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The expulsion of runaway electrons (REs) during different types of tokamak instabilities is analysed by means of a Cherenkov probe inserted into the scrape-off layer of the FTU tokamak. One such type of instability, the well-known tearing mode, is involved in disruptive plasma termination events, during which the risk of RE avalanche multiplication is highest. The second type, known as anomalous Doppler instability, influences RE dynamics by enhancing pitch angle scattering. Three scenarios are analysed here, characterised by different RE generation rates and mechanisms. The main conclusions are drawn from correlations between the Cherenkov probe and other diagnostics. In particular, the Cherenkov probe permits the detection of fast electron expulsion with a high level of detail, presenting peaks with 100% signal contrast during tearing mode growth and rotation, and sub-peak structures reflecting the interplay between the magnetic island formed by the tearing mode, RE diffusion during island rotation and the geometry of obstacles in the vessel. Correlations between the Cherenkov signal, hard x-ray emission and electron cyclotron emission reveal the impulsive development of the anomalous Doppler instability with instability rise time in the microsecond scale resolved by the high time-resolution of the Cherenkov probe.

In this study, the feasibility of measuring the Sb content in different plastic materials by laser induced plasma spectroscopy (LIBS) is explored. Measurements were performed initially on a sample of pure Sb in order to identify the most prominent element transitions before different consumer plastics of varying matrix, composition and color were examined. The experimental set-up was based on a single pulse laser excitation at 1064 nm and a detection system consisting of an array of three compact spectrometers covering the range 236-796 nm. On pure Sb material, many atomic lines, particularly intense in the UV region, were observed, together with much weaker ionic transitions mainly in the visible spectral region. Unfortunately, all of the strong Sb transitions partially overlapped with those from Si, Fe and Ti, elements common in many plastic materials. For constructing the calibration curve for Sb content we exploited the Sb concentration values obtained by X-ray fluorescence (XRF) spectrometry, which varied from the detection limit (∼200 ppm) up to 65000 ppm. The analytical Sb I line at 276.99 nm was selected because, even if it has a weak contribution from one Fe I transition, its empirical subtraction leads to a well-correlated linear calibration graph. The corresponding detection limit was around 1400 ppm while in the absence of Fe, having an intense ionic transition at 259.93 nm, it is possible to use a more intense Sb I transition at 259.81 nm, achieving sensitivity on the order of 100 ppm. © 2018 The Royal Society of Chemistry.

In this work we describe a method for preparation and analysis of oils by Laser Induced Breakdown Spectroscopy (LIBS), aimed to minimize the necessary sample volume and the matrix effect while maximizing the detection sensitivity and measurement's repeatability. The preparation procedure consists in stabilizing the oil sample and silica wafer substrate at a fixed temperature, here of 40 °C, and in delivering an oil droplet on the wafer rotated by a spin coater. In this way, a uniform oil film is obtained, which thickness is controlled through the rotation speed. So prepared target is then scanned by using the LIBS instrument. From comparative measurements on the pure oil and oil containing 2100 ppm of various elements, we studied different potentials sources of the matrix effect. During the sample preparation, above a certain rotation speed the thickness of the liquid film is the same for the two oils although their kinematic viscosities are very different, meaning that the volume sampled by LIBS is the same. The measured oil transmissivity at the laser wavelength of 1064 nm significantly decreases with concentration of impurities, but this effect could be neglected when dealing with very thin films. The plasma formation threshold measured on the bulk oil samples decreases with the impurity content. In case of pure oil, also for the maximum laser energy here used (165 mJ), the plasma is mainly initiated on the wafer while the presence of impurities increases screening of the substrate by the plasma formed directly on the oil. The matrix effect disappears on a very thin film, here of 0.74 μm, where the C I line intensity in plasma does not vary with the total concentration of impurities between zero and 2100 ppm; simultaneously, the plasma emission becomes stable from one laser pulse to another, contrary to the case of a thick liquid layer. At 0.5 μs from the laser pulse the plasma electron density is much higher in presence of oil than on the bare substrate because of the initial plume confinement. In the optimized experimental conditions the plasma emission from oil was very intense although the sample volume probed by each laser pulse was of 0.3 nL only. By choosing properly the signal acquisition delay and the calibration procedure, the latter is dependent on the excitation energy of the analytical lines, we obtained the detection limits of 3.9 ppm, 0.49 ppm, 0.16 ppm and 0.082 ppm for Zn, Cd, Cu and Cr in oil, respectively.

