Possibilities of low-level determination of silicon in biological materials by activation analysis

The capabilities of neutron and photon activation analysis (NAA and PAA, respectively) for low-level determination of silicon in biological materials have been examined. Sensitivities of a variety of modes of NAA and PAA with radiochemical separation have been evaluated. Results are presented for silicon in reference materials CSRM 12–2-03 Lucerne, Bowen’s Kale, NIST SRM-1571 Orchard Leaves, and NIST SRM-1515 Apple Leaves. The results were obtained by employing the ²⁹Si(n,p)²⁹Al reaction with fast reactor neutrons and the radiochemical procedure developed for aluminium separation. Possibilities of further improvement of the silicon determination limit down to the μg g^–1 level by employing NAA and PAA with radiochemical separation are outlined.     

Determination of iodine in biological materials by neutron activation analysis

A method of determination of iodine (total and PBI) in serum, urine and other biological materials has been developed. The method consists in a gamma-spectrometric measurement of¹²⁸I activity after its radiochemical separation. The radiochemical separation procedure includes wet decomposition of the samples in a nitric acid medium followed by a few separation steps, the essential step being the substoichiometric extraction of iodide with a chloroform solution of tetraphenylarsonium chloride. Owing to the application of the substoichiometric separation, a high radiochemical purity of the separated iodine is achieved and the determination of the yield of radiochemical separation is not necessary.     

Possibilities of low-level determination of silicon in biological materials by activation analysis

The capabilities of neutron and photon activation analysis (NAA and PAA, respectively) for low-level determination of silicon in biological materials have been examined. Sensitivities of a variety of modes of NAA and PAA with radiochemical separation have been evaluated. Results are presented for silicon in reference materials CSRM 12-2-03 Lucerne, Bowen's Kale, NIST SRM-1571 Orchard Leaves, and NIST SRM-1515 Apple Leaves. The results were obtained by employing the 29Si(n,p)29Al reaction with fast reactor neutrons and the radiochemical procedure developed for aluminium separation. Possibilities of further improvement of the silicon determination limit down to the microg g(-1) level by employing NAA and PAA with radiochemical separation are outlined.     

Evolution and applications of radiochemical procedures: From Marie Curie to Darleane Hoffman

Marie Curie carried out the first radiochemical separations which eventually lead to the discovery of polonium and radium, two new elements. Nearly a century later Darleane Hoffman and her collaborators are devising new radiochemical separation procedures for studying the chemical properties of newly discovered transactinide elements. Safety requirements as well as changes necessitated by fast decaying radionuclides have transformed the nature of radiochemical separations. Further, applications in a wide variety of areas such as analysis of trace lements in food to radioimmunoassay have broadened the use of radiochemical separations. Examples of some early, historically important, radiochemical separations are described in this article. In addition, recent trends in the use of radiochemical separations in neutron activation analysis. in dating applications. in fission product studies and in the study of transactinide elements are briefly described with specific examples.     

Experimental Simulation on Separation of Alpha-Particle Induced Rhenium Isotopes from Bulk Tantalum

Trace level tantalum and rhenium, ¹⁸²Ta and ^186,188Re, have been separated with liquid anion exchanger, TOA from HNO₃ medium. The feasibility of the separation process has also been verified for the separation of trace level rhenium from bulk or macro quantity of tantalum. The developed radiochemical scheme will be useful for the separation of carrier-free rhenium radionuclides produced in -particle activated matrix target.     

Rapid determination of 90Sr/90Y in water samples by liquid scintillation and Cherenkov counting

Strontium-90 (⁹⁰Sr) is a ubiquitous contaminant at nuclear facilities, found at high concentrations in spent nuclear fuel and radioactive waste. Due to its long half-life and ability to be transported in groundwater, an accurate method for measuring ⁹⁰Sr in water samples is critical to the monitoring program of any nuclear facility. To address this need, a rapid procedure for sequential separation of Sr/Y was developed and tested in groundwater samples collected from an area of riverbed affected by a ⁹⁰Sr groundwater plume. Sixteen samples, plus spike and water blanks, were analyzed. Five different measurements were performed to determine the ⁹⁰Sr and yttrium-90 (⁹⁰Y) activities in the samples: direct triple-to-double-coincidence ratio (TDCR) Cherenkov counting of ⁹⁰Y, liquid scintillation (LS) counting for ⁹⁰Sr following radiochemical separation, LS counting for ⁹⁰Y following radiochemical separation, Cherenkov counting for ⁹⁰Y following radiochemical separation and LS counting of the Sr samples for ⁹⁰Y in-growth. The counting was done using a low-level Hidex 300SL TDCR counter. Each measurement method was compared for accuracy, sensitivity and efficiency. The results following Cherenkov counting and radiochemical separation were in very good agreement with one another.     

