Nuclear Activation Analysis Research Articles

Compositional Analysis of Metal(IV) Phosphate and Phosphonate Materials—Pitfalls and Best Practices

Metal(IV) phosphate and phosphonates materials have increasingly found their applications in water purification, heterogeneous catalysis, drug delivery, and proton-exchange membrane fuel cells. The strong linkage between tetravalent metal cations and phosphate/phosphonate groups offers a unique bottom-up design platform, resulting in chemically stable inorganics or hybrids. Task-specific physiochemical functionalities could be deposited by modifying the phosphate/phosphonate groups before the material synthesis. The high reactivity between the metal centre and the phosphorus-containing linker, on the other hand, often leads to obtaining unordered materials (amorphous solids or coordination polymers). The chemical composition of the prepared materials is a key parameter in guiding the synthetic approach and in governing their performances. This narrative review focuses on critically summarising the traditional and advanced analytical methods for probing the composition of these materials. The reader is introduced to and guided on the advances and restrictions of different analysis techniques when probing metal(IV) phosphates/phosphonates. Both solution-based and solid-state spectroscopic techniques are covered with a focus on understanding the quantity and the linkage status of the phosphorus-containing moieties. These techniques include atomic spectroscopy, mass spectroscopy, nuclear magnetic resonance spectroscopy, X-ray-based methods, and neutron activation analysis.

Optimization of cementitious composite for heavyweight concrete preparation using conduction calorimetry

The present work investigates the hydration heat of different cement composites by means of conduction calorimetry to optimize the composition of binder in the design of heavyweight concrete as biological shielding. For this purpose, Portland cement CEM I 42.5 R was replaced by a different portion of supplementary cementitious materials (blast furnace slag, metakaolin, silica fume/limestone) at 75%, 65%, 60%, 55%, and 50% levels to obtain low hydration heat lower than 250 j g−1. All ingredients were analyzed by energy dispersive X-ray fluorescence (EDXRF) and nuclear activation analysis (NAA) to assess the content of major elements and isotopes. A mixture of two high-density aggregates (barite and magnetite) was used to prepare three heavyweights concretes with compressive strength exceeding 45 MPa and bulk density ranging between 3400 and 3500 kg m−3. After a short period of volume expansion (up to 4 h), a slight shrinkage (max. 0.3°/°°) has been observed. Also, thermophysical properties (thermal conductivity, volumetric specific heat, thermal diffusivity) and other properties were determined. The results showed that aggregate content and not binder is the main factor influencing the engineering properties of heavyweight concretes.

High-saturation magnetization in small nanoparticles of Fe3O4 coated with natural oils

The enhancement of nanoparticle’s magnetic properties with a suitable coating is the main tool to increase their potential as an effective candidate for applications in different areas, especially in biomedicine. In the work here reported, Fe3O4 nanoparticles coated with natural oils were synthesized by iron (III) acetylacetonate thermal decomposition and the effects of the coating on the magnetic properties of these particles have been investigated. The oils were extracted from three Amazon fruits seeds: acai, ucuuba, and bacaba by CO2 supercritical extraction process, and the relative percentage composition of fatty acids were determined by gas chromatography. A systematic study of crystalline, morphological, and magnetic properties revealed a saturation magnetization (Ms) enhancement and high values of the anisotropy constant for Fe3O4 samples when coated with acai and ucuuba oils, which present a large percentage of saturated total fatty acid. Our results indicate that nanoparticles with sizes smaller than around 5 nm present Ms values as high as that found for bulk Fe3O4 and, consequently, much higher than Ms values for nanoparticles usually coated with oleic acid. The nuclear techniques neutron activation analysis and perturbed angular correlations were used to better characterize the nanoparticles.

