Accurate measurement of bromine contents in plastic samples by instrumental neutron activation analysis

Accurate measurements of bromine contents in plastic samples were made by the direct comparator instrumental neutron activation analysis (INAA). Individual factors affecting the measurements were comprehensively evaluated and compensated, including the volatility loss of bromine from standard comparators, the background bromine level in the filter papers used for preparation of the standard comparators, nuclear interference, γ-ray spectral interference and the variance among replicates of the samples. Uncertainty contributions from those factors were thoroughly evaluated and included in the uncertainty budgeting of the INAA measurement. ⁸¹Br was chosen as the target isotope, and the INAA measurements for bromine were experimentally confirmed to exhibit good linearity within a bromine content range of 10–170 μg. The established method has been applied to the analysis of eight plastic samples: four commercially available certified reference materials (CRMs) of polyethylene and polystyrene and four acrylonitrile butadiene styrene (ABS) samples prepared as the candidate reference materials (KRISS CRM 113-01-012, -013, -014 and -015). The bromine contents of the samples were calculated at three different γ-ray energies and compared, showing good agreement. The results of the four CRMs also showed good consistency with their certified values within the stated uncertainties. Finally, the bromine contents of the ABS samples were determined with expanded uncertainties (at a 95% level of confidence) between 2.5% and 5% in a bromine content range of 25–900 mg kg⁻¹.     

Application of instrumental neutron activation analysis to ceramic solid electrolytes

Beta" alumina isomorphs with different conducting cations were produced by ion exchange in molten salts. The concentration of the main component (Al), of conducting ions (Na⁺, Sr⁺⁺, Ba⁺⁺) and of chlorides from residues of the melt inside the exchanged material was determined by instrumental neutron activation analysis (INAA).Dedicated to Professor Günther Tölg on the occasion of his 60th birthday     

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.     

Instrumental neutron activation analysis of mass fractions of toxic metals in plastic

It is very challenging to decompose a plastic product for the purpose of analysis of hazardous elements contained. To circumvent such technical problem, it is imperative that an analyst employ a nondestructive analytical method free of any pretreatments. The analytical results of the concentrations of toxic metals such as Cd and Cr in polypropylene for seven samples at two different levels were obtained using the instrumental neutron activation analysis. This work was intended ultimately to establish certified reference materials (CRMs) of these metals in the polypropylene, traceable to the SI. The uncertainties associated with the analytical procedures were estimated in accordance with the ISO guideline. The results were subsequently validated by a comparison with those for CRM-680 and −681 of the Bureau Communautaire de Reference (BCR), which demonstrated acceptable agreement within their uncertainty ranges.     

Metrological role of neutron activation analysis. IA. Inherent characteristics of relative INAA as a primary ratio method of measurement

In a series of three papers, the inherent characteristics of relative instrumental neutron activation analysis (INAA) as a primary ratio method of measurement, the unique functions of parametric INAA as an ideal back-up method of the relative INAA, and the valuable role of INAA in characterization of sampling behavior of individual elements in certified reference materials (CRMs) will be discussed. In this paper, the first of the series, the uncertainty evaluation and the traceability of values measured by neutron activation analysis (NAA), especially instrumental NAA (INAA), will be described to demonstrate the method at its ”the state-of-the-art” level can meet CCQM criteria for a primary ratio method. The scope and examples will be given. Received: 19 March 2001 Accepted: 2 October 2001     

Determination of elemental concentrations in environmental plant samples by instrumental neutron activation analysis

The intake of leafy vegetables in daily diet is very important to meet our nutritional needs. Vegetables provide the essential elements which are necessary and recommended for human growth. However, due to rapid industrialization and urbanization our environment becomes polluted and this affects the normal growth of agricultural products and composition of environmental species. The elemental concentrations present in the environmental samples are good indicators to assess the toxicological levels due to pollution affects. In the present work we have analysed several vegetable plant samples by instrumental neutron activation analysis to determine the elemental concentrations at major, minor and trace levels. The leafy vegetables like spinach, red leafy veagetable, pui, gourd leaf, lettuce and katoua were chosen as these are extensively consumed by local peple in eastern part of India. We have determined 15 elements in the above mentioned vegetable samples and some of these are essential elements and some are toxic elements. It was found that Na and K were present as major elements, Fe and Zn as minor elements and As, Ce, Cr, Co, La, Mo, Rb, Sc, Sm, Sr as trace elements. The concentration level of Cr was found to be higher than that of recommended value certified by WHO and National environment quality control for human consumption. The validation of our analytical results have been performed by the Z-score tests through the determination of concentrations of the elements of interest in certified reference materials.     

