Prompt Gamma Neutron Activation Analysis Research Articles

Use of neutron activation analysis for the characterization of single-wall carbon nanotube materials

Instrumental neutron activation analysis (INAA) and prompt gamma neutron activation analysis (PGAA) were used to characterize a variety of single-wall carbon nanotube (SWCNT) materials from different principal production processes, as well as a material containing SWCNTs together with other carbon species, catalyst residues, and trace element contaminants to be issued by the National Institute of Standards and Technology for characterization and distribution as Standard Reference Material SRM 2483 Carbon Nanotube Soot. INAA proved to be well suited for the direct determination of catalyst and contaminant trace elements requiring only minimal sample preparation. PGAA complemented the INAA data in particular with determinations of the light elements. Carbon and hydrogen results provided information on the materials purity and storage properties. Strategies for the quality assurance of the measurements in these new materials were developed. INAA and PGAA data were provided for the value assignment of mass fractions of catalyst and trace elements in the candidate SRM and a systematic overview was obtained of the catalyst and trace element contaminants associated with each of the major production routes.

A brief introduction to NAA facilities of China Advance Research Reactor at CIAE

China Advance Research Reactor (CARR) at China Institute of Atomic Energy (CIAE), with a non-perturbed maximum thermal neutron flux of 1 × 1015 cm−2 s−1 at the center of active area, is one of the most powerful research reactors in the world. Three neutron channels have been allocated for conventional neutron activation analysis (NAA), thermal neutron prompt gamma activation analysis (PGAA) and cold neutron PGAA, respectively. Two irradiation tube systems are installed in the conventional NAA channel. One of them is for short irradiation with the rabbit size of diameter (Φ)19 × 40 mm, the other one is for long irradiation with the rabbit size of Φ39 × 70 mm. The medium temperature is about 45 °C and the thermal neutron flux is about 3 × 1014 cm−2 s−1 at sample positions. The flux gradient is expected to be very small according to the designed neutron flux distribution. Pneumatic systems are used for samples transfer. The speed of rabbits is designed to be about 20 m/s, and it takes 3 s to travel from irradiation position to detector. Three sets of gamma counting systems and one delayed neutron counting system are being equipped for routine analysis. They are designed for running continuously and automatically. And all the functions can be operated at laboratory or office through remote controlled computer. Software has been made domestically for spectrum peak search, concentration calculation with relative method and k0 method with interference corrections and some other functions for the convenience of users.

Development of a prompt gamma neutron activation analysis facility for 10B concentration measurements at RA-3: Design stage

A PGNAA facility is being developed for (10)B concentration measurements at RA-3 reactor. Its design targets detection limits better than tenths of a microgram and irradiation times on the order of minutes. Computational models were developed, which estimated thermal neutron fluxes in irradiation position to be larger than 10(9) n cm(-2) s(-1). Calculated amounts of photons and fast neutrons make necessary for filter/moderator arrangements. An irradiation device was designed and numerically tested, which is being built and is to be used for performing characterizing measurements.

Detection efficiency of low levels of boron and cadmium with a LaBr 3:Ce scintillation detector

The response of a cylindrical 3 in.×3 in. (height×diameter) LaBr 3:Ce detector was measured for low energy prompt gamma-rays from boron and cadmium contaminated water samples using a newly designed portable neutron generator-based Prompt Gamma Neutron Activation Analysis (PGNAA) setup. Prompt gamma-rays were measured from water samples contaminated with 0.031, 0.125, 0.250 and 0.5 wt% boron and 0.0625, 0.125, 0.250 and 0.500 wt% cadmium. The experimental yield of boron and cadmium prompt gamma-rays measured with the LaBr 3:Ce detector based PGNAA setup were compared with the results of Monte Carlo calculations. An excellent agreement between the experimental and calculated yields of 478 keV gamma-ray from boron and 558 keV gamma-rays from cadmium from boron and cadmium contaminated water samples, indicate an excellent response of the LaBr 3:Ce detector for the low energy prompt gamma-rays.