Gd-GLU toward NMR imaging: synthesis, characterization and breast cell uptake assay

Breast cancer cell uptake of Gd-metal is investigated based on the formation of coordinate compounds of gadolinium and glucose (Glu) molecules in solution. The hypothesis is that glucose helps Gd-internalization by complex formations constituted of Gd3+ coordinate to m-glucose molecules, whose valence was complemented by Cl- anions. Such a proposal is an insight toward a metabolic-dependent contrast-agent for cancer and inflammation in magnetic resonance image. A solution was prepared based on anhydrous d-glucose and gadolinium chloride (Gd-Glu). Uptake assays for MDA-MB-231(c231) cells were elaborated collecting incubated c231-cells with Gd-Glu and measuring metal-uptake and their concentrations by Nuclear Activation Analysis (NAA). The ionic solution was studied using Direct-Infusion Electrospray Ionization Mass-Spectrometry (ESI-MS) to identify Gd-Glu interactions. Means and standard deviations of Gd-masses were 13.3±0.8 and 12.5±0.7µg, at 361.5 µg of Gd in 3mL Gd-Glu/PBS solution, in times of 30-50 min, equivalent to the concentrations of 13404±2104 and 11347±2742 µg.g-1 in dried cells. Such values were statistically higher than the control with metal presence. ESI-MS demonstrated the m/z-signals at 516, 552, 696, 923, attributed to positively loaded-species containing Glu, Gd+3 and Cl-. In conclusion, Gd-internalization was increased in aqueous solution due to the gadolinium-glucose coordination. Such findings drive the research to MRI with Gd-Glu complexes.

The inorganic fraction in e-liquids used in vapor products including e-cigarettes

Nowadays, e-cigarettes are largely used, they are considered less dangerous than the traditional cigarettes. Actually, there are a lot of investigations on the health effects of nanoparticles and smoke emitted by them whereas there are very few studies on the e-liquid composition. For the first time this paper would like to investigate the inorganic composition of the e-liquids at different nicotine content (0, 9 and 18 mg mL−1) by means of the instrumental nuclear activation analysis. More than 20 elements at trace/ultra-trace levels were determined: elements such as Na, W, Br, Fe and Co show similar distribution in all the samples, toxic elements as As, Ni and Sb are at μg kg−1 levels whereas Hg is present only in the sample at 0 mg mL−1 nicotine (0.56 µg kg−1). Further, based on transfer rate data of some metals from tobacco to smoke, an evaluation of inhaled element amount during a single vape is also reported.

Instrumental Neutron Activation Analysis (INAA) of Cisadane Estuarine Sediments

Nuclear analytical technique instrumental neutron activation analysis was employed for the multielemental analysis of sediments collected from Cisadane estuary. This analytical technique provides concentration of 20 elementswhich consist of heavy metals and rare earth elements simultaneously. Two sediments cores were collected using core sampler for determining the distribution of all elements in the depth profiles of sediments. Sediment cores were subdivided into 2 cm increment, dried and sent to reactor for irradiation using thermal flux of ?1013 neutrons.cm-2.s-1 for 20 minutes in Research Reactor Siwabessy, National Nuclear Energy Agency (BATAN), Serpong. Irradiated samples were measured using a multichannel analyzer (MCA) gamma spectrometer coupled with high purity germanium detector. Analysis of particle size was done since uptake of heavy metals by sediments is particle-size dependent. The results are presented and discussed.

Biokinetic study of selenium nanoparticles and salt forms in living organisms

An experimental study of absorption, distribution, metabolism, and excretion from the body of radioisotope-labeled nanoparticles (NPs) of elemental Se in comparison with the traditional form of this trace element (sodium selenite) has been performed, being administered in the gastrointestinal tract of rats that were normally supplied with Se or experiencing its nutritional deficiency. Nuclear activation analysis is used for the detection of Se in the biological tissue, which is based on the measurement of a gamma-emitting label [75Se34] that is introduced in the Se NPs or its salt by thermal neutron irradiation in a nuclear reactor. It is shown that Se NPs administered into the gastrointestinal tract have bioavailability comparable to the salt form of this element. According to some experimental data, the metabolic assimilation of both forms of Se is greater in animals that suffer from a deficiency in this element when compared to those that are normally supplied with it. There are some differences in the kinetics of accumulation of Se NPs and its salts in the blood and liver, which can be explained by the presence of limiting steps in the absorption and biotransformation of Se-containing NPs. The retention of Se that is administered in the form of NPs or salts to Se-deficient animals differs significantly. These results demonstrate the capacity of the Se NPs to be a source of Se in a new generation of biologically active food supplements.

