Laser-induced Breakdown Spectroscopy Results Research Articles

An approach for measurement of the magnetic field near the surface of plasma-facing components in tokamak by laser induced breakdown spectroscopy based on Zeeman effect

Laser-induced breakdown spectroscopy (LIBS) has been demonstrated to diagnose the surface element distribution of plasma-facing components (PFCS) in fusion devices. However, the magnetic field intensity and polarity near the wall surface change frequently and cannot be measured in real time, which will affect the analytical accuracy of LIBS results. The determination of the strength and polarity direction of the magnetic field near the surface will be conducive to the quantitative analysis of LIBS and provide valuable information for the distribution of the magnetic field near the surface of PFCs. In this work, the effects of magnetic fields on the characteristics of laser-induced Mo plasma, such as the ablation depth and mass, the spatio-temporal evolution behavior of spectrum and the plasma parameters, were first systematically investigated. The different phenomenon of continuum radiation, Mo I line and Mo II line under the magnetic field were mutually verified by optical emission spectroscopy and fast plasma imaging methods. Meanwhile, an approach for measurement of the magnetic field intensity and polarity near the surface of PFCS by LIBS method has been proposed and investigated. When the magnetic field polarity is changed, the spatial distribution profile of Mo spectrum will drift in the opposite direction affected by of the Lorentz force, which realizes the measurement of magnetic field polarity. Moreover, the splitting distance of Mo I line caused by Zeeman effect with the variable magnetic fields were preliminarily calculated. The experimental values of splitting distance agree well with the theoretical values that calculated by the known magnetic field strength. These results confirm the feasibility of measuring the magnetic field intensity and polarity of PFCs surface by LIBS approach.

Study of Electronic Bands of Diatomic Molecules for the Evaluation of Toxicity of Green Crackers Using LIBS Coupled with Chemometric Method

Laser-induced Breakdown Spectroscopy (LIBS) is primarily an atomic emission spectroscopic method based on analyzing the spectral lines of elements in the laser-induced plasma. However, when the plasma cools down after its ignition, i.e., when one collects the emissions from the plasma after a certain interval of time/gate delay (~1 micro-second), the signature of the electronic bands of diatomic molecules is also observed along with ionic/atomic emission lines. The present manuscript reports the evaluation of toxicity/pollutants in green crackers based on the intensity of the electronic bands of the Aluminum Oxide (AlO), calcium oxide (CaO), and strontium oxide (SrO) molecules observed in the laser-induced plasma of the firecrackers. LIBS spectra of the green crackers show the presence of spectral lines of the heavy/toxic elements such as Al, Ca, Sr, Cr, Cu, and Ba, along with the electronic bands of the AlO, CaO, and SrO. Fourier Transform Infra-Red Spectroscopy (FTIR) has been used to validate the LIBS results and confirm the molecules in these crackers. The concentration of toxic elements in green crackers such as Aluminum (Al), Copper (Cu), and Chromium (Cr) has also been estimated using the Partial Least Square Regression method (PLSR) to evaluate and compare the extent of the toxicity of green crackers.

Stable sensing platform for diagnosing electrolyte disturbance using laser-induced breakdown spectroscopy.

Electrolyte disturbance is very common and harmful, increasing the mortality of critical patients. Hence, rapid and accurate detection of electrolyte levels is vital in clinical practice. Laser-induced breakdown spectroscopy (LIBS) has the advantage of rapid and simultaneous detection of multiple elements, which meets the needs of clinical electrolyte detection. However, the cracking caused by serum drying and the effect of the coffee-ring led to the unstable spectral signal of LIBS and inaccurate detection results. Herein, we propose the ordered microarray silicon substrates (OMSS) obtained by laser microprocessing, to solve the disturbance caused by cracking and the coffee-ring effect in LIBS detection. Moreover, the area of OMSS is optimized to obtain the optimal LIBS detection effect; only a 10 uL serum sample is required. Compared with the silicon wafer substrates, the relative standard deviation (RSD) of the serum LIBS spectral reduces from above 80.00% to below 15.00% by the optimized OMSS, improving the spectral stability. Furthermore, the OMSS is combined with LIBS to form a sensing platform for electrolyte disturbance detection. A set of electrolyte disturbance simulation samples (80% of the ingredients are human serum) was prepared for this platform evaluation. Finally, the platform can achieve an accurate quantitative detection of Na and K elements (Na: RSD < 6.00%, R2 = 0.991; K: RSD < 4.00%, R2 = 0.981), and the detection time is within 5 min. The LIBS sensing platform has a good prospect in clinical electrolyte detection and other blood-related clinical diagnoses.