Synthesis of platinum and platinum–ruthenium-modified diamond nanoparticles

With the aim of developing dimensionally stable-supported catalysts for direct methanol fuel cell application, Pt and Pt–Ru catalyst nanoparticles were deposited onto undoped and boron-doped diamond nanoparticles (BDDNPs) through a chemical reduction route using sodium borohydride as a reducing agent. As-received commercial diamond nanoparticles (DNPs) were purified by refluxing in aqueous nitric acid solution. Prompt gamma neutron activation analysis and transmission electron microscopy (TEM) techniques were employed to characterize the as-received and purified DNPs. The purified diamond nanoparticulates, as well as the supported Pt and Pt–Ru catalyst systems, were subjected to various physicochemical characterizations, such as scanning electron microscopy, energy dispersive analysis, TEM, X-ray diffraction, inductively coupled plasma-mass spectrometry, X-ray photoelectron spectroscopy, and infrared spectroscopy. Physicochemical characterization showed that the sizes of Pt and Pt–Ru particles were only a few nanometers (2–5 nm), and they were homogeneously dispersed on the diamond surface (5–10 nm). The chemical reduction method offers a simple route to prepare the well-dispersed Pt and Pt–Ru catalyst nanoparticulates on undoped and BDDNPs for their possible employment as an advanced electrode material in direct methanol fuel cells.

Estimation of minimum detectable concentration of chlorine in the blast furnace slag cement concrete

The Prompt Gamma Neutron Activation Analysis technique was used to measure the concentration of chloride in the blast furnace slag (BFS) cement concrete to assess the possibility of reinforcement corrosion. The experimental setup was optimized using Monte Carlo calculations. The BFS concrete specimens containing 0.8–3.5 wt.% chloride were prepared and the concentration of chlorine was evaluated by determining the yield of 6.11, 6.62, 7.41, 7.79 and 8.58 MeV gamma-rays. The Minimum Detectable Concentration (MDC) of chlorine in the BFS cement concrete was estimated. The best value of MDC limit of chlorine in the BFS cement concrete was found to be 0.034 ± 0.011 and 0.038 ± 0.012 wt.% for 6.11 and 6.62 MeV prompt gamma-rays. Within the statistical uncertainty the lower bound of the measured MDC of chlorine in the BFS cement concrete meets the maximum permissible limit of 0.03 wt.% of chloride set by the American Concrete Institute.

The feasibility of in vivo detection of gadolinium by prompt gamma neutron activation analysis following gadolinium-based contrast-enhanced MRI

The feasibility of using the McMaster University in vivo prompt gamma neutron activation analysis system for the detection of gadolinium has been investigated. Phantoms have been developed for the kidney, liver, and the leg muscle. The initial detection limits are determined to be 7.2 ± 0.3 ppm for the kidney, 3.0 ± 0.1 ppm for the liver, and 2.33 ± 0.08 ppm for the lower leg muscle. A few system optimizations have been tested and show significant detection limit reduction from these initial values. The technique is promising and shows feasibility for in vivo studies of gadolinium retention.

A benchmarked MCNP model of the in vivo detection of gadolinium by prompt gamma neutron activation analysis

Abstract Gadolinium (Gd)-based contrast agents are a valuable diagnostic aid for magnetic resonance imaging (MRI). The amount of free Gd deposited in tissues following contrast enhanced MRI is of toxicological concern. The McMaster University in vivo prompt gamma neutron activation analysis facility has been adapted for the detection of Gd in the kidney, liver, and the leg muscle. A simple model of the HPGe detector used for detection of the prompt γ-rays following Gd neutron capture has been created using Monte Carlo simulation. A separate simulation describing the neutron collimation and shielding apparatus has been modified to determine the neutron capture rate in the Gd phantoms. The MCNP simulation results have been confirmed by experimental measurement. The deviations between MCNP and the experiment were between 1% and 18%, with an average deviation of 3.8 ± 6.7%. The validated MCNP model is to be used to improve the Gd in vivo measurement sensitivity by determining the best neutron moderator/reflector arrangement.