Radiochemical analysis of the polar agrochemicals validamycin and the metabolite melamine by ion-exchange chromatography

Suitable analytical methods to determine the radiochemical purity of validamycin and melamine are not described in the literature. High performance ion-exchange chromatography for the detection of underivatized validamycin and melamine has been proposed. The compounds were separated on HPLC using a styrene-divinylbenzene copolymer based cation-exchanger. For the separation of validamycin a resin in the hydrogen-form has given a good separation and for melamine in the Na⁺-form. For the first time an ion-exchange separation of validamycin is described allowing the separation of at least four components of commercial validamycin: validamycin A, validamycin B or G, validoxylamine A and validoxylamine B or G without prior derivatization. The methods were applied to determine the radiochemical purity of ¹⁴C- or ³H labeled compounds.This revised version was published online in November 2005 with corrections to the Cover Date.     

Polyurethane foam of the polyether type as a solid polymeric extractant for cobalt and iron from thiocyanate media

By combining instrumental and radiochemical neutron activation analysis, up to 47 elements including major, minor, and trace elements, have been determined in lake sediment samples. Instrumental neutron activation involving both short and long irradiations is used to determine 40 elements including most of the environmentally important ones. A radiochemical separation procedure allows the determination of 7 noble metals. The accuracy and precision of the method are 5–10%.     

Separation of carrier-free47Sc from titanium targets

The radiochemical separation of no-carrier-added (NCA)⁴⁷Sc from^natTi targets has been studied. Scandium-47, a medium-energy -emitter, is intended for use with labelled tumor associated monoclonal antibodies for radiotherapy. Several radiochemical methods for the separation of NCA⁴⁷Sc from macroquantities of titanium and other impurities were tested. Four different procedures based on ion exchange, solvent extraction and extraction chromatography are reported. For each method, parameters such as the distribution coefficient, kinetics and recoveries are reported. The selective separation can be performed rapidly by all methods.     

Cumulative yields of short-lived xenon isotopes in the spontaneous fission of252Cf

Cumulative yields of short-lived xenon isotopes^137,138,139Xe have been determined in the spontaneous fission of²⁵²Cf, using a fast radiochemical separation method followed by gamma spectrometry. Xenon-137 yield is reported for the first time. The measured cumulative yields are converted to chain yields assuming normal charge distribution systematics for comparision with the literature data.     

Ultratrace characterization of AlSiCu sputter targets for Th,U and 35 other elements by neutron activation analysis

Instrumental and radiochemical neutron activation analysis has been applied to a comprehensive trace characterization of AlSiCu sputter targets. By instrumental neutron activation analysis via long-lived indicator radionuclides, up to 33 elements were assayed with detection limits between 0.01 and 200 ng·g^–1. The high activity of⁶⁴Cu and²⁴Na produced from the matrix significantly limits the instrumental performance via short- and medium-lived indicator dionuclides. For this reason, a radiochemical separation was developed based on adsorption of²⁴Na on hydrated antimony pentoxide and extraction of⁶⁴Cu by diethylammonium diethyldithiocarbamate from HCl medium. By this radiochemical method, As, Ga, K, La, Mn, Mo, Re, Sb, U and W could be assayed via medium-lived radionuclides and the achievable limits of detection were between 0.1 and 25 ng·g^–1. Further improvement of detection limits for U and Th was achieved by a selective radiochemical separation of²³⁹Np and²³³Pa on a Dowex 1×8 column in HF and HF/NH₄F medium providing limits of detection for U and Th of 0.06 and 0.02 ng·g^–1, respectively. These techniques were applied to the analysis of two AlSiCu sputter target materials. Results are compared with those of glow discharge mass spectrometry.     

Determination of rhenium by neutron activation

A neutron activation method is proposed for the determination of rhenium in rocks and ores. After the irradiation, the radiochemical separation consists of a one-step anion exchange; β-activities of radiochemically pure ¹⁸⁸Re or ¹⁸⁶Re are counted. The chemical yield averaged 75% and there was a considerable saving of time in the radiochemical work. Results are quoted for the rhenium contents of the standard rock W-1, several molybdenites and pyrolusites.     

Rapid radiochemical separation in neutron activation analysis : Part 1. The use of C18-bonded silica gel and selective complexation for determinations of manganese,copper and zinc in biological materials

A rapid radiochemical separation method based on the removal of metal ions by columns of C₁₈-bonded silica gel after selective complexation by 8-quinolinol, ammonium pyrolidinedithiocarbamate or cupferron is described for the determination of manganese, copper and zinc in neutron-activated biological materials. The removal of the metal ions, either by adsorption or by a combination of filtration and adsorption on columns of C₁₈-bonded silica gel, was investigated to optimise the separation procedure. Analysis of several National Bureau of Standards and International Atomic Energy Agency biological reference materials demonstrated the effectiveness of this technique. The method is simple and reliable and readily adaptable in all radiochemical laboratories. Furthermore, columns of C₁₈-bonded silica gel have been successfully recycled a number of times without deterioration.     

