NAA and ICP analysis of obsidian from Central Europe and the Aegean: Source characterisation and provenance determination

INAA and ICPES are compared for their discriminative power in obsidian source characterisation. Geological samples from the Aegean and Carpathian sources were analysed for Na, Sc, Fe, Co, Rb, Sb, Cs, Ba, La, Ce, Sm, Eu, Tb, Yb, Lu, Hf, Ta, Th, U by INAA and for B, Na, Mg, Al, K, Ca, Sc, Ti, Mn, Fe, Zn, Y, Yr, Cs, Ba, La, Ce, Sm, Eu, Gd, Tb, Yb, Lu, Hf by two ICPES procedures. It is shown that all techniques work successfully, however, INAA is more efficient in the chemical discrimination of neighbouring sources.     

Feasibility of instrumental neutron activation analysis for trace element studies in natural soils

Fifty natural surface soils with strongly variable organic matter content and elemental composition were investigated to see to what extent INAA would prove useful for multi-element surveys. A conventional scheme of irradiations and decay intervals was used and 35 elements were investigated. Detection limits of the various trace elements were studied with respect to the influence of elements giving rise to major radionuclides in activated samples. For the 18 elements Na, Al, K, Sc, Cr, Mn, Fe, Co, Zn, Br, Sb, Cs, Ba, La, Sm, Hf, Th, the performance of INAA was very good. Useful results were also obtained for V, As, Se, Rb, Sr, I, Ta, and Au, while the technique appeared marginal for Cl, Zr, Mo, Ag, and Hg, and unsatisfactory for Mg, Ti, Ni, and Cd.     

Determination of trace element levels in polyethylene by instrumental neutron activation analysis

Elements Al, As, Au, Br, Cl, Co, Cr, Cu, Fe, Hg, K, La, Mn, Mo, Na, Sb, Sc, Sm, V, and Zn were determined by INAA in several brands and batches of high pressure polyethylene (PE) Bralen (Slovnaft Bratislava, Czechoslovakia). A large scatter of trace element contents was found in both granules and foils, indicating an inhomogeneous distribution for the majority of the above mentioned elements present as impurities in PE. Larger amounts of the elements Al, Mn, and Sb were found in foils than in granules. Blank values resulting from using of PE Bralen as a canning material for INAA were compared to trace element concentration in human hair samples, too.     

Determination of elemental levels in radiopharmaceuticals by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) was applied to thedetermination of the concentration levels of Na, Mg, Al, Cl, K, Sc, Ti, V,Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Zr, Mo, Ag, Cd, Sb, I, Cs,Ba, La, Ce, Nd, Sm, Eu, Tb, Dy, Yb, Lu, Hf, Ta, Hg, Th and U in three radiopharmaceuticals.The irradiation of the samples was carried out in a 0.5 kW Bariloche RA-6Research Nuclear Reactor and the induced gamma-activity was measured by gamma-spectrometry.INAA proves to be an accurate and precise technique to obtain a quick informationon the concentration levels of several minor and trace components in radiopharmaceuticals.The quantification of heavy toxic elements is required for the registrationof radiopharmaceuticals.     

Elemental analysis of phosphate rocks: For sustainable agriculture in Pakistan

The concentration of 32 elements was determined in phosphate rock samples from the Hazara phosphate deposits of Pakistan using instrumental neutron activation analysis (INAA) technique employing different irradiation protocols. These included 23 major, minor and trace elements (Al, As, Ba, Br, Co, Cr, Cs, Fe, Ga, Hf, K, Mn, Na, Rb, Sb, Sc, Sn, Ta, Th, U, V, Zn and Zr) and 9 rare earth elements (REEs) namely Ce, Eu, Ho, La, Lu, Nd, Sm, Tb and Yb. The results have been compared with the global values of these elements. The concentrations for most of the elements studied are lower than the concentrations reported in the literature whereas the concentrations of As, Co, Fe, K, Mn, Na and Sb are comparable. Two samples namely HR-4 and HR-5 have the highest concentrations for majority of the REFs with high enrichment factors. The quality assurance of data was performed through the concurrent use of Lake Sediment (SL-1) and GSJ-JR-1 (Rhyolite) reference materials. The acquired data will serve as a reference for the follow-up studies to assess the agronomic effectiveness of the Hazara phosphate rocks.     

