Multi-element analysis of environmental samples by cold and thermal guided neutron induced prompt gamma-ray measurement

Non-destructive multi-element determination in environmental samples by neutron-induced prompt -ray analysis (PGA) has been investigated. Comparative standardization for the elements including H, B, C, N, Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, Mn, Fe, Co, Cd, Sm, Gd, Hg by PGA has been carried out using the cold and thermal guided neutron beams of JRR-3M reactor and then several environmental reference materials have been analyzed. Accuracy and precision of better than 20% were found for these elemental analyses except for H, C, N and Cl in biological samples. Detection limits in various environmental matrices were 25 to 820 ng/g for B, Cd, Sm and Gd, 1.1 to 820 g/g for H, Na, S, Cl, K, Ti, Mn, Co and Hg, and 0.031 to 10% for C, N, Mg, Al, Si, P, Ca and Fe. The present method is being applied to environmental studies of post war Persian Gulf together with INAA and ICP-MS.     

Activation analysis opportunities using cold neutron beams

Guided beams of cold neutrons being installed at a number of research reactors may become increasingly available for analytical research. A guided cold beam will provide higher neutron fluence rates and lower background interferences than in present facilities. In an optimized facility, fluence rates of 10⁹ n·cm^–2·s^–1 are obtainable. Focusing a large area beam onto a small target will further increase the neutron intensity. In addition, the shift to lower neutron energy increases the effective cross sections. The absence of fast neutrons and gamma rays permits detectors to be placed near the sample without intolerable background, and thus the efficiency for counting prompt gamma rays can be much higher than in present systems. Measurements made at the hydrogen cold source of the FRJ-2 (DIDO) reactor at the KFA provide a numerical evaluation of the improvements in PGAA with respect to signal-to-background ratios of important elements and matrices.     

Prompt gamma-ray neutron activation analysis by the absolute method

In this study an investigation into the applicability of the absolute method in Prompt Gamma-ray Neutron Activation Analysis (PGNAA) was undertaken. Although the system parameters are adequately characterized, the scatter in nuclear data for a number of elements is significant. For our particular experimental set up the K-factors were calculated for a number of elements using both Au and Fe as monostandards. A comparison was made between the calculated and experimentally determined K-factors and from this comparison the feasibility of the absolute method in neutron prompt gamma-rays can be realized for a number of elements.     

Prompt gamma-ray neutron activation analysis for multi-element determination in sediment samples

A facility for the irradiation of internal targets has been installed at the research reactor FRG-of the GKSS Research Center. Thermal-neutron induced prompt gamma radiation was detected by pair spectrometer. With this experimental arrangement concentrations of the major and mino elements Na, Al, Si, K, Ca, Ti, Mn, Fe, Zn, Cl, and S, as well as of the trace constituents Cr Ni, Cu Cd, and Hg of samples from a sediment core of the Elbe River could be determined. The results indicate, that prompt gamma-ray neutron activation analysis (PGNAA) is a powerful instrumental tool for a complete characterization of the main sediment constituents and for the detection of the trace elements Cd and Hg which are of considerable ecological relevance.     

Prompt gamma cold neutron activation analysis applied to biological materials

Summary Cold neutrons at the external neutron guide laboratory (ELLA) of the KFA Jülich are used to demonstrate their profitable application for multielement characterization of biological materials. The set-up and experimental conditions of the Prompt Gamma Cold Neutron Activation Analysis (PGCNAA) device is described in detail. Results for C, H, N, S, K, B, and Cd using synthetic standards and the “ratio” technique for calculation are reported for several reference materials and prove the method to be reliable and complementary with respect to the elements being determined by INAA. IAEA fellow at the KFA from 6. 3. 91 to 2. 9. 91 on contract No. VIE/9016R.     

Prompt gamma-ray analysis of archaeological bronze

Prompt γ-ray analysis using the internal monostandard method was applied to voluminous archaeological bronze mirrors produced in ancient China. Sn/Cu content ratios were determined nondestructively by this method. Furthermore, Au/Cu, As/Cu, and Sb/Cu content ratios were determined by means of measuring decay γ-rays emitted from radioactive nuclides produced within samples via (n,γ) reactions. It is clear that the Sn/Cu content ratios in bronze mirrors produced in the Sung era is smaller than in ones produced in between the Han and the Tung era.     

Prompt gamma activation analysis using a chopped neutron beam

A beam chopper has been developed at the cold neutron PGAA facility of the Budapest Research Reactor. In the open phase of the chopper the usual prompt gamma-spectrum is recorded, while in the decay phase short-lived decay lines can be collected with good counting statistics on an extremely low baseline. A series of elements has been measured with the chopped beam technique to assess the capabilities of the new technique. An archaeological sample was also examined, to demonstrate how spectral interferences can be resolved.     