Practical application of Laser-induced Breakdown Spectroscopy (LIBS) for the detection of chlorides in concrete structures

Some reinforced concrete damage is caused by the penetration of harmful substances, such as chlo-rine, into the concrete matrix. This can trigger processes such as corrosion. With LIBS it is possible to measure a high-quality chlorine distribution. The results can be expressed in weight percent and show a 2D representation and a detailed ingress profile. In this presentation we will give an overview of how libs work and what important information this method can provide (carbonation, sulfur detection). In addition, a comparison between the wet chemical (standard procedure) and the LIBS results is shown. The advantages of the LIBS results are presented. Information on how much and how deep the chlorine penetrates is important information for civil engineering. Due to the high-resolution mapping it is pos-sible to measure a large number of measurement points on the sample (~100.000 measurement points, Drill core diameter 50 mm, length 100 mm). Each measuring point contains spectral information about the element concentration (measuring point diameter 100 µm). With this information, the data points that are aggregates can be excluded. For this reason, only measuring points relating to the cement paste matrix are considered. In this presentation, practical results are shown, and the added value of the process is presented.

LIBS and pXRF validation for the removal of Pb by bio-CaCO3 nanoparticles from contaminated water

In this work, laser-induced breakdown spectroscopy (LIBS) was applied to qualitatively evaluate lead adsorbed from industrial wastewater by nano-CaCO3. Eggshell as a natural source of CaCO3 has been used as a sorbent owing to its low cost and unrivalled adsorption capacity to remove Pb from contaminated water. The structure and morphology of CaCO3 nano-powders were investigated using scanning electron microscopy (SEM), transmission electron microscope (TEM) and Fourier transforms infrared (FTIR). LIBS results were experimentally validated by the results obtained using portable X-ray fluorescence spectroscopy (pXRF) and energy dispersive X-ray (EDS), which confirmed the feasibility of using LIBS to detect traces of Pb ions, while the adsorption process is applied under governing parameters. Langmuir and Freundlich isotherm models were used to model the experimental data. The kinetics of adsorption mechanisms were studied using Lagergren's pseudo-first-order and McKay and Ho's pseudo-second-order. The obtained results demonstrated that bio-CaCO3 nanoparticles could be used as an effective lead-sorbent from wastewater. Accordingly, it is possible to utilize this adsorption technique as a promising practical approach for the treatment of lead-contaminated industrial wastewater and its recirculation.Graphical abstractHighlightsNatural nano CaCO3 from eggshell was prepared mechanically as a low-cost adsorbent and characterized by SEM, TEM, and FTIR.The capacity of removing Pb (II) by nano-CaCO3 was dependent on pH, metal concentration and contact time .LIBS was used for qualitative analysis of adsorbed Pb (II) and the results were validated with those obtained by EDX and pXRF spectrometry; in addition, isotherm models and kinetics of adsorption mechanisms were investigated.

Rapid Determination of Arsenic in Traditional Chinese Medicine by Laser-Induced Breakdown Spectroscopy (LIBS)

High arsenic (As) content in medicine may threaten health and its determination is necessary. However, traditional methods cannot achieve rapid analysis because of complex digestion procedures. Exploring rapid and accurate methods for the determination of As is urgent. In this study, the As concentration in niuhuangjiedu tablets (NHJDTs) was accurately and rapidly determined by laser-induced breakdown spectroscopy (LIBS). Furthermore, comprehensive health risks of As were analyzed combined with solubility measurements to evaluate the impact on humans. The results showed that the relative standard deviation and relative error of the LIBS results were less than 10% for detection period of less than 0.3 h, which meets the requirements for rapid, accurate, and convenient As determination. The indices for non-carcinogenic and carcinogenic risk for total As and soluble As in niuhuangjiedu tablets were 966.67, 0.15, 4.37, and 6.72 × 10−4, respectively, indicating the presence of potential health risks. This work provided support for further investigation for quality control of pharmaceutical products.

Rapid Determination and Quantification of Nutritional and Poisonous Metals in Vastly Consumed Ayurvedic Herbal Medicine (Rejuvenator Shilajit) by Humans Using Three Advanced Analytical Techniques.