Natural radioactivity in Brazilian bottled mineral waters and consequent doses

Instrumental neutron activation analysis (INAA) has been applied tomultielement determination of five medicinal plants which are used to curevarious diseases in Ghana. These are: Sirappac powder-E, Tina-A powder, Aphrodisiacpowder, Blighia powder and Olax powder. Concentrations of fifteen elementsAl, Ba, Br, Ca, Cl, Co, K, Mn, Mg, Na, Rb, Sb, Sc, Se, Ta, V and Zn have beendetermined by short, medium, and long irradiation times with a thermal neutronflux of 5 . 10 11 n . cm –2. s –1 . Of these Co, Sb, and Sc arefound to be present at trace level, Br, Mn, Rb, Ta, V and Zn at the minorlevel and Al, Ca, Cl, K, Mg, and Na are generally at the major level. StandardReference Material NIST SRM-1571(Orchard Leaf) was analysed simultaneouslywith the samples. The precision and accuracy of the method was evaluated usingreal samples and the standard reference material. It was found out that theelemental concentrations measured in the NIST SRM-1571 are within ±10%of the reported values.     

Determination of elements in SRM soil 2709a by neutron activation analysis

A combination of instrumental neutron activation analysis (INAA) and prompt gamma-ray activation analysis (PGAA) was used to value assign 35 elements in SRM soil 2709a (San Joaquin Soil). INAA with counting of short-lived radioisotopes was used for determination of Al, Au, Ca, Dy, K, Mg, Mn, Na, Ti, and V. Elements determined by INAA with counting of intermediate and long-lived radioisotopes included As, Ba, Ce, Co, Cr, Cs, Eu, Fe, Hf, La, Lu, Nd, Rb, Sb, Sc, Sm, Sr, Ta, Tb, Yb, Zn, and Zr. Thermal neutron PGAA was used for the determination of H, B, Si, K, Ti, Mn, Fe, Cd and Gd. Expanded uncertainties were determined for all values reported.     

Accelerated denitration by formic acid accompanied with residual acid-electrolytic trimming

The fruit bodies of wild-growing higher fungi (macromycetes), commonly called mushrooms, of various genera and species collected in localities with different geochemical features and man-made burden in the Czech Republic were analyzed by different modes of activation analysis. The elements Na, Mg, Al, S, Cl, K, Ti, V, Mn, Cu, Br, Ba and Dy were determined by short-term instrumental neutron activation analysis (INAA). Short-term epithermal INAA (ENAA) was used for determination of I and other elements, such as Rb, Ag, and U. The elements Na, K, Sc, Cr, Fe, Co, Cu, Zn, As, Se, Br, Rb, Ag, Cd, Sb, Cs, Ba, La, Ce, Sm, Eu, Hf, Au, Hg and Th were determined by long-term INAA, whereas long-term ENAA enabled determination of several other elements, such as Ni, Ta, W and U. The analytical possibilities of instrumental photon activation analysis (IPAA) using a microtron were also explored and found useful for determination of several additional elements, namely Sr, Y, Zr, Nb, and Pb. High concentrations of several essential and toxic trace elements found (up to hundreds of mg^.g^-1, dry mass) should be of concern in nutritional studies, because mushrooms form non-negligible part of diet in many countries, especially in Middle and East Europe.     

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.     

Determination of some trace elements in natural and fertilised Libyan soils using INAA and ED-XRF

Samples of natural and fertilised soils were collected from Al-Gheran region, west of Tripoli, Libya. The samples were investigated by means of INAA and ED-XRF for Al, Si, K, Ca, Sc, Cr, Mn, Fe, Co, Zn, Br, Rb, Sr, Y, Zr, Nb, Cs, Ba, Hf, Ta, Pb and Th. The results indicate that the concentrations of K, Ca, Zn, Sr and Pb are 2–4 fold higher in fertilised compared to natural soil, while the concentrations of Al, Si, Cr, Mn, Fe, Co, Rb, Y, Nb, Cs, Ba Ta and Th are nearly the same in all samples. Mn and Fe values in two arable soils have been found to be 4–6 times lower than the average concentration in the earth's surface soils. This study concludes that, although the levels of some trace elements important for human health are very low in both natural and fertilised soils. Further research is needed to understand the full significance of the distribution transfer and toxicity of trace elements introduced in imported fertilisers.     

Instrumental neutron activation analysis of pottery for provenience study

A scheme for INAA of pottery is proposed. The combination of 3 irradiations-epithermal and pile (short and long time) and 6 measurements (2 times after each irradiation) enables the determination of Al, As, Au, Ba, Br, Ce, Co, Cr, Cs, Dy, Eu, Fe, Hf, K, La, Lu, Mg, Mn, Na, Nd, Rb, Sb, Sc, Si, Sm, Ta, Tb, Th, Ti, U, V and Yb. The accuracy and precision of the method is evaluated by analysis of standard reference materials (USGS-BCR-1, USGS-W-1, ZGI-TB). The applicability of the method is demonstrated by analysis of 15 sgraffito ceramics from XV–XVIII cc. from Tzarevetz, Veliko Tirnovo (Bulgaria). The results from the clustering of the analytical data are presented and discussed.     

