3D elemental sensitive imaging using transmission X-ray microscopy

Determination of the heterogeneous distribution of metals in alloy/battery/catalyst and biological materials is critical to fully characterize and/or evaluate the functionality of the materials. Using synchrotron-based transmission x-ray microscopy (TXM), it is now feasible to perform nanoscale-resolution imaging over a wide X-ray energy range covering the absorption edges of many elements; combining elemental sensitive imaging with determination of sample morphology. We present an efficient and reliable methodology to perform 3D elemental sensitive imaging with excellent sample penetration (tens of microns) using hard X-ray TXM. A sample of an Al-Si piston alloy is used to demonstrate the capability of the proposed method.     

Bulk material analysis using 14 MeV neutrons

There is considerable interest in bulk material analysis using energetic neutrons e.g. on-line coal analysis and down-hole logging. Recent work has indicated that an in-situ analysis of all the major elements of coal, using prompt capture and inelastic neutron scattering reactions, may be an operational possibility. The application of these techniques to oil well logging would allow the determination of lithology, porosity and oil and water saturation. Gamma-ray spectra arising from 14 MeV neutron bombardment of well characterised coal and fluid saturated rocks are presented. The gamma-ray intensities from both capture and scattering reactions are determined. Neutron transport modelling is used to evaluate the effect of variations in material content and the presence of trace neutron poisons. Predictions of carbon and oxygen scattering response are compared with the experimentally determined ratios.     

Activation analysis with fast neutrons using a cyclotron

A systematic study of activation analysis with cyclotron-produced neutrons for (n, 2n), (n, p) and (n, α) reactions is presented. The limits of detection for elements of atomic number from 6 to 80 are given. The possibilities of optimization of irradiation conditions by the choice of the most suitable neutron spectrum are discussed. The potential of this fast neutron activation analysis method is compared with that of 14 MeV neutron activation analysis.     

Detection of dynamical transitions in hydrogenous materials using transmission measurements with very cold neutrons

We have tested the transmission of very cold neutrons as a method to measure dynamical transitions in hydrogenous materials. Transmitted intensities vs. temperature at 30 Å neutron wavelength were measured for four materials that undergo phase transformations associated with changes in dynamics: ammonium iodide, sodium borohydride, hexamethylbenzene, and dicesium dodecahydro-closo-dodecaborate. In some cases, neutron vibrational spectra above and below the transformation temperatures are compared to the transmission results. The measurements show changes in transmission at or near the transition for all these compounds, reflecting dynamical changes. The results demonstrate that the transmission method is sensitive to motional changes due to a wide range of structural transitions, from first-order to much more subtle order–disorder effects and for both small molecular species and larger molecules. The technique is valuable for rapid (ca. hours) scans of new materials to guide neutron inelastic scattering experiments or to complement the results of other techniques.     

Use of spectroscopy of gamma-radiation from the inelastic scattering of reactor fast neutrons for elemental analysis

Gamma-spectra of stainless-steel and soil samples have been measured to study the potentialities of using spectroscopy of γ-radiation from the inelastic scattering of reactor fast neutrons for element analysis of various materials. Contents of iron, chromium, nickel, manganese, silicon and titanium in stainless steel, and those of silicon, iron, aluminium, magnesium, calcium, sodium, titanium, carbon and oxygen in soil have been determined by comparing the spectra of the samples with those of specially prepared mixtures of elements. The distinguishing features, advantages, and limitations of this method are discussed.     

A method for bulk hydrogen analysis based on transmission and back scattering of fast neutrons

A method was proposed for bulk hydrogen analysis. It is based on simultaneous detection of transmitted fast neutrons and back scattered thermal neutrons from the investigated samples by ³He detectors. The fast neutron beams were obtained from ²⁵²Cf and Pu–Be neutron sources. The experimental set-up as well as samples preparation were described. Incident thermal neutrons beams obtained from either ²⁵²Cf or Pu–Be sources, were used to investigate the samples by neutron backscattering. The results obtained from transmission and backscattering of fast neutrons were compared and discussed. The advantage and capabilities of the proposed method were presented. The results obtained using fast neutron beams are more sensitive than those obtained using thermal neutron beams. Validation procedures were proposed to credit the results.     