‏Shilajit is used commonly as Ayurvedic medicine worldwide which is Rasayana herbo-mineral substance and consumed to restore the energetic balance and to prevent diseases like cognitive disorders and Alzheimer. Locally, Shilajit is applied for patients diagnosed with bone fractures. For safety of the patients, the elemental analysis of Shilajit is imperative to evaluate its nutritional quality as well as contamination from heavy metals. The elemental composition of Shilajit was conducted using three advanced analytical techniques (LIBS, ICP, and EDX). For the comparative studies, the two Shilajit kinds mostly sold globally produced in India and Pakistan were collected. Our main focus is to highlight nutritional eminence and contamination of heavy metals to hinge on Shilajit therapeutic potential. In this work, laser-induced breakdown spectroscopy (LIBS) was applied for qualitative and quantitative analysis of the Shilajit. Our LIBS analysis revealed that Shilajit samples composed of several elements like Ca, S, K, Mg, Al, Na, Sr, Fe, P, Si, Mn, Ba, Zn, Ni, B, Cr, Co, Pb, Cu, As, Hg, Se, and Ti. Indian and Pakistani Shilajits were highly enriched with Ca, S, and K nutrients and contained Al, Sr, Mn, Ba, Zn, Ni, B, Cr, Pb, As, and Hg toxins in amounts that exceeded the standard permissible limit. Even though the content of most elements was comparable among both Shilajits, nutrients, and toxins, in general, were accentuated more in Indian Shilajit with the sole detection of Hg and Ti. The elemental quantification was done using self-developed calibration-free laser-induced breakdown spectroscopy (CF-LIBS) method, and LIBS results are in well agreement with the concentrations determined by standard ICP-OES/MS method. To verify our results by LIBS and ICP-OES/MS techniques, EDX spectroscopy was also conducted which confirmed the presence above mentioned elements. This work is highly significant for creating awareness among people suffering due to overdose of this product and save many human lives.

Microwave induced plasma optical emission spectrometry (MIP OES) and laser-induced breakdown spectroscopy (LIBS) for multi-element determination and location in ceramic tableware

In the present study, the microwave induced plasma optical emission spectrometry (MIP OES) and laser-induced breakdown spectroscopy (LIBS) complementary techniques are used to determine and locate metals in ceramic tableware samples. For quantitative analysis by MIP OES, a new method for sample treatment is proposed, preparing the samples using ultrasonic decomposition aided by an acid mixture containing HNO3 and HF. The highest average concentrations were found in the group of Brazilian samples for most of the analytes. The accuracy of the quantitative method was assessed by comparing the results with two methods described in the literature. No significant differences were detected. Aiming at qualitative analysis and analyte locating by LIBS, a sample fragment was already sufficient for the analysis, being possible to observe that Al, Ba, Ca, Fe, K, Li, Mg, Na and Ti are present in the ceramic mass and decorated surface, while Cd, Co, Cr, Cu, Mn, Pb and Zn are found only on the sample surface. Besides, according to LIBS results, it would be essential to pay attention to pigmentation, which contains most of the potentially toxic elements, at locations in direct contact with food to minimize the risk of leaching and avoid human contamination. This study shows that MIP OES and LIBS can be used complementarily to improve the analytical information used to control the ceramic tableware quality and safety. The conclusions of this work can be extended to several other types of samples where both the average contents and the location of the elements are relevant.

Development of a simple method based on LIBS for evaluation of neutron production targets made of hydrogen isotopes

In the present work we propose a fast and simple method, based on Laser Induced Breakdown Spectroscopy (LIBS), to evaluate Neutron Production Targets. Targets of interest consist of hydrogen (particularly deuterium or tritium) contained in a titanium matrix. The method aims to evaluate the relative content of hydrogen within the titanium matrix, in order to determine if the target is “accepted” or “rejected” according to this content. Several deuterium targets have been fabricated (TiDx), with different deuterium concentrations, and different techniques have been used to characterize their surfaces. Optical Coherent Tomography has been used to characterize the size and shape of LIBS holes, in order to determine LIBS depth of analysis. Grazing Incidence X-ray Diffraction has been used to determine a range for deuterium relative content. Elastic Recoil Detection Analysis (ERDA) is proposed for future LIBS calibration, since it provides a single value for relative content, has a depth of analysis similar to LIBS and also allows to distinguish between different isotopes. ERDA first results are reported in comparison with LIBS results.