Determination of 21 elements by INAA for certification of SRM 1570a,Spinach

Analyses for certification have been made by instrumental neutron activation analysis (INAA) for the determination of 21 elements in the National Institute of Standards and Technology (NIST) Spinach renewal reference material, SRM 1570a. Elements determined included ones with short halflife products (Al, V, Ca, Mg), intermediate halflife products (Mn, Na, K, La), and long halflife products (Ba, Co, Cr, Cs, Eu, Fe, Rb, Sb, Sc, Se, Sr, Th, and Zn). For the first time a new robotic sample changer was used in the counting of long halflife indicator isotopes for certification of an SRM. Uncertainties obtained averaged±1.80% for the four major and minor constituents (Ca, K, Mg, Na); ±3.14% for elements with concentrations from 1 to 400 mg/kg (Al, Ba, Cr, Fe, Mn, Rb, Sr, and Zn); and±8.31% for the ultra trace elements (<1 mg/kg) (Co, Cs, Eu, La, Sb, Sc, Se, Th, and V).     

Determination of trace elements in atmospheric wet precipitation by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) methods have been developed for the simultaneous determination of multielement concentrations in both particulate and soluble fractions of atmospheric wet precipitation (AWP). Samples of AWP collected across Canada by Canadian Network for Sampling Precipitation (CANSAP) have been analyzed. The INAA method involves four sequential irradiations and counting after five different decay periods for measuring Ag, Al, As, Au, Ba, Br, Ca, Ce, Cl, Co, Cr, Cu, Dy, Fe, Hf, Hg, I, K, La, Mg, Mn, Na, Rb, Sb, Sc, Se, Sm, Sr, Ti V and Zn. Precision and accuracy of the INAA methods have been evaluated, and detection limits have been calculated.     

Determination of trace elements in Egyptian cane sugar (Deshna Factories) by neutron activation,atomic absorption spectrophotometric and inductively coupled plasma-atomic emission spectrometric analysis

Multielemental instrumental neutron activation (INAA), inductively coupled plasmaatomic emission spectrometric (ICP-AES) and atomic absorption spectrophotometric (AAS) analyses are utilized for the determination of Ag, Al, As, Au, Ba, Be, Br, Ca, Cd, Ce, Cl, Co, Cr, Cu, Eu, Fe, Ga, Hf, K, La, Li, Lu, Mg, Mn, Na, Nb, Ni, P. Pb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Th, Ti, U, V, W and Zn in sugar cane plant, raw juice, juice in different stages, syrup, deposits, molasses, A, B and C sugar, refinery 1 and 2 sugar, and in soil samples picked up from the immediate vicinity of the cane plant roots at surface, 30 and 60 cm depth.     

Use of INAA and ICP-MS for the assessment of trace element mass fractions in adult and geriatric prostate

The variation with age of the mass fraction of 54 trace elements (Ag, Al, As, Au, B, Be, Bi, Br, Cd, Ce, Co, Cr, Cs, Dy, Er, Eu, Fe, Ga, Gd, Hf, Hg, Ho, Ir, La, Li, Lu, Mn, Mo, Nb, Nd, Ni, Pb, Pd, Pr, Pt, Rb, Re, Sb, Sc, Se, Sm, Sn, Ta, Tb, Te, Th, Ti, Tl, Tm, U, Y, Yb, Zn, and Zr) in intact nonhyperplastic prostate of 65 healthy 21–87 year old males was investigated by instrumental neutron activation analysis with high resolution spectrometry of long-lived radionuclides and inductively coupled plasma mass spectrometry. This work revealed that there is a significant tendency for an increase in Bi, Cd, Co, Fe, Hg, Sc, Sn, Th, U, and Zn (p < 0.0014) mass fraction in normal prostate from age 21 years to the sixth decade. In the sixth to ninth decades the mass fractions of almost all chemical elements investigated in nonhyperplastic prostates were maintained at approximately stable levels. Our finding of correlation between pairs of prostatic chemical element mass fractions indicates that there is a great disturbance of prostatic chemical element relationships with increasing age.     

