Facility for non-destructive analysis for major and trace elements using neutron-capture gamma-ray spectrometry

A facility for neutron-capture γ-ray spectroscopy for analytical purposes has been developed and tested at the National Bureau of Standards reactor. The system consists of an internal beam tube with collimators, an external beam tube and irradiation station, a Compton-suppressed Ge(Li) γ-ray detection system, and a minicomputer-based data-collection and-analysis system. Detection limits have been established for many elements and errors arising from neutron self shielding, γ-ray peak overlap, neutron beam variations, and sample matrix evaluated.     

Nuclide analysis of a tantalum target irradiated with high-energy protons

First results of γ-spectrometric measurements of radionuclides produced in a tantalum target irradiated for 500 days with 800 MeV protons are presented. The activities of the γ-ray-emitting nuclides measured after a cooling period of 2–4 years differ by more than four orders of magnitude. Within this cooling period about 95% of the activity of the target is determined by¹⁷²Lu,¹⁷³Lu,¹⁷⁴Lu,¹⁷²Hf (daughter nuclide of¹⁷²Lu) and¹⁸²Ta nuclides. These highly active nuclides, together with some other medium-active nuclides, were measured with good precision by γ-ray spectrometry directly in the sample solution. Weakly active nuclides could not be measured in this way because of the high Compton background in the γ-ray spectrum. For the sensitive measurement of many other nuclides present in weaker activities a simple chemical separation procedure was developed to separate Lu, Hf and Ta. With the separation of these elements and simultaneously of the high-active nuclides, the Compton background in the γ-ray spectra could be drastically reduced and many weakly active nuclides additionally measured.     

Measurements of Ir concentration in geological standard samples using neutron activation analysis with multiple gamma-ray coincidence method

In this study, the Ir concentrations in some standard rock samples were determined by using the multiple γ-ray detection method. The use of the multiple γ-ray detection method, which was developed for nuclide quantification, yielded better resolution and sensitivity than the ordinary singles γ-ray detection method. Iridium is one of the least abundant elements in Earth’s crust, with an average mass fraction of 0.001 ppm in a crust rock. However, iridium is relatively more abundant (concentration: 0.5 ppm or more) in undifferentiated meteorites. Therefore iridium abundance anomalies in geological samples provide important information about meteorite impact. The standard rock samples used in this study were SARM-76, FC-1 and FC-2. The SARM-76 was prepared from a platinum ore, and issued by the south African bureau of standards. FC-1 and FC-2 were obtained from fish clay sediment samples from Stevens Klint, Denmark.     

Fast neutron activation analysis: High resolution gamma spectroscopy

The purpose of this study was to demonstrate the versatility of combining the use of high resolution, Ge(Li) γ-detectors with the techniques of fast neutron activation analysis. A compilation of γ-ray spectra are presented for irradiation of 30 elements with 14.8 MeV neutrons under standard conditions and the origin of all major photopeaks is determined.     

Pulsed neutron-based on-line coal analysis

A neutron generator-based on-line coal analysis system is described, capable of measuring the content of the major and minor elements in coal. The system utilizes reactions produced from fast and themal neutrons, as well as from neutron activation with half lives of seconds or minutes. Characteristic γ-rays, detected with BGO detectors are used for the identification of the various chemical elements. The method for the analysis of the γ-ray spectra is presented, and the measurements of coal density, carbon and sulfur content are shown.     

A compilation of X- and gamma-ray sensitivities from isotopes produced by the (n, γ) reaction for utilization in instrumental neutron activation analysis

A comprehensive compilation of X- and γ-ray emitting isotopes produced by the (n, γ) reaction is reported in this paper for application to instrumental neutron activation analysis (INAA). The X- and γ-ray sensitivities are computed theoretically by a computer code. Interfering photons from isotopes of neighbouring elements are identified by the code and the percentage interference is computed. Additionally an advantage factor (X-ray: γ-ray sensitivity) is computed, which is a figure of merit for X-ray spectroscopy in INAA. Further, mathematical representation of background continua for typical matrices encountered in INAA allow the calculation of elemental detection limits for the X-ray and γ-ray photons.     

The use of non-destructive high energy gamma photon activation for trace element survey analysis

An empirical study has been made of the potential of high energy γ photon activation and high resolution γ-ray spectrometry for the survey analysis of trace elements in a variety of materials. Human blood, urine, bone ash, standard glass (NBS, SRM 612) and air particulates, along with synthetic multi-element standards, have been studied following irradiation with γ photons of maximum energy 17–45 MeV. Elements found to be suited to determination by γ activation include Sb, As, Bi, Cd, Cs, Ca, Ce, Cr, Fe, Au, Pb, Mg, Mo, Ni, Nb, Rb, Sr, Tl, Ti, Tm, Zn and Zr. γ spectra, elemental concentrations measured, and/or limits of detection observed, for the matrices studied are given.     

