Quantitative analysis of titanium concentration using calibration-free laser-induced breakdown spectroscopy (LIBS)

Science.gov (United States)

Zaitun; Prasetyo, S.; Suliyanti, M. M.; Isnaeni; Herbani, Y.

2018-03-01

Laser-induced breakdown spectroscopy (LIBS) can be used for quantitative and qualitative analysis. Calibration-free LIBS (CF-LIBS) is a method to quantitatively analyze concentration of elements in a sample in local thermodynamic equilibrium conditions without using available matrix-matched calibration. In this study, we apply CF-LIBS for quantitative analysis of Ti in TiO2 sample. TiO2 powder sample was mixed with polyvinyl alcohol and formed into pellets. An Nd:YAG pulsed laser at a wavelength of 1064 nm was focused onto the sample to generate plasma. The spectrum of plasma was recorded using spectrophotometer then compared to NIST spectral line to determine energy levels and other parameters. The value of plasma temperature obtained using Boltzmann plot is 8127.29 K and electron density from calculation is 2.49×1016 cm-3. Finally, the concentration of Ti in TiO2 sample from this study is 97% that is in proximity with the sample certificate.

ANALISIS UNSUR Ag PADA SAMPEL CAIR DENGAN LASER INDUCED BREAKDOWN SPECTROSCOPY (LIBS

Directory of Open Access Journals (Sweden)

Sinaga Natalia Declarossy

2014-02-01

Full Text Available It has been done research on the analysis of Ag element in the liquid electrolyte with Laser Induced Breakdown Spectroscopy (LIBS through electrolysis method. Observations conducted by LIBS using Nd-YAG laser (1064nm, 7ns. Prior to analyze, first looking for the optimum conditions of experiments had been done. The results showed that the optimum laser energy to the characterization of the elements Ag was 100 mJ and optimum conditions of electric current and time deposition on electrolysis process were 4.93 mA and 10 minutes, respectively. These conditions, next, for the application of quantitative analysis of Ag solution that started from concentration 300 ppm to the lowest concentration and limit of detection obtained 1 ppm.

Laser-Induced Breakdown Spectroscopy (LIBS) in a Novel Molten Salt Aerosol System.

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Williams, Ammon N; Phongikaroon, Supathorn

2017-04-01

In the pyrochemical separation of used nuclear fuel (UNF), fission product, rare earth, and actinide chlorides accumulate in the molten salt electrolyte over time. Measuring this salt composition in near real-time is advantageous for operational efficiency, material accountability, and nuclear safeguards. Laser-induced breakdown spectroscopy (LIBS) has been proposed and demonstrated as a potential analytical approach for molten LiCl-KCl salts. However, all the studies conducted to date have used a static surface approach which can lead to issues with splashing, low repeatability, and poor sample homogeneity. In this initial study, a novel molten salt aerosol approach has been developed and explored to measure the composition of the salt via LIBS. The functionality of the system has been demonstrated as well as a basic optimization of the laser energy and nebulizer gas pressure used. Initial results have shown that this molten salt aerosol-LIBS system has a great potential as an analytical technique for measuring the molten salt electrolyte used in this UNF reprocessing technology.

Multi-Pulse Excitation for Underwater Analysis of Copper-Based Alloys Using a Novel Remote Laser-Induced Breakdown Spectroscopy (LIBS) System.

Science.gov (United States)

Guirado, Salvador; Fortes, Francisco J; Laserna, J Javier

2016-04-01

In this work, the use of multi-pulse excitation has been evaluated as an effective solution to mitigate the preferential ablation of the most volatile elements, namely Sn, Pb, and Zn, observed during laser-induced breakdown spectroscopy (LIBS) analysis of copper-based alloys. The novel remote LIBS prototype used in this experiments featured both single-pulse (SP-LIBS) and multi-pulse excitation (MP-LIBS). The remote instrument is capable of performing chemical analysis of submersed materials up to a depth of 50 m. Laser-induced breakdown spectroscopy analysis was performed at air pressure settings simulating the conditions during a real subsea analysis. A set of five certified bronze standards with variable concentration of Cu, As, Sn, Pb, and Zn were used. In SP-LIBS, signal emission is strongly sensitive to ambient pressure. In this case, fractionation effect was observed. Multi-pulse excitation circumvents the effect of pressure over the quantitative analysis, thus avoiding the fractionation phenomena observed in single pulse LIBS. The use of copper as internal standard minimizes matrix effects and discrepancies due to variation in ablated mass. © The Author(s) 2016.

Qualitative Analysis of Dairy and Powder Milk Using Laser-Induced Breakdown Spectroscopy (LIBS).

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Alfarraj, Bader A; Sanghapi, Herve K; Bhatt, Chet R; Yueh, Fang Y; Singh, Jagdish P

2018-01-01

Laser-induced breakdown spectroscopy (LIBS) technique was used to compare various types of commercial milk products. Laser-induced breakdown spectroscopy spectra were investigated for the determination of the elemental composition of soy and rice milk powder, dairy milk, and lactose-free dairy milk. The analysis was performed using radiative transitions. Atomic emissions from Ca, K, Na, and Mg lines observed in LIBS spectra of dairy milk were compared. In addition, proteins and fat level in milks can be determined using molecular emissions such as CN bands. Ca concentrations were calculated to be 2.165 ± 0.203 g/L in 1% of dairy milk fat samples and 2.809 ± 0.172 g/L in 2% of dairy milk fat samples using the standard addition method (SAM) with LIBS spectra. Univariate and multivariate statistical analysis methods showed that the contents of major mineral elements were higher in lactose-free dairy milk than those in dairy milk. The principal component analysis (PCA) method was used to discriminate four milk samples depending on their mineral elements concentration. In addition, proteins and fat level in dairy milks were determined using molecular emissions such as CN band. We applied partial least squares regression (PLSR) and simple linear regression (SLR) models to predict levels of milk fat in dairy milk samples. The PLSR model was successfully used to predict levels of milk fat in dairy milk sample with the relative accuracy (RA%) less than 6.62% using CN (0,0) band.

Determination of Rare Earth Elements in Geological Samples Using Laser-Induced Breakdown Spectroscopy (LIBS).

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Bhatt, Chet R; Jain, Jinesh C; Goueguel, Christian L; McIntyre, Dustin L; Singh, Jagdish P

2018-01-01

Laser-induced breakdown spectroscopy (LIBS) was used to detect rare earth elements (REEs) in natural geological samples. Low and high intensity emission lines of Ce, La, Nd, Y, Pr, Sm, Eu, Gd, and Dy were identified in the spectra recorded from the samples to claim the presence of these REEs. Multivariate analysis was executed by developing partial least squares regression (PLS-R) models for the quantification of Ce, La, and Nd. Analysis of unknown samples indicated that the prediction results of these samples were found comparable to those obtained by inductively coupled plasma mass spectrometry analysis. Data support that LIBS has potential to quantify REEs in geological minerals/ores.

Laser-induced breakdown spectroscopy (LIBS): an overview of recent progress and future potential for biomedical applications.

Science.gov (United States)

Rehse, S J; Salimnia, H; Miziolek, A W

2012-02-01

The recent progress made in developing laser-induced breakdown spectroscopy (LIBS) has transformed LIBS from an elemental analysis technique to one that can be applied for the reagentless analysis of molecularly complex biological materials or clinical specimens. Rapid advances in the LIBS technology have spawned a growing number of recently published articles in peer-reviewed journals which have consistently demonstrated the capability of LIBS to rapidly detect, biochemically characterize and analyse, and/or accurately identify various biological, biomedical or clinical samples. These analyses are inherently real-time, require no sample preparation, and offer high sensitivity and specificity. This overview of the biomedical applications of LIBS is meant to summarize the research that has been performed to date, as well as to suggest to health care providers several possible specific future applications which, if successfully implemented, would be significantly beneficial to humankind.

Identification of offal adulteration in beef by laser induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Velioglu, Hasan Murat; Sezer, Banu; Bilge, Gonca; Baytur, Süleyman Efe; Boyaci, Ismail Hakki

2018-04-01

Minced meat is the major ingredient in sausages, beef burgers, and similar products; and thus it is the main product subjected to adulteration with meat offal. Determination of this kind of meat adulteration is crucial due to religious, economic and ethical concerns. The aim of the present study is to discriminate the beef meat and offal samples by using laser induced breakdown spectroscopy (LIBS). To this end, LIBS and multivariate data analysis were used to discriminate pure beef and offal samples qualitatively and to determine the offal mixture adulteration quantitatively. In this analysis, meat samples were frozen and LIBS analysis were performed. The results indicate that by using principal component analysis (PCA), discrimination of pure offal and offal mixture adulterated beef samples can be achieved successfully. Besides, adulteration ratio can be determined using partial least square analysis method (PLS) with 0.947 coefficient of determination (R 2 ) and 3.8% of limit of detection (LOD) values for offal mixture adulterated beef samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

Analysis of heterogeneous gallstones using laser-induced breakdown spectroscopy (LIBS) and wavelength dispersive X-ray fluorescence (WD-XRF).

Science.gov (United States)

Jaswal, Brij Bir S; Kumar, Vinay; Sharma, Jitendra; Rai, Pradeep K; Gondal, Mohammed A; Gondal, Bilal; Singh, Vivek K

2016-04-01

Laser-induced breakdown spectroscopy (LIBS) is an emerging analytical technique with numerous advantages such as rapidity, multi-elemental analysis, no specific sample preparation requirements, non-destructiveness, and versatility. It has been proven to be a robust elemental analysis tool attracting interest because of being applied to a wide range of materials including biomaterials. In this paper, we have performed spectroscopic studies on gallstones which are heterogeneous in nature using LIBS and wavelength dispersive X-ray fluorescence (WD-XRF) techniques. It has been observed that the presence and relative concentrations of trace elements in different kind of gallstones (cholesterol and pigment gallstones) can easily be determined using LIBS technique. From the experiments carried out on gallstones for trace elemental mapping and detection, it was found that LIBS is a robust tool for such biomedical applications. The stone samples studied in the present paper were classified using the Fourier transform infrared (FTIR) spectroscopy. WD-XRF spectroscopy has been applied for the qualitative and quantitative analysis of major and trace elements present in the gallstone which was compared with the LIBS data. The results obtained in the present paper show interesting prospects for LIBS and WD-XRF to study cholelithiasis better.

Wavelength dependence of laser induced breakdown spectroscopy (LIBS) on questioned document investigation.

Science.gov (United States)

Elsherbiny, Nany; Aied Nassef, O

2015-07-01

The fast and nearly non-destructive criteria of laser induced breakdown spectroscopy (LIBS) technique has been exploited for forensic purposes, specifically, document investigation. The dependence of the optical emission spectra of different black gel ink samples on the excitation laser wavelength, namely the visible wavelength at λ=532 nm and the IR wavelength at λ=1064 nm, was studied. The inks of thirty black gel-ink pens comprising ten brands were analyzed to determine the variation of the chemical composition of ink and to discriminate among them with minimum mass removal and minimum damage to the document's paper. Under the adopted experimental conditions, the ability of the visible LIBS to differentiate among the different ink samples was successful compared to IR LIBS at the same laser pulse energy (~25 mJ/pulse, laser fluence is ~1400J·cm(-2) for visible laser and ~1100J·cm(-2) for IR laser) which could be attributed to the IR absorption effects by the black ink. However, the visible LIBS produces deeper crater with respect to that produced by IR LIBS. Applying IR LIBS with higher pulse energy of ~87mJ (laser fluence is ~4100J·cm(-2)), identification and differentiation of the adopted samples was performed with producing a larger-diameter but superficial crater. The plasma parameters are discussed at the adopted experimental conditions. The results support the potential of LIBS technique using both the visible and IR lasers to be commercially developed for forensic document examination. Copyright © 2015 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

Study of atomic and molecular emission spectra of Sr by laser induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Bhatt, Chet R; Alfarraj, Bader; Ayyalasomayajula, Krishna K; Ghany, Charles; Yueh, Fang Y; Singh, Jagdish P

2015-12-01

Laser Induced Breakdown Spectroscopy (LIBS) is an ideal analytical technique for in situ analysis of elemental composition. We have performed a comparative study of the quantitative and qualitative analysis of atomic and molecular emission from LIBS spectra. In our experiments, a mixture of SrCl2 and Al2O3 in powder form was used as a sample. The atomic emission from Sr and molecular emission from SrCl and SrO observed in LIBS spectra were analyzed. The optimum laser energies, gate delays, and gate widths for selected atomic lines and molecular bands were determined from spectra recorded at various experimental parameters. These optimum experimental conditions were used to collect calibration data, and the calibration curves were used to predict the Sr concentration. Limits of detection (LODs) for selected atomic and molecular emission spectra were determined.

Characterization and forensic analysis of soil samples using laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Jantzi, Sarah C; Almirall, José R

2011-07-01

A method for the quantitative elemental analysis of surface soil samples using laser-induced breakdown spectroscopy (LIBS) was developed and applied to the analysis of bulk soil samples for discrimination between specimens. The use of a 266 nm laser for LIBS analysis is reported for the first time in forensic soil analysis. Optimization of the LIBS method is discussed, and the results compared favorably to a laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method previously developed. Precision for both methods was LIBS limits of detection were LIBS method successfully discriminated samples from two different sites in Dade County, FL. Analysis of variance, Tukey's post hoc test and Student's t test resulted in 100% discrimination with no type I or type II errors. Principal components analysis (PCA) resulted in clear groupings of the two sites. A correct classification rate of 99.4% was obtained with linear discriminant analysis using leave-one-out validation. Similar results were obtained when the same samples were analyzed by LA-ICP-MS, showing that LIBS can provide similar information to LA-ICP-MS. In a forensic sampling/spatial heterogeneity study, the variation between sites, between sub-plots, between samples and within samples was examined on three similar Dade sites. The closer the sampling locations, the closer the grouping on a PCA plot and the higher the misclassification rate. These results underscore the importance of careful sampling for geographic site characterization.

Forensic Discrimination of Latent Fingerprints Using Laser-Induced Breakdown Spectroscopy (LIBS) and Chemometric Approaches.

Science.gov (United States)

Yang, Jun-Ho; Yoh, Jack J

2018-01-01

A novel technique is reported for separating overlapping latent fingerprints using chemometric approaches that combine laser-induced breakdown spectroscopy (LIBS) and multivariate analysis. The LIBS technique provides the capability of real time analysis and high frequency scanning as well as the data regarding the chemical composition of overlapping latent fingerprints. These spectra offer valuable information for the classification and reconstruction of overlapping latent fingerprints by implementing appropriate statistical multivariate analysis. The current study employs principal component analysis and partial least square methods for the classification of latent fingerprints from the LIBS spectra. This technique was successfully demonstrated through a classification study of four distinct latent fingerprints using classification methods such as soft independent modeling of class analogy (SIMCA) and partial least squares discriminant analysis (PLS-DA). The novel method yielded an accuracy of more than 85% and was proven to be sufficiently robust. Furthermore, through laser scanning analysis at a spatial interval of 125 µm, the overlapping fingerprints were reconstructed as separate two-dimensional forms.

Detection of heavy metals in soils by laser-induced breakdown spectroscopy (LIBS)

International Nuclear Information System (INIS)

Sirven, Jean-Baptiste

2006-01-01

In the fields of analysis, control and physical measurement, the laser constitutes a particularly powerful and multi-purpose metrological tool, capable to bring concrete solutions to various matters, including of a societal nature. Among the latter, contamination of sites and soils by heavy metals is an important issue of public health which requires to have measurement means adapted to existing regulations and whose use be sufficiently flexible. As a fast technique which does not need any sample preparation, laser-induced breakdown spectroscopy (LIBS) offers very interesting advantages for making on-site measurements of heavy metals content at the 10-ppm level; the design of a portable system is conceivable in the medium term. In this work we first show that the femtosecond regime presents no advantages with respect to the standard nanosecond regime for our issue. Then we implement an advanced treatment of LIBS spectra by chemometric techniques whose performances significantly improve the results of qualitative and quantitative analyses of soils samples. (author)

Rapid Analysis of Ash Composition Using Laser-Induced Breakdown Spectroscopy (LIBS)

Energy Technology Data Exchange (ETDEWEB)

Tyler L. Westover

2013-01-01

Inorganic compounds are known to be problematic in the thermochemical conversion of biomass to syngas and ultimately hydrocarbon fuels. The elements Si, K, Ca, Na, S, P, Cl, Mg, Fe, and Al are particularly problematic and are known to influence reaction pathways, contribute to fouling and corrosion, poison catalysts, and impact waste streams. Substantial quantities of inorganic species can be entrained in the bark of trees during harvest operations. Herbaceous feedstocks often have even greater quantities of inorganic constituents, which can account for as much as one-fifth of the total dry matter. Current methodologies to measure the concentrations of these elements, such as inductively coupled plasma-optical emission spectrometry/mass spectrometry (ICP-OES/MS) are expensive in time and reagents. This study demonstrates that a new methodology employing laser-induced breakdown spectroscopy (LIBS) can rapidly and accurately analyze the inorganic constituents in a wide range of biomass materials, including both woody and herbaceous examples. This technique requires little or no sample preparation, does not consume any reagents, and the analytical data is available immediately. In addition to comparing LIBS data with the results from ICP-OES methods, this work also includes discussions of sample preparation techniques, calibration curves for interpreting LIBS spectra, minimum detection limits, and the use of internal standards and standard reference materials.

A Simple Laser Induced Breakdown Spectroscopy (LIBS) System for Use at Multiple Levels in the Undergraduate Chemistry Curriculum

Science.gov (United States)

Randall, David W.; Hayes, Ryan T.; Wong, Peter A.

2013-01-01

A LIBS (laser induced breakdown spectroscopy) spectrometer constructed by the instructor is reported for use in undergraduate analytical chemistry experiments. The modular spectrometer described here is based on commonly available components including a commercial Nd:YAG laser and a compact UV-vis spectrometer. The modular approach provides a…

Homogeneity testing and quantitative analysis of manganese (Mn in vitrified Mn-doped glasses by laser-induced breakdown spectroscopy (LIBS

Directory of Open Access Journals (Sweden)

V. K. Unnikrishnan

2014-09-01

Full Text Available Laser-induced breakdown spectroscopy (LIBS, an atomic emission spectroscopy method, has rapidly grown as one of the best elemental analysis techniques over the past two decades. Homogeneity testing and quantitative analysis of manganese (Mn in manganese-doped glasses have been carried out using an optimized LIBS system employing a nanosecond ultraviolet Nd:YAG laser as the source of excitation. The glass samples have been prepared using conventional vitrification methods. The laser pulse irradiance on the surface of the glass samples placed in air at atmospheric pressure was about 1.7×109 W/cm2. The spatially integrated plasma emission was collected and imaged on to the spectrograph slit using an optical-fiber-based collection system. Homogeneity was checked by recording LIBS spectra from different sites on the sample surface and analyzing the elemental emission intensities for concentration determination. Validation of the observed LIBS results was done by comparison with scanning electron microscope- energy dispersive X-ray spectroscopy (SEM-EDX surface elemental mapping. The analytical performance of the LIBS system has been evaluated through the correlation of the LIBS determined concentrations of Mn with its certified values. The results are found to be in very good agreement with the certified concentrations.

Feasibility of atomic and molecular laser induced breakdown spectroscopy (LIBS) to in-situ determination of chlorine in concrete : final report.

Science.gov (United States)

2016-10-01

Laser-induced breakdown spectroscopy (LIBS) has been studied as a fast method of detecting chlorine in concrete samples. Both single pulse (SP) and double pulse (DP) experiments have been tested. Several combinations of lasers (Neodymium-Yttrium Alum...

The determination of V and Mo by dispersive liquid–liquid microextraction (DLLME) combined with laser-induced breakdown spectroscopy (LIBS)

OpenAIRE

Jesus, Amanda M. D. de; Aguirre Pastor, Miguel Ángel; Hidalgo Núñez, Montserrat; Canals Hernández, Antonio; Pereira-Filho, Edenir R.

2014-01-01

Laser-induced breakdown spectroscopy (LIBS) is a promising analytical technique with well-known advantages and limitations. However, despite its growing popularity, this technique has been applied mainly to solid samples and there have been a smaller number of studies devoted to liquid samples. This lack of studies is mainly due to experimental difficulties in the analysis of liquid matrices. Sensitivity can be improved and matrix effects minimized in the LIBS analysis of aqueous samples by u...

Laser induced spectroscopy breakdown (LIBS) application to heavy metal detection in soils; Applicazioni della tecnica Laser induced breakdown spectroscopy (LIBS) alla determinazione dei metalli pesanti nei suoli

Energy Technology Data Exchange (ETDEWEB)

Barbini, R.; Fantoni, R.; Palucci, A.; Ribezzo, S.; Colao, F. [ENEA, Centro Ricerche Frascati, Frascati, RM (Italy). Div. Fisica Applicata; Capitelli, F. [Bari, Univ., Bari (Italy). Dipt. di Biologia e Chimica Agroforestale ed Ambientale

2000-07-01

LIBS (Laser induced breakdown spectroscopy) is a new spectroscopic technique suitable to the use in the analysis of samples of environmental interest, such as soils and rocks, and of industrial interest, such as alloys. Results dealing with the application of the technique to heterogeneous soil samples certified by Ispra Joint Research Centre in the contest of heavy metals (Cd, Cr, Cu, Fe, Mn, Ni, Pb, Zn) with an agronomical interest are presented in this report. In the LIBS technique, a high power laser beam is focused onto the sample in order to generate a small volume of plasma at its surface. Emissions from single atomic species are collected by a lens system coupled to an optical fiber bundle, dispersed on a monochromator and analyzed by an iCCD. the identification and the assignment of emission lines relevant to single atomic species allows to determine the sample elemental composition and, after calibration against reference samples, to perform quantitative analysis for a large number of species. This technique requires no sample pre-treatment, a part from eventually compacting powders by mechanical press. This is a considerable advantage with respect to traditional spectroscopic techniques, such as the ICP (Inductively Coupled Plasma) which needs sample mineralization by acid attack. Measurements performed on soil samples by means of the LIBS technique at ENEA Frascati were compared with the results obtained by ICP, which is considered a traditional technique for this kind of analysis. Results showed a general overestimation of the LIBS values with respect to the ICP ones, probably due to differences in lytologic matrix between the analyzed samples and the standard. The phenomenon is usually referred to the matrix effect, which is held responsible for the deviation from linearity between single element concentration and its row intensity. The effect is due to local plasma density variations and limit the correlation between the plasma elemental composition

Remote quantitative analysis of minerals based on multispectral line-calibrated laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Wan, Xiong; Wang, Peng

2014-01-01

Laser-induced breakdown spectroscopy (LIBS) is a feasible remote sensing technique used for mineral analysis in some unapproachable places where in situ probing is needed, such as analysis of radioactive elements in a nuclear leak or the detection of elemental compositions and contents of minerals on planetary and lunar surfaces. Here a compact custom 15 m focus optical component, combining a six times beam expander with a telescope, has been built, with which the laser beam of a 1064 nm Nd ; YAG laser is focused on remote minerals. The excited LIBS signals that reveal the elemental compositions of minerals are collected by another compact single lens-based signal acquisition system. In our remote LIBS investigations, the LIBS spectra of an unknown ore have been detected, from which the metal compositions are obtained. In addition, a multi-spectral line calibration (MSLC) method is proposed for the quantitative analysis of elements. The feasibility of the MSLC and its superiority over a single-wavelength determination have been confirmed by comparison with traditional chemical analysis of the copper content in the ore.

Laser-Induced Breakdown Spectroscopy (LIBS) for the Measurement of Spatial Structures and Fuel Distribution in Flames.

Science.gov (United States)

Kotzagianni, Maria; Kakkava, Eirini; Couris, Stelios

2016-04-01

Laser-induced breakdown spectroscopy (LIBS) is used for the mapping of local structures (i.e., reactants and products zones) and for the determination of fuel distribution by means of the local equivalence ratio ϕ in laminar, premixed air-hydrocarbon flames. The determination of laser threshold energy to induce breakdown in the different zones of flames is employed for the identification and demarcation of the local structures of a premixed laminar flame, while complementary results about fuel concentration were obtained from measurements of the cyanogen (CN) band Β(2)Σ(+)--Χ(2)Σ(+), (Δυ = 0) at 388.3 nm and the ratio of the atomic lines of hydrogen (Hα) and oxygen (O(I)), Hα/O. The combination of these LIBS-based methods provides a relatively simple to use, rapid, and accurate tool for online and in situ combustion diagnostics, providing valuable information about the fuel distribution and the spatial variations of the local structures of a flame. © The Author(s) 2016.

Monitoring of Cr, Cu, Pb, V and Zn in polluted soils by laser induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Dell'Aglio, Marcella; Gaudiuso, Rosalba; Senesi, Giorgio S; De Giacomo, Alessandro; Zaccone, Claudio; Miano, Teodoro M; De Pascale, Olga

2011-05-01

Laser Induced Breakdown Spectroscopy (LIBS) is a fast and multi-elemental analytical technique particularly suitable for the qualitative and quantitative analysis of heavy metals in solid samples, including environmental ones. Although LIBS is often recognised in the literature as a well-established analytical technique, results about quantitative analysis of elements in chemically complex matrices such as soils are quite contrasting. In this work, soil samples of various origins have been analyzed by LIBS and data compared to those obtained by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). The emission intensities of one selected line for each of the five analytes (i.e., Cr, Cu, Pb, V, and Zn) were normalized to the background signal, and plotted as a function of the concentration values previously determined by ICP-OES. Data showed a good linearity for all calibration lines drawn, and the correlation between ICP-OES and LIBS was confirmed by the satisfactory agreement obtained between the corresponding values. Consequently, LIBS method can be used at least for metal monitoring in soils. In this respect, a simple method for the estimation of the soil pollution degree by heavy metals, based on the determination of an anthropogenic index, was proposed and determined for Cr and Zn.