In-situ LIBS and NRA deuterium retention study in porous W-O and compact W coatings loaded by Magnum-PSI

The purpose of this study is to investigate the applicability of in-situ laser induced breakdown spectroscopy (LIBS) for deuterium retention measurements in tungsten coatings with different morphology and oxygen content. These were exposed to a Gaussian beam of deuterium plasma in the Magnum-PSI linear plasma device. The deuterium line intensities determined by LIBS were compared with the deuterium content measured by nuclear reaction analysis (NRA).Both LIBS and NRA results showed that higher deuterium retention was achieved in the coating region corresponding to the periphery of the plasma beam. This decreasing deuterium retention in the central region can be attributed to higher surface temperature. At the same time, the deuterium retention in different coating types assessed by LIBS D intensity was markedly different from the retention determined by NRA. Porous W-O coating with high oxygen content had the highest deuterium retention according to NRA while D intensity obtained by LIBS was an order of magnitude smaller when compared with other coatings. The deuterium retention in compact W coating and thick W coating was almost the same and LIBS D intensities were also comparable for these coatings. The results demonstrate the LIBS applicability and its limits in different coating types.

Combination of analytic techniques to chemical characterization and preservation of Jurassic clam shrimp carapaces from La Matilde Formation, Patagonia

Chemical studies of fossil clam shrimps have taken relevance in the possibility of inferring about fossilization processes. Laser–induced Breakdown Spectroscopy (LIBS) is an attractive technique for geological analyses because the laser can ablate a few micrograms directly from a small area on the solid sample. On the other hand, RAMAN spectroscopy is a technique that allows rapid and non-destructive in situ detection of the components of the samples and has been used in micropalaeontology to identify carbonaceous materials. In this study, the aim was an analysis of the preservation of the clam shrimp Eosolimnadiopsis? santacrucensis Gallego, 1994 from La Matilde Formation (Jurassic) using diverse methods including LIBS, RAMAN and X–ray fluorescence (XRF) techniques as well as surrounding rock. Afterwards LIBS results were evaluated using principal component analysis (PCA). According to XRF data, Si was the main element, indicating that the rock sample consists primarily of silicate minerals. Our results of LIBS and PCA analysis indicate chemical changes between the points from carapaces and rock matrix. Some areas of the carapace showed high peaks of Ca, Na, Mg and it was variable for Si, while in other parts of the carapace and rock matrix the Si remained at high intensity. Also, RAMAN spectroscopic analysis revealed the presence of amorphous carbon. This is the first report and evaluation on the LIBS and RAMAN techniques applied to fossil clam shrimps and contributes to obtaining a range of additional information to subsequently establish the different mechanisms involved in the taphonomic history of these organisms.

Investigation of compositional analysis and physical properties for Ni-Cr-Nb alloys using laser-induced breakdown spectroscopy

In this work, laser-induced breakdown spectroscopy (LIBS) analysis is optimized for direct estimation of elemental composition, thermal conductivity and hardness for Ni-Cr-Nb alloys. These alloys were chosen with a variable elemental content of niobium and chromium. The influence of laser energy and shot numbers on measuring line intensity was investigated. Based on the ratio between two spectral lines, calibration curves were formed to estimate the element concentration and LIBS results were confirmed with related energy-dispersive X-ray spectroscopy (EDS) data. Hardness and thermal conductivity estimation using LIBS were done by measuring the ratio between two spectral lines, plasma excitation temperature and electron density for different samples. Semi-empirical formulas correlated hardness and thermal conductivity with plasma temperature were established.

LIBS study of ITER relevant tungsten–oxygen coatings exposed to deuterium plasma in Magnum-PSI

We discuss the applicability of laser induced breakdown spectroscopy (LIBS) for deuterium retention analysis in compact and porous tungsten-oxide (W-O) coatings. Deuterium loading was performed by exposing the coatings to deuterium plasma in Magnum-PSI linear plasma device.The deuterium signals obtained by ex-situ LIBS had sufficiently good signal-to-noise ratio for reliable separation of essentially broadened hydrogen and deuterium lines as well as for comparison of the lateral and depth distributions of deuterium in the coatings. Strong deuterium signal was obtained for the first laser shot which corresponded to the surface layer of the W-O coatings whereas deeper in the coating the signal decreased to noise level. In addition, the deuterium signal was highest in the central region of compact W-O coating. For both coatings, depth profiles of elements obtained by LIBS match with those recorded by secondary ion mass spectroscopy (SIMS) in the lateral direction along the sample surface. The results of LIBS and SIMS results were supported by Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD) data which showed that the exposure to deuterium plasma resulted in remarkable changes in the surface morphology along the sample surface. The study demonstrates the LIBS potential in deuterium retention measurements in plasma facing components.