Analysis of hydrogen concentration in low-alloy steel

The hydrogen concentration for the reference material low-alloy steel was estimated using prompt gamma neutron activation analysis. The hydrogen concentration had a range of 0.91–1.14 mg/kg as measured by the prompt gamma activation method but the reference value was about 1.0 mg/kg as measured by the ICP/AES method. The relative error appeared to be 14% and the differences showed as the background by blank. The standard reference material (NIST SRM) was used for the analytical control.

Relating Complex Fluid Composition and Thermophysical Properties with the Advanced Distillation Curve Approach

AbstractComplex fluids have long posed a significant challenge in our ability to characterize and model fluid properties. Here, we consider complex fluids to be mixtures with many components that can differ significantly in polarity and polarizability. The penultimate complex fluid is crude oil, although many other fluids such as finished fuels are also highly complex. We have recently introduced a measurement strategy that can simplify these efforts and provides the added potential of linking chemical composition (i.e. analytical) information with physical property information. In addition to chemical characterization, the approach provides the ability to calculate thermodynamic and transport properties for such complex heterogeneous streams. The technique is based on the advanced distillation curve (ADC) metrology, which separates a complex fluid by distillation into fractions that are sampled, and for which thermodynamically consistent temperatures are measured at atmospheric pressure. The collected sample fractions can be analyzed by any method that is appropriate. Analytical methods we have applied include gas chromatography (with flame ionization, mass spectrometric and sulfur chemiluminescence detection), thin‐layer chromatography, FTIR, Karl Fischer coulombic titrimetry, refractometry, corrosivity analysis, neutron activation analysis and cold neutron prompt gamma activation analysis. We have applied this method on product streams such as finished fuels (gasoline, diesel fuels, aviation fuels, rocket propellants), crude oils (including a crude oil made from swine manure) and waste oil streams (used automotive and transformer oils). In this review, we describe the essential features of the ADC metrology with illustrative examples.

Non-destructive analysis of concrete for corrosion studies using nuclear technique

Chloride-induced reinforcement corrosion is the principal cause of deterioration of concrete structures in the Arabian Gulf and the world over. Preventive measures against corrosion require maintaining the chloride and sulphate concentration in concrete below the threshold limits specified by the standards. This requires monitoring the chloride and sulphate concentration in concrete, and a nondestructive technique is preferable for this purpose. The Prompt-Gamma Neutron Activation Analysis (PGNAA) technique can be used to monitor the concentration of corrosive elements in concrete specimens. An accelerator-based PGNAA setup has been developed to measure the chloride and sulphate concentration in concrete. The PGNAA technique has been utilised successfully to measure the elemental composition of concrete. In this regard, several studies were undertaken to determine the calcium, silicon, chloride and sulphate concentration in the concrete specimens. Furthermore, the concentration of compounds, such as lime and silica was also determined. The results of these studies along with a description of the facility are presented in this paper.

Combined application of Monte Carlo method and neural networks to simulate qualitative prompt gamma neutron activation analysis

Prompt gamma spectrum produced by thermal neutron absorption and fast neutron inelastic scattering is simulated using Monte Carlo code MCNP4C. The simulated spectrum is analyzed with artificial neural network techniques. The neural network in our study is trained based on back-propagation algorithm with 138 gamma ray spectra. Elements existing in the 20 different substances are specified. The ANN could identify elements correctly in 96% of input cases.