Comparison of laser induced breakdown spectroscopy and spark induced breakdown spectroscopy for determination of mercury in soils

International Nuclear Information System (INIS)

Srungaram, Pavan K.; Ayyalasomayajula, Krishna K.; Yu-Yueh, Fang; Singh, Jagdish P.

2013-01-01

Mercury is a toxic element found throughout the environment. Elevated concentrations of mercury in soils are quite hazardous to plants growing in these soils and also the runoff of soils to nearby water bodies contaminates the water, endangering the flora and fauna of that region. This makes continuous monitoring of mercury very essential. This work compares two potential spectroscopic methods (laser induced breakdown spectroscopy (LIBS) and spark induced breakdown spectroscopy (SIBS)) at their optimum experimental conditions for mercury monitoring. For LIBS, pellets were prepared from soil samples of known concentration for generating a calibration curve while for SIBS, soil samples of known concentration were used in the powder form. The limits of detection (LODs) of Hg in soil were calculated from the Hg calibration curves. The LOD for mercury in soil calculated using LIBS and SIBS is 483 ppm and 20 ppm, respectively. The detection range for LIBS and SIBS is discussed. - Highlights: • We compared SIBS and LIBS for mercury (Hg) measurements in soil. • Hg 546.07 nm line was selected for both LIBS and SIBS measurements. • Limit of detection for Hg was found to be 20 ppm with SIBS and 483 ppm with LIBS

Comparison of laser induced breakdown spectroscopy and spark induced breakdown spectroscopy for determination of mercury in soils

Energy Technology Data Exchange (ETDEWEB)

Srungaram, Pavan K.; Ayyalasomayajula, Krishna K.; Yu-Yueh, Fang; Singh, Jagdish P., E-mail: singh@icet.msstate.edu

2013-09-01

Mercury is a toxic element found throughout the environment. Elevated concentrations of mercury in soils are quite hazardous to plants growing in these soils and also the runoff of soils to nearby water bodies contaminates the water, endangering the flora and fauna of that region. This makes continuous monitoring of mercury very essential. This work compares two potential spectroscopic methods (laser induced breakdown spectroscopy (LIBS) and spark induced breakdown spectroscopy (SIBS)) at their optimum experimental conditions for mercury monitoring. For LIBS, pellets were prepared from soil samples of known concentration for generating a calibration curve while for SIBS, soil samples of known concentration were used in the powder form. The limits of detection (LODs) of Hg in soil were calculated from the Hg calibration curves. The LOD for mercury in soil calculated using LIBS and SIBS is 483 ppm and 20 ppm, respectively. The detection range for LIBS and SIBS is discussed. - Highlights: • We compared SIBS and LIBS for mercury (Hg) measurements in soil. • Hg 546.07 nm line was selected for both LIBS and SIBS measurements. • Limit of detection for Hg was found to be 20 ppm with SIBS and 483 ppm with LIBS.

In situ semi-quantitative analysis of polluted soils by laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Ismaël, Amina; Bousquet, Bruno; Michel-Le Pierrès, Karine; Travaillé, Grégoire; Canioni, Lionel; Roy, Stéphane

2011-05-01

Time-saving, low-cost analyses of soil contamination are required to ensure fast and efficient pollution removal and remedial operations. In this work, laser-induced breakdown spectroscopy (LIBS) has been successfully applied to in situ analyses of polluted soils, providing direct semi-quantitative information about the extent of pollution. A field campaign has been carried out in Brittany (France) on a site presenting high levels of heavy metal concentrations. Results on iron as a major component as well as on lead and copper as minor components are reported. Soil samples were dried and prepared as pressed pellets to minimize the effects of moisture and density on the results. LIBS analyses were performed with a Nd:YAG laser operating at 1064 nm, 60 mJ per 10 ns pulse, at a repetition rate of 10 Hz with a diameter of 500 μm on the sample surface. Good correlations were obtained between the LIBS signals and the values of concentrations deduced from inductively coupled plasma atomic emission spectroscopy (ICP-AES). This result proves that LIBS is an efficient method for optimizing sampling operations. Indeed, "LIBS maps" were established directly on-site, providing valuable assistance in optimizing the selection of the most relevant samples for future expensive and time-consuming laboratory analysis and avoiding useless analyses of very similar samples. Finally, it is emphasized that in situ LIBS is not described here as an alternative quantitative analytical method to the usual laboratory measurements but simply as an efficient time-saving tool to optimize sampling operations and to drastically reduce the number of soil samples to be analyzed, thus reducing costs. The detection limits of 200 ppm for lead and 80 ppm for copper reported here are compatible with the thresholds of toxicity; thus, this in situ LIBS campaign was fully validated for these two elements. Consequently, further experiments are planned to extend this study to other chemical elements and other

Micro-Laser-Induced Breakdown Spectroscopy (Micro-LIBS) Study on Ancient Roman Mortars.

Science.gov (United States)

Pagnotta, Stefano; Lezzerini, Marco; Ripoll-Seguer, Laura; Hidalgo, Montserrat; Grifoni, Emanuela; Legnaioli, Stefano; Lorenzetti, Giulia; Poggialini, Francesco; Palleschi, Vincenzo

2017-04-01

The laser-induced breakdown spectroscopy (LIBS) technique was used for analyzing the composition of an ancient Roman mortar (5th century A.D.), exploiting an experimental setup which allows the determination of the compositions of binder and aggregate in few minutes, without the need for sample treatment. Four thousand LIBS spectra were acquired from an area of 10 mm 2 , with a 50 µm lateral resolution. The elements of interest in the mortar sample (H, C, O, Na, Mg, Al, Si, K, Ca, Ti, Mn, Fe) were detected and mapped. The collected data graphically shown as compositional images were interpreted using different statistical approaches for the determination of the chemical composition of the binder and aggregate fraction. The methods of false color imaging, blind separation, and self-organizing maps were applied and their results are discussed in this paper. In particular, the method based on the use of self-organizing maps gives well interpretable results in very short times, without any reduction in the dimensionality of the system.

Emission Characteristics of Laser-Induced Plasma Using Collinear Long and Short Dual-Pulse Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Wang, Zhenzhen; Deguchi, Yoshihiro; Liu, Renwei; Ikutomo, Akihiro; Zhang, Zhenzhen; Chong, Daotong; Yan, Junjie; Liu, Jiping; Shiou, Fang-Jung

2017-09-01

Collinear long and short dual-pulse laser-induced breakdown spectroscopy (DP-LIBS) was employed to clarify the emission characteristics from laser-induced plasma. The plasma was sustained and became stable by the long pulse-width laser with the pulse width of 60 μs under free running (FR) conditions as an external energy source. Comparing the measurement results of stainless steel in air using single-pulse LIBS (SP-LIBS) and DP-LIBS, the emission intensity was markedly enhanced using DP-LIBS. The temperature of plasma induced by DP-LIBS was maintained at a higher temperature under different gate delay time and short pulse-width laser power conditions compared with those measured using short SP-LIBS. Moreover, the variation rates of plasma temperatures measured using DP-LIBS were also lower. The superior detection ability was verified by the measurement of aluminum sample in water. The spectra were clearly detected using DP-LIBS, whereas it cannot be identified using SP-LIBS of short and long pulse widths. The effects of gate delay time and short pulse-width laser power were also discussed. These results demonstrate the feasibility and enhanced detection ability of the proposed collinear long and short DP-LIBS method.

Rapid detection of soils contaminated with heavy metals and oils by laser induced breakdown spectroscopy (LIBS).

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Kim, Gibaek; Kwak, Jihyun; Kim, Ki-Rak; Lee, Heesung; Kim, Kyoung-Woong; Yang, Hyeon; Park, Kihong

2013-12-15

A laser induced breakdown spectroscopy (LIBS) coupled with the chemometric method was applied to rapidly discriminate between soils contaminated with heavy metals or oils and clean soils. The effects of the water contents and grain sizes of soil samples on LIBS emissions were also investigated. The LIBS emission lines decreased by 59-75% when the water content increased from 1.2% to 7.8%, and soil samples with a grain size of 75 μm displayed higher LIBS emission lines with lower relative standard deviations than those with a 2mm grain size. The water content was found to have a more pronounced effect on the LIBS emission lines than the grain size. Pelletizing and sieving were conducted for all samples collected from abandoned mining areas and military camp to have similar water contents and grain sizes before being analyzed by the LIBS with the chemometric analysis. The data show that three types of soil samples were clearly discerned by using the first three principal components from the spectral data of soil samples. A blind test was conducted with a 100% correction rate for soil samples contaminated with heavy metals and oil residues. Copyright © 2013 Elsevier B.V. All rights reserved.

[Study on physical deviation factors on laser induced breakdown spectroscopy measurement].

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Wan, Xiong; Wang, Peng; Wang, Qi; Zhang, Qing; Zhang, Zhi-Min; Zhang, Hua-Ming

2013-10-01

In order to eliminate the deviation between the measured LIBS spectral line and the standard LIBS spectral line, and improve the accuracy of elements measurement, a research of physical deviation factors in laser induced breakdown spectroscopy technology was proposed. Under the same experimental conditions, the relationship of ablated hole effect and spectral wavelength was tested, the Stark broadening data of Mg plasma laser induced breakdown spectroscopy with sampling time-delay from 1.00 to 3.00 micros was also studied, thus the physical deviation influences such as ablated hole effect and Stark broadening could be obtained while collecting the spectrum. The results and the method of the research and analysis can also be applied to other laser induced breakdown spectroscopy experiment system, which is of great significance to improve the accuracy of LIBS elements measuring and is also important to the research on the optimum sampling time-delay of LIBS.

Enhancement of laser-induced breakdown spectroscopy (LIBS) Detection limit using a low-pressure and short-pulse laser-induced plasma process.

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Wang, Zhen Zhen; Deguchi, Yoshihiro; Kuwahara, Masakazu; Yan, Jun Jie; Liu, Ji Ping

2013-11-01

Laser-induced breakdown spectroscopy (LIBS) technology is an appealing technique compared with many other types of elemental analysis because of the fast response, high sensitivity, real-time, and noncontact features. One of the challenging targets of LIBS is the enhancement of the detection limit. In this study, the detection limit of gas-phase LIBS analysis has been improved by controlling the pressure and laser pulse width. In order to verify this method, low-pressure gas plasma was induced using nanosecond and picosecond lasers. The method was applied to the detection of Hg. The emission intensity ratio of the Hg atom to NO (IHg/INO) was analyzed to evaluate the LIBS detection limit because the NO emission (interference signal) was formed during the plasma generation and cooling process of N2 and O2 in the air. It was demonstrated that the enhancement of IHg/INO arose by decreasing the pressure to a few kilopascals, and the IHg/INO of the picosecond breakdown was always much higher than that of the nanosecond breakdown at low buffer gas pressure. Enhancement of IHg/INO increased more than 10 times at 700 Pa using picosecond laser with 35 ps pulse width. The detection limit was enhanced to 0.03 ppm (parts per million). We also saw that the spectra from the center and edge parts of plasma showed different features. Comparing the central spectra with the edge spectra, IHg/INO of the edge spectra was higher than that of the central spectra using the picosecond laser breakdown process.

Assessment and forensic application of laser-induced breakdown spectroscopy (LIBS) for the discrimination of Australian window glass.

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El-Deftar, Moteaa M; Speers, Naomi; Eggins, Stephen; Foster, Simon; Robertson, James; Lennard, Chris

2014-08-01

A commercially available laser-induced breakdown spectroscopy (LIBS) instrument was evaluated for the determination of elemental composition of twenty Australian window glass samples, consisting of 14 laminated samples and 6 non-laminated samples (or not otherwise specified) collected from broken windows at crime scenes. In this study, the LIBS figures of merit were assessed in terms of accuracy, limits of detection and precision using three standard reference materials (NIST 610, 612, and 1831). The discrimination potential of LIBS was compared to that obtained using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), X-ray microfluorescence spectroscopy (μXRF) and scanning electron microscopy energy dispersive X-ray spectrometry (SEM-EDX) for the analysis of architectural window glass samples collected from crime scenes in the Canberra region, Australia. Pairwise comparisons were performed using a three-sigma rule, two-way ANOVA and Tukey's HSD test at 95% confidence limit in order to investigate the discrimination power for window glass analysis. The results show that the elemental analysis of glass by LIBS provides a discrimination power greater than 97% (>98% when combined with refractive index data), which was comparable to the discrimination powers obtained by LA-ICP-MS and μXRF. These results indicate that LIBS is a feasible alternative to the more expensive LA-ICP-MS and μXRF options for the routine forensic analysis of window glass samples. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

The 1064 nm laser-induced breakdown spectroscopy (LIBS) inspection to detect the nutrient elements in freshly cut carrot samples

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Yudasari, N.; Prasetyo, S.; Suliyanti, M. M.

2018-03-01

The laser-induced breakdown spectroscopy (LIBS) technique was applied to detect the nutrient elements contained in fresh carrot. Nd:YAG laser the wavelength of 1064 nm was employed in the experiments for ablation. Employing simple set-up of LIBS and preparing the sample with less step method, we are able to detect 18 chemical elements including some fundamental element of carrot, i.e Mg, Al, Fe, Mn, Ti, Ca, and Mn. By applying normalized profiles calculation on some of the element, we are able to compare the concentration level of each element of the outer and inner part of carrot.

Calibration-free quantitative analysis of elemental ratios in intermetallic nanoalloys and nanocomposites using Laser Induced Breakdown Spectroscopy (LIBS).

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Davari, Seyyed Ali; Hu, Sheng; Mukherjee, Dibyendu

2017-03-01

Intermetallic nanoalloys (NAs) and nanocomposites (NCs) have increasingly gained prominence as efficient catalytic materials in electrochemical energy conversion and storage systems. But their morphology and chemical compositions play critical role in tuning their catalytic activities, and precious metal contents. While advanced microscopy techniques facilitate morphological characterizations, traditional chemical characterizations are either qualitative or extremely involved. In this study, we apply Laser Induced Breakdown Spectroscopy (LIBS) for quantitative compositional analysis of NAs and NCs synthesized with varied elemental ratios by our in-house built pulsed laser ablation technique. Specifically, elemental ratios of binary PtNi, PdCo (NAs) and PtCo (NCs) of different compositions are determined from LIBS measurements employing an internal calibration scheme using the bulk matrix species as internal standards. Morphology and qualitative elemental compositions of the aforesaid NAs and NCs are confirmed from Transmission Electron Microscopy (TEM) images and Energy Dispersive X-ray Spectroscopy (EDX) measurements. LIBS experiments are carried out in ambient conditions with the NA and NC samples drop cast on silicon wafers after centrifugation to increase their concentrations. The technique does not call for cumbersome sample preparations including acid digestions and external calibration standards commonly required in Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) techniques. Yet the quantitative LIBS results are in good agreement with the results from ICP-OES measurements. Our results indicate the feasibility of using LIBS in future for rapid and in-situ quantitative chemical characterizations of wide classes of synthesized NAs and NCs. Copyright © 2016 Elsevier B.V. All rights reserved.

Direct Determination of Contaminants and Major and Minor Nutrients in Solid Fertilizers Using Laser-Induced Breakdown Spectroscopy (LIBS).

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Andrade, Daniel F; Pereira-Filho, Edenir Rodrigues

2016-10-11

Contaminants (Cd, Cr, and Pb) as well as minor (B, Cu, Mn, Na, and Zn) and major (Ca and Mg) elements were directly determined in solid fertilizer samples using laser-induced breakdown spectroscopy (LIBS). Factorial designs were used to define the most appropriate LIBS parameters and pellet pressure on solid fertilizers. Emission lines for all of the analytes were collected and employed 12 signal normalization modes. The best results were obtained using a laser energy of 75 mJ, a spot size of 50 μm, a pressure of 10 t/in., and a delay of 2.0 μs. Good correlation was obtained between the calibration model's prediction using the proposed LIBS method and the reference values obtained with ICP-OES. The limits of detection (LOD) for the proposed method varied from 2 mg/kg (for Cd) to 1% (for Zn).

Laser induced spectroscopy breakdown (LIBS) application to heavy metal detection in soils

International Nuclear Information System (INIS)

Barbini, R.; Fantoni, R.; Palucci, A.; Ribezzo, S.; Colao, F.; Capitelli, F.

2000-01-01

LIBS (Laser induced breakdown spectroscopy) is a new spectroscopic technique suitable to the use in the analysis of samples of environmental interest, such as soils and rocks, and of industrial interest, such as alloys. Results dealing with the application of the technique to heterogeneous soil samples certified by Ispra Joint Research Centre in the contest of heavy metals (Cd, Cr, Cu, Fe, Mn, Ni, Pb, Zn) with an agronomical interest are presented in this report. In the LIBS technique, a high power laser beam is focused onto the sample in order to generate a small volume of plasma at its surface. Emissions from single atomic species are collected by a lens system coupled to an optical fiber bundle, dispersed on a monochromator and analyzed by an iCCD. the identification and the assignment of emission lines relevant to single atomic species allows to determine the sample elemental composition and, after calibration against reference samples, to perform quantitative analysis for a large number of species. This technique requires no sample pre-treatment, a part from eventually compacting powders by mechanical press. This is a considerable advantage with respect to traditional spectroscopic techniques, such as the ICP (Inductively Coupled Plasma) which needs sample mineralization by acid attack. Measurements performed on soil samples by means of the LIBS technique at ENEA Frascati were compared with the results obtained by ICP, which is considered a traditional technique for this kind of analysis. Results showed a general overestimation of the LIBS values with respect to the ICP ones, probably due to differences in lytologic matrix between the analyzed samples and the standard. The phenomenon is usually referred to the matrix effect, which is held responsible for the deviation from linearity between single element concentration and its row intensity. The effect is due to local plasma density variations and limit the correlation between the plasma elemental composition

Qualitative and quantitative analysis of milk for the detection of adulteration by Laser Induced Breakdown Spectroscopy (LIBS).

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Moncayo, S; Manzoor, S; Rosales, J D; Anzano, J; Caceres, J O

2017-10-01

The present work focuses on the development of a fast and cost effective method based on Laser Induced Breakdown Spectroscopy (LIBS) to the quality control, traceability and detection of adulteration in milk. Two adulteration cases have been studied; a qualitative analysis for the discrimination between different milk blends and quantification of melamine in adulterated toddler milk powder. Principal Component Analysis (PCA) and neural networks (NN) have been used to analyze LIBS spectra obtaining a correct classification rate of 98% with a 100% of robustness. For the quantification of melamine, two methodologies have been developed; univariate analysis using CN emission band and multivariate calibration NN model obtaining correlation coefficient (R 2 ) values of 0.982 and 0.999 respectively. The results of the use of LIBS technique coupled with chemometric analysis are discussed in terms of its potential use in the food industry to perform the quality control of this dairy product. Copyright © 2017 Elsevier Ltd. All rights reserved.

Laser-induced breakdown spectroscopy (LIBS) for rapid analysis of ash, potassium and magnesium in gluten free flours.

Science.gov (United States)

Markiewicz-Keszycka, Maria; Casado-Gavalda, Maria P; Cama-Moncunill, Xavier; Cama-Moncunill, Raquel; Dixit, Yash; Cullen, Patrick J; Sullivan, Carl

2018-04-01

Gluten free (GF) diets are prone to mineral deficiency, thus effective monitoring of the elemental composition of GF products is important to ensure a balanced micronutrient diet. The objective of this study was to test the potential of laser-induced breakdown spectroscopy (LIBS) analysis combined with chemometrics for at-line monitoring of ash, potassium and magnesium content of GF flours: tapioca, potato, maize, buckwheat, brown rice and a GF flour mixture. Concentrations of ash, potassium and magnesium were determined with reference methods and LIBS. PCA analysis was performed and presented the potential for discrimination of the six GF flours. For the quantification analysis PLSR models were developed; R 2 cal were 0.99 for magnesium and potassium and 0.97 for ash. The study revealed that LIBS combined with chemometrics is a convenient method to quantify concentrations of ash, potassium and magnesium and present the potential to classify different types of flours. Copyright © 2017 Elsevier Ltd. All rights reserved.

Laser-induced breakdown spectroscopy (LIBS), part II: review of instrumental and methodological approaches to material analysis and applications to different fields.

Science.gov (United States)

Hahn, David W; Omenetto, Nicoló

2012-04-01

The first part of this two-part review focused on the fundamental and diagnostics aspects of laser-induced plasmas, only touching briefly upon concepts such as sensitivity and detection limits and largely omitting any discussion of the vast panorama of the practical applications of the technique. Clearly a true LIBS community has emerged, which promises to quicken the pace of LIBS developments, applications, and implementations. With this second part, a more applied flavor is taken, and its intended goal is summarizing the current state-of-the-art of analytical LIBS, providing a contemporary snapshot of LIBS applications, and highlighting new directions in laser-induced breakdown spectroscopy, such as novel approaches, instrumental developments, and advanced use of chemometric tools. More specifically, we discuss instrumental and analytical approaches (e.g., double- and multi-pulse LIBS to improve the sensitivity), calibration-free approaches, hyphenated approaches in which techniques such as Raman and fluorescence are coupled with LIBS to increase sensitivity and information power, resonantly enhanced LIBS approaches, signal processing and optimization (e.g., signal-to-noise analysis), and finally applications. An attempt is made to provide an updated view of the role played by LIBS in the various fields, with emphasis on applications considered to be unique. We finally try to assess where LIBS is going as an analytical field, where in our opinion it should go, and what should still be done for consolidating the technique as a mature method of chemical analysis. © 2012 Society for Applied Spectroscopy

In-vitro analysis of early calcification in aortic valvular interstitial cells using Laser-Induced Breakdown Spectroscopy (LIBS).

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Davari, Seyyed Ali; Masjedi, Shirin; Ferdous, Zannatul; Mukherjee, Dibyendu

2018-01-01

Calcific aortic valve disease (CAVD) is a major cardiovascular disorder caused by osteogenic differentiation of valvular interstitial cells (VICs) within aortic valves. Conventional methods like colorimetric assays and histology fail to detect small calcium depositions during in-vitro VIC cultures. Laser-induced breakdown spectroscopy (LIBS) is a robust analytical tool used for inorganic materials characterizations, but relatively new to biomedical applications. We employ LIBS, for the first time, for quantitative in-vitro detection of calcium depositions in VICs at various osteogenic differentiation stages. VICs isolated from porcine aortic valves were cultured in osteogenic media over various days. Colorimetric calcium assays based on arsenazo dye and Von Kossa staining measured the calcium depositions within VICs. Simultaneously, LIBS signatures for Ca I (422.67 nm) atomic emission lines were collected for estimating calcium depositions in lyophilized VIC samples. Our results indicate excellent linear correlation between the calcium assay and our LIBS measurements. Furthermore, unlike the assay results, the LIBS results could resolve calcium signals from cell samples with as early as 2 days of osteogenic culture. Quantitatively, the LIBS measurements establish the limit of detection for calcium content in VICs to be ∼0.17±0.04 μg which indicates a 5-fold improvement over calcium assay. Picture: Quantitative LIBS enables in-vitro analysis for early stage detection of calcium deposition within aortic valvular interstitial cells (VICs). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Standoff Laser-Induced Breakdown Spectroscopy (LIBS) Using a Miniature Wide Field of View Spatial Heterodyne Spectrometer with Sub-Microsteradian Collection Optics.

Science.gov (United States)

Barnett, Patrick D; Lamsal, Nirmal; Angel, S Michael

2017-04-01

A spatial heterodyne spectrometer (SHS) is described for standoff laser-induced breakdown spectroscopy (LIBS) measurements. The spatial heterodyne LIBS spectrometer (SHLS) is a diffraction grating based interferometer with no moving parts that offers a very large field of view, high light throughput, and high spectral resolution in a small package. The field of view of the SHLS spectrometer is shown to be ∼1° in standoff LIBS measurements. In the SHLS system described here, the collection aperture was defined by the 10 mm diffraction gratings in the SHS and standoff LIBS measurements were made up to 20 m with no additional collection optics, corresponding to a collection solid angle of 0.2 μsr, or f/2000, and also using a small telescope to increase the collection efficiency. The use of a microphone was demonstrated to rapidly optimize laser focus for 20 m standoff LIBS measurements.

Characterization of laser-induced breakdown spectroscopy (LIBS) for application to space exploration

International Nuclear Information System (INIS)

Knight, Andrew K.; Scherbarth, Nancy L.; Cremers, David A.; Ferris, Monty J.