Gamma-ray yield dependence on bulk density and moisture content of a sample of a PGNAA setup: A Monte Carlo study

Monte Carlo calculations were carried out to study the dependence of γ-ray yield on the bulk density and moisture content of a sample in a thermal-neutron capture-based prompt gamma neutron activation analysis (PGNAA) setup. The results of the study showed a strong dependence of the γ-ray yield upon the sample bulk density. An order of magnitude increase in yield of 1.94 and 6.42 MeV prompt γ-rays from calcium in a Portland cement sample was observed for a corresponding order of magnitude increase in the sample bulk density. On the contrary the γ-ray yield has a weak dependence on sample moisture content and an increase of only 20% in yield of 1.94 and 6.42 MeV prompt γ-rays from calcium in the Portland cement sample was observed for an order of magnitude increase in the moisture content of the Portland cement sample. A similar effect of moisture content has been observed on the yield of 1.167 MeV prompt γ-rays from chlorine contaminants in Portland cement samples. For an order of magnitude increase in the moisture content of the sample, a 7 to 12% increase in the yield of the 1.167 MeV chlorine γ-ray was observed for the Portland cement samples containing 1 to 5 wt.% chlorine contaminants. This study has shown that effects of sample moisture content on prompt γ-ray yield from constituents of a Portland cement sample are insignificant in a thermal-neutrons capture-based PGNAA setup.     

List-mode coincidence data analysis for highly selective and low background detection of gamma-nuclides in activated samples

Highly selective and sensitive γ-ray detection was performed by coincidence and anticoincidence event analysis after list-mode data acquisition using an HPGe spectrometer equipped with NaI(Tl) and plastic scintillation detectors. In order to obtain the most suitable detection of specific nuclides, coincidence or anticoincidence spectra could be freely constructed by extracting events with particular time and energy correlations. Although the detector arrangement of this system was the same as that of a typical Compton suppression spectrometer, background counts were drastically reduced and γ-rays of particular nuclides could be selectively detected by using γ-γ, γ-X, γ-X-X, and γ-β⁺ coincidences.     

Multi-element standard for routine instrumental activation analysis of trace elements in rocks and tectites

The use of high-resolution Ge(Li) detectors in non-destructive instrumental neutron activation analysis (INAA) of mineral materials makes possible the simultaneous determination of a number of trace elements. In routine applications of INAA the use of a multi-element standard (MES) has proved to have advantages over a set of standards for each determined element. An MES has been prepared containing 8 trace elements mixed in a suitable proportion and giving, after neutron activation, long-lived γ-emitters, the γ-ray lines of which regularly occur in the γ-ray spectra of silicate mineral materials. This method has been used in the determination of Sc, Cr, Co, Rb. Cs, Eu, Hf and Th in samples of standard rocks and moldavites.     

Quantitative analysis of phosphorus by (p, γ) reactions

Measured values of the intensities of characteristic γ-rays emitted under the bombardment of protons on a thick target of phosphorus are tabulated. The intensity of each characteristic γ-ray is measured and used for quantitative analysis of phosphorus in any sample with a sensitivity of 50 to 1000 ppm.     

The investigation of the resolution enhancement transformation and the analysis of complex overlapping peaks in gamma-ray spectra

A method is proposed for the resolution enhancement transformation (RET) of the γ-ray spectrum, which is not only a simple convolution operation but also have a definite analytical significance because of the introduction of the parameter ω representing the degree of the resolution enhancement. We apply the RET to the peak detection method for complex overlapping peaks. The validity of this method is ascertained by the analysis of X-ray overlapping peaks.     

A neutron induced prompt gamma-ray spectroscopy system using a 252Cf neutron source for quantitative analysis of aqueous samples

A neutron induced prompt γ -ray spectrometry (NIPS) facility has been developed at the Nuclear Chemistry Research Division, of the Korea Atomic Energy Research Institute (KAERI) with the aim of analyzing the major components of various elements in aqueous samples. The facility is equipped with a ²⁵²Cf neutron source and a γ-γ coincidence setup with two n-type coaxial HPGe detectors based on NIM spectrometric modules in association with data acquisition and spectral analysis systems. The development of the system, its set-up and the calibration of detection efficiency up to 8 MeV using a set of radionuclides and the (n,γ) reactions of chlorine are described in the paper. This revised version was published online in July 2006 with corrections to the Cover Date.     

Automatic interpretation of gamma-ray data obtained in non-destructive activation analysis

The procedure in use at our institute for the extraction of the desired element concentrations in a sample from the peak data obtained by a spectrum analysis program, is described in detail. The method is based on the use of zinc as a single comparator and takes into consideration primary activation products as well as their daughter isotopes. After assigning isotopes to spectrum peaks on the basis of γ-ray energies, the list of possible isotopes is reduced to a list of present isotopes with their concentrations using criteria based on half life, specificity and intensity of γ-rays. For elements not observed, detection limits are estimated. The procedure has been used extensively during the last two years and has shown to produce reliable results.     

