Multi-elemental analysis of commercial wheat flours by ICP-MS triple quadrupole in function of the milling degree.

This preliminary study is focused on an elemental analysis of 60 samples of different commercial grains' flour, including various typologies of refined product, researching transition metals and trace elements. All the samples were first digested with a microwave digestion system and then analyzed by a triple quadrupole (TQ) inductively coupled plasma mass spectrometer (ICP-MS-QQQ) located in a Clean Room ISO class 6. The minimum value of most of the elements (Li, Be, Na, Ca, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, As, Se, Rb, Sr) are in the wheat flour "00" type and in the wheat flour "0" type (B, Na, Mg, Al, Cu, Ag, Cd, In, Cs, Pb, Bi). On the opposite, the maximum value of these elements is found in whole wheat flour (B, Mg, K, Ca, Mn, Zn, Ga, Rb, Sr, Ba) and in the wheat flour "0" type (Na, Al, V, Cr, Fe, Co, Ni, As). Relating rare-earth elements (REE), all of them show value similar to each other and not under the detection limits thanks to the use of a TQ in the clean room. The final aim is to create a large database, with a high data bank and easily enlargeable, that could be used in future to analyze unknown flour samples and to set up traceability analysis. The purpose of this work is to find some trends of analyzed elements in function of different parameters, such as milling degree or geographical origin, also with a statistical point of view.

Preparation and Characterization of Isostructural Na2MoO4 and Na2WO4 and a Study of the Composition of Their Mixed System.

Na2MoO4 and Na2WO4 are isostructural semiconductors, belonging to the spinel class. They have interesting properties and find applications in numerous sectors. These properties can be tuned by controlling the composition of their solid solutions. Here, different methods to obtain these compounds are presented, both wet and solid-state synthesis. The obtained results show a possible dependence of the material properties on the chosen synthesis method. The pure compounds and their mixtures were characterized by Raman spectroscopy, scanning electron microscopy, and X-ray diffraction.

Halide Perovskites Films for Ionizing Radiation Detection: An Overview of Novel Solid-State Devices.

Halide perovskites are a novel class of semiconductors that have attracted great interest in recent decades due to their peculiar properties of interest for optoelectronics. In fact, their use ranges from the field of sensors and light emitters to ionizing radiation detectors. Since 2015, ionizing radiation detectors exploiting perovskite films as active media have been developed. Recently, it has also been demonstrated that such devices can be suitable for medical and diagnostic applications. This review collects most of the recent and innovative publications regarding solid-state devices for the detection of X-rays, neutrons, and protons based on perovskite thin and thick films in order to show that this type of material can be used to design a new generation of devices and sensors. Thin and thick films of halide perovskites are indeed excellent candidates for low-cost and large-area device applications, where the film morphology allows the implementation on flexible devices, which is a cutting-edge topic in the sensor sector.

Dissolution of Molybdenum in Hydrogen Peroxide: A Thermodynamic, Kinetic and Microscopic Study of a Green Process for 99mTc Production.

99mTc-based radiopharmaceuticals are the most commonly used medical radioactive tracers in nuclear medicine for diagnostic imaging. Due to the expected global shortage of 99Mo, the parent radionuclide from which 99mTc is produced, new production methods should be developed. The SORGENTINA-RF (SRF) project aims at developing a prototypical medium-intensity D-T 14-MeV fusion neutron source specifically designed for production of medical radioisotopes with a focus on 99Mo. The scope of this work was to develop an efficient, cost-effective and green procedure for dissolution of solid molybdenum in hydrogen peroxide solutions compatible for 99mTc production via the SRF neutron source. The dissolution process was extensively studied for two different target geometries: pellets and powder. The first showed better characteristics and properties for the dissolution procedure, and up to 100 g of pellets were successfully dissolved in 250-280 min. The dissolution mechanism on the pellets was investigated by means of scanning electron microscopy and energy-dispersive X-ray spectroscopy. After the procedure, sodium molybdate crystals were characterized via X-ray diffraction, Raman and infrared spectroscopy and the high purity of the compound was established by means of inductively coupled plasma mass spectroscopy. The study confirmed the feasibility of the procedure for production of 99mTc in SRF as it is very cost-effective, with minimal consumption of peroxide and controlled low temperature.

Set up and test of an anticoincidence system for the detection of radioactive xenon by gamma spectrometry system.

