Potassium 3-phenylmethyldithiocarbazate as substoichiometric reagent: Determination of silver

An accurate and rapid radiochemical method has been developed for the determination of silver based on the substoichiometric extraction of its complex with potassium 3-phenylmethyldithiocarbazate into chloroform from pH 5.5 acetate buffer. Microgram amounts of silver could be determined with an average error of ±1.1% and the effect of diverse metal ions was critically examined. The method developed was applied to evaluate the silver content of photofilm washings.     

Substoichiometric Isotope Dilution Analysis for the Determination of Iron in Biological Materials and Comparison with Substoichiometric Isotope Dilution Mass Spectrometry

Substoichiometric isotope dilution analysis for the determination of trace iron has been studied by using synergistic extraction of iron(III) with a substoichiometric amount of 4-isopropyltropolone (Hipt) in the presence of an excess of 3,5-dichlorophenol (DCP) in heptane. Optimum conditions for the substoichiometric extraction of iron(III) in g to sub-g levels were examined and the high selectivity for iron(III) toward various metal ions encountered in the analysis of biological materials was confirmed. The present method was applied to a biological reference material (NIES, CRM No.9, sargasso) without any pre-separation and was successfully evaluated. Furthermore, substoichiometric stable isotope dilution mass spectrometry using the present extraction method was also used with the above sample. Applicability and practicability was compared for both substoichiometric methods.     

Use of thenoyltrifluoroacetone for the determination of manganese by activation analysis

A new procedure for the substoichiometric extraction of bivalent manganese by thenoyltrifluoroacetone into ethyl acetate has been developed and used in activation analysis. The value of the extraction constant has been found to be 3.1 x 10(-6); the pH range in which the extraction can be performed is 7.8-9.2. The influence of oxalate, citrate, tartrate, fluoride and cyanide ions has been studied. A selective substoichiometric extraction of manganese in the presence of Zr, Hf, Nb, Th, Fe and Sc is possible at pH 8-8.5, tartrate and fluoride being used as masking agents. Copper and cobalt can be screened by ammonia and cyanide respectively. The method has been used for the determination of manganese in biological materials, potassium fluoride and zirconium.     

Solvent extraction of Ni/II/ with isonitrosobenzoylacetone into chloroform

A method has been developed for the quantitative extraction of Ni/II/ with isonitrosobenzoylacetone /HINBA/ into chloroform. The effect of various parameters on the extraction coefficient value such as pH, time of equilibration, effect of solvents, anions, cations etc. have been studied. The stoichiometry of the metal: reagent determined by the method of substoichiometric extraction and slope ratio method was found to be 12. Decontamination factors for many elements in the substoichiometric extraction of Ni/II/ were also evaluated.     

Estimation of selenium in biological samples utilizing potassium benzyl xanthate

In the present investigation, a simple and selective radioanalytical method for the evaluation of selenium in microgram amounts by substoichiometric isotope dilution analysis has been developed. Potassium benzyl xanthate has been employed as the reagent. The colorless selenium-benzyl xanthate complex was extracted into chloroform. The influence of various ions during the extraction was also critically examined. The method developed has been successfully applied for the analysis of a few agricultural products for selenium.     

Determination of cobalt by substoichiometric extraction with β-hydroxy-naphthaldoxime

A substoichiometric radiochemical solventextraction method is described for the determination of cobalt, employing β-hydroxy-naphthaldoxime and chloroform as reagent and extractant, respectively. The extraction behaviour of the complex of cobalt with the reagent in the pH-range 8–9.5 and the effects of various metal ions on the extraction are critically studied. The method is used to determine the cobalt content in some pharmaceutical drugs.     

Solvent extraction of Ru(III) with 2-mercaptobenzimidazole into n-butanol

A new and rapid method has been developed for the quantitative extraction of Ru(III) with 2-mercaptobenzimidazole into n-butanol. The extraction coefficient of Ru(III) between n-butanol and an ethanolic solution of 1% 2-mercaptobenzimidazole showed a maximum value ofE=161 at a pH of 2.0. The effect of various other parameters on the extraction coefficient value of Ru(III) such as solvent effect, anions, cations, etc. have also been studied. The stoichiometry of metal to reagent has also been determined by the method of substoichiometric extraction and by the slope ratio method and was found to be 1∶3. Decontamination factor for various elements in the substoichiometric extraction of Ru(III) were also evaluated.     

Substoichiometric extraction of mercury with malonic anilide

Determination of mercury (II) by substoichiometric extraction with malonic anilide into a mixture of ether and MIBK is reported. The method has been applied in the estimation of the metal in industrial effluents.     

Determination of cadmium by substoichiometric thermal neutron activation analysis

A rapid and selective method has been developed for the determination of cadmium in environmental samples by thermal neutron activation analysis, employing substoichiometric solvent extraction technique. Alcoholic solution of 2-mercaptobenzothiazole /2-HMBT/ has been used for the substoichiometric extraction of Cd/II/ from an aqueous solution of pH 7.0 into methyl iso-butyl ketone /MIBK/.     

Substoichiometry for multielement separation by metal chelate extraction and its application in activation analysis

The method of substoichiometric separation is completed for radioactivity measurements using special nuclear measurement methods in a way that along with the substoichiometric extraction of a given metal the simultaneous quantitative separation of other metals can also be effected. Some general relationships have been derived for the substoichiometric multielement separation of MA _m -type metal chelates. Particularly, the primary dithizonates of silver and copper(II) have been studied, and the application of the method is demonstrated by the separation of silver and copper from cobalt.     