2000-01-01

Early in the next century, several space missions are planned with the goal of landing craft on asteroids, comets, the Moon, and Mars. To increase the scientific return of these missions, new methods are needed to provide (1) significantly more analyses per mission lifetime, and (2) expanded analytical capabilities. One method that has the potential to meet both of these needs for the elemental analysis of geological samples is laser-induced breakdown spectroscopy (LIBS). These capabilities are possible because the laser plasma provides rapid analysis and the laser pulse can be focused on a remotely located sample to perform a stand-off measurement. Stand-off is defined as a distance up to 20 m between the target and laser. Here we present the results of a characterization of LIBS for the stand-off analysis of soils at reduced air pressures and in a simulated Martian atmosphere (5-7 torr pressure of CO 2 ) showing the feasibility of LIBS for space exploration. For example, it is demonstrated that an analytically useful laser plasma can be generated at distances up to 19 m by using only 35 mJ/pulse from a compact laser. Some characteristics of the laser plasma at reduced pressure were also investigated. Temporally and spectrally resolved imaging showed significant changes in the plasma as the pressure was reduced and also showed that the analyte signals and mass ablated from a target were strongly dependent on pressure. As the pressure decreased from 590 torr to the 40-100 torr range, the signals increased by a factor of about 3-4, and as the pressure was further reduced the signals decreased. This behavior can be explained by pressure-dependent changes in the mass of material vaporized and the frequency of collisions between species in the plasma. Changes in the temperature and the electron density of the plasmas with pressure were also examined and detection limits for selected elements were determined. (c) 2000 Society for Applied Spectroscopy

Characterization of laser-induced breakdown spectroscopy (LIBS) for application to space exploration

Energy Technology Data Exchange (ETDEWEB)

Knight, Andrew K. [Group CST-1, MS J565, Chemical Science and Technology Division, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States); Scherbarth, Nancy L. [Group CST-1, MS J565, Chemical Science and Technology Division, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States); Cremers, David A. [Group CST-1, MS J565, Chemical Science and Technology Division, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States); Ferris, Monty J. [Group CST-1, MS J565, Chemical Science and Technology Division, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States)

2000-03-01

Early in the next century, several space missions are planned with the goal of landing craft on asteroids, comets, the Moon, and Mars. To increase the scientific return of these missions, new methods are needed to provide (1) significantly more analyses per mission lifetime, and (2) expanded analytical capabilities. One method that has the potential to meet both of these needs for the elemental analysis of geological samples is laser-induced breakdown spectroscopy (LIBS). These capabilities are possible because the laser plasma provides rapid analysis and the laser pulse can be focused on a remotely located sample to perform a stand-off measurement. Stand-off is defined as a distance up to 20 m between the target and laser. Here we present the results of a characterization of LIBS for the stand-off analysis of soils at reduced air pressures and in a simulated Martian atmosphere (5-7 torr pressure of CO{sub 2}) showing the feasibility of LIBS for space exploration. For example, it is demonstrated that an analytically useful laser plasma can be generated at distances up to 19 m by using only 35 mJ/pulse from a compact laser. Some characteristics of the laser plasma at reduced pressure were also investigated. Temporally and spectrally resolved imaging showed significant changes in the plasma as the pressure was reduced and also showed that the analyte signals and mass ablated from a target were strongly dependent on pressure. As the pressure decreased from 590 torr to the 40-100 torr range, the signals increased by a factor of about 3-4, and as the pressure was further reduced the signals decreased. This behavior can be explained by pressure-dependent changes in the mass of material vaporized and the frequency of collisions between species in the plasma. Changes in the temperature and the electron density of the plasmas with pressure were also examined and detection limits for selected elements were determined. (c) 2000 Society for Applied Spectroscopy.

Detection of pesticides and dioxins in tissue fats and rendering oils using laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Multari, Rosalie A; Cremers, David A; Scott, Thomas; Kendrick, Peter

2013-03-13

In laser-induced breakdown spectroscopy (LIBS), a series of powerful laser pulses are directed at a surface to form microplasmas from which light is collected and spectrally analyzed to identify the surface material. In most cases, no sample preparation is needed, and results can be automated and made available within seconds to minutes. Advances in LIBS spectral data analysis using multivariate regression techniques have led to the ability to detect organic chemicals in complex matrices such as foods. Here, the use of LIBS to differentiate samples contaminated with aldrin, 1,2,3,4,6,7,8-heptachlorodibenzo-p-dioxin, chlorpyrifos, and dieldrin in the complex matrices of tissue fats and rendering oils is described. The pesticide concentrations in the samples ranged from 0.005 to 0.1 μg/g. All samples were successfully differentiated from each other and from control samples. Sample concentrations could also be differentiated for all of the pesticides and the dioxin included in this study. The results presented here provide first proof-of-principle data for the ability to create LIBS-based instrumentation for the rapid analysis of pesticide and dioxin contamination in tissue fat and rendered oils.

Detection and quantification of a toxic salt substitute (LiCl) by using laser induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Sezer, Banu; Velioglu, Hasan Murat; Bilge, Gonca; Berkkan, Aysel; Ozdinc, Nese; Tamer, Ugur; Boyaci, Ismail Hakkı

2018-01-01

The use of Li salts in foods has been prohibited due to their negative effects on central nervous system; however, they might still be used especially in meat products as Na substitutes. Lithium can be toxic and even lethal at higher concentrations and it is not approved in foods. The present study focuses on Li analysis in meatballs by using laser induced breakdown spectroscopy (LIBS). Meatball samples were analyzed using LIBS and flame atomic absorption spectroscopy. Calibration curves were obtained by utilizing Li emission lines at 610nm and 670nm for univariate calibration. The results showed that Li calibration curve at 670nm provided successful determination of Li with 0.965 of R 2 and 4.64ppm of limit of detection (LOD) value. While Li Calibration curve obtained using emission line at 610nm generated R 2 of 0.991 and LOD of 22.6ppm, calibration curve obtained at 670nm below 1300ppm generated R 2 of 0.965 and LOD of 4.64ppm. Copyright © 2017. Published by Elsevier Ltd.

Comparative Study of Elemental Nutrients in Organic and Conventional Vegetables Using Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Bhatt, Chet R; Alfarraj, Bader; Ghany, Charles T; Yueh, Fang Y; Singh, Jagdish P

2017-04-01

In this study, the laser-induced breakdown spectroscopy (LIBS) technique was used to identify and compare the presence of major nutrient elements in organic and conventional vegetables. Different parts of cauliflowers and broccolis were used as working samples. Laser-induced breakdown spectra from these samples were acquired at optimum values of laser energy, gate delay, and gate width. Both univariate and multivariate analyses were performed for the comparison of these organic and conventional vegetable flowers. Principal component analysis (PCA) was taken into account for multivariate analysis while for univariate analysis, the intensity of selected atomic lines of different elements and their intensity ratio with some reference lines of organic cauliflower and broccoli samples were compared with those of conventional ones. In addition, different parts of the cauliflower and broccoli were compared in terms of intensity and intensity ratio of elemental lines.

Determination of the penetration hardness and analysis of stainless steel alloys by means of Laser Induced Breakdown Spectroscopy (LIBS

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mohamad Vahid Dastjerdi

2017-11-01

Full Text Available A significant feature of alloys is the surfaces hardness that is always accompanied by challenges when it’s measured by common mechanical techniques. In this investigation, we used Laser Induced Breakdown Spectroscopy (LIBS as a replacement method for common mechanical techniques to measure the surfaces hardness of different alloys. After recording the spectrum of alloy samples in order to identify the surface hardness of analyzed sample, K-Nearest Neighbors method (KNN was used and obtained results showed that the LIBS-KNN method can separate and identify the surfaces hardness of samples with precision of 93.3%. In addition, in order to identify the percentage of constituent elements of alloys and their hardness, calibration approach was investigated that showed there is an appropriate linear relation between recorded emission lines from the LIB spectra of sample alloys and the percentage of their constituent elements and also their Vickers hardness numbers. Therefore, According to exclusive advantages of LIBS technique i.e. high speed analysis, non-destructive analysis and being portable, some of available difficulties in conventional mechanical techniques can be removed.

Evaluation of laser-induced breakdown spectroscopy (LIBS) for measurement of silica on filter samples of coal dust.

Science.gov (United States)

Stipe, Christopher B; Miller, Arthur L; Brown, Jonathan; Guevara, Edward; Cauda, Emanuele

2012-11-01

Airborne silica dust (quartz) is common in coal mines and represents a respiratory hazard that can lead to silicosis, a potentially fatal lung disease. With an eye toward developing a portable monitoring device for rapid analysis of silica dust, laser-induced breakdown spectroscopy (LIBS) was used to quantify quartz in coal dust samples collected on filter media. Pure silica (Min-U-Sil™ 5), Georgia kaolin, and Pittsburgh-4 and Illinois-6 coal dusts were deposited separately and at multiple mass loadings onto 37-mm polyvinylchloride (PVC) filters. LIBS-generated silicon emission was monitored at 288.16 nm, and non-silica contributions to that signal from kaolinite were removed by simultaneously detecting aluminum. Measurements of the four samples were used to calculate limits of detection (LOD) for silicon and aluminum of approximately 0.08 μg/cm(2) and 0.05 μg/cm(2), respectively (corresponding to 0.16 μg/cm(2) and 0.20 μg/cm(2) for silica and kaolinite, respectively). Relative errors of prediction are around 10%. Results demonstrate that LIBS can dependably quantify silica on filter samples of coal dust and confirm that accurate quantification can be achieved for very lightly loaded samples, which supports the potential application of LIBS for rapid, in-field monitoring.

Partial Least Squares and Neural Networks for Quantitative Calibration of Laser-induced Breakdown Spectroscopy (LIBs) of Geologic Samples

Science.gov (United States)

Anderson, R. B.; Morris, Richard V.; Clegg, S. M.; Humphries, S. D.; Wiens, R. C.; Bell, J. F., III; Mertzman, S. A.

2010-01-01

The ChemCam instrument [1] on the Mars Science Laboratory (MSL) rover will be used to obtain the chemical composition of surface targets within 7 m of the rover using Laser Induced Breakdown Spectroscopy (LIBS). ChemCam analyzes atomic emission spectra (240-800 nm) from a plasma created by a pulsed Nd:KGW 1067 nm laser. The LIBS spectra can be used in a semiquantitative way to rapidly classify targets (e.g., basalt, andesite, carbonate, sulfate, etc.) and in a quantitative way to estimate their major and minor element chemical compositions. Quantitative chemical analysis from LIBS spectra is complicated by a number of factors, including chemical matrix effects [2]. Recent work has shown promising results using multivariate techniques such as partial least squares (PLS) regression and artificial neural networks (ANN) to predict elemental abundances in samples [e.g. 2-6]. To develop, refine, and evaluate analysis schemes for LIBS spectra of geologic materials, we collected spectra of a diverse set of well-characterized natural geologic samples and are comparing the predictive abilities of PLS, cascade correlation ANN (CC-ANN) and multilayer perceptron ANN (MLP-ANN) analysis procedures.

Long-Wave Infrared (LWIR) Molecular Laser-Induced Breakdown Spectroscopy (LIBS) Emissions of Thin Solid Explosive Powder Films Deposited on Aluminum Substrates.

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Yang, Clayton S-C; Jin, Feng; Trivedi, Sudhir B; Brown, Ei E; Hommerich, Uwe; Tripathi, Ashish; Samuels, Alan C

2017-04-01

Thin solid films made of high nitro (NO 2 )/nitrate (NO 3 ) content explosives were deposited on sand-blasted aluminum substrates and then studied using a mercury-cadmium-telluride (MCT) linear array detection system that is capable of rapidly capturing a broad spectrum of atomic and molecular laser-induced breakdown spectroscopy (LIBS) emissions in the long-wave infrared region (LWIR; ∼5.6-10 µm). Despite the similarities of their chemical compositions and structures, thin films of three commonly used explosives (RDX, HMX, and PETN) studied in this work can be rapidly identified in the ambient air by their molecular LIBS emission signatures in the LWIR region. A preliminary assessment of the detection limit for a thin film of RDX on aluminum appears to be much lower than 60 µg/cm 2 . This LWIR LIBS setup is capable of rapidly probing and charactering samples without the need for elaborate sample preparation and also offers the possibility of a simultaneous ultraviolet visible and LWIR LIBS measurement.

Investigation of non-uniformity and inclusions in 6LiInSe2 utilizing laser induced breakdown spectroscopy (LIBS)

Science.gov (United States)

Wiggins, Brenden; Tupitsyn, Eugene; Bhattacharya, Pijush; Rowe, Emmanuel; Lukosi, Eric; Chvala, Ondrej; Burger, Arnold; Stowe, Ashley

2013-09-01

Impurity analysis and compositional distribution studies have been conducted on a crystal of LiInSe2, a compound semiconductor which recently has been shown to respond to ionizing radiation. IR microscopy and laser induced breakdown spectroscopy (LIBS) revealed the presence of inclusions within the crystal lattice. These precipitates were revealed to be alkali and alkaline earth elemental impurities with non-uniform spatial distribution in the crystal. LIBS compositional maps correlate the presence of these impurities with visual color differences in the crystal as well as a significant shift of the band gap. Further, LIBS revealed variation in the ratio of I-III-VI2 elemental constituents throughout the crystal. Analysis of compositional variation and impurities will aid in discerning optimal synthesis and crystal growth parameters to maximize the mobility-lifetime product and charge collection efficiency in the LiInSe2 crystal. Preliminary charge trapping calculations have also been conducted with the Monte Carlo N-particle eXtended (MCNPx) package indicating preferential trapping of holes during irradiation with thermal neutrons.

Estimation of Soil Nitrate (NO3) Level Using Laser-Induced Breakdown Spectroscopy (LIBS)

Science.gov (United States)

Angkat, A. R.; Seminar, K. B.; Rahmat, M.; Sutandi, A.

2018-05-01

Laser-Induced Breakdown Spectroscopy (LIBS) is a method for measuring level of nitrogen (N) in the soil in the form of N-nitrate (NO3) rapidly without going through the process of sieving and drying. The sample soil in the form of pellets subjected to laser pulses using a wavelength of 532 nm, pulse duration 5.5 ns, repetition rate of 10 Hz, and Q-switch delay of 150 μs. Emissions are captured by the spectrometer with the wavelength range of 190-1130 nm. Spectrum characterization was processed through the second derivative in order to obtain a wavelength identity that could be rapidly used to estimate the nitrate content of the soil with a determination coefficient of (R2) 0.9254 and a coefficient of variation (CV) of 8.41%. The results of this study are very potential to be applied for rapid measurement of soil nitrate.

The effect of bacterial environmental and metabolic stresses on a laser-induced breakdown spectroscopy (LIBS) based identification of Escherichia coli and Streptococcus viridans.

Science.gov (United States)

Mohaidat, Qassem; Palchaudhuri, Sunil; Rehse, Steven J

2011-04-01

In this paper we investigate the effect that adverse environmental and metabolic stresses have on the laser-induced breakdown spectroscopy (LIBS) identification of bacterial specimens. Single-pulse LIBS spectra were acquired from a non-pathogenic strain of Escherichia coli cultured in two different nutrient media: a trypticase soy agar and a MacConkey agar with a 0.01% concentration of deoxycholate. A chemometric discriminant function analysis showed that the LIBS spectra acquired from bacteria grown in these two media were indistinguishable and easily discriminated from spectra acquired from two other non-pathogenic E. coli strains. LIBS spectra were obtained from specimens of a nonpathogenic E. coli strain and an avirulent derivative of the pathogen Streptococcus viridans in three different metabolic situations: live bacteria reproducing in the log-phase, bacteria inactivated on an abiotic surface by exposure to bactericidal ultraviolet irradiation, and bacteria killed via autoclaving. All bacteria were correctly identified regardless of their metabolic state. This successful identification suggests the possibility of testing specimens that have been rendered safe for handling prior to LIBS identification. This would greatly enhance personnel safety and lower the cost of a LIBS-based diagnostic test. LIBS spectra were obtained from pathogenic and non-pathogenic bacteria that were deprived of nutrition for a period of time ranging from one day to nine days by deposition on an abiotic surface at room temperature. All specimens were successfully classified by species regardless of the duration of nutrient deprivation. © 2011 Society for Applied Spectroscopy

Laser-induced breakdown spectroscopy theory and applications

CERN Document Server

Perini, Umberto

2014-01-01

This book deals with the Laser-Induced Breakdown Spectroscopy (LIBS), a widely used atomic emission spectroscopy technique for elemental analysis of materials. It is based on the use of a high-power, short pulse laser excitation. The book is divided into two main sections: the first one concerning theoretical aspects of the technique, the second one describing the state of the art in applications of the technique in different scientific/technological areas. Numerous examples of state of the art applications provide the readers an almost complete scenario of the LIBS technique. The LIBS theoretical aspects are reviewed. The book helps the readers who are less familiar with the technique to understand the basic principles. Numerous examples of state of the art applications give an almost complete scenario of the LIBS technique potentiality. These examples of applications may have a strong impact on future industrial utilization. The authors made important contributions to the development of this field.

Depth-resolved multilayer pigment identification in paintings: combined use of laser-induced breakdown spectroscopy (LIBS) and optical coherence tomography (OCT).

Science.gov (United States)

Kaszewska, Ewa A; Sylwestrzak, Marcin; Marczak, Jan; Skrzeczanowski, Wojciech; Iwanicka, Magdalena; Szmit-Naud, Elżbieta; Anglos, Demetrios; Targowski, Piotr

2013-08-01

A detailed feasibility study on the combined use of laser-induced breakdown spectroscopy with optical coherence tomography (LIBS/OCT), aiming at a realistic depth-resolved elemental analysis of multilayer stratigraphies in paintings, is presented. Merging a high spectral resolution LIBS system with a high spatial resolution spectral OCT instrument significantly enhances the quality and accuracy of stratigraphic analysis. First, OCT mapping is employed prior to LIBS analysis in order to assist the selection of specific areas of interest on the painting surface to be examined in detail. Then, intertwined with LIBS, the OCT instrument is used as a precise profilometer for the online determination of the depth of the ablation crater formed by individual laser pulses during LIBS depth-profile analysis. This approach is novel and enables (i) the precise in-depth scaling of elemental concentration profiles, and (ii) the recognition of layer boundaries by estimating the corresponding differences in material ablation rate. Additionally, the latter is supported, within the transparency of the object, by analysis of the OCT cross-sectional views. The potential of this method is illustrated by presenting results on the detailed analysis of the structure of an historic painting on canvas performed to aid planned restoration of the artwork.

Laser-Induced Breakdown Spectroscopy for Qualitative Analysis of Metals in Simulated Martian Soils

Science.gov (United States)

Mowry, Curtis; Milofsky, Rob; Collins, William; Pimentel, Adam S.

2017-01-01

This laboratory introduces students to laser-induced breakdown spectroscopy (LIBS) for the analysis of metals in soil and rock samples. LIBS employs a laser-initiated spark to induce electronic excitation of metal atoms. Ensuing atomic emission allows for qualitative and semiquantitative analysis. The students use LIBS to analyze a series of…

A brief history of laser-induced breakdown spectroscopy: From the concept of atoms to LIBS 2012

International Nuclear Information System (INIS)

Radziemski, Leon; Cremers, David

2013-01-01

LIBS did not appear de novo in 1962, but was built upon accomplishments of the past. These started with very old concepts of indivisible units (atomos), chemical and physical experiments and theoretical advances that took place in the late 19th and early 20th centuries, the development of the laser, the discovery of gas breakdown, and the realization of the application to spectrochemistry. We sketch the historical developments and focus as well on the advances in LIBS methodology and instrumentation over the past 50 years, culminating with a synopsis of the LIBS 2012 Conference in Luxor, Egypt

A brief history of laser-induced breakdown spectroscopy: From the concept of atoms to LIBS 2012

Energy Technology Data Exchange (ETDEWEB)

Radziemski, Leon, E-mail: ljrbwr@comcast.net [Tucson, AZ (United States); Cremers, David [Applied Research Associates Inc., Albuquerque, NM (United States)

2013-09-01

LIBS did not appear de novo in 1962, but was built upon accomplishments of the past. These started with very old concepts of indivisible units (atomos), chemical and physical experiments and theoretical advances that took place in the late 19th and early 20th centuries, the development of the laser, the discovery of gas breakdown, and the realization of the application to spectrochemistry. We sketch the historical developments and focus as well on the advances in LIBS methodology and instrumentation over the past 50 years, culminating with a synopsis of the LIBS 2012 Conference in Luxor, Egypt.

Remote Raman - laser induced breakdown spectroscopy (LIBS) geochemical investigation under Venus atmospheric conditions

Energy Technology Data Exchange (ETDEWEB)

Clegg, Sanuel M [Los Alamos National Laboratory; Barefield, James E [Los Alamos National Laboratory; Humphries, Seth D [Los Alamos National Laboratory; Wiens, Roger C [Los Alamos National Laboratory; Vaniman, D. T. [Los Alamos National Laboratory; Sharma, S. K. [UNIV OF HAWAII; Misra, A. K. [UNIV OF HAWAII; Dyar, M. D. [MT. HOLYOKE COLLEGE; Smrekar, S. E. [JET PROPULSION LAB.

2010-12-13

The extreme Venus surface temperatures ({approx}740 K) and atmospheric pressures ({approx}93 atm) create a challenging environment for surface missions. Scientific investigations capable of Venus geochemical observations must be completed within hours of landing before the lander will be overcome by the harsh atmosphere. A combined remote Raman - LIBS (Laser Induced Breakdown Spectroscopy) instrument is capable of accomplishing the geochemical science goals without the risks associated with collecting samples and bringing them into the lander. Wiens et al. and Sharma et al. demonstrated that both analytical techniques can be integrated into a single instrument capable of planetary missions. The focus of this paper is to explore the capability to probe geologic samples with Raman - LIBS and demonstrate quantitative analysis under Venus surface conditions. Raman and LIBS are highly complementary analytical techniques capable of detecting both the mineralogical and geochemical composition of Venus surface materials. These techniques have the potential to profoundly increase our knowledge of the Venus surface composition, which is currently limited to geochemical data from Soviet Venera and VEGA landers that collectively suggest a surface composition that is primarily tholeiitic basaltic with some potentially more evolved compositions and, in some locations, K-rich trachyandesite. These landers were not equipped to probe the surface mineralogy as can be accomplished with Raman spectroscopy. Based on the observed compositional differences and recognizing the imprecise nature of the existing data, 15 samples were chosen to constitute a Venus-analog suite for this study, including five basalts, two each of andesites, dacites, and sulfates, and single samples of a foidite, trachyandesite, rhyolite, and basaltic trachyandesite under Venus conditions. LIBS data reduction involved generating a partial least squares (PLS) model with a subset of the rock powder standards to

Laser-induced breakdown spectroscopy for quantification of heavy metals in soils and sediments

CSIR Research Space (South Africa)

Ambushe, AA

2010-09-01

Full Text Available Laser-induced breakdown spectroscopy (LIBS) will be used to determine the contents of heavy metals in soils and sediments. LIBS results will be compared with the results obtained by inductively coupled plasma-optical emission spectrometry (ICP...

Prospects for laser-induced breakdown spectroscopy for biomedical applications: a review.

Science.gov (United States)

Singh, Vivek Kumar; Rai, Awadhesh Kumar

2011-09-01

We review the different spectroscopic techniques including the most recent laser-induced breakdown spectroscopy (LIBS) for the characterization of materials in any phase (solid, liquid or gas) including biological materials. A brief history of the laser and its application in bioscience is presented. The development of LIBS, its working principle and its instrumentation (different parts of the experimental set up) are briefly summarized. The generation of laser-induced plasma and detection of light emitted from this plasma are also discussed. The merit and demerits of LIBS are discussed in comparison with other conventional analytical techniques. The work done using the laser in the biomedical field is also summarized. The analysis of different tissues, mineral analysis in different organs of the human body, characterization of different types of stone formed in the human body, analysis of biological aerosols using the LIBS technique are also summarized. The unique abilities of LIBS including detection of molecular species and calibration-free LIBS are compared with those of other conventional techniques including atomic absorption spectroscopy, inductively coupled plasma atomic emission spectroscopy and mass spectroscopy, and X-ray fluorescence.

Heavy metal concentrations in soils as determined by laser-induced breakdown spectroscopy (LIBS), with special emphasis on chromium

International Nuclear Information System (INIS)

Senesi, G.S.; Dell'Aglio, M.; Gaudiuso, R.; De Giacomo, A.; Zaccone, C.; De Pascale, O.; Miano, T.M.; Capitelli, M.

2009-01-01

Soil is unanimously considered as one of the most important sink of heavy metals released by human activities. Heavy metal analysis of natural and polluted soils is generally conducted by the use of atomic absorption spectroscopy (AAS) or inductively coupled plasma optical emission spectroscopy (ICP-OES) on adequately obtained soil extracts. Although in recent years the emergent technique of laser-induced breakdown spectroscopy (LIBS) has been applied widely and with increasing success for the qualitative and quantitative analyses of a number of heavy metals in soil matrices with relevant simplification of the conventional methodologies, the technique still requires further confirmation before it can be applied fully successfully in soil analyses. The main objective of this work was to demonstrate that new developments in LIBS technique are able to provide reliable qualitative and quantitative analytical evaluation of several heavy metals in soils, with special focus on the element chromium (Cr), and with reference to the concentrations measured by conventional ICP spectroscopy. The preliminary qualitative LIBS analysis of five soil samples and one sewage sludge sample has allowed the detection of a number of elements including Al, Ca, Cr, Cu, Fe, Mg, Mn, Pb, Si, Ti, V and Zn. Of these, a quantitative analysis was also possible for the elements Cr, Cu, Pb, V and Zn based on the obtained linearity of the calibration curves constructed for each heavy metal, i.e., the proportionality between the intensity of the LIBS emission peaks and the concentration of each heavy metal in the sample measured by ICP. In particular, a triplet of emission lines for Cr could be used for its quantitative measurement. The consistency of experiments made on various samples was supported by the same characteristics of the laser-induced plasma (LIP), i.e., the typical linear distribution confirming the existence of local thermodynamic equilibrium (LTE) condition, and similar excitation

Heavy metal concentrations in soils as determined by laser-induced breakdown spectroscopy (LIBS), with special emphasis on chromium.

Science.gov (United States)

Senesi, G S; Dell'Aglio, M; Gaudiuso, R; De Giacomo, A; Zaccone, C; De Pascale, O; Miano, T M; Capitelli, M

2009-05-01

Soil is unanimously considered as one of the most important sink of heavy metals released by human activities. Heavy metal analysis of natural and polluted soils is generally conducted by the use of atomic absorption spectroscopy (AAS) or inductively coupled plasma optical emission spectroscopy (ICP-OES) on adequately obtained soil extracts. Although in recent years the emergent technique of laser-induced breakdown spectroscopy (LIBS) has been applied widely and with increasing success for the qualitative and quantitative analyses of a number of heavy metals in soil matrices with relevant simplification of the conventional methodologies, the technique still requires further confirmation before it can be applied fully successfully in soil analyses. The main objective of this work was to demonstrate that new developments in LIBS technique are able to provide reliable qualitative and quantitative analytical evaluation of several heavy metals in soils, with special focus on the element chromium (Cr), and with reference to the concentrations measured by conventional ICP spectroscopy. The preliminary qualitative LIBS analysis of five soil samples and one sewage sludge sample has allowed the detection of a number of elements including Al, Ca, Cr, Cu, Fe, Mg, Mn, Pb, Si, Ti, V and Zn. Of these, a quantitative analysis was also possible for the elements Cr, Cu, Pb, V and Zn based on the obtained linearity of the calibration curves constructed for each heavy metal, i.e., the proportionality between the intensity of the LIBS emission peaks and the concentration of each heavy metal in the sample measured by ICP. In particular, a triplet of emission lines for Cr could be used for its quantitative measurement. The consistency of experiments made on various samples was supported by the same characteristics of the laser-induced plasma (LIP), i.e., the typical linear distribution confirming the existence of local thermodynamic equilibrium (LTE) condition, and similar excitation

Recent advances in the use of laser-induced breakdown spectroscopy (LIBS) as a rapid point-of-care pathogen diagnostic

Science.gov (United States)

Rehse, Steven J.; Miziolek, Andrzej W.