Characterization of an Am–Be PGNAA set-up developed for in situ liquid analysis: Application to domestic waste water and industrial liquid effluents analysis

A prompt gamma neutron activation analysis (PGNAA) set-up with an Am–Be source developed for in situ analysis of liquid samples is described. The linearity of its response was tested for chlorine and cadmium dissolved in water. Prompt gamma efficiency of the system has been determined experimentally using prompt gamma of chlorine dissolved in water and detection limits for different elements have been derived for domestic waste water. A methodology to analyze any kind of liquid is then proposed. This methodology consists mainly on using standards with water as bulk or in the case of absolute method, to use gamma efficiency determined with prompt gammas emitted by chlorine dissolved in water. To take into account the thermal neutron flux variations inside the samples, flux monitoring was carried out using a He-3 neutron detector placed at the external sample container surface. Finally, to correct for the differences in gamma attenuation, average gamma attenuations factors were calculated using MCNP5 code. This method was then checked successfully by determining cadmium in industrial phosphoric acid and our result was in good agreement with that obtained with inductively coupled plasma (ICP) method.

Design, construction and characterization of a prompt gamma activation analysis facility at the Oregon State University TRIGA® reactor

A prompt gamma neutron activation analysis facility has been designed, built, and characterized at the Oregon State University TRIGA® reactor. This facility was designed for versatile multi-elemental analyses. The facility utilizes the leakage neutrons originating from beam port #4 of the Oregon State University TRIGA® reactor. The neutrons are collimated through a series of lead and Boral® collimators, and filtered through both a bismuth filter and single-crystal sapphire. Samples are irradiated in a sample chamber outside the biological shielding of the reactor, and the resulting gamma radiation produced from neutron interactions within the sample is monitored using a high-purity germanium detector (HPGe). The thermal and epithermal neutron fluxes were measured using gold-foil irradiations and found to be 2.81 × 107 and 1.70 × 104 cm−2 s−1, respectively. The resulting cadmium ratio was 106. Measured detection limits for boron, chlorine, and potassium in a NIST SRM 1571 orchard leaf were 5.6 × 10−4 mg/g, 8.2 × 10−2 mg/g, and 1.0 mg/g, respectively. Detection limits for additional elements and samples are presented.

Increasing the Personnel Safety of a Landmine Detection System using Proper Shielding Materials

It has been proven that landmine detection systems based on prompt gamma neutron activation analysis method can be used effectively in detecting low metal content mines. Unfortunately, neutron and gamma radiations of these systems are inevitable. Therefore, the personnel safety of these devices is one of the major limitations in using these systems. In this work, a system composed of a moderated americium-beryllium neutron source was considered. We have investigated different thicknesses of proper neutron shielding materials such as polyethylene and boric acid around the system to shield neutrons and increase the safety conditions for the operators. The effect of using different thicknesses of a cylindrical lead shield (around the source) for shielding the gamma radiation of the source was also studied. Several experiments were done to measure neutron and gamma dose equivalent rate at different distances from the source. Most of the results were compared with the results obtained by Monte Carlo N-particle transport 4C code. Finally, we found a system that is safe for the operators who work at about a 1 m distance from the landmine detection system.

Determination of chlorine concentrations in whole rock: Comparison between prompt-gamma activation and isotope-dilution AMS analysis

Accurate determination of chlorine concentrations in terrestrial rocks is of importance for the interpretation of terrestrial in-situ cosmogenic 36Cl. Neutron capture by 35Cl, together with production from Ca and K, is one of the three major production pathways of 36Cl in rocks. Here, we present an inter-comparison of chlorine determinations by two procedures. The first approach is an independent Cl determination by prompt-gamma (neutron) activation analysis (PGAA). The second method is isotope-dilution based on isotopically enriched stable chlorine carrier added during chemical sample preparation for accelerator mass spectrometry (ID-AMS). Twenty-six (26) whole rock samples have been processed for PGAA and ID-AMS analysis. This study constitutes the first published inter-comparison for concentrations below 100 μgCl/g. Our results show no significant difference in Cl concentrations between methods. This agreement indicates good retention of chloride during the procedure we employ for whole rock sample dissolution. No significant loss of stable chlorine from either the spike or the sample occurs before isotopic equilibrium is reached, prior to AgCl precipitation. Uncertainties, which are <5% for both methods, affect the uncertainty of the total 36Cl production rate less than 2% for our samples. The Cl concentration measured by PGAA can be used to calculate the amount of isotopically enriched spike for AMS-ID sample preparation with the aim to optimize 36Cl analysis. Furthermore, PGAA offers an advance for the interpretation of 36Cl measurements. It allows measurement of concentrations of major, minor and trace elements including the elements for 36Cl production (Cl, K, Ca, Ti, and Fe), as well as of neutron absorbers and neutron moderators (H, B, Sm and Gd). These measurements are performed simultaneously and with a precision necessary for calculating the relative contributions to 36Cl production from the different mechanisms.