Substoichiometric determination of zinc with potassium ethyl xanthate

A rapid radiochemical method has been designed for the determination of microgram quantities of zinc, based on the substoichiometric isotope dilution, using potassium ethyl xanthate as the extraction reagent. pH 5.5 in acetate buffers and chloroform as the extractant were found to be suitable for quantitative substoichiometric extraction. The influence of the diverse ions on the extraction was studied. The zinc contents of a medicinal preparation and biological samples were determined by the present method.     

Solvent extraction of Os(IV) with 2-mercaptobenzothiazole into chloroform

2-mercaptobenzothiazole has been used for the solvent extraction of Os(IV) in acidic medium. The extraction of Os(IV) was found to be better than 90% over the pH range of 3.0 to 5.0 with an equilibration time of 5.0 minutes. The stoichiometry of metal:reagent determined by substoichiometric extraction and slope ratio method was found to be 1∶4. Decontamination factor for various elements in the substoichiometric extraction of Os(IV) were also evaluated.     

A new and rapid method for the solvent extraction of Ru/III/ with 1,2,3-benzotriazole into 1-pentanol

A new and rapid method has been developed for the quantitative extraction of Ru/III/ with 1,2,3-benzotriazole /1,2,3-BT/ into 1-pentanol. The extraction coefficient value of Ru/III/ between 1-pentanol and an aqueous 5% solution of 1,2,3-BT in 2M sodium acetate-acetic acid buffer showed a maximum value of E=46 at pH 4.5. The effect of various other parameters on the extraction coefficient of Ru/III/ such as solvents, anions, cations, etc. have also been studied. The stoichiometry of metal:reagent determined by the method of substoichiometric extraction and slope ratio method was found to be 13. Decontamination factors for many elements in the substoichiometric extraction of Ru/III/ were also evaluated.     

Determination of cobalt by substoichiometric extraction with β-hydroxy-naphthaldoxime

A substoichiometric radiochemical solventextraction method is described for the determination of cobalt, employing β-hydroxy-naphthaldoxime and chloroform as reagent and extractant, respectively. The extraction behaviour of the complex of cobalt with the reagent in the pH-range 8–9.5 and the effects of various metal ions on the extraction are critically studied. The method is used to determine the cobalt content in some pharmaceutical drugs. Received: 10 January 1997 / Revised: 11 March 1997 / Accepted: 25 March 1997     

The determination of zinc by substoichiometric isotope dilution

Recently, R??I?KA et al. proposed a determination of zinc in highly pure germanium dioxide by a substoichiometric extraction technique. In the present work, the effects on the substoichiometric extraction of equilibrium time, pH and interfering ions were investigated by radioactive tracer techniques and spectrophotometric measurements. The sensitivity of the procedure is limited by the blanks and the addition of oxalate ions can give rise to inaccurate results. The specific activity of ⁶⁵Zn was also determined by substoichiometric extraction.     

Solvent extraction of W(VI) with rhodamine-B in nitrobenzene

A rapid and selective method has been developed for the extraction of W(VI) with rhodamine-B in nitrobenzene. The extraction coefficient value for the extraction between aqueous solution and nitrobenzene showed a maximum value of E=63 at a pH of 5.0. The stoichiometry of metal to reagent has been determined by the method of substoichiometric extraction and slope ratio method.     

Determination of caesium microamounts by isotope dilution with substoichiometric separation

Selectivity of isotope dilution analysis with substoichiometric separation for caesium determination has been investigated. Caesium can be extracted with a substoichiometric amounts of bis 1,2-dicarbollylcobaltate in nitrobenzene in the presence of dibenzo-18-crown-6. The method is selective. Other metal ions (K⁺, Na⁺, Mg²⁺, Ca²⁺, Fe³⁺, Al³⁺) do not interfere.     

Redox substoichiometry in isotope dilution analysis

Isotope dilution analysis using the redox substoichiometric principle has been applied to the determination of antimony content in metallic zinc. As the substoichiometric reaction, the oxidation of trivalent to pentavalent antimony with potassium permanganate was used, followed by separation of these species by the BPHA extraction of trivalent antimony. Determination of antimony contents less than 0.5 μg was found to be possible with good accuracy, without separation of zinc ions. The antimony content in metallic zinc was determined to be 19.7±0.8 ppm, in good agreement with the results obtained by the other analytical methods.     

Solvent extraction of Au(III) using 2-mercaptobenzimidazole into n-butanol

A method has been developed for the extraction of Au(III) with 2-mercaptobenzimidazole into n-butanol.¹⁹⁹Au has been used as a tracer for establishing the ideal extraction parameters such as effect of pH, time of equilibration, solvents and anions. Separation factor and decontamination factor have also been evaluated to determine the selectivity of the method with respect to various elements. The interfering elements were suppressed by the use of suitable masking agents which increased the selectivity. The stoichiometry of metal to reagent was determined by the method of substoichiometric extraction and slope ratio method.     

Solvent extraction of Cu/II/ with 1,2,3-benzotriazole into chloroform

1,2,3-Benzotriazole/1,2,3-BT/ has been used for the extraction of Cu/II/ into chloroform. The effect of various parameters on the extraction coefficient of Cu/II/ was evaluated. The stoichiometry of metal:reagent, determined by the method of substoichiometric extraction and slope ratio was found to be 12. Separation factor for a number of elements in the extraction of Cu/II/ has been evaluated.