Prompt gamma-ray neutron activation analysis methodology for determination of boron from trace to major contents

Prompt gamma ray neutron activation analysis methodologies were standardized using a reflected neutron beam and Compton suppressed γ-ray spectrometer to quantify boron from trace to major concentrations. Neutron self-shielding correction factors for higher boron contents (0.2–10 mg) in samples were obtained from the sensitivity of chlorine by irradiating KCl with and without boron. This method was validated by determining boron concentrations in six boron compounds and applied to three borosilicate glass samples with boron contents in the range of 1–10 mg. Low concentrations of boron (10–58 mg kg⁻¹) were also determined in two samples and five reference materials from NIST and IAEA.     

Determination of boron in materials by cold neutron prompt gamma-ray activation analysis

An instrument for cold neutron prompt gamma-ray activation analysis (PGAA), located at the NIST Center for Neutron Research (NCNR), has proven useful for the measurement of boron in a variety of materials. Neutrons, moderated by passage through liquid hydrogen at 20 K, pass through a (58)Ni coated guide to the PGAA station in the cold neutron guide hall of the NCNR. The thermal equivalent neutron fluence rate at the sample position is 9 x 10(8) cm(-2) s(-1). Prompt gamma rays are measured by a cadmium- and lead-shielded high-purity germanium detector. The instrument has been used to measure boron mass fractions in minerals, in NIST SRM 2175 (Refractory Alloy MP-35-N) for certification of boron, and most recently in semiconductor-grade silicon. The limit of detection for boron in many materials is <10 ng g(-1).     

Improvements in food analysis by thermal neutron capture prompt gamma-ray spectrometry

Summary The thermal neutron prompt gamma-ray activation analysis (PGAA) facility, operated by the US Food and Drug Administration and National Institute of Standards and Technology Center for Neutron Research, has been redesigned to lower background radiation levels and improved analytical capabilities. Analysis of 22 element standards and food and botanical certified reference materials revealed significant sensitivity increases and lower limits of detection for H, B, C, N, Na, Al, P, S, Cl, K, Ca, Fe, and Cd. Mass fractions for these elements, as well as Mg, Al, Si, Ti, Mn, Fe, Cu, I, Zn, Sm, and Gd, were determined for 6 dietary supplements.     

Coincidence and anti-coincidence measurements in prompt gamma neutron activation analysis with pulsed cold neutron beams

A novel approach is implemented to alleviate some persistent problems in neutron capture prompt gamma activation analysis (PGAA). Detection sensitivities of PGAA are often restricted by the following factors: poor signal to noise ratios, interferences from background signals, and, in some cases, overlapping energy lines from different origins, namely ultra short-lived decay lines interfering with prompt decay. Timing the gamma-ray acquisition with the actual capture events using a pulsed beam of cold neutrons allows discrimination between prompt and delayed emissions from a sample source as well as against background events. Coincidence gating selects the prompt gamma-ray emissions. Contributions of background capture gamma-rays are suppressed because of different flight times of neutrons to the sources of background radiation, providing a reduction in direct gamma-ray interferences. Anti-coincidence gating allows measurement of only decay radiation that originates from short-lived activated states of the nuclides after capture. Spectra of decaying nuclides are free of interfering prompt activities, as well as have lower continuum background from Compton scattering of high-energy prompt gamma-rays in the detector. The measurements provide the opportunity to use ultra-short half-life nuclides for analytical purposes, no sample transfer times are lost, and repetitive activation and counting cycles are achieved with the use of pulsed neutron beams.     

Multielement analysis of major and minor elements by thermal neutron induced capture gamma-ray spectrometry

The utility of prompt gamma-rays from thermal neutron capture for the measurement of nine elements (Si, Al, Fe, Na, K, Ca, Ti, Mg and P) in major and minor abundance has been investigated. National Bureau of Standards (NBS) and United States Geological Survey (USGS) standards were used to demonstrate generally good agreement between experimental measurements and certified values. Usually accuracies and precisions of ±10% were observed.     

Development of a procedure for measuring nitrogen by cold neutron prompt gamma-ray activation analysis

An instrument for cold neutron prompt gamma-ray activation analysis (CNPGAA) has been used for the nondestructive determination of nitrogen. The samples were analyzed in an evacuated box to minimize background from neutron capture by atmospheric nitrogen. The system features lower background and lower detection limits than obtainable with the University of Maryland-National Institute of Standards and Technology (NIST) thermal neutron PGAA instrument. CNPGAA has been used to measure nitrogen in standard reference materials which included biological materials and soils; the results are in agreement with certified values. The detection limit for nitrogen in most biological and geological samples is near 1000 mg kg-1.     