The aim of this work is based on the optimisation of a gamma spectrometry system in anticoincidence for the detection of noble gases, in particular the radioactive isotopes of xenon. These four radionuclides are of particular interest for the Comprehensive Nuclear Test-Ban Treaty (CTBT). The Laboratory of the ENEA Research Centre of Brasimone, where the experimental apparatus has been set up to carry out the measurements of 131mXe, 133Xe, 133mXe and 135Xe, is able to provide, if necessary, data and analysis on noble gases. The apparatus provides for the sampling of outdoor air, the passage through filters and in activated carbons maintained at cryogenic temperatures to allow xenon absorption. Finally, gas extraction and xenon volumes are analyzed by means of gas chromatography and a thermal conductivity detector. At the end of the extraction an aluminium cylinder containing radioxenon is analyzed by high resolution gamma spectroscopy using a High Purity Germanium Detector P-type. The signals produced by the interaction of cosmic rays with the crystal have been recognized as the main cause of the increase of the detector background because they give rise to the Compton continuum and, as a result, they affect the value of the minimum detectable activity (MDA). In order to overcome this effect, a system in anticoincidence has been developed using two plastic scintillators, placed over the shielding of the HPGe detector, which send pulses recording within a time delay window located in the germanium multichannel analyzer: at the time the signal arrives from the scintillator, the gate blocks data acquisition to avoid recording pulses generated by cosmic radiation. For both configurations of the system (with and without the anticoincidence apparatus operating) the energy, and efficiency calibrations have been carried out using a certified multigamma-ray calibration source to assess the performance.

Profiling and imaging of forensic evidence - A pan-European forensic round robin study part 1: Document forgery.

The forensic scenario, on which the round robin study was based, simulated a suspected intentional manipulation of a real estate rental agreement consisting of a total of three pages. The aims of this study were to (i) establish the amount and reliability of information extractable from a single type of evidence and to (ii) provide suggestions on the most suitable combination of compatible techniques for a multi-modal imaging approach to forgery detection. To address these aims, seventeen laboratories from sixteen countries were invited to answer the following tasks questions: (i) which printing technique was used? (ii) were the three pages printed with the same printer? (iii) were the three pages made from the same paper? (iv) were the three pages originally stapled? (v) were the headings and signatures written with the same ink? and (vi) were headings and signatures of the same age on all pages? The methods used were classified into the following categories: Optical spectroscopy, including multispectral imaging, smartphone mapping, UV-luminescence and LIBS; Infrared spectroscopy, including Raman and FTIR (micro-)spectroscopy; X-ray spectroscopy, including SEM-EDX, PIXE and XPS; Mass spectrometry, including ICPMS, SIMS, MALDI and LDIMS; Electrostatic imaging, as well as non-imaging methods, such as non-multimodal visual inspection, (micro-)spectroscopy, physical testing and thin layer chromatography. The performance of the techniques was evaluated as the proportion of discriminated sample pairs to all possible sample pairs. For the undiscriminated sample pairs, a distinction was made between undecidability and false positive claims. It was found that none of the methods used were able to solve all tasks completely and/or correctly and that certain methods were a priori judged unsuitable by the laboratories for some tasks. Correct results were generally achieved for the discrimination of printer toners, whereas incorrect results in the discrimination of inks. For the discrimination of paper, solid state analytical methods proved to be superior to mass spectrometric methods. None of the participating laboratories deemed addressing ink age feasible. It was concluded that correct forensic statements can only be achieved by the complementary application of different methods and that the classical approach of round robin studies to send standardised subsamples to the participants is not feasible for a true multimodal approach if the techniques are not available at one location.

Forensic Analysis of Commercial Inks by Laser-Induced Breakdown Spectroscopy (LIBS).

Laser-induced breakdown spectroscopy (LIBS) was tested for all of the relevant issues in forensic examinations of commercial inks, including classification of pen inks on one paper type and on different paper types, determination of the deposition order of layered inks, and analysis of signatures and toners on one questioned document. The scope of this work was to determine the potential of a single LIBS setup that is compatible with portable instruments for different types of ink analysis, rather than building a very large database for inks and papers. We identified up to seven metals characteristic for the examined inks, which allowed to fully discriminate all eight black inks on one type of printing paper. When the inks were tested on ten different papers, the correct classification rates for some of them were reduced for reasons thoroughly studied and explained. The replicated tests on three crossing points, each one involving a pair of blue or black inks, were successful in five cases out of six. In the test simulating documents of forensic interest (questioned documents), LIBS was able to correctly identify the differences in three inks used for signatures on one of the three pages and the use of different printing inks on each page of the document.