Multi-elemental composition of Slovenian milk: analytical approach and geographical origin determination

The main objective in multi-elemental analysis in food is to obtain the best results in the shortest time and with minimal contamination and reagent consumption. Three different methods were investigated in the present study to obtain the elemental content in milk samples: energy dispersive X-ray fluorescence spectrometry (EDXRF), k<sub>0</sub>-instrumental nuclear activation analysis (k<sub>0</sub>-INAA) and the inductively coupled plasma mass spectrometry (ICP-MS). Quality assurance including intercomparison exercises of these measurements proved entirely satisfactory and was typical of that previously established for this technique. It was found that EDXRF was the cheapest, simplest and environmental friendly method for analysis of multi-elemental composition (P, S, Cl, K, Ca, Zn, Br, Rb, Sr) in milk samples, while for determination of Mn, Fe, Cu, Se content and possible identification of pollutants such as As, Cd and Pb ICP-MS was a method of choice due to its excellent sensitivity and accuracy. These two methods were also used to determine the multi-elemental composition in Slovenian raw cow milk from different geographical regions: Alpine, Mediterranean. Dinaric and Panoninan in December 2013. Linear discriminant analysis (LDA) was used to explore multi-elemental analysis of milk samples to obtain classification according to geographical regions. Regional discrimination was most successful taking into account Ca, S, P, K, and Cl with prediction ability of 66.7%.

Development of Three-Dimensional Trajectory Model for Detecting Source Region of the Radioactive Materials Released into the Atmosphere

Background: It is necessary to consider the overall countermeasure for analysis of nuclear activities according to the increase of the nuclear facilities like nuclear power and reprocessing plants in the neighboring countries including China, Taiwan, North Korea, Japan and South Korea. South Korea and comprehensive nuclear-test-ban treaty organization (CTBTO) are now operating the monitoring instruments to detect radionuclides released into the air. It is important to estimate the origin of radionuclides measured using the detection technology as well as the monitoring analysis in aspects of investigation and security of the nuclear activities in neighboring countries. Materials and methods: A three-dimensional forward/backward trajectory model has been developed to estimate the origin of radionuclides for a covert nuclear activity. The developed trajectory model was composed of forward and backward modules to track the particle positions using finite difference method. Results and discussion: A three-dimensional trajectory model was validated using the measured data at Chernobyl accident. The calculated results showed a good agreement by using the high concentration measurements and the locations where was near a release point. The three-dimensional trajectory model had some uncertainty according to the release time, release height and time interval of the trajectory at each release points. An atmospheric dispersion model called long-range accident dose assessment system (LADAS), based on the fields of regards (FOR) technique, was applied to reduce the uncertainties of the trajectory model and to improve the detective technology for estimating the radioisotopes emission area. Conclusion: The detective technology developed in this study can evaluate in release area and origin for covert nuclear activities based on measured radioisotopes at monitoring stations, and it might play critical tool to improve the ability of the nuclear safety field.

Assessment of Total Suspended Particulates (TSP) in Ikot Abasi L. G. A., Nigeria

Concentrations of major, minor and trace elements in the total suspended particulate (TSP) matter around Ikot Abasi were determined by instrumental nuclear activation analysis (INAA) technique using the thermal neutrons from the first Nigerian nuclear research reactor (NIRR-1) at centre for energy research and training (CERT), Ahmadu Bello University, Zaria. Total suspended particulate (TSP) concentrations ranged between 139±22 µgm-3 and 23±07 µgm-3. The total TSP concentrations from different source groups revealed the commercial sector as the highest contributor of TSP level to the area with a value of 254.64 µgm-3. This value is slightly higher than the µgm-3 standard set by the federal environmental protection agency FEPA. The INAA of the TSP samples show the presence of Al, Na and Mn. Their contributions range between 19.8±3.7 – 119.1±10.1 ppm for Al; 57.4±10.2 - 184±16 ppm for Na and 1.2±0.3 – 4.7±0.4 ppm for Mn in the TSP samples around the study area.

Characterization of Old Nuclear Waste Packages Coupling Photon Activation Analysis and Complementary Non-Destructive Techniques

Radiological characterization of nuclear waste packages is an industrial issue in order to select the best mode of storage. The characterization becomes crucial particularly for waste packages produced at the beginning of the French nuclear industry. For the latter, available information is often incomplete and some key parameters are sometimes missing (content of the package, alpha-activity, fissile mass...) In this case, the use of non-destructive methods, both passive and active, is an appropriate solution to characterize nuclear waste packages and to obtain all the information of interest. In this article, we present the results of a complete characterization carried out on the TE 1060 block, which is a nuclear waste package produced during the 1960's in Saclay. This characterization is part of the DEMSAC (Dismantling of Saclay's facilities) project (ICPE part). It has been carried out in the SAPHIR facility, located in Saclay and housing a linear electron accelerator. This work enables to show the great interest of active methods (photon activation analysis and high-energy imaging) as soon as passive techniques encounter severe limitations.