Platinum determination by instrumental neutron activation analysis with special reference to the spectral interference of Sc-47 on the platinum indicator nuclide Au-199

A method of instrumental neutron activation analysis (INAA) is developed for the determination of platinum by the ¹⁹⁹Au daughter of ¹⁹⁹Pt in the presence of the spectral interference from the ⁴⁷Sc daughter of ⁴⁷Ca. The contributions of the Pt and Ca signals to the integral 157–161 keV peak were separated by calculating the number of disintegrations due to the ⁴⁷Sc from the signal of her parent ⁴⁷Ca at 1297.1 keV γ-ray. The method was used to calculate the trace concentrations of Pt in air samples, collected on filters.     

Metrological role of neutron activation analysis. III. Role of INAA in sampling behavior characterization

The minimum sample size, usually 100 mg or larger, is often the only information given on certificates of existing certified reference materials (CRMs) to describe sampling behavior. This value is not only too large for quality control requirements of microanalysis, but also too general to reflect the strong element-specific nature of the sampling behavior of solid materials. In this paper, the third and final of the series, we explain the need for CRMs with sampling behavior characterized for individual elements and describe the unique role of instrumental neutron activation analysis in sampling behaviour characterization. Received: 19 March 2001 Accepted: 2 October 2001     

Progress in neutron activation analysis for uranium

A new type of extractant, sym-dibenzo-16-crown-5-oxyhydroxamic acid (HL) is introduced. The extractions of UO22+, Na+, K+, Sr2+, Ba2+ and Br- were studied with HL in chloroform. The results obtained show that UO22+ can be quantitatively extracted at pH values above 5, whereas the extractions of K+, Na+, Sr2+, Ba2+ and Br- are negligible in the pH range of 2 - 7. The dependence of the distribution ratio of U(VI) on both the concentration of the HL and pH are linear, and they have the same slope of 2. This suggests that U(VI) appears to form a 1:2 complex with ligand. Uranium(VI) can be selectively separated and concentrated from interfering elements such as Na, K, Sr and Br by solvent extraction with HL under specific conditions. The recovery of uranium is nearly 100% and the radionudear purity of uranium is greater than 99.99%. Therefore, neutron activation analysis has greatly improved the sensitivity and accuracy for the detection of trace uranium from seawater.     

Instrumental neutron activation analysis of trace element contents in the rib bone of healthy men

The effect of age on trace element contents in rib bone of 24 healthy 16–55-year old men was investigated by INAA. Mean values (M ± SΕΜ) for mass fraction of Co, Fe, Rb, Sr, and Zn (mg/kg on dry weight basis) were: 0.0030 ± 0.0005, 150 ± 20, 1.70 ± 0.30, 260 ± 30, and 76 ± 4, respectively. The upper limit of mean contents of Ce, Cs, Eu, Hg, and Se were: ≤0.03, ≤0.01, ≤0.001, ≤0.008, and ≤0.03, respectively. The contents of Ag, As, Au, Ba, Br, Cd, Cr, Gd, Hf, La, Lu, Nd, Sb, Sc, Sm, Ta, Tb, Th, U, Yb, and Zr were under detection limits. No changes of trace element contents with age were found.     

Preparation and characterization of a new set of IAEA reference air filters using instrumental neutron activation analysis, proton-induced X-ray emission and Rutherford backscattering

A new set of reference air filters was prepared for proficiency testing of laboratories involved in air pollution studies organized by the International Atomic Energy Agency (IAEA). The set consists of one filter loaded with airborne particulate matter (APM) and one blank filter. Target values and their standard deviations were established using instrumental neutron activation analysis (INAA) and proton induced X-ray emission (PIXE) with proven accuracy. Rutherford backscattering (RBS) was used to help in deriving the necessary corrections in PIXE. Losses of individual elements from APM due to the wet deposition procedure were evaluated.     

