Determination of multielement in optical waveguide and standard reference materials by instrumental neutron activation analysis

Trace amounts of transition elements (Co, Cr, Cu, Fe, Mn and V) and other seven elements in optical waveguide samples were determined by INAA. The contents of impurities in ultra-pure materials are less than those of high-purity materials and of G.R. grade. The increase of contamination of trace transition elements and iridium from furnace or crucible are observed in the production of optical glass fibers. Up to seventeen elements were determined in five NBS biological standard reference materials: Oyster Tissue: SRM-1566, Brewers Yeast: SRM-1569, Spinach: SRM-1570, Orchard Leaves: SRM-1571 and Tuna Fish, and in four Japanese biological standard reference materials: Tea Leaves B&C, Pepperbush and Shark Meat. The analytical results in NBS and Japanese standard reference materials are in good agreement with published values and certified values by NBS.     

An example for activation analysis by low-level radioisotope neutron soruce

A 1 Ci Pu−Be neutron source and a low-background beta-spectrometer were used to activate and to measure the beta-rays of low-activity. The main characteristics of this method can be given as follow: The determined S/N ratio increases because the background beta-rays are lower than the gamma-rays. For example, the sensitivity obtained for quantitative analysis of sulphur in silicon is 100 ppm in case of S/N=1.0.     

The software and information system for development of neutron activation techniques with optimal characteristics

An optimal software and information system for NAA techniques has been developed. The system includes a data base and software complex. A number of original analog simulation algorithms of the gamma-spectrum of an activated sample were tested. The calculations of the metrological characteristics of optimal AA conditions were used as a basis. The analog simulation program for activation in a reactor, neutron generator, or with a²⁵²Cf radiation source simulates the -spectrum of a sample taking into account the decay chains up to the 15th link. A research of the optimal activation conditions for the determination of elements is conducted within a wide range of variations using the data base management system.     

Methodological developments and applications of neutron activation analysis

The paper reviews the author’s experience acquired and achievements made in methodological developments of neutron activation analysis (NAA) of mostly biological materials. These involve epithermal neutron activation analysis, radiochemical neutron activation analysis using both single-and multi-element separation procedures, use of various counting modes, and the development and use of self-verification principle. The role of NAA in the detection of analytical errors is discussed and examples of applications of the procedures developed are given.     

Industrial applications of instrumental neutron activation analysis

Neutron activation analysis is shown as a useful diagnostic technique in semiconductor industry. A better acceptance of the method for applications in industry has been achieved through a specialized analytical service. Its main application is the characterization of high purity silicon in all stages of production. Irradiation of large sample volumes allowes a very sensitive detection of impurities in silicon with detection limits down to 10^–16 g/g. Other applications discussed are the analysis of silicon carbide, quartz, pure water and titanium. Special techniques described are autoradiography, depth profiling and surface analysis. In semiconductor process technology NAA was used to monitor contamination of silicon wafers.     

In-vivo neutron activation analysis for medical applications

This paper describes the design of the system and the uses of in-vivo neutron activation analysis (IVNAA) for the determination of total body calcium (TBCa) and total body nitrogen (TBN) in humans. TBCa and TBN assay are useful in a variety of clinical situations dealing with the diagnosis and management of patients with osteopenia, nutritional deficiency, renal dysfunction, transplantation, cancer, thyroid dysfunction and many others. The system can be put together with readily available nuclear components and within a reasonable cost. This paper examines the present status of IVNAA for medical applications in a hospital setting.     

Analytical applications of delayed and instrumental neutron activation analysis

Delayed neutron activation analysis (DNAA) is a rapid and sensitive analytical method for the determination of fissile elements in a variety of samples. The present work describes two different analytical applications of delayed neutron activation for the analysis of biological and environmental samples, respectively. In the first application, DNAA was utilized to determine the natural uranium content in NIST standard reference materials (SRM) 1547 peach leaves and 1573a tomato leaves. Measured uranium mass fractions are comparable to the non-certified values listed on the certificates for these materials. In the second application, delayed neutron activation is coupled with instrumental neutron activation analysis (INAA) for the measurement of rare earth elements (REE) (cerium, lanthanum, neodymium, and ytterbium) in NIST SRM 2586, Trace Elements in Soil Containing Lead from Paint. DNAA was utilized to determine the uranium mass fraction in SRM 2586 for the subsequent application of a correction factor to account for cerium, lanthanum, and neodymium produced as part of the INAA irradiation. Measured and corrected mass fractions for the REEs described here are all within the uncertainty limits provided on the NIST certificate for SRM 2586. These results and the demonstrated sensitivity of the DNAA system establish and validate the use of this method for the determination of REEs and for potential nuclear forensics applications.     

Preconcentration techniques for trace analysis via neutron activation

A review is given of the methods that have been proposed for enrichment of trace elements in samples that are to be analysed by neutron-activation methods. The emphasis is on classification of methods, with full illustrations by means of practical examples.     

Updating analytical techniques for fast neutron activation analysis

Two improvements in the analytical techniques used for fast neutron activation analysis have been developed and put into routine use. The first is neutron shielding of a NaI (TL) counting system, which reduces the counting noise encountered during neutron generation. The second is a modification of batch type irradiation for long lived nuclides so they can be done simultaneously with other test.     

Multielement content of coal by neutron activation analysis techniques

Due to the interaction with components present in natural waters, radionuclides may be present in different physico-chemical forms, varying in size, charge and density. The distribution pattern will influence the transport, mobility and biological uptake of the radionuclides. Size fractionation based on hollow fiber is useful for the determination of the size distribution pattern of radionuclides in natural waters. Furthermore, a continuous mixing and separation system has been developed for the investigation of the association of radionuclides with naturally occurring colloids. Results based on radionuclides in waste water from the Forsmark nuclear power plant, Sweden, will illustrate the potential usefulness of the technique.     