2012-06-01

Laser-induced breakdown spectroscopy (LIBS) has made tremendous progress in becoming a viable technology for rapid bacterial pathogen detection and identification. The significant advantages of LIBS include speed (present the latest advances achieved in LIBS-based bacterial sensing including the ability to uniquely identify species from more than five bacterial genera with high-sensitivity and specificity. Bacterial identifications are completely unaffected by environment, nutrition media, or state of growth and accurate diagnoses can be made on autoclaved or UV-irradiated specimens. Efficient discrimination of bacteria at the strain level has been demonstrated. A rapid urinary tract infection diagnosis has been simulated with no sample preparation and a one second diagnosis of a pathogen surrogate has been demonstrated using advanced chemometric analysis with a simple "stop-light" user interface. Stand-off bacterial identification at a 20-m distance has been demonstrated on a field-portable instrument. This technology could be implemented in doctors' offices, clinics, or hospital laboratories for point-of-care medical specimen analysis; mounted on military medical robotic platforms for in-the- field diagnostics; or used in stand-off configuration for remote sensing and detection.

Classification of red wine based on its protected designation of origin (PDO) using Laser-induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Moncayo, S; Rosales, J D; Izquierdo-Hornillos, R; Anzano, J; Caceres, J O

2016-09-01

This work reports on a simple and fast classification procedure for the quality control of red wines with protected designation of origin (PDO) by means of Laser Induced Breakdown Spectroscopy (LIBS) technique combined with Neural Networks (NN) in order to increase the quality assurance and authenticity issues. A total of thirty-eight red wine samples from different PDO were analyzed to detect fake wines and to avoid unfair competition in the market. LIBS is well known for not requiring sample preparation, however, in order to increase its analytical performance a new sample preparation treatment by previous liquid-to-solid transformation of the wine using a dry collagen gel has been developed. The use of collagen pellets allowed achieving successful classification results, avoiding the limitations and difficulties of working with aqueous samples. The performance of the NN model was assessed by three validation procedures taking into account their sensitivity (internal validation), generalization ability and robustness (independent external validation). The results of the use of a spectroscopic technique coupled with a chemometric analysis (LIBS-NN) are discussed in terms of its potential use in the food industry, providing a methodology able to perform the quality control of alcoholic beverages. Copyright © 2016 Elsevier B.V. All rights reserved.

Laser-induced breakdown spectroscopy (LIBS) technique for the determination of the chemical composition of complex inorganic materials

Science.gov (United States)

Łazarek, Łukasz; Antończak, Arkadiusz J.; Wójcik, Michał R.; Kozioł, Paweł E.; Stepak, Bogusz; Abramski, Krzysztof M.

2014-08-01

Laser-induced breakdown spectroscopy (LIBS) is a fast, fully optical method, that needs little or no sample preparation. In this technique qualitative and quantitative analysis is based on comparison. The determination of composition is generally based on the construction of a calibration curve namely the LIBS signal versus the concentration of the analyte. Typically, to calibrate the system, certified reference materials with known elemental composition are used. Nevertheless, such samples due to differences in the overall composition with respect to the used complex inorganic materials can influence significantly on the accuracy. There are also some intermediate factors which can cause imprecision in measurements, such as optical absorption, surface structure, thermal conductivity etc. This paper presents the calibration procedure performed with especially prepared pellets from the tested materials, which composition was previously defined. We also proposed methods of post-processing which allowed for mitigation of the matrix effects and for a reliable and accurate analysis. This technique was implemented for determination of trace elements in industrial copper concentrates standardized by conventional atomic absorption spectroscopy with a flame atomizer. A series of copper flotation concentrate samples was analyzed for contents of three elements, that is silver, cobalt and vanadium. It has been shown that the described technique can be used to qualitative and quantitative analyses of complex inorganic materials, such as copper flotation concentrates.

Laser-induced breakdown spectroscopy (LIBS) to measure quantitatively soil carbon with emphasis on soil organic carbon. A review.

Science.gov (United States)

Senesi, Giorgio S; Senesi, Nicola

2016-09-28

Soil organic carbon (OC) measurement is a crucial factor for quantifying soil C pools and inventories and monitoring the inherent temporal and spatial heterogeneity and changes of soil OC content. These are relevant issues in addressing sustainable management of terrestrial OC aiming to enhance C sequestration in soil, thus mitigating the impact of increasing CO2 concentration in the atmosphere and related effects on global climate change. Nowadays, dry combustion by an elemental analyzer or wet combustion by dichromate oxidation of the soil sample are the most recommended and commonly used methods for quantitative soil OC determination. However, the unanimously recognized uncertainties and limitations of these classical laboursome methods have prompted research efforts focusing on the development and application of more advanced and appealing techniques and methods for the measurement of soil OC in the laboratory and possibly in situ in the field. Among these laser-induced breakdown spectroscopy (LIBS) has raised the highest interest for its unique advantages. After an introduction and a highlight of the LIBS basic principles, instrumentation, methodologies and supporting chemometric methods, the main body of this review provides an historical and critical overview of the developments and results obtained up-to-now by the application of LIBS to the quantitative measurement of soil C and especially OC content. A brief critical summary of LIBS advantages and limitations/drawbacks including some final remarks and future perspectives concludes this review. Copyright © 2016 Elsevier B.V. All rights reserved.

Improved intact soil-core carbon determination applying regression shrinkage and variable selection techniques to complete spectrum laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Bricklemyer, Ross S; Brown, David J; Turk, Philip J; Clegg, Sam M

2013-10-01

Laser-induced breakdown spectroscopy (LIBS) provides a potential method for rapid, in situ soil C measurement. In previous research on the application of LIBS to intact soil cores, we hypothesized that ultraviolet (UV) spectrum LIBS (200-300 nm) might not provide sufficient elemental information to reliably discriminate between soil organic C (SOC) and inorganic C (IC). In this study, using a custom complete spectrum (245-925 nm) core-scanning LIBS instrument, we analyzed 60 intact soil cores from six wheat fields. Predictive multi-response partial least squares (PLS2) models using full and reduced spectrum LIBS were compared for directly determining soil total C (TC), IC, and SOC. Two regression shrinkage and variable selection approaches, the least absolute shrinkage and selection operator (LASSO) and sparse multivariate regression with covariance estimation (MRCE), were tested for soil C predictions and the identification of wavelengths important for soil C prediction. Using complete spectrum LIBS for PLS2 modeling reduced the calibration standard error of prediction (SEP) 15 and 19% for TC and IC, respectively, compared to UV spectrum LIBS. The LASSO and MRCE approaches provided significantly improved calibration accuracy and reduced SEP 32-55% over UV spectrum PLS2 models. We conclude that (1) complete spectrum LIBS is superior to UV spectrum LIBS for predicting soil C for intact soil cores without pretreatment; (2) LASSO and MRCE approaches provide improved calibration prediction accuracy over PLS2 but require additional testing with increased soil and target analyte diversity; and (3) measurement errors associated with analyzing intact cores (e.g., sample density and surface roughness) require further study and quantification.

Laser-induced breakdown spectroscopy fundamentals and applications

CERN Document Server

Noll, Reinhard

2012-01-01

This book is a comprehensive source of the fundamentals, process parameters, instrumental components and applications of laser-induced breakdown spectroscopy (LIBS). The effect of multiple pulses on material ablation, plasma dynamics and plasma emission is presented. A heuristic plasma modeling allows to simulate complex experimental plasma spectra. These methods and findings form the basis for a variety of applications to perform quantitative multi-element analysis with LIBS. These application potentials of LIBS have really boosted in the last years ranging from bulk analysis of metallic alloys and non-conducting materials, via spatially resolved analysis and depth profiling covering measuring objects in all physical states: gaseous, liquid and solid. Dedicated chapters present LIBS investigations for these tasks with special emphasis on the methodical and instrumental concepts as well as the optimization strategies for a quantitative analysis. Requirements, concepts, design and characteristic features of LI...

Inclusion Detection in Aluminum Alloys Via Laser-Induced Breakdown Spectroscopy

Science.gov (United States)

Hudson, Shaymus W.; Craparo, Joseph; De Saro, Robert; Apelian, Diran

2018-04-01

Laser-induced breakdown spectroscopy (LIBS) has shown promise as a technique to quickly determine molten metal chemistry in real time. Because of its characteristics, LIBS could also be used as a technique to sense for unwanted inclusions and impurities. Simulated Al2O3 inclusions were added to molten aluminum via a metal-matrix composite. LIBS was performed in situ to determine whether particles could be detected. Outlier analysis on oxygen signal was performed on LIBS data and compared to oxide volume fraction measured through metallography. It was determined that LIBS could differentiate between melts with different amounts of inclusions by monitoring the fluctuations in signal for elements of interest. LIBS shows promise as an enabling tool for monitoring metal cleanliness.

Laser-Induced Breakdown Spectroscopy Infrared Emission From Inorganic and Organic Substances

National Research Council Canada - National Science Library

Yang, C.S; Brown, E; Hommerich, U; Trivedi, S. B; Snyder, A. P; Samuels, A. C

2006-01-01

Laser-induced breakdown spectroscopy (LIBS) has been established as a powerful method for identifying trace elemental contaminants by analyzing the atomic spectral emission lines that result subsequent to plasmas generated by laser power...

Nanoparticle detection in aqueous solutions using Raman and Laser Induced Breakdown Spectroscopy

NARCIS (Netherlands)

Sovago, M.; Buis, E.-J.; Sandtke, M.

2013-01-01

We show the chemical identification and quantification of the concentration and size of nanoparticle (NP) dispersions in aqueous solutions by using a combination of Raman Spectroscopy and Laser Induced Breakdown Spectroscopy (LIBS). The two spectroscopic techniques are applied to demonstrate the NP

Elemental profiling of laser cladded multilayer coatings by laser induced breakdown spectroscopy and energy dispersive X-ray spectroscopy

Science.gov (United States)

Lednev, V. N.; Sdvizhenskii, P. A.; Filippov, M. N.; Grishin, M. Ya.; Filichkina, V. A.; Stavertiy, A. Ya.; Tretyakov, R. S.; Bunkin, A. F.; Pershin, S. M.

2017-09-01

Multilayer tungsten carbide wear resistant coatings were analyzed by laser induced breakdown spectroscopy (LIBS) and energy dispersive X-ray (EDX) spectroscopy. Coaxial laser cladding technique was utilized to produce tungsten carbide coating deposited on low alloy steel substrate with additional inconel 625 interlayer. EDX and LIBS techniques were used for elemental profiling of major components (Ni, W, C, Fe, etc.) in the coating. A good correlation between EDX and LIBS data was observed while LIBS provided additional information on light element distribution (carbon). A non-uniform distribution of tungsten carbide grains along coating depth was detected by both LIBS and EDX. In contrast, horizontal elemental profiling showed a uniform tungsten carbide particles distribution. Depth elemental profiling by layer-by-layer LIBS analysis was demonstrated to be an effective method for studying tungsten carbide grains distribution in wear resistant coating without any sample preparation.

Analysis of organic vapors with laser induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Nozari, Hadi; Tavassoli, Seyed Hassan [Laser and Plasma Research Institute, Shahid Beheshti University, G. C, 1983963113 Evin, Tehran (Iran, Islamic Republic of); Rezaei, Fatemeh, E-mail: fatemehrezaei@kntu.ac.ir [Department of Physics, K. N. Toosi University of Technology, 15875-4416 Shariati, Tehran (Iran, Islamic Republic of)

2015-09-15

In this paper, laser induced breakdown spectroscopy (LIBS) is utilized in the study of acetone, ethanol, methanol, cyclohexane, and nonane vapors. Carbon, hydrogen, oxygen, and nitrogen atomic emission spectra have been recorded following laser-induced breakdown of the organic vapors that are mixed with air inside a quartz chamber at atmospheric pressure. The plasma is generated with focused, Q-switched Nd:YAG radiation at the wavelength of 1064 nm. The effects of ignition and vapor pressure are discussed in view of the appearance of the emission spectra. The recorded spectra are proportional to the vapor pressure in air. The hydrogen and oxygen contributions diminish gradually with consecutive laser-plasma events without gas flow. The results show that LIBS can be used to characterize organic vapor.

Analysis of organic vapors with laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Nozari, Hadi; Tavassoli, Seyed Hassan; Rezaei, Fatemeh

2015-01-01

In this paper, laser induced breakdown spectroscopy (LIBS) is utilized in the study of acetone, ethanol, methanol, cyclohexane, and nonane vapors. Carbon, hydrogen, oxygen, and nitrogen atomic emission spectra have been recorded following laser-induced breakdown of the organic vapors that are mixed with air inside a quartz chamber at atmospheric pressure. The plasma is generated with focused, Q-switched Nd:YAG radiation at the wavelength of 1064 nm. The effects of ignition and vapor pressure are discussed in view of the appearance of the emission spectra. The recorded spectra are proportional to the vapor pressure in air. The hydrogen and oxygen contributions diminish gradually with consecutive laser-plasma events without gas flow. The results show that LIBS can be used to characterize organic vapor

Quantitative analysis of Al-Si alloy using calibration free laser induced breakdown spectroscopy (CF-LIBS)

Science.gov (United States)

Shakeel, Hira; Haq, S. U.; Aisha, Ghulam; Nadeem, Ali

2017-06-01

The quantitative analysis of the standard aluminum-silicon alloy has been performed using calibration free laser induced breakdown spectroscopy (CF-LIBS). The plasma was produced using the fundamental harmonic (1064 nm) of the Nd: YAG laser and the emission spectra were recorded at 3.5 μs detector gate delay. The qualitative analysis of the emission spectra confirms the presence of Mg, Al, Si, Ti, Mn, Fe, Ni, Cu, Zn, Sn, and Pb in the alloy. The background subtracted and self-absorption corrected emission spectra were used for the estimation of plasma temperature as 10 100 ± 300 K. The plasma temperature and self-absorption corrected emission lines of each element have been used for the determination of concentration of each species present in the alloy. The use of corrected emission intensities and accurate evaluation of plasma temperature yield reliable quantitative analysis up to a maximum 2.2% deviation from reference sample concentration.

Comparing predictive ability of Laser-Induced Breakdown Spectroscopy to Near Infrared Spectroscopy for soil texture and organic carbon determination

DEFF Research Database (Denmark)

Knadel, Maria; Peng, Yi; Gislum, René

Soil organic carbon (SOC) and texture have a practical value for agronomy and the environment. Thus, alternative techniques to supplement or substitute for the expensive conventional analysis of soil are developed. Here the feasibility of laser-induced breakdown spectroscopy (LIBS) to determine SOC...... and texture was tested and compared with near infrared spectroscopy (NIRS) technique and traditional laboratory analysis. Calibration models were developed on 50 topsoil samples. For all properties except silt, higher predictive ability of LIBS than NIRS models was obtained. Successful calibrations indicate...... that LIBS can be used as a fast and reliable method for SOC and texture estimation....

STUDI PERBANDINGAN ANALISIS UNSUR PLUMBUM (PB DARI HASIL ELEKTROLISIS ANTARA METODE LASER- INDUCED BREAKDOWN SPECTROSCOPY (LIBS DENGAN METODE KONVENSIONAL

Directory of Open Access Journals (Sweden)

H. S. Suyanto

2014-07-01

Full Text Available Penelitian ini bertujuan menganalisis unsur Pb hasil proses elektrolisis dengan metode alternatif laser-induced breakdown spectroscopy (LIBS dan metode konvensional. Elektrolisis menggunakan tembaga (Cu sebagai katoda dan karbon sebagai anoda. Unsur Pb yang terdeposisi pada katoda diirradiasi laser Nd-YAG (model CFR 200, 1064nm dan emisinya (Pb I 405.7 nm ditangkap spektrometer HR 2500++ yang kemudian ditampilkan dalam intensitas fungsi panjang gelombang. Hasil penelitian menunjukkan bahwa energi laser, arus listrik dan waktu deposisi proses elektrolisis yang optimum untuk karakterisasi unsur Pb masing - masing adalah 100 mJ, 5,28 mA dan 15 menit. Aplikasi metode ini untuk analisis kuantitatif larutan Pb dengan membuat kurva kalibrasi dari kosentrasi 300 ppm sampai kosentrasi terendah yaitu 0,5 ppm, serta diperoleh deteksi limit sebesar 0,44 ppm. Sebagai perbandingan metode deteksi dengan LIBS ini telah dilakukan analisis dengan metode konvensional dengan menentukan selisih massa katoda sebelum dan sesudah elektrolisis dan diperoleh hasil yang sebanding.ABSTRACTThe aim of this research was to compare between a method of laser-induced breakdown spectroscopy (LIBS and the conventional one to analyse of Plumbum (Pb element resulted from electrolysis process. Electrolysis used copper (Cu and carbon (C as cathode and anode respectively. Plumbum element which was deposited on cathode was irradiated by Nd-YAG laser (model CFR 200, 1064nm and its emission intensity of neutral Pb I 405.7 nm in the plasma was captured by HR 2500++ spectrometer and displayed in a form of intensity as a function of wavelength. The experiment result showed that the optimum condition parameters of electrolysis: laser energy, electric current and electrolysis time duration were 100 mJ, 5.28 mA and 15 minutes respectively. An application of these conditions was done to make calibration curve of Pb element in liquid sample from 300 ppm to 0.5 ppm and resulted a limit of

Development of a compact underwater laser-induced breakdown spectroscopy (LIBS) system and preliminary results in sea trials.

Science.gov (United States)

Guo, Jinjia; Lu, Yuan; Cheng, Kai; Song, Jiaojian; Ye, Wangquan; Li, Nan; Zheng, Ronger

2017-10-10

The exploitation and research of deep-sea hydrothermal vent has been an issue of great interest in ocean research in recent years. Laser-induced breakdown spectroscopy (LIBS) has great potential for ocean application due to the capabilities of stand-off, multiphase, and multielement analysis. In this work, a newly developed compact 4000 m rated LIBS system (LIBSea) is introduced with preliminary results of sea trials. The underwater system consists of an Nd:YAG single-pulsed laser operating at 1064 nm, an optical fiber spectrometer, an optics module, and an electronic controller module. The whole system is housed in an L800  mm×ϕ258  mm pressure housing with an optical window on the end cap. It was deployed on the remote operated vehicle Faxian on the research vessel Kexue, and in June 2015 was successfully applied for hydrothermal field measurements at the Manus area. The obtained results are shown that the LIBS system is capable of detecting elements Li, Na, K, Ca, and Mg in the hydrothermal area. Profiles of LIBS signals of elements K and Ca have also been obtained during the sea trial. The results show that the K emission line is gradually broadened with depth from sea surface to sea floor (1800 m or so); the K intensity shows a hump shape with maximum value at about 1050 m. The Ca emission line is rapidly broadened below 400 m and slowly narrowed to the sea floor; the Ca intensity shows no obvious change below 400 m and increases continuously to sea floor. A very interesting finding is that the small fluctuations of intensity profile curve of Ca show a degree of correlation with seawater temperature change. The sea trial results prove the performance of LIBSea. After further optimization, it is hoped to apply the LIBS system to the in situ mineral deposits and hydrothermal vent fluid detection in deep sea.

Laser-Induced Breakdown Spectroscopy of Cinematographic Film

Science.gov (United States)

Oujja, M.; Abrusci, C.; Gaspard, S.; Rebollar, E.; Amo, A. del; Catalina, F.; Castillejo, M.

Laser-induced breakdown spectroscopy (LIBS) was used to characterize the composition of black-and-white, silver-gelatine photographic films. LIB spectra of samples and reference gelatine (of various gel strengths, Bloom values 225 and 75 and crosslinking degrees) were acquired in vacuum by excitation at 266 nm. The elemental composition of the gelatine used in the upper protective layer and in the underlying emulsion is revealed by the stratigraphic analysis carried out by delivering successive pulses on the same spot of the sample. Silver (Ag) lines from the light-sensitive silver halide salts are accompanied by iron, lead and chrome lines. Fe and Pb are constituents of film developers and Cr is included in the hardening agent. The results demonstrate the analytical capacity of LIBS for study and classification of different gelatine types and the sensitivity of the technique to minor changes in gelatine composition. In addition LIBS analysis allows extracting important information on the chemicals used as developers and hardeners of archival cinematographic films.

Elemental and mineralogical imaging of a weathered limestone rock by double-pulse micro-Laser-Induced Breakdown Spectroscopy

Science.gov (United States)

Senesi, Giorgio S.; Campanella, Beatrice; Grifoni, Emanuela; Legnaioli, Stefano; Lorenzetti, Giulia; Pagnotta, Stefano; Poggialini, Francesco; Palleschi, Vincenzo; De Pascale, Olga

2018-05-01

The present work aims to evaluate the alteration conditions of historical limestone rocks exposed to urban environment using the Laser-Induced Breakdown Spectroscopy (LIBS) technique. The approach proposed is based on the microscale three dimensional (3D) compositional imaging of the sample through double-pulse micro-Laser-Induced Breakdown Spectroscopy (DP-μLIBS) in conjunction with optical microscopy. DP-μLIBS allows to perform a quick and detailed in-depth analysis of the composition of the weathered artifact by creating a 'virtual thin section' (VTS) of the sample which can estimate the extent of the alteration processes occurred at the limestone surface. The DP-μLIBS analysis of these thin sections showed a reduction with depth of the elements (mainly Fe, Si and Na) originating from atmospheric dust, particulate deposition and the surrounding environment (due to the proximity of the sea), whereas, the LIBS signal of Ca increased in intensity from the black crust to the limestone underneath.

Quantitative mixture fraction measurements in combustion system via laser induced breakdown spectroscopy

KAUST Repository

Mansour, Mohy S.; Imam, Hisham; Elsayed, Khaled A.; Elbaz, Ayman M.; Abbass, Wafaa

2015-01-01

Laser induced breakdown spectroscopy (LIBS) technique has been applied to quantitative mixture fraction measurements in flames. The measured spectra of different mixtures of natural gas and air are used to obtain the calibration parameters for local

Investigation of the differentiation of ex vivo nerve and fat tissues using laser-induced breakdown spectroscopy (LIBS): Prospects for tissue-specific laser surgery.

Science.gov (United States)

Mehari, Fanuel; Rohde, Maximillian; Kanawade, Rajesh; Knipfer, Christian; Adler, Werner; Klämpfl, Florian; Stelzle, Florian; Schmidt, Michael

2016-10-01

In the present study, the elemental compositions of fat and nerve tissue during their plasma mediated laser ablation are studied in the context of tissue differentiation for laser surgery applications by using Laser-Induced Breakdown Spectroscopy (LIBS). Tissue samples of porcine fat and nerve were prepared as ex vivo experimental objects. Plasma mediated laser ablation is performed using an Nd : YAG laser in open air and under normal stray light conditions. The performed measurements suggest that the two tissue types show a high similarity in terms of qualitative elemental composition while at the same time revealing a distinct difference in the concentration of the constituent elements. Different analysis approaches are evaluated and discussed to optimize the tissue-differentiation performance of the LIBS approach. Plasma mediated laser tissue ablation. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantitative analysis of chromium concentration in nickel based alloys by laser induced breakdown spectroscopy at atmospheric pressure using a nanosecond ultraviolet Nd:YAG laser

International Nuclear Information System (INIS)

Gupta, G.P.; Suri, B.M.; Verma, A.; Sundararaman, M.; Unnikrishnan, V.K.; Alti, K.; Kartha, V.B.; Santhosh, C.

2010-01-01

Laser-induced breakdown spectroscopy (LIBS) has been well recognized as a simple, fast and direct analytical technique of elemental analysis of multi-element materials by a number of research groups all over the world. It is based on the focusing of a high-power pulsed laser beam with a power density > 100 MW/cm 2 onto a sample surface followed by optical emission spectroscopy of the plasma produced over the surface. In the present work, they have carried out the quantitative analysis of chromium in nickel-based-alloys using laser-induced breakdown spectroscopy (LIBS) in air at atmospheric pressure. In the present work the quantitative analysis of chromium in nickel-based-alloys using laser-induced break-down spectroscopy (LIBS) in air at atmospheric pressure has been carried out

Effect of sodium chloride concentration on elemental analysis of brines by laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Goueguel, Christian; Singh, Jagdish P; McIntyre, Dustin L; Jain, Jinesh; Karamalidis, Athanasios K

2014-01-01

Leakage of injected carbon dioxide (CO2) or resident fluids, such as brine, is a major concern associated with the injection of large volumes of CO2 into deep saline formations. Migration of brine could contaminate drinking water resources by increasing their salinity or endanger vegetation and animal life as well as human health. The main objective of this study was to investigate the effect of sodium chloride (NaCl) concentration on the detection of calcium and potassium in brine samples using laser-induced breakdown spectroscopy (LIBS). The ultimate goals were to determine the suitability of the LIBS technique for in situ measurements of metal ion concentrations in NaCl-rich solution and to develop a chemical sensor that can provide the early detection of brine intrusion into formations used for domestic or agricultural water production. Several brine samples of NaCl-CaCl2 and NaCl-KCl were prepared at NaCl concentrations between 0.0 and 3.0 M. The effect of NaCl concentration on the signal-to-background ratio (SBR) and signal-to-noise ratio (SNR) for calcium (422.67 nm) and potassium (769.49 nm) emission lines was evaluated. Results show that, for a delay time of 300 ns and a gate width of 3 μs, the presence of and changes in NaCl concentration significantly affect the SBR and SNR for both emission lines. An increase in NaCl concentration from 0.0 to 3.0 M produced an increase in the SNR, whereas the SBR dropped continuously. The detection limits obtained for both elements were in the milligrams per liter range, suggesting that a NaCl-rich solution does not severely limit the ability of LIBS to detect trace amount of metal ions.