Determination of elemental levels in medicinally important Indian leaves by instrumental neutron activation analysis

Levels of As, Ba, Br, Ca, Ce, Cl, Cr, Cs, Eu, Fe, Hg, I, K, La, Mg, Mn, Na, Ni, Rb, Sb, Sc, Sm, Sr, Th, Zn, and U have been determined in ten leaves widely used in ayurvedic medicine by instrumental neutron activation analysis (INAA). The neutron irradiations were performed with a 100 kW Triga nuclear reactor and the induced activity was counted with a gamma-ray spectrometer. Based on elemental levels obtained the utility of these leaves in medicine are discussed.     

Determination of the elemental distribution in cigarette components and smoke by instrumental neutron activation analysis

Cigarette smoking is a major source of particles released in indoor environments. A comprehensive study of the elemental distribution in cigarettes and cigarette smoke has been completed. Specifically, concentrations of thirty elements have been determined for the components of 15 types of cigarettes. Components include tobacco, ash, butts, filters, and cigarette paper. In addition, particulate matter from mainstream smoke (MS) and sidestream smoke (SS) were analyzed. The technique of elemental determination used in the study is instrumental neutron activation analysis. The results show that certain heavy metals, such as As, Cd, K, Sb and Zn, are released into the MS and SS. These metals may then be part of the health risk of exposure to smoke. Other elements are retained, for the most part, in cigarette ash and butts. The elemental distribution among the cigarette components and smoke changes for different smoking conditions.     

Assessing sediment pollution from the Julian Adame-Alatorre dam by instrumental neutron activation analysis

The rapid industrial development in regions of Mexico during recent years has had the side effect of introducing toxic metals, fertilizers, and pesticides into the ecosystem. Sediment cores were collected from eight locations around the Julian Adame-Alatorre dam located in the Municipality of Villanueva in the State of Zacatecas, México. The cores were analyzed for 32 major, trace, and rare earth elements (As, La, Lu, Nd, Sm, U, Yb, Ce, Co, Cr, Cs, Eu, Fe, Hf, Rb, Sb, Sc, Sr, Ta, Tb, Th, Zn, Zr, Al, Ba, Ca, Dy, K, Mn, Na, Ti, and V) in order to estimate the health risk. The samples were analyzed by instrument neutron activation analysis (INAA) using thermal neutron fluxes of 8 × 10¹³ and 5 × 10¹³ n cm⁻² s⁻¹ for short and long irradiations, respectively. The results of the contamination levels for elements such as As, Ba, Cr, Fe, Mn, Ta, V, and Zn were compared with the Mexican regulations and the guidelines of USEPA. Enrichment factors for quantified elements identified high As, Sb, Hf, and Cs contents using Fe as a crustal reference.     

Determination of aluminium contents in selected food samples by instrumental neutron activation analysis

Food and food products are the main sources of Aluminium entering the human body. In order to know aluminium contents in food and food products, selected 26 samples from local market were analyzed by instrumental neutron activation analysis (INAA) using reactor neutrons and high resolution gamma-ray spectrometry. INAA using 1,779 keV γ-ray of ²⁸Al (2.24 min) was used for aluminium concentrations in the range of 33–529 mg kg^?1. Two NIST standard reference materials (SRMs) and two IAEA reference materials (RMs) were analyzed by INAA for quantification of aluminium as a part of method validation.     