In order to answer to some specific unsolved questions regarding ancient Roman frescoes from Villa della Piscina, already examined by other spectroscopic techniques, LIBS stratigraphic measurements were performed on the most representative sample fragments. We found that taking into account just the line intensities or applying a single normalization approach based on ratio of the element's analytical line and a selected transition from a main sample constituent, here of Ca, might produce misleading results of depth profiling by LIBS. During the laser induced ablation, parameters of the detected plasma might change both due to the crater development and different overlaid matrix materials, as in case of heterogeneous painted samples, possibly realized with different techniques. We performed the theoretical simulations to select the pair of Cu I and Ca I lines less sensitive to variations of the plasma temperature in presence of local thermal equilibrium (LTE). However, when using not gated detectors as here, the experimental results showed that only a partial LTE holds. For this reason, the choice of the optimum normalization line must take into account also the energy gap between the excited levels of the species, which energies affect the emission lifetime and consequently, the intensity captured by not gated detectors. In following, to the each element's analytical line a specific Ca I line was attributed for deducing the relative element distribution in sample. Following this approach and by detecting simultaneously up to 20 elements per laser pulse, it was possible to distinguish clearly by LIBS also thin overpainted layers of similar colour, and to recognize the painting technique used. Through detection of trace and light elements and studies of their correlations with other elements during ablation of on painted layer, in some cases it was possible also to establish the geographical provenance of the material used.

Here, we describe an innovative Integrated Laser Sensor (ILS) that combines four spectroscopic techniques and two vision systems into a unique, transportable device. The instrument performs Raman and Laser-Induced Fluorescence (LIF) spectroscopy excited at 355 nm and Laser-Induced Breakdown Spectroscopy (LIBS) excited at 1064 nm, and it also detects Laser Scattering (LS) from the target under illumination at 650 nm. The combination of these techniques supplies information about: material change from one scanning point to another, the presence of surface contaminants, and the molecular and elemental composition of top target layers. Switching between the spectroscopic techniques and the laser wavelengths is fully automatic. The instrument is equipped with an autofocus, and it performs scanning with a chosen grid density over an interactively-selected target area. Alternative to the spectroscopic measurements, it is possible to switch the instrument to a high magnification target viewing. The working distances tested until now are between 8.5 and 30 m. The instrument is self-powered and remotely controlled via wireless communication. The ILS has been fully developed at ENEA for security applications, and it was successfully tested in two outdoor campaigns where an automatic recognition of areas containing explosives in traces had been implemented. The strategies for the identification of nitro-compounds placed on various substrates as fingerprints and the results obtained at a working distance of 10 m are discussed in the following.

Optical and spectroscopic techniques offer unique possibilities for non destructive or micro-destructive characterization of surfaces, with widespread applications, starting from in-line monitoring of industrial processes. A significant group of industrial applications concerns nuclear grade material characterization and plasma diagnostics relevant to the thermonuclear fusion process. However, technologies and methodologies originally developed for specific in-vessel utilization, can easily find additional in-situ and remote application to environmental and cultural heritage (CH) diagnostics addressed to preventive conservation and restoration of surfaces. At ENEA Frascati different prototypes have been developed and patented to collect reflectance and fluorescence images excited at different ultraviolet and visible laser wavelengths, Raman and LIBS signals. Portable integrated instruments suitable for operation at different distances from a 1.5 to 30 m, have been assembled and operated in laboratory on multilayered samples and in field campaigns for Security and on CH painted surfaces. Significant results relevant to the cross fertilization among different applications will be presented and discussed.