Source identification of inorganic airborne particle fraction (PM10) at ultratrace levels by means of INAA short irradiation

Many studies have focused their attention on the determination of elements of toxicological and environmental interest in atmospheric particulate matter using analytical techniques requiring chemical treatments. The instrumental nuclear activation analysis technique allows achieving high sensitivity, good precision, and excellent limit of detection without pretreatment, also considering the problems related to the radioisotope characteristics (e.g., half-life time, interfering reactions, spectral interferences). In this paper, elements such as Al, As, Br, Cl, Cu, I, La, Mg, Mn, Na, Sb, Si, Ti, and V are studied in atmospheric PM10 sampled in downtown Rome: The relative radionuclides after activation of the sample are characterized by very short (ranging from 2.24 to 37.2 min) and short (ranging from 2.58 h to 2.70 days) half-lives. Furthermore, As, Br, La, Mn, and Sb were also determined for evaluating the aerosol characteristics. The results, elaborated considering the matrix effects and the interfering reaction contribution to the radioisotope formation (e.g., (28)Al generated by both (n,γ) reaction from (27)Al and (n,p) reaction from (28)Si), show interesting values of As (0.3-6.1 ng m(-3)), Cu (22-313 ng m(-3)), Mn (17-125 ng m(-3)), V (7-63 ng m(-3)), higher than those determined in an area not influenced by autovehicular traffic, and significant levels of I (1-11 ng m(-3)) and Ti (25-659 ng m(-3)) in Rome PM10. The other elements show a pattern similar to the very few data present in the literature. It should be underlined the good correlation (r (2)) of Al vs. Mg (0.915) and Al vs. La (0.726), indicating a same sources for these species as well as Br-Sb showing a little lower correlation (0.623). This last hypothesis is confirmed by the study of the enrichment factors: Sb and Br may be attributed to anthropogenic sources; Cu, Cl, and I show a mixed origin (natural and anthropogenic), whereas Al, Si, Ti, Mn, Na, Mg, and As are of crustal origin. For having more information, a statistical approach based on the principal component analysis and the canonical discriminant analysis has been performed: All the samples (except one) are grouped in a cluster, and elements such as As, Br, Cu, I, La, Mn, Sb, Ti, and V are highly correlated, whereas Na and Cl and Mg and Al assemble in two different clusters. Finally, a comparison with other similar studies is reported showing interesting values for Al, As, Mg, Mn, and Ti.

The detection of signals hidden in noise

This paper examines signal detection in the presence of noise, with particular emphasis on nuclear activation analysis. The specific problem is to decide whether the signal-plus-background or the no-signal hypothesis fits the data better. Our solution is based on the use of Bayesian inferences to test the two hypotheses.

Nuclear analytical techniques for quantification of uranium for its recovery from seawater

Nuclear analytical techniques namely fission track technique using solid state nuclear track detector (SSNTD) and instrumental neutron activation analysis (INAA) have been standardized and applied for quantification of low uranium concentrations in liquid samples such as feed, elute and brine and solid sorbent samples respectively. The quantification of uranium is required for its recovery study from seawater, which is one of the potential sources of uranium. The uranium concentration of a liquid sample obtained by SSNTD method was compared with the other well established conventional techniques like ICP-MS, ICP-AES, adsorptive stripping voltametry and alpha spectrometry. INAA was applied for uranium concentration determination in the radiation grafted polyamidoxime sorbent samples.

Review of analytical methods for the quantification of iodine in complex matrices

Iodine is an essential element of human nutrition. Nearly a third of the global population has insufficient iodine intake and is at risk of developing Iodine Deficiency Disorders (IDD). Most countries have iodine supplementation and monitoring programs. Urinary iodide (UI) is the biomarker used for epidemiological studies; only a few methods are currently used routinely for analysis. These methods either require expensive instrumentation with qualified personnel (inductively coupled plasma-mass spectrometry, instrumental nuclear activation analysis) or oxidative sample digestion to remove potential interferences prior to analysis by a kinetic colorimetric method originally introduced by Sandell and Kolthoff ∼75 years ago. The Sandell–Kolthoff (S–K) method is based on the catalytic effect of iodide on the reaction between Ce 4+ and As 3+. No available technique fully fits the needs of developing countries; research into inexpensive reliable methods and instrumentation are needed. There have been multiple reviews of methods used for epidemiological studies and specific techniques. However, a general review of iodine determination on a wide-ranging set of complex matrices is not available. While this review is not comprehensive, we cover the principal developments since the original development of the S–K method.

