concentration, and the interferences from various ions are reported.     

Substitutions of organopalladium(II) species with benzimidazole derivatives

The [Pd(cod)(cotl)]ClO₄ complex (cod = cycloocta-1,5-diene; cotl = cyclooctenyl, C₁₈H₁₃ ^–) undergoes substitutions with new Schiff base ligands containing benzimidazole L [L = 2-(2-N-n-propylidenephenyl)benzimidazole (L¹); 2-(2-N-i-propylidenephenyl)benzimidazole (L²); 2-(2-N-n-butylidenephenyl)benzimidazole (L³); 2-(2-N-i-butylidenephenyl)benzimidazole (L⁴)]. Facile displacement of cod by L occurs to produce complexes of the type [Pd(cotl)L]ClO₄· nMe₂CO (n= 0; L = L¹, L² or L³; n= 2, L = L⁴). Dihalobridge complexes of the type [Pd(cotl)X]₂(X = Cl or Br) undergo halogen-bridge cleavage with L¹–L⁴ to give mononuclear complexes of the type Pd(cotl)LX · nH₂O (n= 2, X = Cl, L = L¹; n= 0, X = Br, L = L¹; n= 0, X = Cl, L = L²; n= 0, X = Cl or Br, L = L³; n= 0, X = Cl, L = L⁴; n= 2, X = Br, L = L⁴) and a binuclear complex [Pd(cotl)Br]₂L². The complexes were characterised by physical properties, i.r., ¹H- and ¹³C-n.m.r. spectral techniques and by mass spectra. Probable structures have been proposed.     

Vanadametry Estimation of Thiosulphate

1.(a) We have found that sodium thiosulphate is quantitatively oxidized to tetrathionate in five minutes at room temperature (28°) by excess sodium vanadate in a medium containing sulphuric acid at 0.06N to 0.1N concentration and a little copper sulphate as catalyst. (b) Quantitative emulation of sodium thiosulphate to tetrathionate has also been achieved by the action of excess sodium vanadate during five minutes at room temperature in a medium containing 2.0N—8.0N acetic acid and a little copper salt as catalyst. Further oxidation to sulphate does not occur, even if the mixture is heated to boiling. (c) The excess of unreacted vanadate in 1(a) and 1(b) can be titrated with a standard solution of ferrous ammonium sulphate using diphenylbenzidine as indicator, after adding the requisite quantity of syrupy phosphoric acid. 2. On the other hand, sodium thiosulphate is easily and quantitatively oxidized to sulphate at room temperature, when. acted upon by excess sodium vanadate in a medium containing hydrochloric acid at an overall concentration of 5-6N and 1.0 ml of iodine monochloride as catalyst. The time required for reaction is ten minutes. The unreacted vanadate can be estimated by titration with a standard solution of ferrous ammonium sulphate, using N-phenylanthranilic acid as indicator or with diphenylbenzidine as indicator after suitably diluting and adding phosphoric acid.     

Synthesis and characterization of oligomeric molybdenum complexes of N-alkylphenothiazines

Summary Polynuclear molybdenum(IV/V) oxide - phenothiazine complexes which are oligomeric in nature have been prepared. The complexes were characterized by elemental analyses and spectroscopic data. The molecular formulae of the new complexes are [Mo₄O₉(OH₂)₂(PTZ)₂], PTZ = chlorpromazine or promethazine, [Mo_{4 8}(OH₂)₂(TR)₂], TR = thioridazine, [Mo₅O₁₀(OH_O2)₂(EP)₂], EP = ethopropazine, and [Mo₆O₁₂(OH₂)₂(TF)₂], TF = trifluoperazine. Tentative structures are proposed.     

Promethazine hydrochloride as a new redox indicator in vanadametry

Promethazine hydrochloride is proposed as a new redox indicator in vanadametry. It has been tested rigorously in the titration of iron(II), hydroquinone, uranium(IV) and antimony(III) with sodium vanadate. The indicator gives a very sharp reversible colour change from green to violet at the equivalence point. It has advantages over all the proposed redox indicators in vanadametry. Its redox and transition potentials are reported.     