Design of a new instrument for cold neutron prompt gamma-ray activation analysis at NIST

A new instrument for cold neutron prompt gamma-ray activation analysis (CNPGAA) is being designed and constructed at the NIST Center for Neutron Research (NCNR). The new instrument is expected to have lower gamma-ray and neutron background and better detection limits for most elements than the current cold neutron PGAA instrument. Other advantages over the current facility will include the ability to analyze larger samples and greater overall measurement capability due to the addition of scanning stages, cryostats, and sample changers.     

Characterization of the wavelength spectrum of guided neutron beams

Summary A simple method is introduced for the determination of the effective temperature of neutron beams. It is mathematically derived that the thermal equivalent neutron flux measured with a thin foil made from a 1/<Emphasis Type=Italic>v</Emphasis>-nuclide is proportional to the product of the real flux and the average wavelength. The real flux can be determined using fully absorbent materials. From the ratio of the two fluxes the average wavelength and the effective temperature can be determined. The method has been tested in thermal and cold neutron beams.     

Prompt and delayed radiation measurements in the elemental analysis of biological materials: The case for neutron induced gamma-ray emission tomography

Nuclear and atomic methods of analysis, which rely on the detection of prompt and delayed radiations, emitted as a result of interactions between radiation probe and target, for determining the elemental concentration in vivo and in vitro, are summarily reviewed, with reference to bone analysis; the demand for methods which provide information about elemental distribution is highlighted. The way neutrons can be used as probes to investigate the composition and structure of objects by employed the principles of computerised tomography are outlined and the novel modes of utilisation are briefly described: neutron transmission tomography, neutron induced prompt gammaray emission tomography and neutron induced delayed gamma-ray emission tomography. The latter method, alternatively termed neutron activation tomography, is then used to determine on-destructively the distribution of Na in selected planes of a human tibia, in vitro, by measuring the activity of²⁴Na using a NaI(Tl) and a Ge(Li) detector in a tomographic scanner which incorporates a microcomputer for control, data acquisition and image reconstruction. The problems of attenuation and scattering are discussed as are the limitations for quantitative results of this useful new mode of tomography which provided information about composition and elemental distribution in a material.     

The use of element ratios to eliminate analytical bias in cold neutron prompt gamma-ray activation analysis

Analytical bias due to neutron scattering and absorption in cold neutron prompt gamma-ray activation analysis (CNPGAA) is largely eliminated for homogeneous samples when element ratios are measured. Application of sensitivity ratios (measured relative to titanium) to the multielement analysis of the Allende meteorite increases both the speed and accuracy of the measurement. Greater measurement accuracy is achieved for some samples when ratios of element concentrations are reported. Problems are encountered when applying the ratio method to measurement of elements which deviate from 1/v behavior, and when gamma-ray attenuation or sample heterogeneity are significant.     

Prompt gamma neutron activation analysis of boron with a 241Am-Be neutron source

A prompt gamma neutron activation analysis (PGAA) setup installed at ANRTC has been used to analyze boron. It consists of a 22.6% REGe detector and a 740 GBq ²⁴¹Am-Be neutron source moderated with water and paraffin. At the sample irradiation position, the thermal neutron fluence rate measured was 2.36·10⁴ n·m^–2· s^–1 and the corresponding Cd-ratio was 22 for gold monitor. The absolute detection efficiency in the range of 120–1500 keV was determined using ¹⁵²Eu standard solution. The sensitivity and detection limit for standard boric acid samples has been determined. The boron content in boric acid prepared from Turkish borate ores is measured to be 15.91±0.46% wt.     

Some practical procedures in computerized thermal neutron activation analysis with Ge(Li) gamma-ray spectrometry

The practical use of a correction procedure for random coincidence losses, the determination of the detection limit and the standardization of measuring conditions are described. Special correction methods for the interference of the Cu analysis by²⁴Na, the burn-up of the radioactive nuclide formed and the interference of the Pt determination by Au are also given.     

Prompt gamma-ray activation analysis for certification of sulfur in fuel oil SRMs

A combination of cold neutron prompt gamma-ray activation analysis (CNPGAA) and thermal neutron (TN) PGAA was used to determine sulfur in fuel oils to develop a method to provide values for certification. CNPGAA was used to measure S/H mass ratios, and TNPGAA to measure hydrogen mass fractions. Measurements were combined to determine sulfur mass fractions (with expanded uncertainties) of 2.159 ± 0.072 % for SRM 1622e, 0.7066 ± 0.0120 % for SRM 1619b, and 0.1266 ± 0.0030 % for SRM 1617b, in agreement with certified values. The results validate the method as suitable for certification of sulfur at mass fractions ≥0.1 %.