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All sources NASA NTRS DOE OSTI

DOE OSTI2013

Neutron Damage in Mechanically-Cooled High-Purity Germanium Detectors for Field-Portable Prompt Gamma Neutron Activation Analysis (PGNAA) Systems

Prompt Gamma Neutron Activation (PGNAA) systems require the use of a gamma-ray spectrometer to record the gamma-ray spectrum of an object under test and allow the determination of the object’s composition. Field-portable systems, such as Idaho National Laboratory’s PINS system, have used standard liquid-nitrogen-cooled high-purity germanium (HPGe) detectors to perform this function. These detectors have performed very well in the past, but the requirement of liquid-nitrogen cooling limits their use to areas where liquid nitrogen is readily available or produced on-site. Also, having a relatively large volume of liquid nitrogen close to the detector can impact some assessments, possibly leading to a false detection of explosives or other nitrogen-containing chemical. Use of a mechanically-cooled HPGe detector is therefore very attractive for PGNAA applications where nitrogen detection is critical or where liquid-nitrogen logistics are problematic. Mechanically-cooled HPGe detectors constructed from p-type germanium, such as Ortec’s trans-SPEC, have been commercially available for several years. In order to assess whether these detectors would be suitable for use in a fielded PGNAA system, Idaho National Laboratory (INL) has been performing a number of tests of the resistance of mechanically-cooled HPGe detectors to neutron damage. These detectors have been standard commercially-available p-type HPGe detectors as well as prototype n-type HPGe detectors. These tests compare the performance of these different detector types as a function of crystal temperature and incident neutron fluence on the crystal.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2020

Comparison of active interrogation methods for source location in a scattering and absorbing medium, consisting of PGNAA, and an AmBe quasi-forward biased directional source

Source location of Special Nuclear Material (SNM) encompassing 95% 235 U and 239 Pu is identified by utilizing a directional source from Patent No: US20190013109A1 using Prompt Gamma Neutron Activation Analysis (PGNAA) and neutron spectroscopy simulated with Monte-Carlo N-Particle transport 6.2 (MCNP). BC-408, HPGe, LaBr 3 detector arrays were used to identify the location of the SNM using total counts incident on each detector, and PGNAA photopeaks from HPGe and LaBr 3 detector arrays in a polyethylene shield. The conducted simulations varied the volume and location of the SNM in the MCNP input files to observe how the source location method behaved. PGNAA photopeaks used for source identification include 61 keV from fission, 2.223 MeV prompt gamma from hydrogen, 511 keV annihilation, and a single and double escape peaks from the prompt gamma interaction from hydrogen. The capabilities of each detector systems to acquire well resolved photopeaks with a 1% relative error or less, and total relative error for F4 and F8 tallies were less than 0.015% relative error. Source predictions of the SNM with uneven amounts of polyethylene shielding between the source and detectors was observed to overpredict and give invalid source location predictions. Source locations of the SNM with even amounts of polyethylene material between the source and each detector were found to be valid. With a 1 Ci 241 Am source activity, it was determined that 1630 s were needed to obtain the results for each detector system with the quasi-forward directional AmBe source. Coupling source and material identification together would increase acquisition time but would only require one system to determine.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