Extractive spectrophotometric methods for the assay of sildenafil citrate (Viagra) in pure form and in pharmaceutical formulations

Two simple and sensitive extractive spectrophotometric methods for the determination of sildenafil citrate (SC) are proposed. The methods are based on the formation of ion-association complexes of sildenafil citrate with bromocresol green (BCG, method A) and with chromoxane cyanine R (CCR, method B) in aqueous acidic buffer. The complex species, extractable to chloroform phase, were quantitatively measured at 415 and 460 nm for methods A and B, respectively. Beer's law was obeyed in the SC concentration range 1.25-25 mug ml(-1) with a limit of detection 0.16 mug ml(-1) and 1.5-60 mug ml(-1) with a limit of detection 0.18 mug ml(-1), respectively, for methods A and B. The methods have been successfully applied to the analysis of bulk drug and its tablets. No interference was observed from common pharmaceutical adjuvants.     

Rapid spectrophotometric determination of platinum with trifluoperazine dihydrochloride

Trifluoperazine dihydrochloride reacts with platinum(IV) in sodium acetate-hydrochloric acid buffer containing copper(II) catalyst to form a bluish-green 1:1 complex with absorbance maximum at 504 nm. A 50-fold ratio of reagent to metal ion is necessary for complete complexation. Beer's law is valid over the concentration range 0.5-8 ppm of platinum(IV) with optimum concentration range 1-7 ppm. The molar absorptivity is 6.50 x 10(3) l.mole(-1).cm(-1). The effects of pH, time, temperature, concentration of reagent and copper, order of addition of reagents, and the interferences from various ions are reported.     

Oxidimetric determination of methionine and its metal complexes with chloramine-B and dichloramine-B

Simple, rapid, and reproducible methods for the determination of methionine (HMt) and its metal complexes, [NiMt]ClO₄₊ and Na[AgMt₂], in aqueous solutions have been developed, based on their oxidation with chloramine-B and dichloramine-B at room temperature. The direct titration, with a visual or potentiometric endpoint, involves a two-electron change corresponding to the formation of methionine sulfoxide. Several amino acids and common anions and cations do not interfere under these conditions. In the back-titration procedure methionine and its complexes are oxidized by excess CAB in 0.1 N NaOH medium with a four-electron change corresponding to the formation of methionine sulfone. The amino acid and its complexes are, however, oxidized to the respective nitrile, with excess DCB with an eight-electron change.     

Preparation and certification of high-grade gold geochemical reference material

One high-grade gold geochemical reference material-BND 3401.01 has been prepared by the National Geophysical Research Institute (NGRI), Hyderabad in collaboration with the Hutti Gold Mines Company Limited (HGML), Hutti and National Physical Laboratory (NPL), New Delhi, in India. The sample is a sheared gold-sulphide-bearing quartz vein emplaced in a sheared acid volcanic rock that was collected at the 2400-foot level from the middle reef of Hutti deposit located in the north-western periphery of the late-Archaean Hutti-Maski greenstone belt, Karnataka, India. Fifteen institutions in India, Canada, China and Tanzania having experience in geochemical analysis had participated in this collaborative analysis programme. The sample was extensively characterized for its major, minor, trace and ultra-trace element composition by using a variety of analytical techniques. Usable values were provided for major, minor and several trace elements including all rare earth elements (REE). The certified value for the gold concentration in BND 3401.01 gold ore is 12.1±0.7 mg/kg.     

N-substituted phenothiazines as redox indicators in titrations with chloramine-T and chloramine-B

Profenamine hydrochloride, fluphenazine dihydrochloride, trifluopromazine hydrochloride, cyamepromazine maleate, perphenazine dihydrochloride and mepazine hydrochloride are proposed as redox indicators in the titration of hydroquinone, metol and ascorbic acid with chloramine-T and chloramine-B in sulphuric, hydrochloric and acetic acid media. They give a sharp reversible colour change at the equivalence point. A simple but accurate method for the determination of hydroquinone, metol and ascorbic acid is described. The conditional potentials and molar absorptivities of the indicators and redox potential of chloramine-B are reported.