Instrumental neutron activation analysis of monomineral fractions of sulfide minerals and quartzes

A method has been worked out of multi-elemental instrumental neutron-activation analysis INAA of small weights some mg of monomineral fractions of sulfide minerals pyrites, galenites, chalcopyrites, arsenopyrites, bornites, chalcosines and quartzes. The samples were irradiated in a nuclear reactor under a flux of 1.3·10¹³ n·cm⁻²·s⁻¹. For measuring the gamma radiation of the exposed samples Ge(Li) gamma-spectrometers with semiconductor detectors were used. Determined in sulfide monofractions were the elements: Co, Sc, Ag, Se, Sb, Cr, Fe, Zr; rare-earth elements: Ce, Sm, Eu and others at content levels of 10⁻¹−10⁻⁴%. In quartzes they were: Mn, Na, Sb, Cr, Sc, Fe, Co at content levels of 10⁻⁵−10⁻⁷% and Au to n×10⁻⁹%. A special method has been worked out for the determination of In in sulfides with the irradiation of samples in a cadmium screen. An example is cited of using the method for studying some peculiar features of the genetics of copper pyrite deposits. The data on the distribution of admixture elements in sulfide monofractions produced in this work made it possible to conclude that the oreformation in the deposits has a stage-by-stage character.     

Instrumental neutron absorption activation analysis

We present and discuss a modification of instrumental neutron activation analysis (INAA) that is sensitive for nuclides that do not yield (suitable) activation products but have high cross sections for neutron absorption. Their presence in a sample may thwart INAA by neutron flux suppression inside the sample, but they remain undetected and thus unnoticed by the analyst. In particular, this refers to Li, B, Cd and Gd. The proposed method—instrumental neutron absorption activation analysis (INAAA)—takes advantage of the flux depression inside the sample caused by the neutron absorbers. It is made visible by addition of an activatable nuclide (indicator). The concentration of the neutron absorber (analyte) causes a decrease in activity of the indicator. The activity difference between a mixed sample (sample plus indicator) and the pure indicator carries the analytical information. The calibration curve hence follows a reciprocal exponential function. In a proof-of-principle experiment, the applicability for the quantification of boron was exemplified. In presence of only one neutron absorber (whose nature is known), INAAA can be applied easily for quantification of the analyte in powdered or liquid samples. Although INAAA is no trace sensitive method, it has the potential to increase the reliability of INAA analyses by fast and straightforward quality control (even in presence of two or more neutron absorbing nuclides). It is especially suited for research reactors that do not operate a prompt gamma neutron activation analysis (PGNAA) station.     

Instrumental neutron activation analysis of iron and zinc in compact cosmetic products

Summary An instrumental neutron activation analysis method is described for the determination of iron and zinc in compact eye shadow, compact face powder and compact rouge make-up cosmetic products. The steps of the procedure are: irradiation of samples with thermal neutrons, counting of gamma-radioactivity of the radioisotopes of iron and zinc produced by this irradiation and calculation of the concentration of these elements from the gamma-ray spectra of samples and standards. Analysis of the I.A.E.A. standard reference material by this procedure give results in close agreement with certified values. The limit of quantitation is 45 g for iron and 0.35 g for zinc. The developed procedure could possibly be established as an official method for the simultaneous determination of iron and zinc in compact cosmetic products.

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Instrumentelle Neutronenaktivierungsanalyse von Eisen und Zink in festen kosmetischen Erzeugnissen

Zusammenfassung Ein neutronenaktivierungsanalytisches Verfahren wird beschrieben zur Bestimmung von Eisen und Zink in festen kosmetischen Erzeugnissen (Eye shadow, Gesichtspuder, Rouge Make-up). Die Methode umfaßt die Bestrahlung der Probe mit thermischen Neutronen, Messung der Gammaradioaktivität der erzeugten Radioisotope von Fe und Zn, sowie Berechnung der Konzentrationen aus den Gammaspektren von Probe und Standard. Bei der Analyse von Standardreferenzmaterial wurde gute Übereinstimmung mit den zertifizierten Werten erhalten. Die Bestimmungsgrenzen liegen bei 45 g Fe bzw. 0,35 g Zn. Das Verfahren wird als offizielle Methode zur gleichzeitigen Eisen- und Zinkbestimmung in diesen Erzeugnissen empfohlen.

     

Instrumental neutron activation analysis of some ancient punchmark coins from India

A nondestructive instrumental neutron activation analysis technique is applied for the analysis of precious ancient punchmark coins. Coins ranging between 8th century B.C. to 2nd century B.C. were irradiated with thermal neutrons in a²⁵²Cf neutron source facility and analyzed by comparator method of instrumental neutron activation analysis, using high purity germanium detector coupled to a multichannel analyzer, the activities being measured at photopeak energies of the corresponding radioisotopes. It is observed that punchmark coins are mainly of two types: copper or silver based. Other elements present in varying proportions are gold, arsenic and antimony.     