HPGe detector shielding optimization with MCNPX for the MEDINA PGNAA cell

Radioactive waste repositories must guarantee the non-toxicity of the waste in the long term, not only regarding radioactivity but also regarding other environmental contamination such as toxic chemicals. Analytical methods already exist for chemical characterization (ICP-MS, ICP-AES...) but they are based on test sampling. A possible alternative, for waste packages with an appropriate gamma radiation level, is to use Prompt Gamma Neutron Activation Analysis (PGNAA), a non-destructive measurement technique sensitive to several toxic chemicals. In view of the characterization of radioactive wastes in Germany and France, collaboration between the CEA Cadarache (France) and the Forschungszentrum Juelich (Germany) was initiated a few years ago. FZJ holds a PGNAA graphite cell called MEDINA (Multi Element Detection based on Instrumental Neutron Activation), allowing the characterization of 225 L drums. Fast neutrons are emitted from a D-T pulsed 14 MeV neutron generator and thermalized in graphite to induced radiative captures in the waste materials. Prompt capture gamma rays are detected using a 104% relative efficiency n-type HPGe. However, HPGe crystal is sensitive to fast neutron damage and to thermal neutron activation. A thermal neutron shield made of lithium fluorine and lithium carbonate is already used around the detector. In order to further decrease the current of fast and thermal neutrons coming into the crystal without penalizing MEDINA sensitivity (by decreasing the thermal neutron flux and neutron die away time of the cell, the gamma detection efficiency, or increasing the gamma background), some configurations based on easy-to-implement modifications of MEDINA have been simulated with MCNPX with a model of the cell already validated by experiments. Results show that fast and thermal neutron incoming current in the HPGe could easily be reduced by about a factor of 2 by additional quantities of graphite and by replacing lithium carbonate by lithium fluorine with a higher {sup 6}Li concentration. In addition, these modifications slightly increase the thermal neutron flux in the cell without deteriorating the neutron die away time, and reduce the gamma background about a factor of 2 during the neutron pulse but 5 times less after it. More important changes have also been tested, such as the addition of polyethylene and lead between the neutron generator and the HPGe detector, which is more effective regarding neutron shielding but decreases the neutron die away time, partly compensated by a larger initial thermal neutron flux. Concerning gamma background, hydrogen capture gamma ray (2.23 MeV) is increased due to the presence of polyethylene but lead around the HPGe decreases the total gamma background. In conclusion, simple modifications are possible to improve detector shielding and life time before thermal annealing of the crystal, without reducing MEDINA cell performances. Some of these modifications will be tested in the coming months. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

MCNP Simulation of Discrete Gamma-ray Spectra for PGNAA Applications

Prompt Gamma Neutron Activation (PGNAA) systems use the neutron-induced gamma-ray spectra from test objects in order to identify their compositions. The U.S. Army in particular uses these systems to identify the contents of field-recovered munitions in order to determine the presence of chemical warfare materiel (CWM) or explosives. These field-recovered munitions can have a variety of different fills, including experimental fills, have a large range of sizes, and be assessed in different field conditions. All these variations can have a significant effect on the neutron-induced gamma-ray spectrum and therefore a large impact on automatic fill identification algorithms. In order to develop robust identification algorithms, parametric studies of the effects of munition size, fill composition, and assessment conditions are very useful but time-consuming and expensive in the laboratory. Monte Carlo modeling of the system response to these variations is a very attractive alternative, provided the modeling accurately reflects real gamma spectra and can be performed quickly and inexpensively when compared to experiment. At Idaho National Laboratory we have used the Monte Carlo N-Particle (MCNP6) code [2] to calculate the response of the Portable Isotopic Neutron Spectroscopy (PINS) system to a number of simulated chemical warfare munitions as well as performed laboratory measurements with the system. Two versions of PINS system were used; one excited the test object with neutrons from a 252C f source and one with neutrons from a portable deuterium-deuterium (DD) neutron generator. The sets of measurements and simulations with the two different neutron sources provided experimental data for development of automatic fill identification algorithms as well as providing a good test of the agreement between the MCNP calculations and experiment.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2019

Active interrogation of Special Nuclear Material containers using AmBe quasi-forward biased directional source and PGNAA

Special Nuclear Material (SNM) including 95% 235 U and 239 Pu is capable of being identified by utilizing a quasi-forward directional AmBe source from Patent No: US20190013109A1 using Prompt Gamma Neutron Activation Analysis (PGNAA) simulated with Monte-Carlo N-Particle transport 6.2 (MCNP). HPGe and LaBr 3 detector arrays were used to identify and quantify the peak-to-background and peak-to-total ratios of the associated photon spectra from the SNM encased in a polyethylene shield. The conducted simulations varied the volume of the SNM and neutron source strength in the MCNP data card to conduct an uncertainty analysis. Photopeaks identified include K-shell X-rays from 235 U and 239 Pu, 61 keV from fission, 2.223 MeV prompt gamma from hydrogen, 511 keV annihilation, and a single and double escape peak from the prompt gamma interaction from hydrogen. Relationships between peak-to-total and peak-to-background as a function of SNM and particle history were investigated to aid in the analysis. The capabilities of both detector systems to acquire well resolved photopeak with a 5% relative error or less, with a 1 Ci source activity, and a peak-to-background ratio of 1.15. Finally, this was determined to take 326 s for LaBr 3 and 163 s for HPGe which is comparable to current methods for material detection which take between 100 and 900 s to acquire.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Passive high explosive neutron inspection (PHENIX): a new method to confirm the presence or absence of high explosives for nuclear treaty verification