High-sensitive elemental analysis using multi-parameter coincidence spectrometer: GEMINI-II

In this study, using neutron activation analysis with multi-parameter coincidence method which was developed at Japan Atomic Energy Agency (JAEA), a non-destructive, ultra-high sensitive multi-elemental determination has been realized. The multi-parameter coincidence method is carried out with an array of 19 germanium detectors, GEMINI-II. Using this system, very weak γ-rays emitted from trace amounts of elements can be detected. The iridium concentration has been determined by means of neutron activation analysis with multi-parameter coincidence method for Cuban sediment samples across the K/T boundary strata.     

Elemental analysis of aluminium based alloys using 14-MeV neutrons

Elemental concentration has been estimated in aluminium based alloy samples, using 14-MeV neutron activation analysis. The results are in agreement with those obtained by atomic absorption spectroscopy.     

On-line bulk elemental analysis in the resource industries using neutron-gamma techniques

Summary There is an increasing need in industry, arising from both economic and environmental considerations, to reduce costs and improve product quality through the use of automation. The use of on-line analysis instrumentation provides plant operators with a means for continuous measurement and rapid response. This can result in better control of process efficiency, product quality and resource utilization, all of which produce significant economic and environmental benefits. On-line measurement of bulk elemental composition is important in many industrial applications and is best achieved with highly penetrating neutron-gamma techniques. This paper presents recent work by CSIRO Minerals on the development and implementation of such a technique, NITA (neutron inelastic-scattering and thermal-capture analysis). NITA is distinct from the more common PGNAA (prompt neutron gamma activation analysis) technique in its use of fast neutron sources to generate inelastic scattering reactions, and in its consequent ability to excite gamma-rays from industrially important elements such as carbon and oxygen. The paper will compare the features of NITA and PGNAA analysers and will discuss applications of NITA in industry, including the on-line analysis of composition in pyrometallurgical applications and the on-conveyor belt monitoring of cement raw meal and coal.     

Uncertainty estimation in organic elemental analysis using information from proficiency tests

We evaluate the uncertainty in organic elemental analysis of C, H, N, and S. We use data from six proficiency tests (PTs), in which some 35 Spanish laboratories participated. The uncertainty of the technique is estimated from the relative within-laboratory and between-laboratory variances for pure substances and samples with complex matrices (soil, powdered milk, oil, ash, and petroleum coke). We also calculate the relative standard uncertainties for individual laboratories when analysing pure substances using historical data from the participation of each laboratory in different editions of PTs. The uncertainty values obtained for the individual laboratories are comparable with the uncertainty of the technique and correlate with the combined z-scores. The evolution over time of those laboratories participating in common editions of PTs is also evaluated.     

Analysis of fertilizer phosphates using reactor neutrons and 14 MeV neutrons

Instrumental neutron activation analysis (INAA) in the absolute version was applied to 32 fertilizer phosphates of natural and industrial origin including three standard reference materials (NBS-SRM 120b, BCR-SRM No 32 and No 33). With reactor neutrons 48 elements were determined and with 14 MeV neutrons 3 additional elements were found. The results were used to assess the environmental toxicity of the fertilizers and to characterize their different origins.     

Investigation of elemental models in senile dementia and depressives using neutron activation analysis

Instrumental neutron activation analysis has been used to determine the concentration of a range of elements in hair and blood samples, separated into erythrocytes and plasma, obtained from two groups of women, senile demented (9) and depressives (16), and their respective controls (17 and 9). The results suggest that the senile dementia group has significantly higher Al concentrations in erythrocytes and hair relative to the controls but no significant correlation between the aluminium content of hair and that of blood exists. Further, Zn concentrations determined in the erythrocytes and plasma of these subjects were lower compared to the control values. Vanadium levels above our detection limit for the element were found in seven cases out of a total of sixteen in the depressive group. Vanadium was also found to be at higher concentration in the hair of the depressive group compared to the controls. Again no significant correlation was found to exist between the concentration of vanadium in hair and in erythrocyte sample for these seven subjects.     