A comparison between cold and thermal neutron prompt gamma activation analysis in the determination of carbon, nitrogen, and phosphorus in cattail

Methods for the determination of total carbon (TC), total nitrogen (TN), and total phosphorus (TP) in cattail (Typha domingensis) using cold and thermal neutron prompt gamma activation analysis (CNPGAA and TNPGAA) have been developed in the CNPGAA and TNPGAA facilities at the National Institute of Standards and Technology (NIST), and evaluated through the analysis of Standard Reference Materials (SRMs) in previous studies. There are major issues that impact the sensitivities of C, N and P using CNPGAA and TNPGAA including the effects of hydrogen content in samples, sample thickness and Compton scattering. However, interference from chlorine (Cl) in cattails has a major impact on the detection of P. This paper compares the effects of hydrogen content, sample thickness and Compton scattering on the sensitivities of C, N, and P between CNPGAA and TNPGAA and provides a resolution to the Cl interference on P in cattail.

Effects of sample and spectrum characteristics on cold and thermal neutron prompt gamma activation analysis in environmental studies of plants

Previous studies including the development of methods for the determination of carbon, nitrogen, and phosphorus in cattail using cold neutron prompt gamma activation (CNPGAA) and thermal neutron prompt gamma activation analysis (TNPGAA); evaluation of the precision and accuracy of these methods through the analysis of Standard Reference Materials (SRMs); and comparison of the sensitivity of CNPGAA to TNPGAA have been done in the CNPGAA and TNPGAA facilities at the National Institute of Standards and Technology (NIST). This paper integrates the findings from all of these prior studies and presents recommendations for the application of CNPGAA and TNPGAA in environmental studies of plants based on synergistic considerations of the effects of neutron energy, matrix factors such as chlorine content, Compton scattering, hydrogen content, sample thickness, and spectral interferences from Cl on the determination of C, N, and P. This paper also provides a new approach that simulates a sensitivity curve for an element of interest (S), which is a function of hydrogen content (X) and sample thickness (Y) as follows: S = aX + bY + c (where a, b, and c are constants). This approach has provided more accurate results from the analysis of SRMs than traditional methods and an opportunity to use models to optimize experimental conditions.

Combinatorial study of thin film metal hydride by prompt gamma activation analysis

Cold neutron prompt gamma activation analysis (PGAA) was used to determine the mass of hydrogen in Mg hydride thin films with varying hydrogenation times. The results suggest that hydrogenation of the Mg thin films remains unsaturated even after 48 h of treatment, contrary to the indications of inferential hydrogen measurement methods. To demonstrate PGAA as an effective combinatorial methodology for hydride thin films, a continuously varying composition gradient of thin MgyTi(1−y) hydride film with y ranging from 0.65 to 0.94 was prepared and analyzed by both PGAA and instrumental neutron activation analysis (INAA). The variation in the molar ratio of Mg, Ti, and H was obtained for nine 5 mm wide segments of the film.

Simulating the introduction of a sapphire crystal into an epithermal neutron beamline

The epithermal beamline at the Portuguese Research Reactor is being optimized for Prompt Gamma Neutron Activation Analysis (PGNAA). One of the major changes is to thermalise the beam by the introduction of a sapphire crystal into the beamline. Placing the sapphire at the exit of the beamline would greatly reduce the alterations and work necessary to the port and make the crystal easily removable. However, the scattered neutrons from the sapphire would increase both the neutron-induced detector damage and the background radiation. MCNPX was used to simulate the crystal in the beam port and at the exit of the port.