Metrological role of neutron activation analysis. IB. Inherent characteristics of relative INAA as a primary ratio method of measurement

This is the second part of a paper which deals with the advantages and disadvantages of relative instrumental neutron activation analysis concerning traceability and uncertainty, and the current scope and possible future extensions of neutron activation analysis as a primary ratio method. The first part of this paper has been published in this Journal [1]. Received: 19 March 2001 Accepted: 2 October 2001     

Determination of nitrogen in boron carbide by instrumental photon activation analysis

Boron carbide is widely used as industrial material, because of its extreme hardness, and as a neutron absorber. As part of a round-robin exercise leading to certification of a new reference material (ERM-ED102) which was demanded by the industry we analysed nitrogen in boron carbide by inert gas fusion analysis (GFA) and instrumental photon activation analysis (IPAA) using the ¹⁴N(γ,n)¹³N nuclear reaction. The latter approach is the only non-destructive method among all the methods applied. By using photons with energy below the threshold of the ¹²C(γ,n)¹¹C reaction, we hindered activation of matrix and other impurities. A recently installed beam with a very low lateral activating flux gradient enabled us to homogeneously activate sample masses of approximately 1 g. Taking extra precautions, i.e. self-absorption correction and deconvolution of the complex decay curves, we calculated a nitrogen concentration of 2260 ± 100 μg g⁻¹, which is in good agreement with our GFA value of 2303 ± 64 μg g⁻¹. The values are the second and third highest of a rather atypical (non-S-shape) distribution of data of 14 round-robin participants. It is of utmost importance for the certification process that our IPAA value is the only one not produced by inert gas fusion analysis and, therefore, the only one which is not affected by a possible incomplete release of nitrogen from high-melting boron carbide. Figure Twin-Detector system for analyzing spatially extended samples     

Measurement uncertainty of iodine determination in radiochemical neutron activation analysis

The measurement uncertainty of iodine determination in NIST standard reference material (SRM) 1549 using radiochemical neutron activation analysis (RNAA) was studied. This method is based on ignition of the irradiated sample [¹²⁷I(n,)¹²⁸I, t_1/2=25 min, E=422.9 keV] in an oxygen atmosphere, followed by absorption of iodine in a reducing acid solution and its purification by a selective extraction–stripping–reextraction cycle. The purified solution of iodine in CHCl₃ was transferred to a well-type HPGe detector for -ray measurement of the induced radionuclide ¹²⁸I. The detection limit of the method employed under the conditions described was 1 ng/g. The reproducibility of iodine determination in the SRM was 3.6% (12 determinations within 1 month), calculated by the analysis of variance procedure. Using the commercially available software program GUM Workbench and the recommendations of the Eurachem/CITAC Guide, we evaluated the uncertainty budget for this RNAA method and the relative uncertainty obtained was 3.6%. The largest uncertainty contributions were due to the repeatability of the chemical yield determination, the count rate of the induced nuclide in the standard and sample, the mass of the carrier and the mass of the irradiation standard.     

Elemental characterization of mineral supplements by neutron activation analysis

Instrumental neutron activation analysis (INAA) was applied to assess element concentrations in eleven samples of mineral supplements/multivitamins acquired in drugstores and pharmacies in São Paulo city, SP, Brazil. Concentrations of Ca, Co, Cr, Cu, Fe, K, Na, Se and Zn were determined. A comparison was made between the results obtained with the labels of the mineral supplents. Certified reference materials, NIST SRM1400 Bone Ash and NIST SRM 1633b Coal Fly Ash were analyzed for quality control of the analytical results.     

Extraction-chromatographic system TBP-HBr in radiochemical neutron activation analysis of high-purity materials

The extraction and extraction-chromatographic behaviour of a variety of elements in the TBP-HBr system with concentrations from 0.1 to 7M HBr has been studied. The results allowed the development of simple procedures for radiochemical neutron activation determination of 22 impurity elements (Na, K, Sc, Cr, Mn, Fe, Co, Ni, Cu, Ga, As, Se, Rb, Sr, Zn, Mo, Ag, Sb, Te, Ba, La, Hf and W) in high-purity cadmium and indium samples with detection limits from 1 g g^–1 for Fe and Zr to 0.01 ng g^–1 for Na, Sc, Mn with relative standard deviations < 0.15. To increase the selectivity of the extraction-chromatographic separation, use was made of extraction suppression and co-extraction effects. The procedure for the extraction-chromatographic separation of scandium from a number of other elements is described as an example. The procedure can be used for simultaneous quantitative separation of impurity radionuclides from radiation produced long-life scandium radionuclides in the neutron activation analysis of titanium and vanadium.