Influence of time delay between two laser pulses on the LIBS (laser induced breakdown spectroscopy) signal inside liquids was investigated and the results are compared with data from literature. Plasma was produced by laser ablation (LA) of aluminum inside water and its emission after the second laser pulse was characterized by spectrally and time resolved detection. Light propagation through the vapor bubble formed by the first laser pulse was studied by measurements of beam scattering and transmission. Optical absorption by the evolving bubble is not significant, but its growth is accompanied by lowering of its refraction index nb with respect to surrounding liquid; this effect increases defocusing both of the incident beam and of the out-coming plasma radiation. Collection efficiency of the secondary plasma emission rapidly degrades with the cavity growth, but close to its full expansion the LIBS signal partially recovers through Snell's reflections at the liquid-vapor interface, which produce a bright spot close to the bubble center. Such a light redistribution allows detecting of the emission from external plasma volume, otherwise deflected out of the collection system. Except for strong line transitions from the main sample constituents, self-absorbed inside the high-pressure cavity, we observed the highest LIBS signal when sending the second pulse well before the bubble is fully expanded. Transitions of the pressure wave through the focal volume, formed by the first laser pulse and reflected from the cell's walls and sample back-plane, enhances the LIBS signal importantly. The measured lifetime of the secondary plasma rapidly decreases with the bubble expansion. Here, we also discuss the optimization of the optical collection system and some analytical aspects of double-pulse (DP) LIBS inside liquids. © 2013 Elsevier B.V.

Plasma and vapor bubble formation and evolution after a nanosecond laser pulse delivered to aluminum targets inside water were studied by fast photography. This technique was also applied to monitor the plasma produced by a second laser pulse and for different interpulse delays. The bubble growth was evident only after 3 μs from the first laser pulse and the bubble shape changed during expansion and collapse cycles. The evolution and propagation of the initial shockwave and its reflections both from the back sample surface and cell walls were detected by Schlieren photography. The primary plasma develops in two phases: violent particle expulsion and ionization during the first μs, followed by slow plasma growth from the ablation crater into the evolving vapor bubble. The shape of the secondary plasma strongly depends on the inner bubble pressure whereas the particle expulsion into the expanded bubble is much less evident. Both the primary and secondary plasma have similar duration of about 30 μs. Detection efficiency of the secondary plasma is much reduced by light refraction at the curved bubble-water interface, which behaves as a negative lens; this leads to an apparent reduction of the plasma dimensions. Defocusing power of the bubble lens increases with its expansion due to the lowering of the vapor's refraction index with respect to that of the surrounding liquid (Lazic et al., 2012 [1]). Smell's reflections of secondary plasma radiation at the expanded bubble wall redistribute the detected intensity on a wavelength-dependent way and allow gathering of the emission also from the external plasma layer that otherwise, would not enter into the optical system. © 2013 Elsevier B.V.

The laser induced plasma spectroscopy was applied on particles attached on substrate represented by a silica wafer covered with a thin oil film. The substrate itself weakly interacts with a ns Nd:YAG laser (1064 nm) while presence of particles strongly enhances the plasma emission, here detected by a compact spectrometer array. Variations of the sample mass from one laser spot to another exceed one order of magnitude, as estimated by on-line photography and the initial image calibration for different sample loadings. Consequently, the spectral lines from particles show extreme intensity fluctuations from one sampling point to another, between the detection threshold and the detector's saturation in some cases. In such conditions the common calibration approach based on the averaged spectra, also when considering ratios of the element lines i.e. concentrations, produces errors too large for measuring the sample compositions. On the other hand, intensities of an analytical and the reference line from single shot spectra are linearly correlated. The corresponding slope depends on the concentration ratio and it is weakly sensitive to fluctuations of the plasma temperature inside the data set. A use of the slopes for constructing the calibration graphs significantly reduces the error bars but it does not eliminate the point scattering caused by the matrix effect, which is also responsible for large differences in the average plasma temperatures among the samples. Well aligned calibration points were obtained after identifying the couples of transitions less sensitive to variations of the plasma temperature, and this was achieved by simple theoretical simulations. Such selection of the analytical lines minimizes the matrix effect, and together with the chosen calibration approach, allows to measure the relative element concentrations even in highly unstable laser induced plasmas. © 2017 Elsevier B.V.

Droplets of organic liquids on aluminum substrate were probed by an Nd:YAG laser, both in a steady state and during rotation at speeds 18–150 rpm. Rotation transforms the droplet into film, which estimated thickness at high speeds was below 3 μm and 20 μm for diesel and peanut oil, respectively. Line intensities from the liquid (C I) and the support (Al I) material were tracked as a function of the film thickness and the laser energy. By film thinning, the line intensities from liquid sample were enhanced up to a factor 100x; simultaneously, the LIBS signal fluctuations were reduced 5–10 times with respect to the steady droplet. In certain experimental conditions, the line intensities from the support material become very weak with respect to the C I line, indicating an efficient screening of the substrate by highly excited plasma from the liquid layer. At a fixed rotation speed, there is a laser energy threshold, dependent on the liquid thickness, above which the LIBS signal becomes stable. Here, we discuss the relative processes and optimization of the experimental conditions for the LIBS measurements frome one laser shot to another.