Program for elemental analysis using low or medium resolution mass spectra

A program, called ELANAL, has been written in basic which computes all possible empirical formulae for a molecular ion or a fragment ion containing up to eleven common elements. The program then calculates the expected intensities of the peaks following the molecular or fragment ion due to heavier isotopes in the formulae. These calculated intensities are compared with the intensities in an experimentally determined mass spectrum.     

Multi elemental analysis of indigenous food spices in Southern Ethiopia using INAA technique

The objective of this study is a quantitative and qualitative analysis of essential and trace elements of four indigenous Ethiopian spices and herbs using instrumental neutron activation analysis technique. Results obtained for 16 elements: Major elements; Mg, Cl, and K; Minor elements; Na, Fe, and Mn, Zn, Br. While Al, V, Sm, Sc, La, Ba, Eu, Rb were found in traces. The spices, Affromumom korarima and Lippa Adonesis var. Koseret sebsebe were found to be very good sources of essential trace elements like Fe, Zn and Mn. The highest concentration of Mg was found in Ajowan whereas K and Fe were measured in Coriander seeds. The average daily dietary intake of some essential elements from the use of these spices were found to be below the recommended upper limit by WHO.

     

Decomposition methods in elemental trace analysis

Frequently, systematic errors in the decomposition step of a trace analytical multistage procedure lead to erroneous results in spite of the fact that expensive and powerful apparatus has been used for the determination. Of the numerous decomposition methods that have been published only a few meet the requirements of modern trace analysis.     

Comparison and determination of elemental composition in Korean space foods using instrumental neutron activation analysis

A quantitative analysis of mineral contents in several kinds of foods is needed to obtain information on a comprehensive elemental composition as well as an investigation on the effects of human health and nutrition based on the dietary intake of mineral elements. In 2012, six kinds of new Korean space foods (KSF) such as sweet pumpkin porridge, dakgalbi (spicy grilled chicken), Manila clam porridge, ox leg bone-cabbage soup, ginseng-chicken porridge, and chicken curry rice were developed by KAERI, and the contents of more than 15 elements in the samples were determined using an instrumental neutron activation analysis. A certified reference material associated with a biological food sample was used for analytical quality control. The analytical results were evaluated according to the elemental concentrations with KSF samples and compared with the reported values. These results will be applied toward the identification of gamma-irradiated foods.     

Microcomputers in electrochemical trace elemental analysis

The advantages of incorporating digital computers in devices for electrochemical trace elemental analysis are discussed on the basis of examples from the literature. Apart from easing data interpretation, the digital computer may control and monitor electrode processes at a high interaction frequency. For elements undergoing reversible electrode reactions, the resolution and sensitivity of electrochemical techniques can be improved by such rapid real-time interaction. Moreover, for quasi-reversible systems, the application of computerized broad-band potential excitation and simultaneous monitoring of broad band relaxation signals, permits rapid extraction of analytical information from data which represent the electrode process more accurately than do traditional single-frequency a.c. polarographic data.     

State-of-the-art in organic elemental micro and ultramicro analysis

Summary Nernst developed a quartz torsion microbalance in 1903. In consequence of this pioneering work, Emich in the Technical University of Graz, Austria, had systematized a series of chemical operations in microscale as well as a microchemical analysis. Further advances in technique and method of organic microanalysis had been accomplished by Pregl in Graz in 1912. His work had been strongly supported by a new microbalance which was known as Kuhlmann microbalance. Pregl's original methods of analysis were arranged and published in 1916 as Die quantitative organische Mikroanalyse. It is still noteable that the Nobel prize of 1933 had been presented to Dr. Pregl. In accordance with a combination of electronic microbalance and computer techniques, organic elemental microanalysis has grown to include advanced instrumentation and on-line computation. Successful adaptation of microchemical analysis has expanded today not only to pure organic compounds, but on industrial intermediates, polymers, food additives and many other compositions. The paper includes a discussion of the relative merits of traditional and modern analytical techniques together with the progression of microbalances. Recent developments in organic micro and ultramicro analysis in Japan are also described.