Instrumental neutron activation analysis of manganese in some industrially important steel samples

The manganese content of some industrially important steel samples viz. IS-226, spring steel, galvanized iron, high tensile steel, and mild steel is determined by instrumental neutron-activation analysis using a²⁵²Cf neutron source. The analysis is performed by measuring the activity of⁵⁶Mn after /n, / reaction on a 4 k multichannel analyzer coupled to a NaI/Tl/ detector at 847 keV, as well as on a single channel analyzer on integration mode coupled to a NaI/Tl/ detector. The results obtained by both procedures show reasonably good agreement with each other.     

Instrumental neutron activation analysis of urinary calculi

Five kinds of urinary stones from 42 patients have been determined for a total of 19 elements by instrumental neutron activation analysis. Of these elements, Ca, Mg, Sr, Na, and Cl are found to be present in the core of all kinds of stones. The differences in elemental composition among the different kinds of stones as well as across the layers of stone are statistically evaluated.     

Instrumental neutron activation analysis of brewer's yeast

Instrumental neutron activation was used for the determination of 23 trace and minor elements in 4 different samples of brewer's yeast. Detection limits for these elements vary from 2 ppb to 100 ppm. The following average concentrations were found (ppm, dry weight): Al 597, Br 0.36, Cl 1473, Co 0.21, Cu 19, Fe 285, K 16 400, Mg 1355, Mn 8.4, Na 2330, Rb 19, Sb 0.053, Se 1.2, V 2.2 and Zn 80. NBS standard 1569 was also analyzed and the following concentrations (in ppm) were measured: Al 2300, Br 0.65, Ce 0.23, Cl 460, Co 0.26, Cr 2.12, Cu 11, Fe 707, Gd 7.1, Hf 0.13, K 15 500, Mg 1780, Mn 7, Na 510, Rb 16, Sb 0.075, Sc 0.18, Se 0.92, Th 3.7, Ti 38, U 0.49, V 4.1 and Zn 70.     

Instrumental neutron activation analysis of gunpowder residues

A procedure has been developed for the detection of gunpowder residues deposited on the hand of a person firing a gun. The method is based on neutron activation analysis of the antimony level on the surface of the hand. The surface materials are removed by a film made by spraying a 4% solution of cellulose acetate in acetone, which sets to form a thin film that can readily be stripped off. This technique was found to be preferable to the paraffin-lift technique which is in common use. Following neutron activation of the film in a nuclear reactor, antimony is assayed by high-resolution Ge(Li) spectrometry without prior chemical processing. The sensitivity of the method is about 5·10⁻⁹ g Sb, with a precision of about ±10% at a neutron flux of 5·10¹³ n·cm⁻²·sec⁻¹. Analysis of twenty samples taken from the hands of persons who had fired a pistol gave Sb levels of 0.4±0.2 μg, compared with 0.024±0.013 μg found on the hands of persons who had not fired a revolver. The possible extension of the present technique to include the determination of additional elements is discussed. Project carried out with the support of the Office of the Chief Scientist to the Ministry of Defense and with the collaboration of the Israel Police.     

Instrumental neutron activation analysis of blood serum

Instrumental neutron activation analysis has been used to determine 15 trace elements in twelve blood serum samples taken from healthy students at Bilkent University in Ankara. The method allowed the determination of Sc, Cr, Mn, Fe, Co, Zn, Se, Rb, Cs, Ce, Eu, Tb, Hf, Ta and Hg, which occur at the g.ml^–1 to ng.ml^–1 levels. There are no values reported for Tb, Hf, Ce, Eu and Ta before. The other results are compared with the values reported in the literature. Most are in the range of the reported values except for Fe, Zn, Se and Cs.     

Instrumental thermal neutron activation analysis of tobacco

A group of 27 tobacco samples was submitted to INAA. Bowen's Kale was analyzed with the samples. The resulting data for 21 elements in tobacco were processed by a cluster programme. This combination proves to be a convenient tool for discrimination within one group of samples.     

Instrumental neutron activation analysis of Obsidian rock

An instrumental neutron activation analysis technique has been developed for the simultaneous determination of up to 30 elements including major, minor and trace elements in Obsidian Rock (a proposed NBS-SRM-278). INAA method involves both short and long irradiations followed by gamma-ray activity measurement with a Ge(Li) detector. The accuracy of the procedure has been checked by analyzing IAEA Reference Materials.     

Instrumental neutron activation analysis of wheat bunt spores

The concentrations of seventeen elements in two species of fungus which cause wheat bunt disease,Tilletia caries (DC.) Tul. andTilletia controversa Kühn, were determined by instrumental neutron activation analysis. Differences in the K and Cl concentrations between these two species of spores are large and therefore can be used as a criterion for distinguishing between the two species of fungus.     

Instrumental neutron activation analysis of fly ashes and emissions

Instrumental neutron activation analysis (INAA) has been utilized for the analysis of 19 different fly ashes, 1 sample of coal and 3 samples of industrial emissions. Both short and long irradiations in a nuclear reactor have been used. The irradiated samples have been measured by means of a computer-based Ge(Li) gamma-ray spectrometer. The concentrations of 27 elements have been determined in the samples.     