Half-life determination of inorganic-organic hybrid nanomaterials in mice using laser-induced breakdown spectroscopy

Inorganic or inorganic-organic hybrid nanomaterials have great potential for applications in the biomedical fields. Biological half-life is an essential pharmacokinetic parameter for these materials to function in vivo. Compared to inductively coupled plasma mass spectrometry (ICP-MS), which is the gold standard, laser-induced breakdown spectroscopy (LIBS) is a faster and more efficient elemental detection method. We investigated an efficient way to quantify the metabolic rate using LIBS. Nanoparticle platforms, such as manganese dioxide-bovine serum albumin (MnO2-BSA) or boehmite-bovine serum albumin (AlO(OH)-BSA) were injected into mice through intravenous administration for LIBS spectrum acquisition. First, the spectral background was corrected using the polynomial fitting method; The spectral interference was eliminated by Lorentz fitting for each LIBS spectrum simultaneously. The support vector regression (SVR) was then used for LIBS quantitative analyses. Finally, the LIBS results were compared with the ICP-MS ones. The half-lives of MnO2-BSA calculated by LIBS and ICP-MS were 2.49 and 2.42 h, respectively. For AlO(OH)-BSA, the half-lives detected by LIBS and ICP-MS were 3.46 and 3.57 h, respectively. The relative error of LIBS is within 5% compared to ICP-MS. The results demonstrate that LIBS is a valuable tool for quantifying the metabolic rates with a high degree of accuracy.

Potentialities of a Laser-Induced Breakdown Spectroscopy Technique in the Study of Polymer Composites.

A laser-induced breakdown spectroscopy (LIBS) technique was used to evaluate the filler content in particulate epoxy-copper composites. A potential application for a direct and fast measurement of the filler in composites through the LIBS results is suggested using calibrated samples. The methodology used in this work makes possible the incorporation of LIBS as a quantitative technique for the study of particle metal-filled epoxy composites, providing a method to obtain a direct estimation of the filler volume fraction.

Determination of Lead and Chromium in Aloe Vera Pulp and Aloe Vera-Based Cosmetics by Laser-Induced Breakdown Spectroscopy (LIBS)

This study focuses on the application of laser-induced breakdown spectroscopy (LIBS) to determine lead and chromium in pristine aloe vera and aloe vera based beauty soaps using the second harmonic (532 nm) of a Q-switched Nd:YAG laser. The optimal experimental conditions were evaluated to improve the sensitivity of the detection system by a parametric dependence study. The atomic transition lines at 405.7 nm and 425.4 nm were used as the analytical lines to determine lead and chromium, respectively. The LIBS system was calibrated for these toxic elements and the samples under analysis included 8.00–15.00 ppm by mass of lead and 5.00–12.00 ppm by mass of chromium, which are far above the safe permissible levels of these elements (i.e., 0.50 ppm for Pb and 1.00 ppm for Cr). The quantitative results were checked before and after normalization with the background and better outcomes were obtained when the spectrum was normalized with the background. The LIBS results were compared to the outcomes of selected samples by a standard analytical method, inductively coupled plasma – optical emission spectroscopy (ICP-OES). Both outcomes were in outstanding conformity implying the reliability of the LIBS measurements. The current study is attractive for the general evaluation of human health and specifically for the analysis of aloe vera based cosmetics.

Quantitative analysis of saindha salt using laser induced breakdown spectroscopy and cross-validation with ICP-MS

Saindha salt is considered to be more advantageous than the other edible salts for the patients suffering from diabetes, blood pressure and kidney diseases. To explore the constituent elements of this salt, laser induced breakdown spectroscopy (LIBS) has been exploited for its qualitative and quantitative analysis. The third harmonic (355 nm) of a Q-switched Nd:YAG laser has been used to produce the saindha salt plasma and the time integrated optical emission spectra were registered using a set of six miniature spectrometers covering the spectral range of 230–805 nm. The spectroscopic analysis of the emission spectra predominately revealed numerous neutral or singly ionized emission lines of Ca, Mg, Na, K, Fe, Sr, Si, Li and Al. The laser produced plasma was characterized by calculating the electron temperature from the Boltzmann plots and the electron number density from the Stark broadened line profile as a function of laser irradiance and distance from the target sample. The relative concentration of the constituent elements was extracted by the integrated line intensities of the strongest spectral line of each element using the self-calibration-LIBS (SC-LIBS) and one-line calibration free-LIBS (OLCF-LIBS) methods. For cross-validation, the LIBS results have been compared with that obtained from the inductively coupled plasma-mass spectroscopy (ICP-MS) showing good agreement.