Computer-assisted qualitative analysis of gamma-ray spectra

A computer program is described to perform the identification of isotopes in neutron activated samples. The γ-ray energies as obtained from a Ge(Li) γ-ray spectrum are compared with those of a library, containing data for about 250 isotopes. Isotopes whose γ-ray energies match closely with the unknowns are selected as possible constituents. Unlikely attributions are then eliminated by a careful inspection of the γ-rays found. Further exploitation of half-life, the way of production and the sensitivity for the given irradiation and measurement conditions, allow the selection of the most likely constituents in the source. The results of the automated identification agree closely to those obtained by an experienced investigator. The program is written in FORTRAN IV for a PDP-9 computer with a 16 K word memory.     

Accurate and efficient determination of boron content in volcanic rocks by neutron induced prompt gamma-ray analysis

An accurate and efficient analytical method using neutron-induced prompt γ-ray was developed for the determination of boron contents in volcanic rocks. We corrected the effect of sample geometry and flux fluctuation by using silicon as an internal standard. However, we found that the slopes of the calibration line vary among volcanic samples with different matrix. Because the increase of boron activity correlates positively with γ-ray count rate of hydrogen (water), we call this as the hydrogen effect. The hydrogen effect was confirmed by our experiment in which the boron activities showed systematic increase with the amount of added hydrogen (water). Most volcanic rocks, however, contain little water (<2 wt.%) to show this effect. We determined boron contents in various volcanic rocks in order to confirm the validity of the procedure that we established. The analyzed boron contents agreed well with the previous reported values. For efficient PGA of boron in volcanic rocks, we recommend JB-2 (GSJ standard rock) as a single geochemical standard, because of its high boron content (31.2 ppm).     

Radiological characterization of commercially available “radon spa sources”

Nowadays, artificial “radon spa sources” for home baths are commercially available. Although these sources could give a potential radiation exposure to the users, few studies have been reported on their radiological measurements. In the present study, five types of radon spa sources were collected and their radiological characterization was investigated. The followings were estimated for these samples: (1) radon emanation coefficients (dry and water-saturated conditions), (2) surface γ-ray dose rate, (3) surface count rates for α- and β-rays, (4) activity concentrations of ²²⁶Ra, ²³²Th and ⁴⁰K, and (5) concentrations of radon and thoron generated from the sources located in an air flow system. The activity concentrations were very high (except for one sample (named “sample B”), although radon emanation coefficient was low compared with soil. This leads to high concentrations of radon/thoron generated from the sample. The maximum surface γ-ray dose rate was observed for sample A (2.7 μGy h⁻¹). If people stay very close to the sample for a long time, the exposure might be significant.     

Rapid determination of antimony in biological and environmental samples using instrumental neutron activation analysis

A rapid non-destructive activation analysis method has been developed for the determination of antimony. A high resolution low energy Ge detector is used to measure the 61.6 keV γ-ray from^122mSb (T=4.2 min). Sensitivities and detection limits for biological and environmental samples activated with thermal and epithermal neutrons are listed. The time required for the anlaysis is about 12 min per sample using thermal activation and 22 minutes using epithermal activation analysis.     

Prompt gamma-ray yields from proton bombardment of transition elements (Ti to Zn)

Gamma-ray yields from bombardment with protons of thick targets of Ti, V, Mn, Cr, Fe, Co, Ni, Cu and Zn are tabulated for proton energies ranging between 0.6 and 3.2 MeV. The applications of these reactions for quantitative analysis of these chemical elements are discussed. The sensitivity of this technique of analysis is poorer than the PIXE method for these transition elements, but is sufficient for rapid and accurate quantitative analysis of alloys when elements are present in concentrations down to 1%. The knowledge of the γ-ray energies and intensities produced by the bombardment of these elements with protons is also necessary for solving interferences with several γ-rays induced in light elements, for which the proton induced γ-ray technique is sensitive, without any correction for photon attenuation.     

Determination of boron in Japanese geochemical reference samples by neutron-induced prompt gamma-ray analysis

Determination of ppm levels of B in 21 igneous and sedimentary rocks of the Japanese geochemical reference samples prepared by the Geological Survey of Japan (GSJ) has been performed by neutron-induced prompt γ-ray analysis (PGA) using cold and thermal guided neutron beams of the JRR-3M. Owing to the Doppler broadened γ-ray line of B 478 keV, many elements such as Na, Ni, Cl and so on showed spectral interference in the determination of B. The interference was corrected by computer fitting and a reference peak method. The analytical results obtained by the present method almost agreed with the GSJ values recommended in 1994 within the standard deviation of the recommended values. Sodium contents determined by the PGA in the reference rock samples are also reported.