Medical Applications of Laser Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Pathak, A K; Rai, N K; Singh, Ankita; Rai, A K; Rai, Pradeep K; Rai, Pramod K

2014-01-01

Sedentary lifestyle of human beings has resulted in various diseases and in turn we require a potential tool that can be used to address various issues related to human health. Laser Induced Breakdown Spectroscopy (LIBS) is one such potential optical analytical tool that has become quite popular because of its distinctive features that include applicability to any type/phase of samples with almost no sample preparation. Several reports are available that discusses the capabilities of LIBS, suitable for various applications in different branches of science which cannot be addressed by traditional analytical methods but only few reports are available for the medical applications of LIBS. In the present work, LIBS has been implemented to understand the role of various elements in the formation of gallstones (formed under the empyema and mucocele state of gallbladder) samples along with patient history that were collected from Purvancal region of Uttar Pradesh, India. The occurrence statistics of gallstones under the present study reveal higher occurrence of gallstones in female patients. The gallstone occurrence was found more prevalent for those male patients who were having the habit of either tobacco chewing, smoking or drinking alcohols. This work further reports in-situ LIBS study of deciduous tooth and in-vivo LIBS study of human nail

Detection of calculus by laser-induced breakdown spectroscopy (LIBS) using an ultra-short pulse laser system (USPL)

Science.gov (United States)

Schelle, F.; Brede, O.; Krueger, S.; Oehme, B.; Dehn, C.; Frentzen, M.; Braun, A.

2011-03-01

The aim of this study was to assess the detection of calculus by Laser Induced Breakdown Spectroscopy (LIBS). The study was performed with an Nd:YVO4 laser, emitting pulses with a duration of 8 ps at a wavelength of 1064 nm. A repetition rate of 500 kHz at an average power of 5 W was used. Employing a focusing lense, intensities of the order of 1011 W/cm2 were reached on the tooth surface. These high intensities led to the generation of a plasma. The light emitted by the plasma was collimated into a fibre and then analyzed by an echelle spectroscope in the wavelength region from 220 nm - 900 nm. A total number of 15 freshly extracted teeth was used for this study. For each tooth the spectra of calculus and cementum were assessed separately. Comprising all single measurements median values were calculated for the whole spectrum, leading to two specific spectra, one for calculus and one for cementum. For further statistical analysis 28 areas of interest were defined as wavelength regions, in which the signal strength differed regarding the material. In 7 areas the intensity of the calculus spectrum differed statistically significant from the intensity of the cementum spectrum (p calculus. Further studies are necessary to verify that LIBS is a minimally invasive method allowing a safe application in laser-guided dentistry.

Combining Raman and laser induced breakdown spectroscopy by double pulse lasing.

Science.gov (United States)

Lednev, Vasily N; Pershin, Sergey M; Sdvizhenskii, Pavel A; Grishin, Mikhail Ya; Fedorov, Alexander N; Bukin, Vladimir V; Oshurko, Vadim B; Shchegolikhin, Alexander N

2018-01-01

A new approach combining Raman spectrometry and laser induced breakdown spectrometry (LIBS) within a single laser event was suggested. A pulsed solid state Nd:YAG laser running in double pulse mode (two frequency-doubled sequential nanosecond laser pulses with dozens microseconds delay) was used to combine two spectrometry methods within a single instrument (Raman/LIBS spectrometer). First, a low-energy laser pulse (power density far below ablation threshold) was used for Raman measurements while a second powerful laser pulse created the plasma suitable for LIBS analysis. A short time delay between two successive pulses allows measuring LIBS and Raman spectra at different moments but within a single laser flash-lamp pumping. Principal advantages of the developed instrument include high quality Raman/LIBS spectra acquisition (due to optimal gating for Raman/LIBS independently) and absence of target thermal alteration during Raman measurements. A series of high quality Raman and LIBS spectra were acquired for inorganic salts (gypsum, anhydrite) as well as for pharmaceutical samples (acetylsalicylic acid). To the best of our knowledge, the quantitative analysis feasibility by combined Raman/LIBS instrument was demonstrated for the first time by calibration curves construction for acetylsalicylic acid (Raman) and copper (LIBS) in gypsum matrix. Combining ablation pulses and Raman measurements (LIBS/Raman measurements) within a single instrument makes it an efficient tool for identification of samples hidden by non-transparent covering or performing depth profiling analysis including remote sensing. Graphical abstract Combining Raman and laser induced breakdown spectroscopy by double pulse lasing.

New Approach to Quantitative Analysis by Laser-induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Lee, D. H.; Kim, T. H.; Yun, J. I.; Jung, E. C.

2009-01-01

Laser-induced breakdown spectroscopy (LIBS) has been studied as the technique of choice in some particular situations like screening, in situ measurement, process monitoring, hostile environments, etc. Especially, LIBS can fulfill the qualitative and quantitative analysis for radioactive high level waste (HLW) glass in restricted experimental conditions. Several ways have been suggested to get quantitative information from LIBS. The one approach is to use the absolute intensities of each element. The other approach is to use the elemental emission intensities relative to the intensity of the internal standard element whose concentration is known already in the specimen. But these methods are not applicable to unknown samples. In the present work, we introduce new approach to LIBS quantitative analysis by using H α (656.28 nm) emission line as external standard

Identification of Polymers by Means of LIBS

Science.gov (United States)

Anzano, Jesús M.; Bello-Gálvez, Cristina; Lasheras, Roberto J.

Laser-induced breakdown spectroscopy (LIBS) is mainly an elemental analysis technique which is applied several fields. However, molecular materials are almost entirely atomized when exposed to intense laser radiation sufficient for breakdown. This limitation has been solved by researchers using statistical tools as chemometric techniques. In this chapter, the authors expose one review about the identification of polymeric materials using LIBS; and particularly, the different chemometric techniques.

Online analysis of potassium fertilizers by Laser-Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Groisman, Y.; Gaft, M.

2010-01-01

Presently, online analysis in potassium fertilizers industry is performed by Natural Radioactivity Analyzers. Laser Distance Spectrometry (LDS) has tested, by laboratory scale, the possibility of Laser-Induced Breakdown Spectroscopy (LIBS) technique implementation for online fertilizers production control. The main advantage of the system comparing to the existing technique is the principal possibility to analyze all relevant elements, such as K, Na, Mg, and not only K40 isotope as done in natural radiation analytical systems. Good correlations between online LIBS results with chemical analysis data of K, Na and Mg impurities of samples from Russia, Belarus and Israel demonstrate that LIBS system is a perspective tool for online control of those elements in field conditions.

Ultrafast Laser-Based Spectroscopy and Sensing: Applications in LIBS, CARS, and THz Spectroscopy

Science.gov (United States)

Leahy-Hoppa, Megan R.; Miragliotta, Joseph; Osiander, Robert; Burnett, Jennifer; Dikmelik, Yamac; McEnnis, Caroline; Spicer, James B.

2010-01-01

Ultrafast pulsed lasers find application in a range of spectroscopy and sensing techniques including laser induced breakdown spectroscopy (LIBS), coherent Raman spectroscopy, and terahertz (THz) spectroscopy. Whether based on absorption or emission processes, the characteristics of these techniques are heavily influenced by the use of ultrafast pulses in the signal generation process. Depending on the energy of the pulses used, the essential laser interaction process can primarily involve lattice vibrations, molecular rotations, or a combination of excited states produced by laser heating. While some of these techniques are currently confined to sensing at close ranges, others can be implemented for remote spectroscopic sensing owing principally to the laser pulse duration. We present a review of ultrafast laser-based spectroscopy techniques and discuss the use of these techniques to current and potential chemical and environmental sensing applications. PMID:22399883

Ultrafast Laser-Based Spectroscopy and Sensing: Applications in LIBS, CARS, and THz Spectroscopy

Directory of Open Access Journals (Sweden)

Megan R. Leahy-Hoppa

2010-04-01

Full Text Available Ultrafast pulsed lasers find application in a range of spectroscopy and sensing techniques including laser induced breakdown spectroscopy (LIBS, coherent Raman spectroscopy, and terahertz (THz spectroscopy. Whether based on absorption or emission processes, the characteristics of these techniques are heavily influenced by the use of ultrafast pulses in the signal generation process. Depending on the energy of the pulses used, the essential laser interaction process can primarily involve lattice vibrations, molecular rotations, or a combination of excited states produced by laser heating. While some of these techniques are currently confined to sensing at close ranges, others can be implemented for remote spectroscopic sensing owing principally to the laser pulse duration. We present a review of ultrafast laser-based spectroscopy techniques and discuss the use of these techniques to current and potential chemical and environmental sensing applications.

Double-pulse laser-induced breakdown spectroscopy analysis of scales from petroleum pipelines

Science.gov (United States)

Cavalcanti, G. H.; Rocha, A. A.; Damasceno, R. N.; Legnaioli, S.; Lorenzetti, G.; Pardini, L.; Palleschi, V.

2013-09-01

Pipeline scales from the Campos Bay Petroleum Field near Rio de Janeiro, Brazil have been analyzed by both Raman spectroscopy and by laser-induced breakdown spectroscopy (LIBS) using a double-pulse, calibration-free approach. Elements that are characteristic of petroleum (e.g. C, H, N, O, Mg, Na, Fe and V) were detected, in addition to the Ca, Al, and Si which form the matrix of the scale. The LIBS results were compared with the results of micro-Raman spectroscopy, which confirmed the nature of the incrustations inferred by the LIBS analysis. Results of this preliminary study suggest that diffusion of pipe material into the pipeline intake column plays an important role in the growth of scale. Thanks to the simplicity and relative low cost of equipment and to the fact that no special chemical pre-treatment of the samples is needed, LIBS can offer very fast acquisition of data and the possibility of in situ measurements. LIBS could thus represent an alternative or complementary method for the chemical characterization of the scales by comparison to conventional analytical techniques, such as X-ray diffraction or X-ray fluorescence.

Laser-induced breakdown spectroscopy for the study of the pattern of silicon deposition in leaves of saccharum species

NARCIS (Netherlands)

Tripathi, D.K.; Kumar, R.; Chauhan, D.K.; Rai, A.K.; Bicanic, D.D.

2011-01-01

The spatial distribution pattern of silicon in the leaves of three species of Saccharum has been demonstrated by means of laser induced breakdown spectroscopy (LIBS). The in-situ point detection capability of LIBS was used to determine different elements in leaf samples. The concentrations of

Micro spatial analysis of seashell surface using laser-induced breakdown spectroscopy and Raman spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Lu, Yuan; Li, Yuandong; Li, Ying [Optics and Optoelectronics Lab, Ocean University of China, Qingdao 266100 (China); Wang, Yangfan; Wang, Shi; Bao, Zhenmin [Life Science College, Ocean University of China, Qingdao 266003 (China); Zheng, Ronger, E-mail: rzheng@ouc.edu.cn [Optics and Optoelectronics Lab, Ocean University of China, Qingdao 266100 (China)

2015-08-01

The seashell has been studied as a proxy for the marine researches since it is the biomineralization product recording the growth development and the ocean ecosystem evolution. In this work a hybrid of Laser Induced Breakdown Spectroscopy (LIBS) and Raman spectroscopy was introduced to the composition analysis of seashell (scallop, bivalve, Zhikong). Without any sample treatment, the compositional distribution of the shell was obtained using LIBS for the element detection and Raman for the molecule recognition respectively. The elements Ca, K, Li, Mg, Mn and Sr were recognized by LIBS; the molecule carotene and carbonate were identified with Raman. It was found that the LIBS detection result was more related to the shell growth than the detection result of Raman. The obtained result suggested the shell growth might be developing in both horizontal and vertical directions. It was indicated that the LIBS–Raman combination could be an alternative way for the shell researches. - Highlights: • A LIBS–Raman hybrid system was developed. • A seashell has been analyzed for the elementary and molecular distribution with a system. • The shell growth development was studied on the surface and in the depth.

Application of laser-induced breakdown spectroscopy to the analysis of algal biomass for industrial biotechnology

International Nuclear Information System (INIS)

Pořízka, P.; Prochazka, D.; Pilát, Z.; Krajcarová, L.; Kaiser, J.; Malina, R.; Novotný, J.; Zemánek, P.; Ježek, J.; Šerý, M.; Bernatová, S.; Krzyžánek, V.; Dobranská, K.; Novotný, K.; Trtílek, M.; Samek, O.

2012-01-01

We report on the application of laser-induced breakdown spectroscopy (LIBS) to the determination of elements distinctive in terms of their biological significance (such as potassium, magnesium, calcium, and sodium) and to the monitoring of accumulation of potentially toxic heavy metal ions in living microorganisms (algae), in order to trace e.g. the influence of environmental exposure and other cultivation and biological factors having an impact on them. Algae cells were suspended in liquid media or presented in a form of adherent cell mass on a surface (biofilm) and, consequently, characterized using their spectra. In our feasibility study we used three different experimental arrangements employing double-pulse LIBS technique in order to improve on analytical selectivity and sensitivity for potential industrial biotechnology applications, e.g. for monitoring of mass production of commercial biofuels, utilization in the food industry and control of the removal of heavy metal ions from industrial waste waters. - Highlights: ► We realized laser-induced breakdown spectroscopy (LIBS) analysis of algal biomass. ► We used water jet setup, bulk liquid arrangement and algal biofilms. ► LIBS analysis of macro- and micro-element concentrations in algae was shown. ► LIBS can be of assistance in research of sustainable biofuel generation. ► LIBS can be used in research of algal food applications and bioremediation.

Application of laser-induced breakdown spectroscopy to the analysis of algal biomass for industrial biotechnology

Energy Technology Data Exchange (ETDEWEB)

Porizka, P.; Prochazka, D. [X-ray micro CT and nano CT research group, CEITEC-Central European Institute of Technology, Brno University of Technology, Technicka 3058/10, 616 00 Brno (Czech Republic); Pilat, Z. [Institute of Scientific Instruments of the ASCR v.v.i., Academy of Sciences of the Czech Republic, Kralovopolska 147, Brno 61669 (Czech Republic); Krajcarova, L. [Department of Chemistry, Faculty of Sciences, Masaryk University, Kotlarska 2, Brno 611 37 (Czech Republic); Kaiser, J., E-mail: kaiser@fme.vutbr.cz [X-ray micro CT and nano CT research group, CEITEC-Central European Institute of Technology, Brno University of Technology, Technicka 3058/10, 616 00 Brno (Czech Republic); Malina, R.; Novotny, J. [X-ray micro CT and nano CT research group, CEITEC-Central European Institute of Technology, Brno University of Technology, Technicka 3058/10, 616 00 Brno (Czech Republic); Zemanek, P.; Jezek, J.; Sery, M.; Bernatova, S.; Krzyzanek, V.; Dobranska, K. [Institute of Scientific Instruments of the ASCR v.v.i., Academy of Sciences of the Czech Republic, Kralovopolska 147, Brno 61669 (Czech Republic); Novotny, K. [Department of Chemistry, Faculty of Sciences, Masaryk University, Kotlarska 2, Brno 611 37 (Czech Republic); Trtilek, M. [Photon Systems Instruments, Drasov 470, 664 24 Drasov (Czech Republic); Samek, O. [Institute of Scientific Instruments of the ASCR v.v.i., Academy of Sciences of the Czech Republic, Kralovopolska 147, Brno 61669 (Czech Republic)

2012-08-15

We report on the application of laser-induced breakdown spectroscopy (LIBS) to the determination of elements distinctive in terms of their biological significance (such as potassium, magnesium, calcium, and sodium) and to the monitoring of accumulation of potentially toxic heavy metal ions in living microorganisms (algae), in order to trace e.g. the influence of environmental exposure and other cultivation and biological factors having an impact on them. Algae cells were suspended in liquid media or presented in a form of adherent cell mass on a surface (biofilm) and, consequently, characterized using their spectra. In our feasibility study we used three different experimental arrangements employing double-pulse LIBS technique in order to improve on analytical selectivity and sensitivity for potential industrial biotechnology applications, e.g. for monitoring of mass production of commercial biofuels, utilization in the food industry and control of the removal of heavy metal ions from industrial waste waters. - Highlights: Black-Right-Pointing-Pointer We realized laser-induced breakdown spectroscopy (LIBS) analysis of algal biomass. Black-Right-Pointing-Pointer We used water jet setup, bulk liquid arrangement and algal biofilms. Black-Right-Pointing-Pointer LIBS analysis of macro- and micro-element concentrations in algae was shown. Black-Right-Pointing-Pointer LIBS can be of assistance in research of sustainable biofuel generation. Black-Right-Pointing-Pointer LIBS can be used in research of algal food applications and bioremediation.

Correlation between laser-induced breakdown spectroscopy signal and moisture content

International Nuclear Information System (INIS)

Liu, Yuan; Gigant, Lionel; Baudelet, Matthieu; Richardson, Martin

2012-01-01

The possibility of using Laser-Induced Breakdown Spectroscopy (LIBS) for measuring the moisture content of fresh food samples is studied. The normalized line emission of oxygen is highly correlated with the moisture content of the sample, cheese in our case, and can be used as a moisture marker in situations where oxygen interference from the matrix is not a critical issue. The linear correlation between the oxygen signal and the moisture content in the sample shows great potential for using LIBS as an alternative spectroscopic method for moisture monitoring. - Highlights: ► Quantitative moisture measurement by LIBS. ► Use of matrix effects and normalization for physical information on the sample. ► Use of signal from oxygen and CN radical in air background for moisture measurement.

Recent advances in the use of laser-induced breakdown spectroscopy (LIBS) as a rapid point-of-care pathogen diagnostic

Science.gov (United States)

Rehse, Steven; Trojand, Daniel; Putnam, Russell; Gillies, Derek; Woodman, Ryan; Sheikh, Khadija; Daabous, Andrew

2013-05-01

There is a well-known and urgent need in the fields of medicine, environmental health and safety, food-processing, and defense/security to develop new 21st Century technologies for the rapid and sensitive identification of bacterial pathogens. In only the last five years, the use of a real-time elemental (atomic) analysis performed with laser-induced breakdown spectroscopy (LIBS) has made tremendous progress in becoming a viable technology for rapid bacterial pathogen detection and identification. In this talk we will show how this laser-based optical emission spectroscopic technique is able to sensitively assay the elemental composition of bacterial cells in situ. We will also present the latest achievements of our lab to fully develop LIBS-based bacterial sensing including simulation of a rapid urinary tract infection diagnosis and investigation of a variety of autonomous multivariate analysis algorithms. Lastly, we will show how this technology is now ready to be transitioned from the laboratory to field-portable and potentially man-portable instrumentation. The introduction of such a technology into popular use could very well transform the field of bacterial biosensing - a market valued at approximately 10 billion/year world-wide. Funding for this project was provided in part by a Natural Sciences and Engineering Research Council of Canada Discovery Grant.

Characterization of hard coatings produced by laser cladding using laser-induced breakdown spectroscopy technique

Energy Technology Data Exchange (ETDEWEB)

Varela, J.A.; Amado, J.M.; Tobar, M.J.; Mateo, M.P.; Yañez, A.; Nicolas, G., E-mail: gines@udc.es

2015-05-01

Highlights: • Chemical mapping and profiling by laser-induced breakdown spectroscopy (LIBS) of coatings produced by laser cladding. • Production of laser clads using tungsten carbide (WC) and nickel based matrix (NiCrBSi) powders. • Calibration by LIBS of hardfacing alloys with different WC concentrations. - Abstract: Protective coatings with a high abrasive wear resistance can be obtained from powders by laser cladding technique, in order to extend the service life of some industrial components. In this work, laser clad layers of self-fluxing NiCrBSi alloy powder mixed with WC powder have been produced on stainless steel substrates of austenitic type (AISI 304) in a first step and then chemically characterized by laser-induced breakdown spectroscopy (LIBS) technique. With the suitable laser processing parameters (mainly output power, beam scan speed and flow rate) and powders mixture proportions between WC ceramics and NiCrBSi alloys, dense pore free layers have been obtained on single tracks and on large areas with overlapped tracks. The results achieved by LIBS technique and applied for the first time to the analysis of laser clads provided the chemical composition of the tungsten carbides in metal alloy matrix. Different measurement modes (multiple point analyses, depth profiles and chemical maps) have been employed, demonstrating the usefulness of LIBS technique for the characterization of laser clads based on hardfacing alloys. The behavior of hardness can be explained by LIBS maps which evidenced the partial dilution of some WC spheres in the coating.

Study of Bacterial Samples Using Laser Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Farooq W A; Atif M; Tawfik W; Alsalhi M S; Alahmed Z A; Sarfraz M; Singh J P

2014-01-01

Laser-induced breakdown spectroscopy (LIBS) technique has been applied to investigate two different types of bacteria, Escherichia coli (B1) and Micrococcus luteus (B2) deposited on glass slides using Spectrolaser 7000. LIBS spectra were analyzed using spectrolaser software. LIBS spectrum of glass substrate was compared with bacteria spectra. Ca, Mg, Na, K, P, S, Cl, Fe, Al, Mn, Cu, C, H and CN-band appeared in bacterial samples in air. Two carbon lines at 193.02 nm, 247.88 nm and one hydrogen line at 656.28 nm with intensity ratios of 1.9, 1.83 and 1.53 appeared in bacterial samples B1 and B2 respectively. Carbon and hydrogen are the important components of the bio-samples like bacteria and other cancer cells. Investigation on LIBS spectra of the samples in He and Ar atmospheres is also presented. Ni lines appeared only in B2 sample in Ar atmosphere. From the present experimental results we are able to show that LIBS technique has a potential in the identification and discrimination of different types of bacteria. (plasma technology)

Elemental analysis of cotton by laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Schenk, Emily R.; Almirall, Jose R.

2010-05-01

Laser-induced breakdown spectroscopy (LIBS) has been applied to the elemental characterization of unprocessed cotton. This research is important in forensic and fraud detection applications to establish an elemental fingerprint of U.S. cotton by region, which can be used to determine the source of the cotton. To the best of our knowledge, this is the first report of a LIBS method for the elemental analysis of cotton. The experimental setup consists of a Nd:YAG laser that operates at the fundamental wavelength as the LIBS excitation source and an echelle spectrometer equipped with an intensified CCD camera. The relative concentrations of elements Al, Ba, Ca, Cr, Cu, Fe, Mg, and Sr from both nutrients and environmental contributions were determined by LIBS. Principal component analysis was used to visualize the differences between cotton samples based on the elemental composition by region in the U.S. Linear discriminant analysis of the LIBS data resulted in the correct classification of >97% of the cotton samples by U.S. region and >81% correct classification by state of origin.

Monitoring uranium, hydrogen, and lithium and their isotopes using a compact laser-induced breakdown spectroscopy (LIBS) probe and high-resolution spectrometer.

Science.gov (United States)

Cremers, David A; Beddingfield, Alan; Smithwick, Robert; Chinni, Rosemarie C; Jones, C Randy; Beardsley, Burt; Karch, Larry

2012-03-01

The development of field-deployable instruments to monitor radiological, nuclear, and explosive (RNE) threats is of current interest for a number of assessment needs such as the on-site screening of suspect facilities and nuclear forensics. The presence of uranium and plutonium and radiological materials can be determined through monitoring the elemental emission spectrum using relatively low-resolution spectrometers. In addition, uranium compounds, explosives, and chemicals used in nuclear fuel processing (e.g., tributyl-phosphate) can be identified by applying chemometric analysis to the laser-induced breakdown (LIBS) spectrum recorded by these spectrometers. For nuclear forensic applications, however, isotopes of U and Pu and other elements (e.g., H and Li) must also be determined, requiring higher resolution spectrometers given the small magnitude of the isotope shifts for some of these elements (e.g., 25 pm for U and 13 pm for Pu). High-resolution spectrometers will be preferred for several reasons but these must fit into realistic field-based analysis scenarios. To address the need for field instrumentation, we evaluated a previously developed field-deployable hand-held LIBS interrogation probe combined with two relatively new high-resolution spectrometers (λ/Δλ ~75,000 and ~44,000) that have the potential to meet field-based analysis needs. These spectrometers are significantly smaller and lighter in weight than those previously used for isotopic analysis and one unit can provide simultaneous wide spectral coverage and high resolution in a relatively small package. The LIBS interrogation probe was developed initially for use with low resolution compact spectrometers in a person-portable backpack LIBS instrument. Here we present the results of an evaluation of the LIBS probe combined with a high-resolution spectrometer and demonstrate rapid detection of isotopes of uranium and hydrogen and highly enriched samples of (6)Li and (7)Li. © 2012 Society for

Roughness effects on the hydrogen signal in laser-induced breakdown spectroscopy

DEFF Research Database (Denmark)

Rapin, W.; Bousquet, B.; Lasue, J.

2017-01-01

On Mars, Laser-Induced Breakdown Spectroscopy (LIBS) as performed by the ChemCam instrument can be used to measure the hydrogen content of targets in situ, under a low pressure CO2 atmosphere. However, unexpected variations observed in the Martian dataset suggest an effect related to target...... roughness. Here, we present a series of laboratory experiments that reproduce the effect observed on Mars and explore possible causes. We show that the hydrogen peak intensity increases significantly with increasing exposure of the target surface to the LIBS plasma, and that these variations are specific......, this effect should be taken into account for the quantification of hydrogen in any LIBS applications where the roughness of the target is significant....

Laser-induced breakdown spectroscopy with laser irradiation resonant with vibrational transitions

International Nuclear Information System (INIS)

Khachatrian, Ani; Dagdigian, Paul J.