In this work we present studies of spatial and temporal plasma evolution after single pulse ablation of an aluminium target in water. The laser ablation was performed using 20 ns long pulses emitted at 1064 nm. The plasma characterization was performed by fast photography, the Schlieren technique, shadowgraphy and optical emission spectroscopy. The experimental results indicate the existence of two distinct plasma stages: the first stage has a duration of approximately 500 ns from the laser pulse, and is followed by a new plasma growth starting from the crater center. The secondary plasma slowly evolves inside the growing vapor bubble, and its optical emission lasts over several tens of microseconds. Later, the hot glowing particles, trapped inside the vapor cavity, were detected during the whole cycle of the bubble, where the first collapse occurs after 475 μs from the laser pulse. Differences in the plasma properties during the two evolution phases are discussed, with an accent on the optical emission since its detection is of primary importance for LIBS. Here we demonstrate that the LIBS signal quality in single pulse excitation underwater can be greatly enhanced by detecting only the secondary plasma emission, and also by applying long acquisition gates (in the order of 10-100 μs). The presented results are of great importance for LIBS measurements inside a liquid environment, since they prove that a good analytical signal can be obtained by using nanosecond pulses from a single commercial laser source and by employing cost effective, not gated detectors. © the Owner Societies 2016.

This paper provides an overview of the laser induced breakdown spectroscopy (LIBS) inside liquids, applied for detection of the elements present in the media itself or in the submerged samples. The processes inherent to the laser induced plasma formation and evolution inside liquids are discussed, including shockwave generation, vapor cavitation, and ablation of solids. Types of the laser excitation considered here are single pulse, dual pulse and multi-pulse. The literature relative to the LIBS measurements and applications inside liquids is reviewed and the most relevant results are summarized. Finally, we discuss the analytical aspects and release some suggestions for improving the LIBS sensitivity and accuracy in liquid environment.

With the aim to study alteration processes of the rock hewn churches from Lalibela (Ethiopia), we applied Laser Induced Breakdown Spectroscopy (LIBS) technique to measure the elemental composition both of the bulk rock materials and their external layers, exposed to the environmental factors. The analytical plasma was generated by nanosecond pulses of an Nd: YAG laser emitting at 1064 nm. Different major and minor sample constituents were detected, including Ca, Mg, Na, Fe, Ti, Al and K. The detected O emission originates both from air surrounding and the sample, while the intensity of N lines, coming exclusively from air, was used for the LIBS signal normalization. By depth profiling of the weathered basalt rock, we observed a lower presence of K in the external layers, corresponding to the first 5 laser shots. The emission from this element is anti-correlated with the line intensities from O, and this was attributed to the variations in relative abundances of clay minerals and K-feldspar. The analogue measurements were performed on the tuff rock, and compared to the spectra from powder samples containing only the external soft material, scratched from the rocks. These analyses show an abundance of H in the weathered, wetted layers and suggest that cations are lost from the constituent primary minerals and replaced by H+; this process disrupts the lattice structure and causes a marked loss of strength. The studies presented here demonstrate that LIBS is a useful technique for studying the alteration processes in the rocks, caused by environmental factors. © 2013 Elsevier Ltd.

The amount of tritium (T) retained in plasma facing components (PFCs) and in-vessel structures has to be carefully monitored in ITER because of the limits fixed by safety issues. Laser-Induced-Breakdown-Spectroscopy (LIBS) is one of the eligible techniques for this task because it does not require any sample pre-treatment (or removal), it can work both in atmospheric pressure or in vacuum, with different background gases. LIBS can be set up both on a robotic arm entering the vacuum vessel or outside it, for analyses during shut-down periods or in-between plasma discharges. In this paper we describe a new, compact LIBS system, mounted on the Frascati Tokamak Upgrade (FTU) robotic arm, to perform measurements on ITER-relevant samples placed in the FTU mock-up. The samples, composed of thin layers (few μm) of W, Al, D, simulate the co-deposition of Be with T on ITER divertor tiles (Be and T are replaced by Al and D in the samples). W, Al, D emission lines has been clearly detected, both as major constituents or in trace quantities, with different background gases using a single laser pulse.