Advanced instruments and methods need to be developed now to create a technical basis to support the negotiation of future nuclear arms control treaties. One new capability that is anticipated is the ability to confirm either the declared presence or declared absence of high explosive (HE) material in the presence of special nuclear material (SNM). Towards this goal, Passive HE Neutron Inspection (PHENIX) has been developed and demonstrated as a method for confirming the presence or absence of HE in the presence of plutonium. The method exploits the inherent presence of neutrons associated with the decay of plutonium as an internal probe source for performing prompt gamma-ray neutron activation analysis (PGNAA), searching for the presence of HE as revealed by the emission of characteristic gamma rays following neutron absorption in hydrogen and nitrogen which are building blocks of present-day, military-grade HE. Tests using stoichiometrically-correct hemishells of mock HE with plutonium show that a system can be expected to positively confirm the presence or absence of these signatures, supporting determination of HE presence or absence with Pu, in a few hours. To protect other potentially sensitive gamma-ray signatures from a treaty accountable item, an analog information barrier has been conceptualized and tested which physically prevents the collection of gamma-ray spectral data outside of user selected energy windows strategically chosen to view only narrow spectral regions corresponding to the hydrogen (2223.2 keV) and nitrogen (9807.2 keV, 10,318.2 keV, and 10,829.2 keV) PGNAA signatures.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2022

Discrimination of phosgene from cyanogen chloride in recovered chemical munitions using tagged neutron interrogation with high-resolution gamma-ray spectroscopy

The Associated Particle technique has recently been utilized with a germanium-based high-resolution $\gamma$-ray spectrometer and assessed for its capability to improve field identification of recovered chemical warfare (CW) materiel through prompt gamma-ray neutron activation analysis (PGNAA) measurements. An accurate chemical identification is necessary for the safe handling, destruction, and disposal of such hazardous items. A particularly challenging pair of CW agents commonly found in recovered munitions are phosgene (CG) and cyanogen chloride (CK), which have two of three elements in common, i.e. chlorine and carbon, but differ in the third being either oxygen or nitrogen. The detection of both latter elements is complicated by high oxygen concentration in the field environment which interferes with the small signal produced from the chemical agents. The matter is further complicated by the precautionary field practice of overpacking recovered munitions with vermiculite in larger steel multiple round containers (MRCs), which places additional oxygen-rich material around the munition while further attenuating an already weak signal emitted from the munition center. Here, this work reports quantitative results from realistic field measurements of CG and CK simulants in mock 4.2-inch mortar rounds overpacked with vermiculite in a large MRC. Results obtained with the AP technique are compared to those obtained with the traditional PGNAA approach for both overpacked- and bare-munition measurements. The AP technique is shown to provide a much more confident discrimination between the two chemicals, particularly for the more challenging field-relevant overpacked measurements, where a significant gain in sensitivity to all the key elements chlorine, carbon, nitrogen and oxygen is achieved.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2022

Assessment of the associated particle technique with high-resolution gamma-ray spectroscopy for in-field identification of chemical warfare agents and explosives

In this work, high-resolution prompt γ-ray neutron activation analysis (PGNAA) is performed using the associated particle (AP) technique with a deuterium-tritium neutron generator and high-purity germanium detector. Although the time resolution is inferior compared to similar systems employing fast scintillation γ-ray detectors, the strong background suppression combined with the high γ-ray energy resolution provides an important boost in sensitivity to certain key elements, especially relevant to field measurements of complex chemicals encased within thick layers of metal, such as in the case of recovered chemical warfare (CW) munitions. Results for various CW and explosive simulants contained within mock munitions are presented and compared with results obtained from traditional PGNAA measurements without the aid of the AP technique. Significant improvements in identification and discrimination between certain chemicals are achieved with the high energy resolution AP technique.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2016

Prompt Gamma Neutron Activation Analysis of Niobium for Characterization of Light Interstitials