2010-01-01

An investigation of laser-induced breakdown spectroscopy (LIBS) of polymers, both in bulk form and spin coated on Si wafers, with laser irradiation in the mid-infrared spectral region is presented. Of particular interest is whether the LIBS signals are enhanced when the laser wavelength is resonant with a fundamental vibrational transition of the polymer. Significant increases in the LIBS signals were observed for irradiation on hydride stretch fundamental transitions, and the magnitude of the enhancement showed a strong dependence on the mode excited. The role of the substrate was investigated by comparison of results for bulk and spin-coated samples. The polymers investigated were Nylon 12 and poly(vinyl alcohol-co-ethylene).

Characterization of organic photovoltaic devices using femtosecond laser induced breakdown spectroscopy

Science.gov (United States)

Banerjee, S. P.; Sarnet, Thierry; Siozos, Panayiotis; Loulakis, Michalis; Anglos, Demetrios; Sentis, Marc

2017-10-01

The potential of laser induced breakdown spectroscopy (LIBS) as a non-contact probe, for characterizing organic photovoltaic devices during selective laser scribing, was investigated. Samples from organic solar cells were studied, which consisted of several layers of materials including a top electrode (Al, Mg or Mo), organic layer, bottom electrode (indium tin oxide), silicon nitride barrier layer and substrate layer situated from the top consecutively. The thickness of individual layers varies from 115 to 250 nm. LIBS measurements were performed by use of a 40 femtosecond Ti:Sapphire laser operated at very low pulse energy (solar cell structure, demonstrating the potential of LIBS for fast, non-contact characterization of organic photovoltaic coatings.

Combination of laser-induced breakdown spectroscopy and Raman spectroscopy for multivariate classification of bacteria

Science.gov (United States)

Prochazka, D.; Mazura, M.; Samek, O.; Rebrošová, K.; Pořízka, P.; Klus, J.; Prochazková, P.; Novotný, J.; Novotný, K.; Kaiser, J.

2018-01-01

In this work, we investigate the impact of data provided by complementary laser-based spectroscopic methods on multivariate classification accuracy. Discrimination and classification of five Staphylococcus bacterial strains and one strain of Escherichia coli is presented. The technique that we used for measurements is a combination of Raman spectroscopy and Laser-Induced Breakdown Spectroscopy (LIBS). Obtained spectroscopic data were then processed using Multivariate Data Analysis algorithms. Principal Components Analysis (PCA) was selected as the most suitable technique for visualization of bacterial strains data. To classify the bacterial strains, we used Neural Networks, namely a supervised version of Kohonen's self-organizing maps (SOM). We were processing results in three different ways - separately from LIBS measurements, from Raman measurements, and we also merged data from both mentioned methods. The three types of results were then compared. By applying the PCA to Raman spectroscopy data, we observed that two bacterial strains were fully distinguished from the rest of the data set. In the case of LIBS data, three bacterial strains were fully discriminated. Using a combination of data from both methods, we achieved the complete discrimination of all bacterial strains. All the data were classified with a high success rate using SOM algorithm. The most accurate classification was obtained using a combination of data from both techniques. The classification accuracy varied, depending on specific samples and techniques. As for LIBS, the classification accuracy ranged from 45% to 100%, as for Raman Spectroscopy from 50% to 100% and in case of merged data, all samples were classified correctly. Based on the results of the experiments presented in this work, we can assume that the combination of Raman spectroscopy and LIBS significantly enhances discrimination and classification accuracy of bacterial species and strains. The reason is the complementarity in

Laser-induced breakdown spectroscopy for analysis of plant materials: A review

International Nuclear Information System (INIS)

Santos, Dário; Nunes, Lidiane Cristina; Gustinelli Arantes de Carvalho, Gabriel; Gomes, Marcos da Silva; Souza, Paulino Florêncio de; Leme, Flavio de Oliveira; Gustavo Cofani dos Santos, Luis; Krug, Francisco José

2012-01-01

Developments and contributions of laser-induced breakdown spectroscopy (LIBS) for the determination of elements in plant materials are reviewed. Several applications where the solid samples are interrogated by simply focusing the laser pulses directly onto a fresh or dried surface of leaves, roots, fruits, vegetables, wood and pollen are presented. For quantitative purposes aiming at plant nutrition diagnosis, the test sample presentation in the form of pressed pellets, prepared from clean, dried and properly ground/homogenized leaves, and the use of univariate or multivariate calibration strategies are revisited. - Highlights: ► Qualitative and quantitative LIBS analysis of plant materials are reviewed. ► Fresh or dried leaves, fruits, roots and pellets can be easily interrogated by LIBS. ► LIBS is a powerful tool for plant nutrition diagnosis and elemental mapping. ► Intended LIBS users will find a survey of applications in a comprehensive table.

Laser Induced Breakdown Spectroscopy, advances in resolution and portability

International Nuclear Information System (INIS)

Ponce, L.; Flores, T.; Arronte, M.; Moreira, L.; Hernandez, L. C.; Posada, E. de

2009-01-01

Laser Induced Breakdown Spectroscopy (LIBS), can be considered as one of the most dynamic and promising technique in the field of analytical spectroscopy. LIBS has turned into a powerful alternative for a wide front of applications, from the geological exploration to the industrial inspection, including the environmental monitoring, the biomedical analysis, the study of patrimonial works, the safety and defense. The advances in LIBS instrumentation have allowed improving gradually the analysis services and quality, on the basis of a better knowledge of the technology principles. Recently, systems of double pulse have facilitated a better dosing of energy, the improvement of the signal-noise relation and the study of the different process stages. Femtosecond lasers offers the possibility of study in detail the ablation and atomic emission processes. New advances like multi-pulse or multi-wavelength systems -in fact stilling without exploring, must offer new information to advance in this knowledge. Finally, which it does to this technology really attractive, is the aptitude to be employed in field conditions, or for the detection of the elementary composition at long distances. In this presentation there are discussed the designs of portable instrumentation, compact and low cost, which can improve substantially the LIBS possibilities. (Author)

Double-pulse laser-induced breakdown spectroscopy analysis of scales from petroleum pipelines

International Nuclear Information System (INIS)

o – CEP 24210-346 – Niterói, Rio de Janeiro (Brazil))" data-affiliation=" (Physics Department of University Federal Fluminense, Av. Gal. Milton Tavares de Souza, s/no – CEP 24210-346 – Niterói, Rio de Janeiro (Brazil))" >Cavalcanti, G.H.; Rocha, A.A.; Damasceno, R.N.; Legnaioli, S.; Lorenzetti, G.; Pardini, L.; Palleschi, V.

2013-01-01

Pipeline scales from the Campos Bay Petroleum Field near Rio de Janeiro, Brazil have been analyzed by both Raman spectroscopy and by laser-induced breakdown spectroscopy (LIBS) using a double-pulse, calibration-free approach. Elements that are characteristic of petroleum (e.g. C, H, N, O, Mg, Na, Fe and V) were detected, in addition to the Ca, Al, and Si which form the matrix of the scale. The LIBS results were compared with the results of micro-Raman spectroscopy, which confirmed the nature of the incrustations inferred by the LIBS analysis. Results of this preliminary study suggest that diffusion of pipe material into the pipeline intake column plays an important role in the growth of scale. Thanks to the simplicity and relative low cost of equipment and to the fact that no special chemical pre-treatment of the samples is needed, LIBS can offer very fast acquisition of data and the possibility of in situ measurements. LIBS could thus represent an alternative or complementary method for the chemical characterization of the scales by comparison to conventional analytical techniques, such as X-ray diffraction or X-ray fluorescence. - Highlights: • Samples of scales from petroleum pipelines were analyzed using double pulse LIBS. • LIBS is proposed as an alternative method to conventional analytical techniques. • The scale growth is influenced by the product of corrosion in the column of production. • The diffusion of pipe material into the inlay is important for the growth of scale

Effect of sample preparation on the discrimination of bacterial isolates cultured in liquid nutrient media using laser induced breakdown spectroscopy

Science.gov (United States)

Laser induced breakdown spectroscopy (LIBS) is used as the basis for discrimination between 2 genera of gram-negative bacteria and 2 genera of gram-positive bacteria representing pathogenic threats commonly found in poultry processing rinse waters. Because LIBS-based discrimination relies primarily ...

Spectroscopic studies of different brands of cigarettes using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Sayyad, M. H.; Saleem, M.; Shah, M.; Baig, M. A.; Shaikh, N. M.

2008-01-01

In this work the technique of laser-induced breakdown spectroscopy (LIBS) has been used for the elemental analysis of cigarettes. For this purpose emission spectra have been measured of eleven different kinds of cigarette brands sold and/or produced in Pakistan. Analysis of the spectral peaks observed shows that Na, Mg, Al, K, Ca, Cr, Fe, Sr and Ba are contained in all brands. Exhibiting the LIBS results, the powerful potential of this method for the identification of the elemental content of cigarettes is demonstrated

Elemental content of enamel and dentin after bleaching of teeth (a comparative study between laser-induced breakdown spectroscopy and x-ray photoelectron spectroscopy)

Energy Technology Data Exchange (ETDEWEB)

Imam, H. [National Institute of Laser Enhanced Sciences, NILES, Cairo University, Giza (Egypt); Ahmed, Doaa [Department of Restorative Sciences, Faculty of Dentistry, Alexandria University, Alexandria (Egypt); Eldakrouri, Ashraf [National Institute of Laser Enhanced Sciences, NILES, Cairo University, Giza (Egypt); Department of Optometry and Vision Science, College of Applied Medical Science, King Saud University, Riyadh (Saudi Arabia)

2013-06-21

The elemental content of the superficial and inner enamel as well as that of dentin was analyzed using laser-induced breakdown spectroscopy (LIBS) and x-ray photoelectron spectroscopy (XPS) of bleached and unbleached tooth specimens. It is thus clear from the spectral analysis using both the LIBS and XPS technique that elemental changes (though insignificant within the scopes of this study) of variable intensities do occur on the surface of the enamel and extend deeper to reach dentin. The results of the LIBS revealed a slight reduction in the calcium levels in the bleached compared to the control specimens in all the different bleaching groups and in both enamel and dentin. The good correlation found between the LIBS and XPS results demonstrates the possibility of LIBS technique for detection of minor loss in calcium and phosphorus in enamel and dentin.

Elemental content of enamel and dentin after bleaching of teeth (a comparative study between laser-induced breakdown spectroscopy and x-ray photoelectron spectroscopy)

International Nuclear Information System (INIS)

Imam, H.; Ahmed, Doaa; Eldakrouri, Ashraf

2013-01-01

The elemental content of the superficial and inner enamel as well as that of dentin was analyzed using laser-induced breakdown spectroscopy (LIBS) and x-ray photoelectron spectroscopy (XPS) of bleached and unbleached tooth specimens. It is thus clear from the spectral analysis using both the LIBS and XPS technique that elemental changes (though insignificant within the scopes of this study) of variable intensities do occur on the surface of the enamel and extend deeper to reach dentin. The results of the LIBS revealed a slight reduction in the calcium levels in the bleached compared to the control specimens in all the different bleaching groups and in both enamel and dentin. The good correlation found between the LIBS and XPS results demonstrates the possibility of LIBS technique for detection of minor loss in calcium and phosphorus in enamel and dentin.

Evaluation of elemental profiling methods, including laser-induced breakdown spectroscopy (LIBS), for the differentiation of Cannabis plant material grown in different nutrient solutions.

Science.gov (United States)

El-Deftar, Moteaa M; Robertson, James; Foster, Simon; Lennard, Chris

2015-06-01

Laser-induced breakdown spectroscopy (LIBS) is an emerging atomic emission based solid sampling technique that has many potential forensic applications. In this study, the analytical performance of LIBS, as well as that of inductively coupled plasma mass spectrometry (ICP-MS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and X-ray microfluorescence (μXRF), was evaluated for the ability to conduct elemental analyses on Cannabis plant material, with a specific investigation of the possible links between hydroponic nutrients and elemental profiles from associated plant material. No such study has been previously published in the literature. Good correlation among the four techniques was observed when the concentrations or peak areas of the elements of interest were monitored. For Cannabis samples collected at the same growth time, the elemental profiles could be related to the use of particular commercial nutrients. In addition, the study demonstrated that ICP-MS, LA-ICP-MS and LIBS are suitable techniques for the comparison of Cannabis samples from different sources, with high discriminating powers being achieved. On the other hand, μXRF method was not suitable for the discrimination of Cannabis samples originating from different growth nutrients. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Correlation between laser-induced breakdown spectroscopy signal and moisture content

Energy Technology Data Exchange (ETDEWEB)

Liu, Yuan [Townes Laser Institute, CREOL - The College of Optics and Photonics, University of Central Florida, 4000 Central Florida Boulevard, Orlando, FL 32816 (United States); Gigant, Lionel [Townes Laser Institute, CREOL - The College of Optics and Photonics, University of Central Florida, 4000 Central Florida Boulevard, Orlando, FL 32816 (United States); Universite Bordeaux 1, 351 cours de la Liberation 33405 Talence Cedex (France); Baudelet, Matthieu, E-mail: baudelet@creol.ucf.edu [Townes Laser Institute, CREOL - The College of Optics and Photonics, University of Central Florida, 4000 Central Florida Boulevard, Orlando, FL 32816 (United States); Richardson, Martin [Townes Laser Institute, CREOL - The College of Optics and Photonics, University of Central Florida, 4000 Central Florida Boulevard, Orlando, FL 32816 (United States)

2012-07-15

The possibility of using Laser-Induced Breakdown Spectroscopy (LIBS) for measuring the moisture content of fresh food samples is studied. The normalized line emission of oxygen is highly correlated with the moisture content of the sample, cheese in our case, and can be used as a moisture marker in situations where oxygen interference from the matrix is not a critical issue. The linear correlation between the oxygen signal and the moisture content in the sample shows great potential for using LIBS as an alternative spectroscopic method for moisture monitoring. - Highlights: Black-Right-Pointing-Pointer Quantitative moisture measurement by LIBS. Black-Right-Pointing-Pointer Use of matrix effects and normalization for physical information on the sample. Black-Right-Pointing-Pointer Use of signal from oxygen and CN radical in air background for moisture measurement.

Laser-induced breakdown spectroscopy (LIBS) analysis of calcium ions dissolved in water using filter paper substrates: an ideal internal standard for precision improvement.

Science.gov (United States)

Choi, Daewoong; Gong, Yongdeuk; Nam, Sang-Ho; Han, Song-Hee; Yoo, Jonghyun; Lee, Yonghoon

2014-01-01

We report an approach for selecting an internal standard to improve the precision of laser-induced breakdown spectroscopy (LIBS) analysis for determining calcium (Ca) concentration in water. The dissolved Ca(2+) ions were pre-concentrated on filter paper by evaporating water. The filter paper was dried and analyzed using LIBS. By adding strontium chloride to sample solutions and using a Sr II line at 407.771 nm for the intensity normalization of Ca II lines at 393.366 or 396.847 nm, the analysis precision could be significantly improved. The Ca II and Sr II line intensities were mapped across the filter paper, and they showed a strong positive shot-to-shot correlation with the same spatial distribution on the filter paper surface. We applied this analysis approach for the measurement of Ca(2+) in tap, bottled, and ground water samples. The Ca(2+) concentrations determined using LIBS are in good agreement with those obtained from flame atomic absorption spectrometry. Finally, we suggest a homologous relation of the strongest emission lines of period 4 and 5 elements in groups IA and IIA based on their similar electronic structures. Our results indicate that the LIBS can be effectively applied for liquid analysis at the sub-parts per million level with high precision using a simple drying of liquid solutions on filter paper and the use of the correct internal standard elements with the similar valence electronic structure with respect to the analytes of interest.

Wavelength comparison for laser induced breakdown spectroscopy caries detection

Science.gov (United States)

Amaral, Marcello M.; Raele, Marcus P.; Ana, Patrícia A.; Núñez, Sílvia C.; Zamataro, Claudia B.; Zezell, Denise M.

2018-02-01

Laser Induced Breakdown Spectroscopy (LIBS) is a technique capable to perform elemental analyses of a variety of samples, independent of matter state. Other spectroscopy techniques may require a destructive and time-consuming sample preparation. On the other hand, LIBS is a less destructive technique with no (or considerably less) sample preparation, using a relatively simple experimental setup. LIBS also provides a multielement analysis into one single spectrum acquisition, applying a Nd:YAG short-pulsed laser to ensure the stoichiometry between the sample and the generated plasma. LIBS have been applied on the study of carious lesions using a Nd:YAG into its fundamental emission at 1064 nm. It was shown that ratio of P/Ca and Zn/Ca can be used to monitor the cariogenic process. Another minor elements, e.g. C and Cu, associated with bacteria biofilm were also measured with the Nd:YAG laser. The fundamental wavelength emission (1064 nm) of Nd:YAG is coincident with a hydroxyapatite transmission window and it may affect the result. In order to address this issue a study used the second harmonic of the Nd:YAG laser at 532 nm. It was show that it is also possible perform LIBS on carious lesion using the Nd:YAG at 532 nm. However, there is not a work direct comparing the LIBS at 532 nm and 1064 nm for carious lesion detection. So, the aim of this work was to investigate the influence of laser wavelength on the LIBS performance for carious lesion detection. In both cases the carious lesion was detected with the advantage of no interference with hydroxyapatite at 532 nm.

Measurement of Cerium and Gadolinium in Solid Lithium Chloride-Potassium Chloride Salt Using Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Williams, Ammon; Bryce, Keith; Phongikaroon, Supathorn

2017-10-01

Pyroprocessing of used nuclear fuel (UNF) has many advantages-including that it is proliferation resistant. However, as part of the process, special nuclear materials accumulate in the electrolyte salt and present material accountability and safeguards concerns. The main motivation of this work was to explore a laser-induced breakdown spectroscopy (LIBS) approach as an online monitoring technique to enhance the material accountability of special nuclear materials in pyroprocessing. In this work, a vacuum extraction method was used to draw the molten salt (CeCl 3 -GdCl 3 -LiCl-KCl) up into 4 mm diameter Pyrex tubes where it froze. The salt was then removed and the solid salt was measured using LIBS and inductively coupled plasma mass spectroscopy (ICP-MS). A total of 36 samples were made that varied the CeCl 3 and GdCl 3 (surrogates for uranium and plutonium, respectively) concentrations from 0.5 wt% to 5 wt%. From these samples, univariate calibration curves for Ce and Gd were generated using peak area and peak intensity methods. For Ce, the Ce 551.1 nm line using the peak area provided the best calibration curve with a limit of detection (LOD) of 0.099 wt% and a root mean squared error of cross-validation (RMSECV) of 0.197 wt%. For Gd, the best curve was generated using the peak intensities of the Gd 564.2 nm line resulting in a LOD of 0.027 wt% and a RMSECV of 0.295 wt%. The RMSECV for the univariate cases were determined using leave-one-out cross-validation. In addition to the univariate calibration curves, partial least squares (PLS) regression was done to develop a calibration model. The PLS models yielded similar results with RMSECV (determined using Venetian blind cross-validation with 17% left out per split) values of 0.30 wt% and 0.29 wt% for Ce and Gd, respectively. This work has shown that solid pyroprocessing salt can be qualitatively and quantitatively monitored using LIBS. This work has the potential of significantly enhancing

A versatile interaction chamber for laser-based spectroscopic applications, with the emphasis on Laser-Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Novotný, J.; Brada, M.; Petrilak, M.; Prochazka, D.; Novotný, K.; Hrdička, A.; Kaiser, J.

2014-01-01

The technical note describes the interaction chamber developed particularly for the laser spectroscopy technique applications, such as Laser-Induced Breakdown Spectroscopy (LIBS), Raman Spectroscopy and Laser-Induced Fluorescence. The chamber was designed in order to provide advanced possibilities for the research in mentioned fields and to facilitate routine research procedures. Parameters and the main benefits of the chamber are described, such as the built-in module for automatic 2D chemical mapping and the possibility to set different ambient gas conditions (pressure value and gas type). Together with the chamber description, selected LIBS application examples benefiting from chamber properties are described. - Highlights: • Development of the interaction chamber for LIBS applications • Example of automated chemical mapping of lead in a chalcopyrite sample • Example of LIBS measurement of fluorine in underpressure • Overview of chamber benefits

Laser-induced breakdown spectroscopy (LIBS), part I: review of basic diagnostics and plasma-particle interactions: still-challenging issues within the analytical plasma community.

Science.gov (United States)

Hahn, David W; Omenetto, Nicoló

2010-12-01

Laser-induced breakdown spectroscopy (LIBS) has become a very popular analytical method in the last decade in view of some of its unique features such as applicability to any type of sample, practically no sample preparation, remote sensing capability, and speed of analysis. The technique has a remarkably wide applicability in many fields, and the number of applications is still growing. From an analytical point of view, the quantitative aspects of LIBS may be considered its Achilles' heel, first due to the complex nature of the laser-sample interaction processes, which depend upon both the laser characteristics and the sample material properties, and second due to the plasma-particle interaction processes, which are space and time dependent. Together, these may cause undesirable matrix effects. Ways of alleviating these problems rely upon the description of the plasma excitation-ionization processes through the use of classical equilibrium relations and therefore on the assumption that the laser-induced plasma is in local thermodynamic equilibrium (LTE). Even in this case, the transient nature of the plasma and its spatial inhomogeneity need to be considered and overcome in order to justify the theoretical assumptions made. This first article focuses on the basic diagnostics aspects and presents a review of the past and recent LIBS literature pertinent to this topic. Previous research on non-laser-based plasma literature, and the resulting knowledge, is also emphasized. The aim is, on one hand, to make the readers aware of such knowledge and on the other hand to trigger the interest of the LIBS community, as well as the larger analytical plasma community, in attempting some diagnostic approaches that have not yet been fully exploited in LIBS.

Application of a spectrum standardization method for carbon analysis in coal using laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Li, Xiongwei; Wang, Zhe; Fu, Yangting; Li, Zheng; Liu, Jianmin; Ni, Weidou

2014-01-01

Measurement of coal carbon content using laser-induced breakdown spectroscopy (LIBS) is limited by its low precision and accuracy. A modified spectrum standardization method was proposed to achieve both reproducible and accurate results for the quantitative analysis of carbon content in coal using LIBS. The proposed method used the molecular emissions of diatomic carbon (C2) and cyanide (CN) to compensate for the diminution of atomic carbon emissions in high volatile content coal samples caused by matrix effect. The compensated carbon line intensities were further converted into an assumed standard state with standard plasma temperature, electron number density, and total number density of carbon, under which the carbon line intensity is proportional to its concentration in the coal samples. To obtain better compensation for fluctuations of total carbon number density, the segmental spectral area was used and an iterative algorithm was applied that is different from our previous spectrum standardization calculations. The modified spectrum standardization model was applied to the measurement of carbon content in 24 bituminous coal samples. The results demonstrate that the proposed method has superior performance over the generally applied normalization methods. The average relative standard deviation was 3.21%, the coefficient of determination was 0.90, the root mean square error of prediction was 2.24%, and the average maximum relative error for the modified model was 12.18%, showing an overall improvement over the corresponding values for the normalization with segmental spectrum area, 6.00%, 0.75, 3.77%, and 15.40%, respectively.

Apparatus, system, and method for laser-induced breakdown spectroscopy

Science.gov (United States)

Effenberger, Jr., Andrew J; Scott, Jill R; McJunkin, Timothy R

2014-11-18

In laser-induced breakdown spectroscopy (LIBS), an apparatus includes a pulsed laser configured to generate a pulsed laser signal toward a sample, a constructive interference object and an optical element, each located in a path of light from the sample. The constructive interference object is configured to generate constructive interference patterns of the light. The optical element is configured to disperse the light. A LIBS system includes a first and a second optical element, and a data acquisition module. The data acquisition module is configured to determine an isotope measurement based, at least in part, on light received by an image sensor from the first and second optical elements. A method for performing LIBS includes generating a pulsed laser on a sample to generate light from a plasma, generating constructive interference patterns of the light, and dispersing the light into a plurality of wavelengths.

Testing a laser-induced breakdown spectroscopy technique on the Arctic sediments

Science.gov (United States)

Han, D.; Nam, S. I.

2017-12-01

Physical and geochemical investigations coupled with the Laser-induced Breakdown Spectroscopy (LIBS) were performed on three surface sediment cores (ARA03B/24BOX, ARA02B/01(A)MUC, ARA02B/02MUC and ARA02B/03(A)MUC) recovered from the western Arctic Ocean (Chukchi Sea) during IBRV ARON expeditions in 2012. The LIBS technique was applied to carry out elemental chemical analysis of the Arctic sediments and compared with that measured by ITRAX X-ray fuorescence (XRF) core scanning. LIBS and XRF have shown similar elemental composition within each sediment core. In this study, mineral composition (XRD), grain size distribution and organic carbon content as well as elemental composition (LIBS) were all considered to understand paleoenvironmental changes (ocean circulation, sea-ice drift, iceberg discharge, and etc.) recorded in the Arctic Holocene sediment. Quantitative LIBS analysis shows a gradually varying distribution of the elements along the sampled core and clear separation between the cores. The cores are geochemically characterized by elevated Mn profile. The gradient of mineral composition and grain sizes among the cores shows regional distribution and variation in sedimentary condition due to geological distance between East Siberian and North America. The present study reveals that a LIBS technique can be employed for in-situ sediment analyses for the Arctic Ocean. Furthermore, LIBS does not require costly equipment, trained operators, and complicated sample pre-treatment processes compared to Atomic absorption spectroscopy (AAS) and inductively coupled plasma emission spectroscopy (ICP), and also known to show relatively high levels of sensitivity, precision, and distinction than XRF analysis, scanning electron microscopy-energy dispersive spectrometry (SEM-EDS), and electron probe X-ray microanalysis (EPMA).