A compact neutron beam generator system designed for prompt gamma nuclear activation analysis

In this work a compact system was designed for bulk sample analysis using the technique of PGNAA. The system consists of (252)Cf fission neutron source, a moderator/reflector/filter assembly, and a suitable enclosure to delimit the resulting neutron beam. The moderator/reflector/filter arrangement has been optimised to maximise the thermal neutron component useful for samples analysis with a suitably low level of beam contamination. The neutron beam delivered by this compact system is used to irradiate the sample and the prompt gamma rays produced by neutron reactions within the sample elements are detected by appropriate gamma rays detector. Neutron and gamma rays transport calculations have been performed using the Monte Carlo N-Particle transport code (MCNP5).

Correlated wear measurements using gold implantation, backscattering, nuclear activation analysis and profilometry

High and ultra-mild wear of Al–Si alloys under lubrication is measured (a) by comparison of initial and retained gold concentration in surfaces, (b) by tracking gold in the effluent lubricant or (c) alloy specific elements, and (d) by stylus profilometry. Wear >1 μm is best captured by method (d). However, (d) fails when both tribologically induced films have formed and wear is below 100 nm. Method (c) is efficient in a broad range of wear if element concentrations can be determined precisely. Methods (a) and (b) satisfy this requirement but they are only efficient for ultra-mild wear.

Assessment of non-traditional isotopic ratios by mass spectrometry for analysis of nuclear activities

This work provides an assessment of suitable forensic indicators that may be measured by portable mass spectrometry systems. Traditional assessments of nuclear fuel cycle manipulation or other nuclear activities often depend upon analyses of uranium and plutonium isotopes in the nuclear fuel. Any entity engaging in shortened fuel cycle activity will recover U and Pu during reprocessing. Fission, capture, and activation products are less valuable and generally regarded as waste products. This work determined isotopic ratios that distinguish nuclear weapons and shortened nuclear fuel cycles from commercial nuclear reactors. Modeling of fuel cycles was conducted via ORIGEN-S, MCNPX, and through custom calculations.

Elemental characterization of impurities at trace and ultra-trace levels in metallurgical lead samples by INAA

The purity of several economically important metals is routinely verified by a reference material. Further, it is essential to provide a means of maintaining the consistency between laboratories and on disseminating the accurate value. This work, developed within an activity of certification promoted by EURATOM, reports the results on impurity determination (Ag, As, Cd, Ni, Sb, Sn, Te and Zn) at trace (µg g − 1 ) and ultra-trace (ng g − 1 ) levels in three metallurgical lead samples (99.99% of purity). Among the different analytical techniques available for the characterization, the use of a nuclear technique, i.e. Instrumental Nuclear Activation Analysis, has allowed to reach high sensitivity and to obtain accurate values for these elements. The irradiations were performed in the rotating rack (Lazy Susan) and in the central channel of the Triga Mark II reactor reaching a total integrated flux of 9.36 × 10 17 n cm − 2 and 2 × 10 19 n cm − 2 , respectively. The results about the determination of elements such as Ni, Sn, Te and Zn present at ultra-trace levels (ng/g), are showed and discussed. This task is very interesting for the radio-analytical and methodological implications: in fact, for analyzing them a radiochemical separation is involved and an anti-Compton gamma spectrometer is necessary due to their very low levels.

Application of the INAA technique for elemental analysis of metallic biomaterials used in dentistry

The sensitive nuclear analytical technique Instrumental Neutron Activation Analysis (INAA) has been applied on several types of metallic biomaterials (Heraenium CE, Ventura Nibon, Wiron 99 and Ducinox which are currently used for restoration in the dental clinics) to study its performance in elemental analysis and identify eventual limitations. The investigation has been performed by two NAA Laboratories and aimed at getting an answer to the question on how the biomaterials compositions influence the patients’ health over the course of time, taking into account the EC Directive 94/27/EC recommendations concerning Ni toxicity.