Instrumental neutron activation analysis of semiconductor grade silicon

The single comparator method in neutron activation analysis has been applied to the investigation of the purity of silicon single-crystals of different origins. The following impurities were determined: Au, Sb, Co, Cu and Na. Studies were also carried out on the surface contamination of silicon samples introduced through steps of sample preparation and irradiation. Up to nineteen elements on the surface of samples were analysed and found to be easily reduced to low levels or detection limits by washing and etching.     

Instrumental neutron activation analysis of air filter samples

Résumé La mesure de traces d'éléments dans l'air ambiant a fait l'objet d'une attention accrue ces derniers mois, en raison d'un intérêt grandissant pour les dangers en puissance pour la santé, qui résultent de l'exposition prolongée à certaines substances toxiques. L'analyse par activation neutronique a été employée avec succès dans la recherche de traces d'éléments, et ce, pour un grand nombre d'études de l'environnement; elle semble convenir de fa?on idéale pour la détermination non-destructive multi-élémentaire de la composition de milieux de particules portées par l'air. Dans cet article, on rend compte des performances de l'analyse instrumentale par activation neutronique comme on le montre dans le cas de 40 échantillons d'air filtrées provenant d'une zone métropolitaine.      

Instrumental neutron activation analysis of spruce needles and trees

Tree rings and needles of young spruce clones from the immission area of the Al-refinery Ranshofen (Upper Austria), which had ceased production in 1992, were investigated by INAA. Short time irradiation was performed for determining, Al, Mn, Ca and Cl, while the elements Na, K, Rb, Ba, Zn, Fe, Sc, Cr, Co, Br and in some samples also Ca were determined via middle- and long-lived radioisotopes. Irradiation and counting conditions are given. Accuracy and sensitivity are sufficient to describe the trends of the element concentrations in needles and with the exception of Cr, Sc and Br, in tree rings. Ca-concentrations derived from⁴⁹Ca (short-time irradiation) and⁴⁷Ca (long-time irradiation) are compared and show good agreement Additionally Mg was determined in some samples by ICP-AES and if possble, by INAA. The results are compared.     

Instrumental neutron activation analysis of sewage sludge and compost

Instrumental neutron activation analysis has been applied for the analysis of four sewage sludges of municpal water treatment plants, one sludge of an industrial water treatment plant one compost of a municipal compostation plant in Belgium. This pilot study showed that concentrations for 41 elements could be obtained. Tests for homogeneity and accuracy indicated the necessity of a thorough grinding and homogenization of the samples before analysis. The concentrations obtained were compared with the mean soil composition and the possible enrichment of heavy metals in the soil calculated when the materials are used as a manure to agricultural land. The Zn concentration is mostly the limiting factor for the agricultural application.     

Instrumental neutron activation analysis of phosphorus in rocks

The possibilities are discussed of the instrumental activation analysis of phosphorus in rocks by the reaction³¹P(n, γ)³²P (T=14.2 d). Results are given for six standard rocks of the U.S. Geological Survey.     

Instrumental neutron activation analysis technique using subsecond radionuclides

The fast irradiation facility Mach-1 installed at the Danish DR 3 reactor has been used in boron determinations by means of Instrumental Neutron Activation Analysis using¹²B with 20-ms half-life. The performance characteristics of the system are presented and boron determinations of NBS standard reference materials as well as fertilizer materials are compared by literature value and spectrophotometric measurements, respectively. In both cases good agreement is obtained.     

Instrumental neutron activation analysis for the elemental analysis of cement

Cement is widely used as a construction material in Libya. Production plants introduce certain contaminants to the environment. The dust from such plants is carried away to neighbouring areas. This dust contains a substantial amount of contaminants depending on the origin of clays used in the production. In this study, a survey of elemental concentration of clay and cement was carried out to assess the environmental impact of such plants, especially those that are situated near residential and agricultural areas. Cement and clay samples, imported and locally produced, were analyzed. Instrumental neutron activation analysis was utilized to determine the elemental concentration of As, Ca, Ce, Co, Cr, Eu, Fe, Hf, La, Na, Rb, Sb, Sc, Sm, Ta, Th, U, Yb and Zn. Elevated concentrations of U and Th were found in a number of cement samples. The two nuclides are part of an elaborate decay scheme producing a range of radioactive elements, which emit alpha-, beta- and gamma-radiation. With ⁴⁰K, they could give elevated levels of background radiation in buildings resulting in higher exposure doses. This could pose a health hazard and a detrimental effect on the well being of residents, especially in poor ventillated buildings. Also, cement is the main component for constructing underground reservoirs for collecting rainwater for drinking in private residences, so some harmful elements could leach into water. This is the first comprehensive survey of commercial cement brands and clays used in Libya. These results are intended to build a database for trace element concentrations using INAA.