High purity niobium metal is used in the construction of superconducting radio frequency (SRF) cavities in superconducting particle accelerators. The Spallation Neutron Source at Oak Ridge National Laboratory is an example of an SRF linear accelerator (LINAC) that requires this high purity niobium material. For the SRF cavities to function well, it is necessary that the cavity wall have a high thermal conductivity so that the radio frequency (RF) power can be dissipated into the liquid helium coolant. For a high thermal conductivity of the niobium metal to be achieved, it is required to have extremely low levels of impurities. The current industry standard for determining the quality of the high purity niobium material is the residual resistivity ratio (RRR) technique. In this technique, the temperature dependency of a niobium metal sample is determined at temperatures near that of liquid helium in order to establish where the superconducting jump occurs. With this method, it is possible to find the general level of impurity of the metal sample, but not the specific elements that are contributing to the impurity. The impurities that are of particular interest to manufacturers of niobium for SRF use are tantalum and light interstitials, such as hydrogen, carbon, nitrogen, and oxygen. In this research, we focus on determining the analytical sensitivity of the detector system and characterizing the light interstitial content in high purity niobium metal through the use of Prompt Gamma Neutron Activation Analysis (PGNAA). PGNAA is an analytical technique that can be utilized to determine the concentration of elemental components in a wide variety of materials with high precision and reproducibility. In this process, neutrons bombard a sample material, causing the emission of gamma rays from the sample. Each element emits a unique spectrum of gamma radiation, which allows for identification of the elements present in the sample. (authors)

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Application of Multivariate Data Analysis Techniques for the Portable Isotopic Neutron Spectroscopy system

The Portable Isotopic Neutron Spectroscopy (PINS) is a commercialized system developed by Idaho National Laboratory (INL) to examine chemical compounds non-destructively, utilizing Prompt Gamma Neutron Activation Analysis (PGNAA) techniques. The PINS systems have been successfully deployed around the world to identify chemical munitions and containers. The PINS system takes advantage of a high-resolution gamma-ray spectrum from a high-purity germanium (HPGe) detector, and gamma-ray peak analysis provides input to its chemical identification logic with the probabilistic decision tree (PDT). Gamma-ray peak analyses, however, require knowledge of pre-selected gamma-ray peaks whose energies, intensities, and origins are well studied, and some peaks might be excluded from the decision making processes due to lack of current nuclear data. In contrast, Multivariate Analysis (MVA) treats a whole gamma-ray spectrum as a collection of multiple variables or a pattern. The effectiveness of chemical identification algorithm is determined by the availability of a wide range of data to train an algorithm to identify chemical fills with accuracy. INL has a collection of gamma-ray spectra of various chemical-fills from the field-deployed PINS systems over the years, and it was envisaged to combine such a database with the principle of multivariate statistics. Therefore, in parallel with the current decision tree algorithm, an MVA-based chemical identification algorithm was developed as an independent verification of the current results. The Principal Component Analysis (PCA) method was adopted to build an MVA-based identification algorithm, using the collected field data to refine and validate the algorithm. A benchmarking study of the MVA-based algorithm’s performance was conducted alongside the current algorithm, with the results presented and discussed in this study.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2019

Application of artificial neural network to prompt gamma neutron activation analysis for chemical warfare agents identification

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2020

Application of Gaussian Bayes classifier to differentiate chlorine-based chemical agents

The Portable Isotopic Neutron Spectroscopy (PINS) is a commercialized system developed by Idaho National Laboratory (INL) to examine chemical warfare agents (CWA) non-destructively, utilizing Prompt Gamma Neutron Activation Analysis (PGNAA) techniques. The PINS system takes advantage of a high-resolution gamma-ray spectrum from a mechanically-cooled high-purity germanium (HPGe) detector. One of the difficult technical challenges is to discriminate the chlorine-based chemical agents. Especially, CN, CNB, CNS and CG have similar chemical compositions to make it hard to discriminate them with a higher confidence. Current identification algorithms for PINS systems with 252-Cf sources have been improved and updated continuously as more field data became available, and new algorithms was studied to complement the current algorithms by adopting the Gaussian Bayes classifier. These new algorithms were intended to be applied to a subset of chlorine-based chemical agents, and their main goal is discriminate CN, CNB, CNS and CG with their ratios of the chlorine neutron inelastic 1763keV peak to the chlorine thermal neutron capture 1959keV peak, which is referred to as the “Cl i/c” or “clic” ratio in this study. The Cl i/c ratios were assumed to follow Gaussian distributions with the means and the standard deviations unique to their corresponding chemical agents. The prior probabilities of these four chemical agents were optimized with a collection of field data to achieve the best performance in terms of precision or positive predictive value (PPV). Finally, their posterior probabilities as functions of the Cl i/c ratio were implemented in the current version of PINS analysis software in order to be tested with more field data.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2022