Modulation and mechanism of shockwaves induced on metals by femtosecond laser double-pulse

An ultrafast pump-probe shadowgraph imaging system and a laser induced breakdown spectroscopy (LIBS) system were used to investigate the modulation and mechanism of shockwaves of nickel (Ni) and aluminum (Al) induced by femtosecond laser double-pulse. With a suitable pulse delay, the bulge in the axial direction of the shockwave can be effectively eliminated and the shockwave expanded evenly in a hemispheric structure. The radial expansion distance of shockwaves of Ni and Al increased by 30% and 50% respectively with double-pulse excitation. The strong coupling of laser with liquid layer and plasma shielding effect were responsible for the enhancement of shockwaves within different regimes of pulse delay. Different enhancement trends were observed for the shockwaves of Ni and Al in the initial regime of pulse delay. Further study indicated that the reduced ablation volume of Al counteracted the enhancement effect of double-pulse on plasma and shockwave and it was the dominant mechanism for the stagnant of Al shockwave. The LIBS results of Ni and Al showed good agreement with the increasing tendency of shockwaves and confirmed the non-negligible effect of the removal volume on the intensity of plasma and shockwave. The results and mechanism exhibited the potential of femtosecond laser double-pulse in plasma and shockwave modulation and application.

Investigation of short-term, high-temperature oxidation of AlCrN coating on WC substrate

A surface analysis was performed on an aluminum chromium nitride (AlCrN) coating formed on a tungsten carbide (WC) substrate subjected to short-term (in minutes) oxidation at an elevated temperature (900 °C) using focused ion beam (FIB), X-ray photoelectron spectroscopy (XPS), grazing incidence X-ray diffraction (GI-XRD), and laser-induced breakdown spectroscopy (LIBS). To separately analyze a coating with a thickness of several micrometers, the GI-XRD method was used. For cross-sectional imaging, the samples were milled using an FIB system, and chemical bonding states and surface elemental concentrations were analyzed by XPS. Within just a few seconds, the color of the AlCrN coating surface changed irregularly and, after 10 min, the entire coating layer surface changed. The entire coating surface oxidation as discoloration progressed in partial areas after 30 min. Based on the GI-XRD and XPS results, after 1 min, alumina and chromium oxides formed on the outermost surface, and after 10 min, Cr-W and Co-W oxide phases appeared, resulting from a reaction with WC near the interface. The atomic concentration of nitrogen in the AlCrN coating decreased after few seconds on the outermost surface and was almost eliminated after 10 min; oxygen showed the opposite trend. Finally, the FIB and LIBS results showed that voids formed within the coating layer and interface at high temperatures, and diffusion of Al and Cr in subsequent reactions was identified. This work demonstrates interesting results from various analyses that differ from previously reported AlCrN coating oxidation behaviors, and could provide a better understanding of long-term reactions for the surface oxidation of AlCrN coatings at high temperatures.

The Use of Laser Induced Breakdown Spectroscopy (LIBS) to Study Catalyst Deactivation of V2O5/γ‐Al2O3 as Compared to Inductively Coupled Plasma Optical Emission Spectrometry

Laser Induced Breakdown Spectroscopy (LIBS) method is introduced as a novel approach in this work to study catalyst deactivation of V2O5/γ‐‐Al2O3 for gas‐phase dehydration of glycerol and producing acrolein. The LIBS results of V2O5/γ‐Al2O3 samples are compared with those data that are obtained by Inductively Coupled Plasma Optical Emission Spectrometry (ICP‐OES). Experimental data of LIBS data specify that line intensities of vanadium are decreased by deactivation of V2O5/γ‐Al2O3 catalyst. A comparison between the results of LIBS test as well as ICP‐OES analysis shows that the amount of vanadium is decreased in the catalyst. Moreover, coke formation changes the surface of the catalyst. The results of deactivation of V2O5/γ‐Al2O3 are also compared with Pd/C catalyst deactivation.