Activity reduction of radioactive mixed wastes for subsequent carboxylate determinations

Instrumental neutron activation analysis (INAA) based on a nuclear reactor and proton induced X-ray emission (PIXE) based on a 2 Me V Van de Graaff accelerator were used to analyse different environmental samples including coal, sawdust, fly ash and landfill materials. These samples represent a large component of the solid waste being buried in the ground, and may be a potential source of toxicity which can have not only adverse effects on the soil and ground water, if diffused during leaching processes, but may also be transferred to humans through the food chain. Both techniques were employed to determine trace element concentrations in these matrices. The concentration of 30 elements were detemined, namely Na, Mg. Cl, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Cd, Ba, La, Sm, Eu, Tb, Ho, Yb, Hf, Ta and Th. The detection limits in the various sample matrices were calculated and a comparison was made for those elements commonly detected by both techniques.     

Separation and Analysis of Theran Volcanic Glass by INAA, XRF and EPMA

 Pumice from the “Minoan eruption” on Thera (Cyclades, Greece) was investigated to reveal the differences between the composition of the bulk material, which contains a certain percentage of crystallites, and the pure glass phase. This is important for the identification of vitric tephra layers found in the Eastern Mediterranean region in archaeological context and in deep sea drilling cores. Eruption products, deposited at some distance, have usually lost their crystalline fraction due to gravity separation and consist only of glass shards. Only major element distributions in such layers and in pumiceous glass phases have been published up to now, but these data are not sufficient for a reliable identification of the volcanic source, as several other eruptions are known to have produced chemically very similar layers in this region (Milos, Nisyros, Yali, Kos). Therefore, a technique has been developed to separate the glass phase from the primary pumice to reveal differences in the trace element distributions obtained by instrumental neutron activation analysis (INAA). X-ray diffractometry and microscopical techniques were applied to check the purity of this fraction. The concentrations of the major constituents, in particular Al, Ca, Fe, K, Mg, Mn, Na, Si, and Ti were determined by X-ray fluorescence (XRF) and electron probe microanalysis (EPMA), those of Al, Ba, Ca, Ce, Co, Cr, Cs, Dy, Eu, Fe, Hf, K, La, Lu, Mn, Na, Nd, Rb, Sb, Sc, Sm, Ta, Ti, Th, U, Yb and Zr by instrumental neutron activation analysis and partly also by X-ray fluorescence. Subtle differences between the compositions of the glass phase and the bulk material are explained by differentiation during partial crystallization and their applicability to the classification of tephra layers is demonstrated.     

Instrumental neutron activation analysis of trace elements in quartz

A scheme for INAA of 32 elements (As, Au, Ba, Br, Ca, Cd, Ce, Co, Cr, Cs, Eu, Fe, Hf, Hg, Ir, K, La, Lu, Mn, Na, Nd, Rb, Sb, Sc, Sm, Ta, Tb, Th, U, W. Yb, Zn) in quartz glass is proposed. The accuracy of the procedure is evaluated by the analysis of two NBS standard reference materials (SRM-1571 and SRM-1632-a). The method is convenient for routine work. The method was used for the determination of impurities in laboratory quartz glass. Dedicated to the 60th birthday of acad. prof. g. bliznakov     

Instrumental neutron activation analysis of rock samples from Ugep area of Cross River State,Nigeria

The theory and analytical procedures in Instrumental Neutron Activation Analysis (INAA) are discussed. Application of the method to the determination of sixteen trace elements: Na, K, Mn, Sm, La, Fe, Th, Sc, Co, Ba, Rb, Br, Sb, Cs and Ta in some rock samples from Ugep in the Lower Benue Region of Nigeria, is described. The high radioactivity observed in some of the samples analyzed has been associated with the higher-than-normal concentrations of Th and K in the samples. Also, Ba and Fe concentrations in some of the samples were found to be anomalous when compared with average expected values in normal sedimentary rocks.     

Determination of 34 elements in Chinese geochemical standard reference materials by instrumental neutron activation analysis

Thirty four elements (Al, As, Ba, Br, Ca, Ce, Co, Cr, Cs, Dy, Eu, Fe, Gd, Hf, Ho, K, La, Lu, Mg, Mn, Na, Nd, Rb, Sb, Sc, Sm, Ta, Tb, Th, Ti, U, V, W, Yb) were determined by instrumental neutron activation analysis in the second set of Chinese geochemical standard reference materials (sediments from GSD-9 to GSD-12, soils from GSS-1 to GSS-8, rocks from GSR-1 to GSR-6) using both thermal and epithermal irradiations. Irradiation schemes designed to utilise short, medium and long-lived nuclides were employed in order to analyse major, minor and trace elements with different half-lives. The gamma-ray spectra were measured by Ge(Li) and HP(Ge) detectors. Relevant nuclear data and possible interferences are listed, and analytical results are presented and discussed.