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- Author or Editor: S. Narayanan x
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Abstract
The extraction equilibria of Co(II) and Zn(II) complexes with 4-benzoyl-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-one in the presence of tributyl phosphate have been investigated in eight ‘inert’ solvents employing the radioisotopes cobalt-60 and zinc-65. The activity coefficients of different species in the organic phase and the solubility parameter of the adduct have been calculated with the help of regular solution theory. A regularity is observed in the correlation between the adduct formation constant and the activity coefficient of the species.
Abstract
Thorium was extracted at pH 5.0 from 0.01 M malonic acid on a column of silica gel coated with Amberlite LA-1. Thorium was separated from alkali and alkaline earths, managenese, iron, cobalt, nickel, zinc, tin, in binary mixtures by taking advantage of the difference in the pH of formation of malonato complexes. Thorium was separated from zirconium, uranium, scandium, molybdenum, titanium, by exploiting the difference in the stability of malonato complexes. The method was extended for the analysis of thorium in monazite.
Abstract
A method has been proposed for the determination of hydrogen sulphide and sulphur dioxide in a mixture. The method is based upon the quantitative oxidation of sulphide and sulphite with an excess of radiochloramine-T in alkaline medium /0.1N NaOH/. The released chloride activity is proportional to the total amount of sulphide and sulphite present. Addition of 1% CdSO4 solution to the mixture of sulphide and sulphite precipitates sulphide, and sulphite in the filtrate determined by the reagent. From the difference in activities, the amount of sulphide can be calculated. This method can be employed for the determination of hydrogen sulphide and sulphur dioxide in air samples.
Abstract
The distribution ciefficients of 4-benzoyl-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-one (BMPP) and its metal chelates with Co(II). Zn(II) and Eu(III) were determined between an aqueous acetate phase (μ=0.1) and eight ‘inert’ organic solvents at 25°C. On the basis of regular solution theory, the correlation between the distribution coefficients of the ligand (PHA) and that of the metal chelate (PM) vas found to be valid satisfactorily in most of the systems. The correlation between the distribution coefficient of the ligand and the solubility parameter of the solvent has been found to conform to regular solution theory.
Abstract
Determination of milligram amounts of monoethanolamine with zinc/II/ by radiometric titration is described.
Abstract
Hydrogen sulphide at trace level can be determined by radiorelease technique using radiochloramine-T. The minimum detection level is 0.25 ppm. Zinc acetate is used to fix H2S from air samples. CS2 does not interfere. Interference by SO2 can be eliminated by oxidizing it with H2O2.
Abstract
Carbon disulphide can be determined at ppm level by converting it into xanthate and then oxidizing it by radiochloramine-T in acid medium. Interference of sulphide, sulphite and nitrite can be eliminated by extracting CS2 from the mixture into carbon tetrachloride and stripping it into aqueous medium as xanthate by the addition of alcoholic KOH to the organic layer.
Abstract
Radiometric titraction of diethanolamine with65ZnSO4 is reported. Determination of individual amounts of mono- and diethanolamines in a mixture is described.
Abstract
The characterized concentrations of 24 impurity elements in New Brunswick Laboratory (NBL) Certified Reference Material (CRM) 124 were reevaluated. A provisional certificate of analysis was issued in September 1983 based upon the “as prepared” values (gravimetric mixing). The provisional certificate does not state uncertainties for the characterized values, or estimate the degree of homogeneity. Since release of the provisional certificate of analysis various laboratories have reported analytical results for CRM 124. Based upon the reported data a re-evaluation of the characterized values with an estimate of their uncertainties was performed in this work. An assessment of the degree of homogeneity was included. The overall difference between the re-evaluated values for the 24 impurity elements and the “as prepared” values from the provisional certificate of analysis is negligible compared to the uncertainties. Therefore, NBL will establish the “as prepared” values as the certified values and use the derived uncertainties from this work for the uncertainties of the certified values. The traceability of the “as prepared” values was established by the gravimetric mixing procedure employed during the preparation of the CRM. NBL further recommends a minimum sample size of 1 g of the CRM material to ensure homogeneity. Samples should be dried by heating up to 110 °C for one hour before use.
Abstract
The International Organization for Standardization (ISO) Guide to the expression of Uncertainty in Measurement (GUM) was developed to meet the demand for a standardized way of evaluating and expressing uncertainties. The Davies and Gray (D&G) titrimetry method is routinely used in nuclear safeguards for uranium accountability measurement and a statement of the uncertainty that can reasonably be attributed to the measured assay value is therefore of importance. A mathematical model for an uncertainty evaluation of D&G measurements in compliance with ISO GUM is presented. This is illustrated by a numerical example and the utilization of the uncertainty budget is explored.
