Richard M. Lindstrom

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.

Prompt Gamma-Ray Activation Analysis: Fundamentals and Applications

Prompt gamma-ray activation analysis (PGAA) is an important nuclear analytical technique that complements conventional neutron activation analysis (NAA). When a target is placed in a beam of neutrons, gamma-rays emitted upon neutron capture are measured by a shielded germanium detector, yielding quantitative elemental analysis. The radiation is penetrating and the analysis both nondestructive and independent of the chemical form of the element(s) being measured. The technique is most useful for measurement of light elements (H, B, C, N, Si, P, S, Cl) which can not be easily measured by other methods. Best sensitivity is achieved with neutron beams from research reactors. Although sample preparation is minimal, care must be taken to select proper standards and blanks, and numerous corrections must sometimes be applied to the data from the complex spectra. PGAA has proven useful for multielement analysis of a wide variety of different materials spanning a broad range of scientific disciplines. Of particular importance has been the measurement of hydrogen in materials.

Prompt-Gamma Activation Analysis using the k0 Approach

Applying thek0 standardization method to prompt-gamma activation analysis (PGAA) offers similar benefits as in instrumental neutron activation analysis. It has been demonstrated that under constant flux conditionsk0-factors obtained by normalizing to a titanium comparator, measured separately, yield consistent analytical sensitivity ratios. The ratio method has been generalized by using stoichiometric compounds for the determination ofk0-factors. Since chlorine forms compounds with essentially everyelement and it also serves as a detector efficiency standard,k0 values have been determined relative to chlorine as an internal standard for several analytically important elements in two reactor facilities: the thermal guided beam at the BRR in Budapest and the cold-neutron beams at the NBSR at NIST.

A low-background gamma-ray assay laboratory for activation analysis☆

Abstract The sources of background in a gamma-ray detector were experimentally determined in underground and surface counting rooms, and an optimized shield was constructed at NIST. The optimum thickness of lead was 10–15 cm, with a greater thickness giving an increased background due to the buildup of tertiary cosmic-ray particles. Neither cadmium, tin, copper nor plastic (hydrocarbon or fluorocarbon) was desirable as a shield liner, since all these increased the background continuum or introduced characteristic peaks into the background spectrum. Two broad peaks in the background result from inelastic scattering of cosmic-ray neutrons (0.02 cm −2 s −1 ) in germanium. These neutrons also excite the lower nuclear levels of lead and structural iron to produce additional gamma-ray peaks in the spectrum. The influence of the 20 MW NIST reactor, located 60 m from the detector, was undetectable. Comparisons among detectors and locations clearly separate cosmic from environmental components of the background.

Cold neutron prompt gamma-ray activation analysis at NIST — Recent developments

The cold neutron capture prompt γ-ray activation analysis (CNPGAA) spectrometer located in the Cold Neutron Research Facility (CNRF) at NIST has proven useful for the analysis of hydrogen and other elements in a wide variety of materials. Modifications of the instrument and the CNRF have resulted in improved measurement capabilities for PGAA. The addition of an atmosphere-controlled sample chamber and Compton suppression have reduced γ-ray background and increased signal-to-noise ratio. More recent revisions are expected to yield still further improvement in analytical capabilities. Replacement of the D2O ice cold source with a liquid H2 moderator is expected to yield a 5–10 fold increase in neutron capture rate, and improved neutron and γ-ray shielding will result in further reduction of the background. Other modifications to the instrument allow easier sample mounting and more precise positioning of samples in the neutron beam. Significant improvements in detection limits and analytical accuracy are expected.

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.

Radioactive particle analysis by digital autoradiography

We have been exploring ways to evaluate the activity of radioactive particles that have been detected by phosphor plate digital autoradiography based on photostimulated luminescence (PSL). A PSL system with 25 μm pixel digitization has been applied to particle analysis problems, both qualitatively and quantitatively. Two data evaluation methods are currently employed: (1) bulk area signal measurement, and (2) discrete event counting which may include spectral evaluation. The first method is conventional, whereas the second method requires high spatial resolution and is presented here for the first time. The counting methods can discriminate between alpha and background counts. The unshielded background signal accumulation rate was determined by the bulk area method. Using the spectral method of evaluation for α-particle events, the mean signal intensity per recorded α-particle was measured, and the detective quantum efficiency (DQE) was found to be nominally 100%. We present a comparison to gamma-spectrometry for sub-Bq 137Cs activities, and demonstrate an application for the qualitative assay of International Atomic Energy Agency swipe samples collected from uranium enrichment facilities.

Neutron captue prompt gamma-ray activation analysis at the NIST Cold Neutron Research Facility

An instrument for neutron capture prompt gamma-ray activation analysis (PGAA) has been constructed as part of the Cold Neutron Research Facility at the 20 MW National Institute of Standards and Technology Research Reactor. The neutron fluence rate (thermal equivalent) is 1.5·108 n ·cm−2·s−1, with negligible fast neutrons and gamma-rays. With compact geometry and hydrogen-free construction, the sensitivity is sevenfold better than an existing thermal instrument. Hydrogen background is thirtyfold lower.

Measuring hydrogen by cold-neutron prompt-gamma activation analysis

By irradiating with cold neutrons and avoiding hydrogenous materials of construction, we have developed a PGAA instrument at the Cold Neutron Research Facility at NIST with hydrogen detection limits in the microgram range in many materials. Quantities of 5–10 μg H/g are presently measurable in gram-sized samples of silicon or quartz, and of order 0.01 wt % can be quantitatively measured in complex silicate rocks.

Precise determination of aluminum by instrumental neutron activation

Because of the short half life of Al-28, the determination of aluminum by neutron activation is subject to many inaccuracies: variation of irradiation conditions between sample and standard, uncertainties in timing, and the effects of high and varying count rate, in addition to other sources of error that must be controlled even in work with long-lived nuclides. These errors can all be made smaller than the fundamental limit set by counting statistics, even when that limit is below 0.5 percent. The transfer function from the observed number of net counts to the counting rate at the end of irradiation is modeled as a product of three processes: radioactive decay and extending and nonextending dead time.The procedure has been applied to the analysis of NBS SRM 1633a Fly Ash. The mean concentration measured was 14.085% Al, with a standard deviation of the mean 0.023% Al for four determinations. The final results showed no significant imprecision beyond counting statistics. The accuracy of the method is shown by the analysis of high-purity single-crystal sapphire.