Neutron activation analysis has become one of the most sensitive and selective analytical technique for the determination of trace elements in a wide variety of matrices. Neutron activation involves the irradiation of the test sample and a standard of the element to be determined with thermal neutrons in a reactor, followed by dissolution of the test sample in the presence of carrier of the element to be determined. The carrier and radioisotopes are separated from the bulk of other induced activities (employing precipitation, solvent extraction, ion exchange etc.) and then the activity induced in the sample is measured on a suitable detector. The standard is treated identically. From the ratios of the activity of the sample and standard and the weight of the standard irradiated, the concentration of element in the test sample is calculated. A rapid, selective and sensitive method of radiochemical separation is subtoichiometric extraction in which the same amount of carrier is added to the irradiated test sample and standard. Exactly the same amount of reagent is added to both the sample and standard but in substoichiometric amounts, followed by the separation of the species formed by extracting it with an organic solvent. The activities of the extracts are measured. The amount of element present in the sample is calculated with help of the ratio of the activities and the weight of the standard taken. The advantages of the method are discussed. Application of substoichiometry in neutron activation has been elucidated with reference to the determination of Au in various samples by substoichiometric neutron activation analysis.
Liver tissues from rat have been analyzed for determining trace amounts of manganese present by employing thermal neutron activation analysis and substoichiometric solvent extraction of Mn/II/ with 1,2,3-benzotriazole into 1-octanol. Three samples and a standard can be processed and counted within three hours.
The reagent 2-mercaptobenzothiazole /2-HMBT/ has been used for the solvent extraction of Ru/III/. The extraction coefficient value of Ru/III/ has been evaluated, based on various parameters such as, effect of molarity of the acid, time of equilibration, time of heating, effect of various solvents and effect of various salts. The stoichiometry of the metal to reagent was determined by the method of substoichiometric extraction of slope-ratio method and was found to be 13. Separation factor and decontamination factor for various elements have also been studied.
A procedure is described for the determination of thallium in complex biological matrices by thermal neutron activation analysis employing substoichiometric extraction of thallium(I) with 2-mercaptobenzothiazole (2-HMBT) at a pH of 7.5 into chloroform, and low-level beta-counting.
The method described here involves the irradiation of biological samples and a g quantity of standard with thermal neutrons at the self-serve position in the CIRUS reactor, followed by dissolution of the sample and standard in the presence of milligram amounts of carrier. Both the sample and the standard are subjected to substoichiometric extraction under controlled experimental conditions with ethyl thioacetoacetate into chloroform. An aliquot of the organic phase is counted on a -spectrometer. The concentration of Hg in various biological samples and the accuracy, precision, and sensitivity of the method are discussed.
A method has been described for the determination of trace amounts of copper in biological samples by thermal neutron activation analysis, involving radiochemical separation of copper from irradiated matrix employing substoichiometric extraction of Cu/II/ with 2-mercaptobenzothiazole /2-HMBT/ into chloroform. 4.01 g of Cu/II/ can be determined with an accuracy of 3.13% and precision of 1.08%.
A rapid and simple method has been developed for the determination of Mn, Zn, Cr and Ag by radiochemical thermal neutron activation analysis, involving solvent extraction and precipitation technique. Mn, Zn, Cr and Ag can be determined with an accuracy of 8.9, 5.8, 7.7 and 7.6%, respectively. The method has been employed for determination of the elements in fish solubles. Two samples and a standard can be analyzed in three hours.
A rapid method for the solvent extraction of Hg(II) into chloroform has been developed, employing thioethylacetoacetate (HETAcAc) as a extracting agent. The extraction of Hg(II) was better than 99% over the pH range 0.3 to 7.3. The extraction equilibrium was reached within 2 min. The effect of various parameters such as anions and cations, solvent effect, etc., on the extraction coefficient has been studied. The stoichiometry metal: reagent was determined by the method of substoichiometric extraction and was found to be 14.
A radiochemical separation method has been developed for the separation of platinum, gold and palladium from various matrices by thermal neutron activation analysis and employing substoichiometric extractions of Pt and Au with 2-mercaptobenzothiazole and Pd with isonitrosobenzoylacetone. Decontamination factors for the individual elements after separation was also studied and was found to be greater than 105 for most of the elements.