Cropland Field Monitoring: MMV Page 1 Montana Cropland Enrolled Farm Fields Carbon Sequestration Field Sampling, Measurement, Monitoring, and Verification: Application of Visible-Near Infrared Diffuse Reflectance Spectroscopy (VNIR) and Laser-induced Breakdown Spectroscopy (LIBS)

Energy Technology Data Exchange (ETDEWEB)

Lee Spangler; Ross Bricklemyer; David Brown

2012-03-15

There is growing need for rapid, accurate, and inexpensive methods to measure, and verify soil organic carbon (SOC) change for national greenhouse gas accounting and the development of a soil carbon trading market. Laboratory based soil characterization typically requires significant soil processing, which is time and resource intensive. This severely limits application for large-region soil characterization. Thus, development of rapid and accurate methods for characterizing soils are needed to map soil properties for precision agriculture applications, improve regional and global soil carbon (C) stock and flux estimates and efficiently map sub-surface metal contamination, among others. The greatest gains for efficient soil characterization will come from collecting soil data in situ, thus minimizing soil sample transportation, processing, and lab-based measurement costs. Visible and near-infrared diffuse reflectance spectroscopy (VisNIR) and laser-induced breakdown spectroscopy (LIBS) are two complementary, yet fundamentally different spectroscopic techniques that have the potential to meet this need. These sensors have the potential to be mounted on a soil penetrometer and deployed for rapid soil profile characterization at field and landscape scales. Details of sensor interaction, efficient data management, and appropriate statistical analysis techniques for model calibrations are first needed. In situ or on-the-go VisNIR spectroscopy has been proposed as a rapid and inexpensive tool for intensively mapping soil texture and organic carbon (SOC). While lab-based VisNIR has been established as a viable technique for estimating various soil properties, few experiments have compared the predictive accuracy of on-the-go and lab-based VisNIR. Eight north central Montana wheat fields were intensively interrogated using on-the-go and lab-based VisNIR. Lab-based spectral data consistently provided more accurate predictions than on-the-go data. However, neither in situ

Laser-induced breakdown spectroscopy in industrial and security applications

International Nuclear Information System (INIS)

Bol'shakov, Alexander A.; Yoo, Jong H.; Liu Chunyi; Plumer, John R.; Russo, Richard E.

2010-01-01

Laser-induced breakdown spectroscopy (LIBS) offers rapid, localized chemical analysis of solid or liquid materials with high spatial resolution in lateral and depth profiling, without the need for sample preparation. Principal component analysis and partial least squares algorithms were applied to identify a variety of complex organic and inorganic samples. This work illustrates how LIBS analyzers can answer a multitude of real-world needs for rapid analysis, such as determination of lead in paint and children's toys, analysis of electronic and solder materials, quality control of fiberglass panels, discrimination of coffee beans from different vendors, and identification of generic versus brand-name drugs. Lateral and depth profiling was performed on children's toys and paint layers. Traditional one-element calibration or multivariate chemometric procedures were applied for elemental quantification, from single laser shot determination of metal traces at ∼10 μg/g to determination of halogens at 90 μg/g using 50-shot spectral accumulation. The effectiveness of LIBS for security applications was demonstrated in the field by testing the 50-m standoff LIBS rasterizing detector.

Determination of Metal Elements in Wine Using Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Bocková, Jana; Tian, Ye; Yin, Hualiang; Delepine-Gilon, Nicole; Chen, Yanping; Veis, Pavel; Yu, Jin

2017-08-01

We developed a method for sensitive elemental analysis of wines using laser-induced breakdown spectroscopy (LIBS). In order to overcome the inefficiency of direct ablation of bulk wine (an organic liquid), a thin layer of wine residue was prepared on a metallic target according to an appropriated heating procedure applied to an amount of liquid wine dropped on the target surface. The obtained ensemble was thus ablated. Such a sample preparation procedure used a very small volume of 2 mL of wine and took only 30 min without reagent or solvent. The results show the detection of tens of metal and non-metal elements including majors (Na, Mg, K, Ca), minors, and traces (Li, B, Si, P, Ti, Mn, Fe, Cu, Zn, Rb, Sr, Ba, and Pb) in wines purchased from local supermarkets and from different production places in France. Commercially available wines were then spiked with certified standard solutions of Ti and Fe. Three series of laboratory reference samples were thus prepared using three different wines (a red wine and a white wine from a same production region and a red wine from another production region) with concentrations of Ti and Fe in the range of 1-40 mg/L. Calibration graphs established with the spiked samples allowed extracting the figures-of-merit parameters of the method for wine analysis such as the coefficient of determination ( R 2 ) and the limits of detection and quantification (LOD and LOQ). The calibration curves built with the three wines were then compared. We studied the residual matrix effect between these wines in the determination of the concentrations of Ti and Fe.

Effect of Atmospheric Conditions on LIBS Spectra

OpenAIRE

Effenberger, Andrew J.; Scott, Jill R.

2010-01-01

Laser-induced breakdown spectroscopy (LIBS) is typically performed at ambient Earth atmospheric conditions. However, interest in LIBS in other atmospheric conditions has increased in recent years, especially for use in space exploration (e.g., Mars and Lunar) or to improve resolution for isotopic signatures. This review focuses on what has been reported about the performance of LIBS in reduced pressure environments as well as in various gases other than air.

Study and development of the laser induced breakdown spectroscopy (LIBS) for the realization of field measurements: application to analysis on-line of metals in liquids

International Nuclear Information System (INIS)

Rosado, J.C.D.

2013-01-01

Metal contamination of water is a major public health issue. Controls and treatments are more drastic and performed on them for human consumption. It is essential for this to possess reliable and sensitive analytical tools adapted to the existing regulations and flexible enough to use. The technique of 'Laser Induced Breakdown Spectroscopy' (LIBS), proven for the analysis of solids, including exo-terrestrial explorations, this very interesting advantages for liquids including, for example, are multi-character elementary and the possibility of in-situ measurements of water contamination by metals. A first part of this study thesis allowed to explore the potential (LIBS) for the analysis of dissolved metals or suspensions in water. Study has found an important effect related to the particle size in the analysis of suspensions. A second prong is to look at the effects of organic matrix represented by humic acid and those natural minerals represented by the bentonite and alumina particles. The matrix effect observed was corrected by normalization by internal standard. (author) [fr

Effect of Sample Preparation on the Discrimination of Bacterial Isolates Cultured in Liquid Nutrient Media Using Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Gamble, Gary R; Park, Bosoon; Yoon, Seung-Chul; Lawrence, Kurt C

2016-03-01

Laser-induced breakdown spectroscopy (LIBS) is used as the basis for discrimination between two genera of gram-negative bacteria and two genera of gram-positive bacteria representing pathogenic threats commonly found in poultry processing rinse waters. Because LIBS-based discrimination relies primarily upon the relative proportions of inorganic cell components including Na, K, Mg, and Ca, this study aims to determine the effects of trace mineral content and pH found in the water source used to isolate the bacteria upon the reliability of the resulting discriminant analysis. All four genera were cultured using tryptic soy agar (TSA) as the nutrient medium, and were grown under identical environmental conditions. The only variable introduced is the source water used to isolate the cultured bacteria. Cultures of each bacterium were produced using deionized (DI) water under two atmosphere conditions, reverse osmosis (RO) water, tap water, phosphate buffered saline (PBS) water, and TRIS buffered water. After 3 days of culture growth, the bacteria were centrifuged and washed three times in the same water source. Bacteria were then freeze dried, mixed with microcrystalline cellulose, and a pellet was made for LIBS analysis. Principal component analysis (PCA) was used to extract related variations in LIBS spectral data among the four bacteria genera and six water types used to isolate the bacteria, and Mahalanobis discriminant analysis (MDA) was used for classification. Results indicate not only that the four genera can be discriminated from each other in each water type, but that each genus can be discriminated by water type used for isolation. It is concluded that in order for LIBS to be a reliable and repeatable method for discrimination of bacteria grown in liquid nutrient media, care must be taken to insure that the water source used in purification of the culture be precisely controlled regarding pH, ionic strength, and proportionate amounts of mineral cations

Laser induced breakdown spectroscopy library for the Martian environment

International Nuclear Information System (INIS)

Cousin, A.; Forni, O.; Maurice, S.; Gasnault, O.

2011-01-01

The NASA Mars Science Laboratory rover will carry the first Laser Induced Breakdown Spectroscopy experiment in space: ChemCam. We have developed a laboratory model which mimics ChemCam's main characteristics. We used a set of target samples relevant to Mars geochemistry, and we recorded individual spectra. We propose a data reduction scheme for Laser Induced Breakdown Spectroscopy data incorporating de-noising, continuum removal, and peak fitting. Known effects of the Martian atmosphere are confirmed with our experiment: better Signal-to-Noise Ratio on Mars compared to Earth, narrower peak width, and essentially no self-absorption. The wavelength shift of emission lines from air to Mars pressure is discussed. The National Institute of Standards and Technology vacuum database is used for wavelength calibration and to identify the elemental lines. Our Martian database contains 1336 lines for 32 elements: H, Li, Be, B, C, N, O, F, Na, Mg, Al, Si, P, S, Cl, K, Ar, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Rb, Sr, Cs, Ba, and Pb. It is a subset of the National Institute of Standards and Technology database to be used for Martian geochemistry. Finally, synthetic spectra can be built from the Martian database. Correlation calculations help to distinguish between elements in case of uncertainty. This work is used to create tools and support data for the interpretation of ChemCam results. - Highlights: ► Chemcam: first Laser Induced Breakdown Spectroscopy technique on Mars. ► Creation of a LIBS specific database to ChemCam on Mars. ► Data reduction scheme is proposed. ► Best signal under Martian conditions. ► LIBS emission lines database: subset of NIST database for Martian geochemistry.

A review of the development of portable laser induced breakdown spectroscopy and its applications

Czech Academy of Sciences Publication Activity Database

Rakovský, Jozef; Čermák, P.; Musset, O.; Veis, P.

2014-01-01

Roč. 101, NOV 2014 (2014), s. 269-287 ISSN 0584-8547 R&D Projects: GA ČR GA13-11635S Institutional support: RVO:61388955 Keywords : Fiber laser * Fieldable LIBS * Laser-induced breakdown spectroscopy Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.176, year: 2014

Atomization efficiency and photon yield in laser-induced breakdown spectroscopy analysis of single nanoparticles in an optical trap

Science.gov (United States)

Purohit, Pablo; Fortes, Francisco J.; Laserna, J. Javier

2017-04-01

Laser-induced breakdown spectroscopy (LIBS) was employed for investigating the influence of particle size on the dissociation efficiency and the absolute production of photons per mass unit of airborne solid graphite spheres under single-particle regime. Particles of average diameter of 400 nm were probed and compared with 2 μm particles. Samples were first catapulted into aerosol form and then secluded in an optical trap set by a 532 nm laser. Trap stability was quantified before subjecting particles to LIBS analysis. Fine alignment of the different lines comprising the optical catapulting-optical trapping-laser-induced breakdown spectroscopy instrument and tuning of excitation parameters conditioning the LIBS signal such as fluence and acquisition delay are described in detail with the ultimate goal of acquiring clear spectroscopic data on masses as low as 75 fg. The atomization efficiency and the photon yield increase as the particle size becomes smaller. Time-resolved plasma imaging studies were conducted to elucidate the mechanisms leading to particle disintegration and excitation.

Effect of Atmospheric Conditions on LIBS Spectra

Science.gov (United States)

Effenberger, Andrew J.; Scott, Jill R.

2010-01-01

Laser-induced breakdown spectroscopy (LIBS) is typically performed at ambient Earth atmospheric conditions. However, interest in LIBS in other atmospheric conditions has increased in recent years, especially for use in space exploration (e.g., Mars and Lunar) or to improve resolution for isotopic signatures. This review focuses on what has been reported about the performance of LIBS in reduced pressure environments as well as in various gases other than air. PMID:22399914

Qualitative and quantitative laser-induced breakdown spectroscopy of bronze objects

International Nuclear Information System (INIS)

Tankova, V; Blagoev, K; Grozeva, M; Malcheva, G; Penkova, P

2016-01-01

Laser-induced breakdown spectroscopy (LIBS) is an analytical technique for qualitative and quantitative elemental analysis of solids, liquids and gases. In this work, the method was applied for investigation of archaeological bronze objects. The analytical information obtained by LIBS was used for qualitative determination of the elements in the material used for manufacturing of the objects under study. Quantitative chemical analysis was also performed after generating calibration curves with standard samples of similar matrix composition. Quantitative estimation of the elemental concentration of the bulk of the samples was performed, together with investigation of the surface layer of the objects. The results of the quantitative analyses gave indications about the manufacturing process of the investigated objects. (paper)

Quantitative Classification of Quartz by Laser Induced Breakdown Spectroscopy in Conjunction with Discriminant Function Analysis

Directory of Open Access Journals (Sweden)

A. Ali

2016-01-01

Full Text Available A responsive laser induced breakdown spectroscopic system was developed and improved for utilizing it as a sensor for the classification of quartz samples on the basis of trace elements present in the acquired samples. Laser induced breakdown spectroscopy (LIBS in conjunction with discriminant function analysis (DFA was applied for the classification of five different types of quartz samples. The quartz plasmas were produced at ambient pressure using Nd:YAG laser at fundamental harmonic mode (1064 nm. We optimized the detection system by finding the suitable delay time of the laser excitation. This is the first study, where the developed technique (LIBS+DFA was successfully employed to probe and confirm the elemental composition of quartz samples.

Determination of elemental composition of coffee using UV-pulsed laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Gondal, M. A.; Baig, Umair; Dastageer, M. A.; Sarwar, Mohsin

2016-01-01

A detection system based on laser induced breakdown spectroscopy (LIBS) was built using 266 nm wavelength pulsed laser from the fourth harmonic of Nd:YAG laser, 500 mm spectrograph and gated ICCD camera with built-in delay generator. The LIBS system was used to study the elemental composition in coffee available in the local market of Saudi Arabia for the detection of elements in coffee samples. The LIBS spectrum of coffee sample revealed the presence magnesium, calcium, aluminum, copper, sodium, barium, bromine, cobalt, chromium, cerium manganese and molybdenum. Atomic transition line of sodium is used to study the parametric dependence of LIBS signal. The study of the dependence of LIBS signal on the laser pulse energy is proven to be linear and the dependence of LIBS signal on the time delay between the excitation and data acquisition showed a typical increase, a peak value and a decrease with the optimum excitation – acquisition delay at 400 ns.

Determination of elemental composition of coffee using UV-pulsed laser induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Gondal, M. A., E-mail: magondal@kfupm.edu.sa; Baig, Umair; Dastageer, M. A.; Sarwar, Mohsin [Laser Research Group, Physics Department, King Fahd University of Petroleum and Minerals, P.O Box 5047, Dhahran 31261 (Saudi Arabia)

2016-06-10

A detection system based on laser induced breakdown spectroscopy (LIBS) was built using 266 nm wavelength pulsed laser from the fourth harmonic of Nd:YAG laser, 500 mm spectrograph and gated ICCD camera with built-in delay generator. The LIBS system was used to study the elemental composition in coffee available in the local market of Saudi Arabia for the detection of elements in coffee samples. The LIBS spectrum of coffee sample revealed the presence magnesium, calcium, aluminum, copper, sodium, barium, bromine, cobalt, chromium, cerium manganese and molybdenum. Atomic transition line of sodium is used to study the parametric dependence of LIBS signal. The study of the dependence of LIBS signal on the laser pulse energy is proven to be linear and the dependence of LIBS signal on the time delay between the excitation and data acquisition showed a typical increase, a peak value and a decrease with the optimum excitation – acquisition delay at 400 ns.

Detection of Minerals in Green Leafy Vegetables Using Laser Induced Breakdown Spectroscopy

Science.gov (United States)

Shukla, P.; Kumar, R.; Raib, A. Kumar

2016-11-01

The distribution of minerals in different green leafy vegetables, such as spinach, chenopodium, chickpea, mustard, and fenugreek, was calculated using laser induced breakdown spectroscopy (LIBS). LIBS can provide an easy, reliable, efficient, low-cost, and in situ chemical analysis with a reasonable precision. In situ LIBS spectra in the range 200-500 nm were carried out using fresh leaves and leaves in the pellet form. As the spectra suggest, magnesium and calcium are present in each vegetable; however, the amount of them varies. It is observed that the amount of iron is maximal in spinach. The nutrition value of the plants was analyzed, and it was revealed that they are low in calories and fat and high in protein, fiber, iron, calcium, and phytochemicals.

Titanium monoxide spectroscopy following laser-induced optical breakdown

International Nuclear Information System (INIS)

Parigger, Christian G.; Woods, Alexander C.; Keszler, Anna; Nemes, László; Hornkohl, James O.

2012-01-01

This work investigates Titanium Monoxide (TiO) in ablation-plasma by employing laser-induced breakdown spectroscopy (LIBS) with 1 to 10 TW/cm 2 irradiance, pulsed, 13 nanosecond, Q-switched Nd:YAG laser radiation at the fundamental wavelength of 1064 nm. The analysis of TiO is based on our first accurate determination of transition line strengths for selected TiO A-X, B-X, and E-X transitions, particularly TiO A-X γ and B-X γ′ bands. Electric dipole line strengths for the A 3 Φ-X 3 δ and B 3 Π-X 3 δ bands of TiO are computed. The molecular TiO spectra are observed subsequent to laser-induced breakdown (LIB). We discuss analysis of diatomic molecular spectra that may occur simultaneously with spectra originating from atomic species. Gated detection is applied to investigate the development in time of the emission spectra following LIB. Collected emission spectra allow one to infer micro-plasma parameters such as temperature and electron density. Insight into the state of the micro-plasma is gained by comparing measurements with predictions of atomic and molecular spectra. Nonlinear fitting of recorded and computed diatomic spectra provides the basis for molecular diagnostics, while atomic species may overlap and are simultaneously identified. Molecular diagnostic approaches similar to TiO have been performed for diatomic molecules such as AlO, C 2 , CN, CH, N 2 , NH, NO and OH.

Double-pulse standoff laser-induced breakdown spectroscopy for versatile hazardous materials detection

Energy Technology Data Exchange (ETDEWEB)

Gottfried, Jennifer L. [U.S. Army Research Laboratory, AMSRD-ARL-WM-BD, Aberdeen Proving Ground, MD, 21005-5069 (United States)], E-mail: jennifer.gottfried@arl.army.mil; De Lucia, Frank C.; Munson, Chase A.; Miziolek, Andrzej W. [U.S. Army Research Laboratory, AMSRD-ARL-WM-BD, Aberdeen Proving Ground, MD, 21005-5069 (United States)

2007-12-15

We have developed a double-pulse standoff laser-induced breakdown spectroscopy (ST-LIBS) system capable of detecting a variety of hazardous materials at tens of meters. The use of a double-pulse laser improves the sensitivity and selectivity of ST-LIBS, especially for the detection of energetic materials. In addition to various metallic and plastic materials, the system has been used to detect bulk explosives RDX and Composition-B, explosive residues, biological species such as the anthrax surrogate Bacillus subtilis, and chemical warfare simulants at 20 m. We have also demonstrated the discrimination of explosive residues from various interferents on an aluminum substrate.

Laser Induced Breakdown Spectroscopy in archeometry: A review of its application and future perspectives

Energy Technology Data Exchange (ETDEWEB)

Spizzichino, Valeria, E-mail: valeria.spizzichino@enea.it; Fantoni, Roberta

2014-09-01

Laser Induced Breakdown Spectroscopy (LIBS) in the last decades has been more and more applied to the field of Cultural Heritage with great results obtained either alone or in combination with complementary laser techniques. Its ability to analyze, with a minimal loss, different kinds of materials in laboratory, in situ and even in hostile environments has been highly appreciated. The main aim of this paper is to present a review of LIBS applications in the interdisciplinary field of archeometry. The LIBS technique is shortly described both from a theoretical and practical point of view, discussing the instrumental setup, also in comparison with typical features of laser induced fluorescence (LIF) and Raman spectroscopy apparata. The complementary with multivariate analysis, a method that can help in reducing data set dimensions and in pulling out effective information, is stressed. In particular the role of LIBS in Cultural Heritage material characterization, recognition of fakes and indirect dating is described, reporting general considerations and case studies on metal alloys, mural paintings, decorated ceramics, glasses, stones and gems. - Highlights: • Applications of LIBS to archeometry are reviewed. • Complementary among LIBS, LIF, Raman and multivariate analysis is highlighted. • Three major areas of successful LIBS application in archeometry are identified. • Significant results have been presented for several different materials.

Classification of alloys using laser induced breakdown spectroscopy with principle component analysis

Science.gov (United States)

Syuhada Mangsor, Aneez; Haider Rizvi, Zuhaib; Chaudhary, Kashif; Safwan Aziz, Muhammad

2018-05-01

The study of atomic spectroscopy has contributed to a wide range of scientific applications. In principle, laser induced breakdown spectroscopy (LIBS) method has been used to analyse various types of matter regardless of its physical state, either it is solid, liquid or gas because all elements emit light of characteristic frequencies when it is excited to sufficiently high energy. The aim of this work was to analyse the signature spectrums of each element contained in three different types of samples. Metal alloys of Aluminium, Titanium and Brass with the purities of 75%, 80%, 85%, 90% and 95% were used as the manipulated variable and their LIBS spectra were recorded. The characteristic emission lines of main elements were identified from the spectra as well as its corresponding contents. Principal component analysis (PCA) was carried out using the data from LIBS spectra. Three obvious clusters were observed in 3-dimensional PCA plot which corresponding to the different group of alloys. Findings from this study showed that LIBS technology with the help of principle component analysis could conduct the variety discrimination of alloys demonstrating the capability of LIBS-PCA method in field of spectro-analysis. Thus, LIBS-PCA method is believed to be an effective method for classifying alloys with different percentage of purifications, which was high-cost and time-consuming before.

Mineral content analysis of root canal dentin using laser-induced breakdown spectroscopy

Science.gov (United States)

2018-01-01

Objectives This study aimed to introduce the use of laser-induced breakdown spectroscopy (LIBS) for evaluation of the mineral content of root canal dentin, and to assess whether a correlation exists between LIBS and scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS) methods by comparing the effects of irrigation solutions on the mineral content change of root canal dentin. Materials and Methods Forty teeth with a single root canal were decoronated and longitudinally sectioned to expose the canals. The root halves were divided into 4 groups (n = 10) according to the solution applied: group NaOCl, 5.25% sodium hypochlorite (NaOCl) for 1 hour; group EDTA, 17% ethylenediaminetetraacetic acid (EDTA) for 2 minutes; group NaOCl+EDTA, 5.25% NaOCl for 1 hour and 17% EDTA for 2 minutes; a control group. Each root half belonging to the same root was evaluated for mineral content with either LIBS or SEM/EDS methods. The data were analyzed statistically. Results In groups NaOCl and NaOCl+EDTA, the calcium (Ca)/phosphorus (P) ratio decreased while the sodium (Na) level increased compared with the other groups (p LIBS and SEM/EDS analyses (r = 0.84, p LIBS method proved to be reliable while providing data for the elemental composition of root canal dentin. PMID:29487841

Contributions to process monitoring by laser-induced breakdown spectroscopy

Science.gov (United States)

Rusak, David Alexander

1998-12-01

When a pulsed laser of sufficient energy and pulse duration is brought to a focus, multi-photon ionization creates free electrons in the focal volume. These electrons are accelerated in a process known as inverse Bremsstrahlung and cause collisional ionization of species in the focal volume. More charge carriers are produced and the process continues for the duration of the laser pulse. The manifestation of this process is a visible spark or plasma which typically lasts for tens of microseconds. This laser-induced plasma can serve as a source in an atomic emission experiment. Because the composition of the plasma is determined in large part by the environment in which it forms, elements in the laser target can be determined spectroscopically. The goal of a laser-induced breakdown spectroscopy (LIBS) experiment is to establish a relationship between the concentration of an element of interest in the target and the intensity of light emitted from the laser-induced plasma at a wavelength characteristic of that element. Because LIBS requires only optical access to the sample and can perform elemental determinations in solids, liquids, or gases with little sample preparation, there is interest in using it as an on-line technique for process monitoring in a number of industrial applications. However, before the technique becomes useful in industrial applications, many issues regarding instrumentation and data analysis need to be addressed in the lab. The first two chapters of this dissertation provide, respectively, the basics of the atomic emission experiment and a background of laser-induced breakdown spectroscopy. The next two chapters examine the effect of target water content on the laser-induced plasma and the use of LIBS for analysis of aqueous samples. Chapter 5 describes construction of a fiber optic LIBS probe and its use to study temporal electron number density evolution in plasmas formed on different metals. Chapter 6 is a study of excitation, vibrational

Preliminary panoramic study of river calm muscle using neodymium:yttrium-aluminum-garnet (Nd: YAG) laser-induced breakdown spectroscopy (LIBS)

Science.gov (United States)

Idris, N.; Lahna, K.; Usmawanda, T. N.; Herman; Ramli, M.; Hedwig, R.; Marpaung, A. M.; Kurniawan, K. H.

2018-04-01

A wide coverage spectral investigation on the muscle of river calm sample has been carried out using laser-induced breakdown spectroscopy for examining the overall profile of the emission spectra from the produced plasma. The basic apparatus of LIBS system used is a Nd-YAG laser and wide coverage optical multichannel analyzer (OMA) system. The river clam samples used is collected from Panga River in Aceh Jaya Regency, Aceh, Indonesia up streaming in a mountain of Gunong Ujeun, which is used as a location of the intensive traditional mining activity. Assuming that heavy metal accumulated in the clam muscle, LIBS experiments were carried out on the muscle of the calm. The sample used was fresh muscle sliced and attached to a copper plate. Plasma was generated by focusing the laser beam on the sample surface under air surrounding gas at 1 atmosphere. It is found that there are only major elements of host organic, namely C, H, O, N and the minor element of salts can be detected from fresh the clam sample when using a high pulse laser energy under air surrounding at high pressure of 1 atmosphere. There is no emission lines from any metal can be detected. Several experimental parameters were explored to study the panoramic dynamic of the emission spectra. It is found that the lower energy and the lower pressure is better for obtaining better emission spectra showing the possibility for determination of the analyte.