Determination of arsenic,chromium, mercury,selenium and zinc in tropical marine fish by neutron activation

Determination of arsenic, chromium, mercury, selenium and zinc in several commonly consumed tropical marine fishes have been carried out by neutron activation followed by radiochemical separation to remove the interfering activities of sodium, potassium, bromine, and phosphorus, etc., in order to establish the baseline data and to measure the levels of contamination, if any. The results of this study positively indicate that the marine fishes of Bangladesh have concentrations much below the permissible levels for these toxic elements. A radiochemical scheme for the separation of seven trace elements in biological material is also presented in this paper.     

Multielemental determination in normal,benign, and cancerous tissues of the human brain

Although the metal content of the human body is only about 3%, metals are very important for human lives. Diseases occur when an excess or deficiency of in-vivo metals appear, when other metal pollutants enter the body, or when poisons or viruses enter into the metal ligand competition. Cancer is caused by carcinogens, which are substances capable of producing tumors in any test species at any dose level. This paper discusses the determination of some elements in diseased tissues of the human brain. As the elements present are mostly at micro- or nano-gram levels, the very sensitive technique of neutron activation analysis involving radiochemical separation has been employed. Substocihiometric estimations were carried out wherever possible. The radiochemical separation procedure includes a solvent extraction and precipitation technique. The elements estimated in the tissue samples are Cu, Au, As, Se, Hg, Co, Zn, Ca, Fe, P, Cr, Na, and K. The accuracy, precision, and radiochemical purity of the method have been discussed. Two samples and a standard can be analyzed in four days.     

The use of 4-nitro-o-phenylene diamine /4-NDP/ and sodium diethyldithiocarbamate /Na-DDTC/ in the radiochemical separation of Cd,Co, Cu,Se and Zn from different biological samples

In this work the use of the reagents 4-NDP and Na-DDTC in the radiochemical separation of Cd, Co, Cu, Se and Zn from a single aliquot of sample shortly after the end of irradiation in a flux of thermal neutrons is described. The performance of the proposed separation method was tested by means of analyses of these elements in a series of SRMs and good agreement with certified values was obtained.Dedicated to the memory of Prof. L. Kosta /1921–1986/.     

A radiochemical procedure for ultratrace determination of chromium in biological materials

Chromium is one of the most difficult elements to accurately determine at the naturally occuring, ultratrace levels normally found in uncontaminated biological samples. In view of the importance of Cr, both as an essential and as a toxic element, efforts have focused on developing a simple, yet reliable, radiochemical procedure for Cr determination using neutron activation analysis. A number of problem areas have been identified in earlier methods, and an improved radiochemical separation procedure, based upon the liquid/liquid extraction of Cr(VI) into a solution of tribenzylamine/chloroform, has been developed. The fast neutron interference from Fe has been evaluated for the highly thermal RT-4 facility of the NBS Research Reactor, and Cr concentrations have been determined in samples of whole human blood collected under clean conditions and in two certified reference materials.     

Radiochemical separation by inorganic ion exchanger and determination of cesium in complex matrices by thermal neutron activation analysis

A rapid and selective method has been developed for radiochemical separation, and determination of Cs in complex matrices by thermal neutron activation analysis. Batch adsorption of ¹³⁴Cs was carried out on zirconium phosphate ion exchanger. A large number of samples of the ore have been analysed for their Cs content and the results are discussed.     

Determination of rare earth elements by charged particle activation analysis in geological materials

The rare earth elements (REE), Pr, Sm, Eu, Gd, Ho, Er and Tm have been determined by charged particle activation analysis using 40 MeV a-particles through radiochemical approach. The radiochemical separation of REE as a group has been carried out from the bulk matrix. It has been shown from the theoretical computation that the products obtained from (a,xn) reactions (x = 1, 2, 3) are more suitable compared to those from (a,pyn) reactions (y = 0, 1, 2) due to the former having higher cross section (of the order of thousand millibarns).     

Low-level determination of silicon in biological materials using radiochemical neutron activation analysis

Summary A new radiochemical neutron activation analysis (RNAA) method has been developed for low-level determination of Si in biological materials, which is based on the ³⁰Si(n,γ)³¹Si nuclear reaction with thermal neutrons. The radiochemical separation consists of an alkaline-oxidative decomposition followed by distillation of SiF₄. Nuclear interferences, namely that of the ³¹P(n,p)³¹Si with fast neutrons, have been examined and found negligible only when irradiation is carried out in an extremely well-thermalized neutron spectrum, such as available at the NIST reactor. The RNAA procedure yields excellent radiochemical purity of the separated fractions, which allows the measurement of the β^--activity of the ³¹Si by liquid scintillation counting. Results for several reference materials, namely Bowen’s Kale, Bovine Liver (NIST SRM 1577b), Non-Fat Milk Powder (NIST SRM 1549) and several intercomparison samples, Pork Liver-1, Pork Liver-2 and Cellulose Avicel, are presented and compared with literature values.