Practical aspects of neutron activation determination of the platinum metals

Triple gamma coincidence counting of¹⁹²Ir allowed the determination of Ir by instrumental neutron activation analysis down to 1 ppb in ultrabasic rocks and down to ca. 20 ppb in some high-furnace slags; the limiting factor for the latter matrix was the presence of¹²⁴Sb. Radiochemical neutron activation analysis of the USGS standard rocks revealed that the Ir contents are up to three orders of magnitude lower than previously reported, except for the ultrabasic rocks. The factor of merit of several scintillation and semiconductor, gamma-ray detectors was determined for the neutron activation determination of Pd, Pt and Os. In the case of radiochemically pure sources, a NaI(Tl) wafer was preferred; in the presence of high-energy gamma-emitters, a Ge(Li) low-energy photon detector was superior.     

Determination of trace elements in semiconductor materials by neutron activation analysis using the radioisotope addition technique

The determination of trace elements in highly activated matrix components was carried out by neutron activation analysis using the radioisotope addition technique. The method is based on the addition to the irradiated test sample of a radioisotope which is a diffeent nuclide of the element to be determined. After separation, the chemical yield is calculated from the radioactivity added and the element is determined by an ordinary technique. Twelve elements in indium phosphide and eight elements in gallium arsenide could be determined by the method.     

Instrumental neutron activation analysis applications in materials science and in forensic surveys

Neutron Activation Analysis (NAA) was applied to the characterization of lithious ceramic materials to be used as tritiogenic breeders in future fusion reactors. After neutron irradiation, measurements by -spectrometry were performed on the activated impurities, particularly on the ones with large neutron cross section. Irradiated samples were then annealed at rising temperatures, to obtain a fractional release of the tritium [formed by (n,) reaction on lithium] as element (HT/T₂) or tritiated water (HTO/T₂O). Barium and antimony were determined by NAA, on request of Italian Courts, as evidence of gunshot residues (GSR), on hands and clothes of suspected people. The sample is left unchanged, even if slightly radioactive, allowing further examinations, in case of controversial results. In some actual cases, NAA was performed on sample already examined by scanning electron microscopy (SEM/EDX), allowing the determination of several more elements and a more definite identification of the ammunitions involved in the crime.     

Characterization of protein-bound metal species by bioanalytical and neutron activation techniques

Several bioanalytical techniques have been employed in conjunction with instrumental neutron activation analysis (INAA) to study metalloproteins and protein-bound trace elements in bovine kidneys. The accuracy of the INAA method developed has been evaluated by analyzing certified reference materials. Up to 29 elements can be reliably determined in biological tissue samples by INAA. Dialysis of the bovine kidney homogenate shows that more than 90% of Ca, Cd, Cu, Fe, Mg, Mn, Mo, Se, V and Zn, and about 20% of Br are bound to macromolecules, mainly proteins. A combination of gel filtration and ion exchange chromatography, chromatofocusing, electrofocusing, ammonium sulphate precipitation and INAA of the bovine kidney microsomecytosol subcellular fraction further indicates that much of the copper is associated with a single protein of an isoelectric point around 5 and a molecular weight of about 30 000 daltons. Some results on manganese proteins are also reported.     

Thin films of peroxopolytungstic acids: applications to optical waveguide components

Thin films of peroxohetero(carbon)polytungstic acid (CW-HPA) and carbon-free isopolytungstic acid (W-IPA) were prepared, and examined in terms of optical and etching properties. Thermal decomposition was found to give good results in removing excess hydrogen peroxide (H₂O₂) during the preparation of CW-HPA and W-IPA. It was shown for the first time that thin films of CW-HPA and W-IPA have very high refractive indices (larger than 2.0) when sufficiently dried. Optical waveguide (OWG) characteristics of these films were examined using a slab-type OWG structure and ARROW (Antiresonance Reflection Optical Waveguide)-type structures. An embossing technique was applied to make diffractional grating couplers.     

Measurement of the neutron flux distribution in a research reactor by neutron activation analysis

Journal of Radioanalytical and Nuclear Chemistry - The neutron flux distribution in the core region of the JRTR was measured through the neutron activation analysis method. Sample mount and a tool...     

The role of neutron activation analysis in VLSI manufacturing and development

Very large scale integrated (VLSI) semiconductor manufacturing and development require trace analyses for materials inspections, process characterization, contamination control, and failure analysis. Improvement in alternate analytical techniques has reduced the relative importance of neutron activation analysis (NAA) in these activities, but, for certain types of problems, NAA can still play a significant role.     

The application and development of k0-standardization method of neutron activation analysis at Dalat research reactor

In recent years the k ₀-NAA method has been applied and developed at the 500 kW Dalat research reactor, which includes (1) the establishment of a PC database of k ₀-NAA-related nuclear parameters, e.g., radionuclide produced, half-lives, k ₀-factors, Q ₀, _r, E _g, etc; the access to the database is able by a k ₀-NAA software or by manual; (2) the detection efficiency calibration of gamma spectrometers used in k ₀-NAA, (3) the determination of reactor neutron spectrum parameters such as a and f factors and neutron fluxes in the irradiation channels, and (4) the validation of the developed k ₀-NAA procedure by analysing some SRMs, namely Coal Fly Ash (NIST-1633b), Bovine Liver (NIST-1577b) and IAEA-Soil7. The analytical results showed the deviations between experimental and certified values were mostly less than 15% with most Z-scores lower than 2. The k ₀-NAA procedure established at the Dalat research reactor has been regarded as a reliable standardization method of NAA and as available for practical applications, in particularly for airborne particulate and crude oil samples.