Improving Coal-Fired Plant Performance Through Integrated Predictive and Condition-Based Monitoring Tools

The project demonstrated the ability to improve boiler performance and reliability through the integrated use of condition-based monitoring (CBM) and predictions of the impacts of coal quality on boiler operations at a full-scale coal-fired power plant. The advanced tool developed actively monitors and manages coal quality and overall boiler conditions that maximizes availability and maintains generating capacity while reducing cost. The tool is used to forecast and alert plant operators and engineers about poor boiler conditions which may occur as a result of incoming coal and/or current power plant operating conditions. The Combustion System Performance Indices (CSPI) and CoalTracker (CT) programs predicts fireside performance of the plant including slagging, fouling, erosion, slag flow, strength development (sintering/densification), and slag layer thickness based on the composition of delivered coal. CT program is tailored for each plant and is used to track the coal from the point of delivery to the burner. The most successful application of the CSPI-CT has been at plants where the coal composition is determined through the use of a full stream elemental analyzers based on prompt gamma neutron analysis (PGNAA). The CSPI-CT program information is used by coal procurement, coal mining and plant operations personnel to select and blend coal properties for the best plant performance.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2023

System and method for predicting the presence of rare earth elements

A system for predicting rare earth elements (REEs) in a feedstock sample includes a measurement instrument that records a measurement for a sample, a processor communicatively coupled to the measuring instrument, and a memory communicatively coupled to the processor and containing machine readable instructions that, when executed by the processor, cause the processor to correlate the measurement series using a model; and predict a presence of one or more rare earth element based at least in part on the correlation. A method for predicting rare earth elements includes measuring feedstock samples via XRF or PGNAA, to generate a measurements of elements of interest with a lower atomic weight than REEs; correlating the measurements with a model; and predicting a presence of one or more rare earth elements based at least in part on the correlation.

Fuka, Matthew↗

DOE OSTI2015

High Energy Performance Tests of Large Volume LaBr{sub 3}:Ce Detector

High energy prompt gamma ray tests of a large volume cylindrical 100 mm x 100 mm (height x diameter) LaBr{sub 3}:Ce detector were carried out using a portable neutron generator-based Prompt Gamma Neutron Activation Analysis (PGNAA) setup. In this study prompt gamma-rays yield were measured from water samples contaminated with toxic elements such nickel, chromium and mercury compounds with gamma ray energies up to 10 MeV. The experimental yield of prompt gamma-rays from toxic elements were compared with the results of Monte Carlo calculations. In spite of its higher intrinsic background due to its larger volume, an excellent agreement between the experimental and calculated yields of high energy gamma-rays from Ni, Cr and Hg samples has been achieved for the large volume LaBr{sub 3}:Ce detector. (authors)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2013

PINS Variance study

The INL’s Portable Isotopic Neutron Spectroscopy System (PINS) non-intrusively identifies the chemical fill of munitions and sealed containers. PINS is used routinely by the U.S. Army, the Defense Threat Reduction Agency, and foreign military units to determine the contents of munitions and other containers suspected to contain explosives, smoke-generating chemicals, and chemical warfare agents such as mustard and nerve gas. The objects assayed with PINS range from softball-sized M139 chemical bomblets to 200 gallon DOT 500X ton containers. INL had previously examined the feasibility of using a similar system for the identification of explosives, and based on this proof-of-principle test, the development of a dedicated system for the identification of explosives in the presence of special nuclear material for emergency responders was started in 2011. INL tested prototype PINS on explosives and mock explosives with kilogram quantities of highly-enriched uranium and weapons-grade plutonium in 2011. In 2012 INL concentrated on making the system more sensitive to identifying explosives, particularly in the detection of the nitrogen content of explosives. This past year INL has been concentrating its efforts in studying the variance in the spectra, in particular the variance in the elemental ratios that are used to identify individual explosives.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2013

PINS-3X Operations

Idaho National Laboratory’s (INL’s) Portable Isotopic Neutron Spectroscopy System (PINS) non-intrusively identifies the chemical fill of munitions and sealed containers. The PINS-3X variant of the system is used to identify explosives and uses a deuterium-tritium (DT) electronic neutron generator (ENG) as the neutron source. Use of the system, including possession and use of the neutron generator and shipment of the system components requires compliance with a number of regulations. This report outlines some of these requirements as well as some of the requirements in using the system outside of INL.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