Laser ablation-laser induced breakdown spectroscopy for the measurement of total elemental concentration in soils.

Science.gov (United States)

Pareja, Jhon; López, Sebastian; Jaramillo, Daniel; Hahn, David W; Molina, Alejandro

2013-04-10

The performances of traditional laser-induced breakdown spectroscopy (LIBS) and laser ablation-LIBS (LA-LIBS) were compared by quantifying the total elemental concentration of potassium in highly heterogeneous solid samples, namely soils. Calibration curves for a set of fifteen samples with a wide range of potassium concentrations were generated. The LA-LIBS approach produced a superior linear response different than the traditional LIBS scheme. The analytical response of LA-LIBS was tested with a large set of different soil samples for the quantification of the total concentration of Fe, Mn, Mg, Ca, Na, and K. Results showed an acceptable linear response for Ca, Fe, Mg, and K while poor signal responses were found for Na and Mn. Signs of remaining matrix effects for the LA-LIBS approach in the case of soil analysis were found and discussed. Finally, some improvements and possibilities for future studies toward quantitative soil analysis with the LA-LIBS technique are suggested.

Real-time control of ultrafast laser micromachining by laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Tong Tao; Li Jinggao; Longtin, Jon P.

2004-01-01

Ultrafast laser micromachining provides many advantages for precision micromachining. One challenging problem, however, particularly for multilayer and heterogeneous materials, is how to prevent a given material from being ablated, as ultrafast laser micromachining is generally material insensitive. We present a real-time feedback control system for an ultrafast laser micromachining system based on laser-induced breakdown spectroscopy (LIBS). The characteristics of ultrafast LIBS are reviewed and discussed so as to demonstrate the feasibility of the technique. Comparison methods to identify the material emission patterns are developed, and several of the resulting algorithms were implemented into a real-time computer control system. LIBS-controlled micromachining is demonstrated for the fabrication of microheater structures on thermal sprayed materials. Compared with a strictly passive machining process without any such feedback control, the LIBS-based system provides several advantages including less damage to the substrate layer, reduced machining time, and more-uniform machining features

Forensic comparative glass analysis by laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Bridge, Candice M.; Powell, Joseph; Steele, Katie L.; Sigman, Michael E.

2007-01-01

Glass samples of four types commonly encountered in forensic examinations have been analyzed by laser-induced breakdown spectroscopy (LIBS) for the purpose of discriminating between samples originating from different sources. Some of the glass sets were also examined by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). Refractive index (RI) measurements were also made on all glass samples and the refractive index data was combined with the LIBS and with the LA-ICP-MS data to enhance discrimination. The glass types examined included float glass taken from front and side automobile windows (examined on the non-float side), automobile headlamp glass, automobile side-mirror glass and brown beverage container glass. The largest overall discrimination was obtained by employing RI data in combination with LA-ICP-MS (98.8% discrimination of 666 pairwise comparisons at 95% confidence), while LIBS in combination with RI provided a somewhat lower discrimination (87.2% discrimination of 1122 pairwise comparisons at 95% confidence). Samples of side-mirror glass were less discriminated by LIBS due to a larger variance in emission intensities, while discrimination of side-mirror glass by LA-ICP-MS remained high

Spectral Analysis of Rare Earth Elements using Laser-Induced Breakdown Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Martin, Madhavi Z [ORNL; Fox, Dr. Richard V [Idaho National Laboratory (INL); Miziolek, Andrzej W [United States Army Research Laboratory; DeLucia, Frank C [United States Army Research Laboratory; Andre, Nicolas O [ORNL

2015-01-01

There is growing interest in rapid analysis of rare earth elements (REEs) both due to the need to find new natural sources to satisfy increased demand in their use in various electronic devices, as well as the fact that they are used to estimate actinide masses for nuclear safeguards and nonproliferation. Laser-Induced Breakdown Spectroscopy (LIBS) appears to be a particularly well-suited spectroscopy-based technology to rapidly and accurately analyze the REEs in various matrices at low concentration levels (parts-per-million). Although LIBS spectra of REEs have been reported for a number of years, further work is still necessary in order to be able to quantify the concentrations of various REEs in realworld complex samples. LIBS offers advantages over conventional solution-based radiochemistry in terms of cost, analytical turnaround, waste generation, personnel dose, and contamination risk. Rare earth elements of commercial interest are found in the following three matrix groups: 1) raw ores and unrefined materials, 2) as components in refined products such as magnets, lighting phosphors, consumer electronics (which are mostly magnets and phosphors), catalysts, batteries, etc., and 3) waste/recyclable materials (aka e-waste). LIBS spectra for REEs such as Gd, Nd, and Sm found in rare earth magnets are presented.

Spectral Analysis of Rare Earth Elements using Laser-Induced Breakdown Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Martin, Madhavi Z [ORNL; Fox, Dr. Richard V [Idaho National Laboratory (INL); Miziolek, Andrzej W [United States Army Research Laboratory; DeLucia, Frank C [United States Army Research Laboratory; Andre, Nicolas O [ORNL

2015-01-01

There is growing interest in rapid analysis of rare earth elements (REEs) both due to the need to find new natural sources to satisfy increased demand in their use in various electronic devices, as well as the fact that they are used to estimate actinide masses for nuclear safeguards and nonproliferation. Laser-Induced Breakdown Spectroscopy (LIBS) appears to be a particularly well-suited spectroscopy-based technology to rapidly and accurately analyze the REEs in various matrices at low concentration levels (parts-per-million). Although LIBS spectra of REEs have been reported for a number of years, further work is still necessary in order to be able to quantify the concentrations of various REEs in real-world complex samples. LIBS offers advantages over conventional solution-based radiochemistry in terms of cost, analytical turnaround, waste generation, personnel dose, and contamination risk. Rare earth elements of commercial interest are found in the following three matrix groups: 1) raw ores and unrefined materials, 2) as components in refined products such as magnets, lighting phosphors, consumer electronics (which are mostly magnets and phosphors), catalysts, batteries, etc., and 3) waste/recyclable materials (aka e-waste). LIBS spectra for REEs such as Gd, Nd, and Sm found in rare earth magnets are presented.

Laboratory feasibility study of fusion vessel inner wall chemical analysis by Laser Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Almaviva, Salvatore; Caneve, Luisa; Colao, Francesco; Fantoni, Roberta; Maddaluno, Giorgio

2012-01-01

Graphical abstract: Laser-Induced-Breakdown-Spectroscopy was used for the determination of the atomic composition of multilayered samples simulating the tiles of plasma facing components in the next generation fusion machines. Highlights: ► Description and characterization of an LIBS set-up for diagnostics in fusion machines. ► Identification of atomic composition of multilayered tiles simulating plasma facing components. ► Qualitative applicability of the Calibration Free method for quantitative analysis. ► Feasibility of large scale application in the processes of control during the tiles fabrication. ► Feasibility of erosion monitoring during operation of fusion machines. - Abstract: Laser Induced Breakdown Spectroscopy (LIBS) is nowadays a well established tool for qualitative, semi-quantitative and quantitative analyses of surfaces, with micro-destructive characteristics and capabilities for stratigraphy. LIBS is an appealing technique compared with many other types of elemental analysis thanks to the set up versatility facilitating non-invasive and remote analyses, as well as suitability to diagnostics in harsh environments. In this work, LIBS capabilities were used for the determination of the atomic composition of multilayered samples simulating the tiles of plasma facing components in the next generation fusion machines such as ITER. A new experimental setup was designed and realized in order to optimize the characteristics of an LIBS system working at low pressure and remotely, as it should be for an in situ system to be applied in monitoring the erosion and redeposition phenomena occurring on the inner walls of a fusion device. The effects of time delay and laser fluence on LIBS sensitivity at reduced pressure were examined, looking for operational conditions suitable to analytical applications. The quantitative analysis of some atomic species in the superficial layer has been carried out using a Calibration Free (CF) approach in the time

Laser-induced breakdown spectroscopy analysis of minerals: Carbonates and silicates

International Nuclear Information System (INIS)

McMillan, Nancy J.; Harmon, Russell S.; De Lucia, Frank C.; Miziolek, Andrzej M.

2007-01-01

Laser-induced breakdown spectroscopy (LIBS) provides an alternative chemical analytical technique that obviates the issues of sample preparation and sample destruction common to most laboratory-based analytical methods. This contribution explores the capability of LIBS analysis to identify carbonate and silicate minerals rapidly and accurately. Fifty-two mineral samples (18 carbonates, 9 pyroxenes and pyroxenoids, 6 amphiboles, 8 phyllosilicates, and 11 feldspars) were analyzed by LIBS. Two composite broadband spectra (averages of 10 shots each) were calculated for each sample to produce two databases each containing the composite LIBS spectra for the same 52 mineral samples. By using correlation coefficients resulting from the regression of the intensities of pairs of LIBS spectra, all 52 minerals were correctly identified in the database. If the LIBS spectra of each sample were compared to a database containing the other 51 minerals, 65% were identified as a mineral of similar composition from the same mineral family. The remaining minerals were misidentified for two reasons: 1) the mineral had high concentrations of an element not present in the database; and 2) the mineral was identified as a mineral with similar elemental composition from a different family. For instance, the Ca-Mg carbonate dolomite was misidentified as the Ca-Mg silicate diopside. This pilot study suggests that LIBS has promise in mineral identification and in situ analysis of minerals that record geological processes

Calibration-Free Laser-Induced Breakdown Spectroscopy: State of the art

Science.gov (United States)

Tognoni, E.; Cristoforetti, G.; Legnaioli, S.; Palleschi, V.

2010-01-01

The aim of this paper is offering a critical review of Calibration-Free Laser-Induced Breakdown Spectroscopy (CF-LIBS), the approach of multi-elemental quantitative analysis of LIBS spectra, based on the measurement of line intensities and plasma properties (plasma electron density and temperature) and on the assumption of a Boltzmann population of excited levels, which does not require the use of calibration curves or matrix-matched standards. The first part of this review focuses on the applications of the CF-LIBS method. Quantitative results reported in the literature, obtained in the analysis of various materials and in a wide range of experimental conditions, are summarized, with a special emphasis on the departure from nominal composition values. The second part is a discussion of the simplifying assumptions which lie at the basis of the CF-LIBS algorithm (stoichiometric ablation and complete atomization, thermal equilibrium, homogeneous plasma, thin radiation, detection of all elements). The inspection of the literature suggests that the CF-LIBS method is more accurate in analyzing metallic alloys rather than dielectrics. However, the full exploitation of the method seems to be still far to come, especially for the lack of a complete characterization of the effects of experimental constraints. However, some general directions can be suggested to help the analyst in designing LIBS measurements in a way which is more suited for CF-LIBS analysis.

Detection of Elemental Composition of Lubricating Grease Using Laser Induced Breakdown Spectroscopy

Directory of Open Access Journals (Sweden)

Cherry Dhiman

2014-12-01

Full Text Available The elemental composition of lubricating soft grease used in rail engines are studied using laser induced breakdown spectroscopy (LIBS technique. LIBS spectra of fresh, partially used and fully used grease samples are recorded using time-gated ICCD spectrometer for verification of compositional degradation of the used grease. LIBS spectra of grease samples are analyzed by comparing with emission spectra of elements published by NIST standard database. Many spectral lines of impurity elements like Fe, Cu, Ba, Mg, Mn, Ni, S, Zn, Si, Pb, Ti, Ca and Al present in the grease in ppm or ppb level in trace level concentrations are observed in excess in the used grease mainly due to wear and tear. On the other hand in fresh grease, spectral lines of Ca, Al and Na are observed predominantly.

Impurity diagnosis of a KSTAR graphite divertor tile using laser induced breakdown spectroscopy technique

Energy Technology Data Exchange (ETDEWEB)

Kim, Minju; Cho, Min Sang; Cho, Byoung Ick, E-mail: bicho@gist.ac.kr

2017-04-15

Laser induced breakdown spectroscopy (LIBS) has been tested to diagnose impurity elements on a Korea Superconducting Tokamak Advanced Research (KSTAR) divertor tile. Spectral lines of various impurity elements such as iron, chromium, and nickel were detected from the divertor surface. The variation of spectra with consecutive laser pulses demonstrates the potential for depth profiling analysis for the deposited impurity layer. The LIBS plasma parameters have been qualitatively determined from analysis of the relative line intensities and linewidths for each element. The validity of this analysis has been checked with atomic spectral simulations.

Field deployment test of laser-induced breakdown spectroscopy (LIBS) technology at the Yucca Mountain Exploratory Studies Facility, Test Alcove No. 1, March 2-9, 1994: Milestone Report LA4047

International Nuclear Information System (INIS)

Blacic, J.; Pettit, D.; Cremers, D.

1996-01-01

A field test in the Exploratory Studies Facility at Yucca Mountain, Nevada was performed to determine the feasibility of real-time elemental analysis of rock encountered in air core drilling using the technique of laser-induced breakdown spectroscopy (LIBS). Over the period March 2-9, 1994, hundreds of LIBS spectra were collected in real-time, reflecting the elemental composition of dust produced at the drill head of the second horizontal core hole in Test Alcove No. 1. The particle-laden, drill-coring effluent air stream served as the means to obtain a representative rock sample immediately surrounding the drill bit. LIBS spectra were taken with the spectral range centered at 250, 330, 410, and 500 nm so that representative, overlapping spectral coverage from 200 to 550 nm was obtained for the dust. Spectral lines for the major elements Si, Al, K, Na, and Fe and the minor elements Ca, Mg, Ti, and Mn were observed. Some simple engineering improvements to the cyclone separator were identified if this approach to dust analysis is pursued in the future

Laser Induced Breakdown Spectroscopy in archeometry: A review of its application and future perspectives

Science.gov (United States)

Spizzichino, Valeria; Fantoni, Roberta

2014-09-01

Laser Induced Breakdown Spectroscopy (LIBS) in the last decades has been more and more applied to the field of Cultural Heritage with great results obtained either alone or in combination with complementary laser techniques. Its ability to analyze, with a minimal loss, different kinds of materials in laboratory, in situ and even in hostile environments has been highly appreciated. The main aim of this paper is to present a review of LIBS applications in the interdisciplinary field of archeometry. The LIBS technique is shortly described both from a theoretical and practical point of view, discussing the instrumental setup, also in comparison with typical features of laser induced fluorescence (LIF) and Raman spectroscopy apparata. The complementary with multivariate analysis, a method that can help in reducing data set dimensions and in pulling out effective information, is stressed. In particular the role of LIBS in Cultural Heritage material characterization, recognition of fakes and indirect dating is described, reporting general considerations and case studies on metal alloys, mural paintings, decorated ceramics, glasses, stones and gems.

Novel estimation of the humification degree of soil organic matter by laser-induced breakdown spectroscopy

Science.gov (United States)

Ferreira, Edilene Cristina; Ferreira, Ednaldo José; Villas-Boas, Paulino Ribeiro; Senesi, Giorgio Saverio; Carvalho, Camila Miranda; Romano, Renan Arnon; Martin-Neto, Ladislau; Milori, Débora Marcondes Bastos Pereira

2014-09-01

Soil organic matter (SOM) constitutes an important reservoir of terrestrial carbon and can be considered an alternative for atmospheric carbon storage, contributing to global warming mitigation. Soil management can favor atmospheric carbon incorporation into SOM or its release from SOM to atmosphere. Thus, the evaluation of the humification degree (HD), which is an indication of the recalcitrance of SOM, can provide an estimation of the capacity of carbon sequestration by soils under various managements. The HD of SOM can be estimated by using various analytical techniques including fluorescence spectroscopy. In the present work, the potential of laser-induced breakdown spectroscopy (LIBS) to estimate the HD of SOM was evaluated for the first time. Intensities of emission lines of Al, Mg and Ca from LIBS spectra showing correlation with fluorescence emissions determined by laser-induced fluorescence spectroscopy (LIFS) reference technique were used to obtain a multivaried calibration model based on the k-nearest neighbor (k-NN) method. The values predicted by the proposed model (A-LIBS) showed strong correlation with LIFS results with a Pearson's coefficient of 0.87. The HD of SOM obtained after normalizing A-LIBS by total carbon in the sample showed a strong correlation to that determined by LIFS (0.94), thus suggesting the great potential of LIBS for this novel application.

Analysis of fresco by laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Caneve, L.; Diamanti, A.; Grimaldi, F.; Palleschi, G.; Spizzichino, V.; Valentini, F.

2010-01-01

The laser-based techniques have been shown to be a very powerful tool for artworks characterization and are used in the field of cultural heritage for the offered advantages of minimum invasiveness, in situ applicability and high sensitivity. Laser induced breakdown spectroscopy, in particular, has been applied in this field to many different kinds of ancient materials with successful results. In this work, a fragment of a Roman wall painting from the archaeological area of Pompeii has been investigated by LIBS. The sample elemental composition resulting from LIBS measurements suggested the presence of certain pigments. The ratio of the intensities of different lines related to some characteristic elements is proposed as an indicator for pigment recognition. The depth profiling permitted to put in evidence the presence of successive paint layers with different compositions. A comparison with the results obtained by the microscopy inspection of the sample has been done.

Investigation of Laser Induced Breakdown Spectroscopy (LIBS) for the Differentiation of Nerve and Gland Tissue—A Possible Application for a Laser Surgery Feedback Control Mechanism

Science.gov (United States)

Mehari, F.; Rohde, M.; Knipfer, C.; Kanawade, R.; Klämpfl, F.; W., Adler; Oetter, N.; Stelzle, F.; Schmidt, M.

2016-06-01

Laser surgery provides clean, fast and accurate modeling of tissue. However, the inability to determine what kind of tissue is being ablated at the bottom of the cut may lead to the iatrogenic damage of structures that were meant to be preserved. In this context, nerve preservation is one of the key challenges in any surgical procedure. One example is the treatment of parotid gland pathologies, where the facial nerve (N. VII) and its main branches run through and fan out inside the glands parenchyma. A feedback system that automatically stops the ablation to prevent nerve-tissue damage could greatly increase the applicability and safety of surgical laser systems. In the present study, Laser Induced Breakdown Spectroscopy (LIBS) is used to differentiate between nerve and gland tissue of an ex-vivo pig animal model. The LIBS results obtained in this preliminary experiment suggest that the measured spectra, containing atomic and molecular emissions, can be used to differentiate between the two tissue types. The measurements and differentiation were performed in open air and under normal stray light conditions.

Optical-fiber-based laser-induced breakdown spectroscopy for detection of early caries

Science.gov (United States)

Sasazawa, Shuhei; Kakino, Satoko; Matsuura, Yuji

2015-06-01

A laser-induced breakdown spectroscopy (LIBS) system targeting for the in vivo analysis of tooth enamel is described. The system is planned to enable real-time analysis of teeth during laser dental treatment by utilizing a hollow optical fiber that transmits both Q-switched Nd:YAG laser light for LIBS and infrared Er:YAG laser light for tooth ablation. The sensitivity of caries detection was substantially improved by expanding the spectral region under analysis to ultraviolet (UV) light and by focusing on emission peaks of Zn in the UV region. Subsequently, early caries were distinguished from healthy teeth with accuracy rates above 80% in vitro.

Development of a fiber-coupled laser-induced breakdown spectroscopy instrument for analysis of underwater debris in a nuclear reactor core

International Nuclear Information System (INIS)

Saeki, Morihisa; Iwanade, Akio; Ohba, Hironori; Ito, Chikara; Wakaida, Ikuo; Thornton, Blair; Sakka, Tetsuo

2014-01-01

To inspect the post-accident nuclear core reactor of the TEPCO Fukushima Daiichi nuclear power plant (F1-NPP), a transportable fiber-coupled laser-induced breakdown spectroscopy (LIBS) instrument has been developed. The developed LIBS instrument was designed to analyze underwater samples in a high-radiation field by single-pulse breakdown with gas flow or double-pulse breakdown. To check the feasibility of the assembled fiber-coupled LIBS instrument for the analysis of debris material (mixture of the fuel core, fuel cladding, construction material and so on) in the F1-NPP, we investigated the influence of the radiation dose on the optical transmittance of the laser delivery fiber, compared data quality among various LIBS techniques for an underwater sample and studied the feasibility of the fiber-coupled LIBS system in an analysis of the underwater sample of the simulated debris in F1-NPP. In a feasible study conducted by using simulated debris, which was a mixture of CeO 2 (surrogate of UO 2 ), ZrO 2 and Fe, we selected atomic lines suitable for the analysis of materials, and prepared calibration curves for the component elements. The feasible study has guaranteed that the developed fiber-coupled LIBS system is applicable for analyzing the debris materials in the F1-NPP. (author)

Analysis of bakery products by laser-induced breakdown spectroscopy.

Science.gov (United States)

Bilge, Gonca; Boyacı, İsmail Hakkı; Eseller, Kemal Efe; Tamer, Uğur; Çakır, Serhat

2015-08-15

In this study, we focused on the detection of Na in bakery products by using laser-induced breakdown spectroscopy (LIBS) as a quick and simple method. LIBS experiments were performed to examine the Na at 589 nm to quantify NaCl. A series of standard bread sample pellets containing various concentrations of NaCl (0.025-3.5%) were used to construct the calibration curves and to determine the detection limits of the measurements. Calibration graphs were drawn to indicate functions of NaCl and Na concentrations, which showed good linearity in the range of 0.025-3.5% NaCl and 0.01-1.4% Na concentrations with correlation coefficients (R(2)) values greater than 0.98 and 0.96. The obtained detection limits for NaCl and Na were 175 and 69 ppm, respectively. Performed experimental studies showed that LIBS is a convenient method for commercial bakery products to quantify NaCl concentrations as a rapid and in situ technique. Copyright © 2015 Elsevier Ltd. All rights reserved.

Laser-induced breakdown spectroscopy of tantalum plasma

International Nuclear Information System (INIS)

Khan, Sidra; Bashir, Shazia; Hayat, Asma; Khaleeq-ur-Rahman, M.; Faizan–ul-Haq

2013-01-01

Laser Induced Breakdown spectroscopy (LIBS) of Tantalum (Ta) plasma has been investigated. For this purpose Q-switched Nd: YAG laser pulses (λ∼ 1064 nm, τ∼ 10 ns) of maximum pulse energy of 100 mJ have been employed as an ablation source. Ta targets were exposed under the ambient environment of various gases of Ar, mixture (CO 2 : N 2 : He), O 2 , N 2 , and He under various filling pressure. The emission spectrum of Ta is observed by using LIBS spectrometer. The emission intensity, excitation temperature, and electron number density of Ta plasma have been evaluated as a function of pressure for various gases. Our experimental results reveal that the optical emission intensity, the electron temperature and density are strongly dependent upon the nature and pressure of ambient environment. The SEM analysis of the ablated Ta target has also been carried out to explore the effect of ambient environment on the laser induced grown structures. The growth of grain like structures in case of molecular gases and cone-formation in case of inert gases is observed. The evaluated plasma parameters by LIBS analysis such as electron temperature and the electron density are well correlated with the surface modification of laser irradiated Ta revealed by SEM analysis

Laser-induced breakdown spectroscopy of tantalum plasma

Energy Technology Data Exchange (ETDEWEB)

Khan, Sidra; Bashir, Shazia; Hayat, Asma; Khaleeq-ur-Rahman, M.; Faizan–ul-Haq [Centre for Advanced Studies in Physics, GC University, Lahore (Pakistan)

2013-07-15

Laser Induced Breakdown spectroscopy (LIBS) of Tantalum (Ta) plasma has been investigated. For this purpose Q-switched Nd: YAG laser pulses (λ∼ 1064 nm, τ∼ 10 ns) of maximum pulse energy of 100 mJ have been employed as an ablation source. Ta targets were exposed under the ambient environment of various gases of Ar, mixture (CO{sub 2}: N{sub 2}: He), O{sub 2}, N{sub 2}, and He under various filling pressure. The emission spectrum of Ta is observed by using LIBS spectrometer. The emission intensity, excitation temperature, and electron number density of Ta plasma have been evaluated as a function of pressure for various gases. Our experimental results reveal that the optical emission intensity, the electron temperature and density are strongly dependent upon the nature and pressure of ambient environment. The SEM analysis of the ablated Ta target has also been carried out to explore the effect of ambient environment on the laser induced grown structures. The growth of grain like structures in case of molecular gases and cone-formation in case of inert gases is observed. The evaluated plasma parameters by LIBS analysis such as electron temperature and the electron density are well correlated with the surface modification of laser irradiated Ta revealed by SEM analysis.

Analysis of preservative-treated wood by multivariate analysis of laser-induced breakdown spectroscopy spectra

International Nuclear Information System (INIS)

Martin, Madhavi Z.; Labbe, Nicole; Rials, Timothy G.; Wullschleger, Stan D.

2005-01-01

In this work, multivariate statistical analysis (MVA) techniques are coupled with laser-induced breakdown spectroscopy (LIBS) to identify preservative types (chromated copper arsenate, ammoniacal copper zinc or alkaline copper quat), and to predict elemental content in preservative-treated wood. The elemental composition of the samples was measured with a standard laboratory method of digestion followed by atomic absorption spectroscopy analysis. The elemental composition was then correlated with the LIBS spectra using projection to latent structures (PLS) models. The correlations for the different elements introduced by different treatments were very strong, with the correlation coefficients generally above 0.9. Additionally, principal component analysis (PCA) was used to differentiate the samples treated with different preservative formulations. The research has focused not only on demonstrating the application of LIBS as a tool for use in the forest products industry, but also considered sampling errors, limits of detection, reproducibility, and accuracy of measurements as they relate to multivariate analysis of this complex wood substrate

Analysis of preservative-treated wood by multivariate analysis of laser-induced breakdown spectroscopy spectra

Energy Technology Data Exchange (ETDEWEB)

Martin, Madhavi Z. [Environmental Sciences Division Oak Ridge National Laboratory, P.O. Box 2008 MS 6422, Oak Ridge TN 37831-6422 (United States); Labbe, Nicole [Forest Products Center, University of Tennessee, 2506 Jacob Drive, Knoxville, TN 37996-4570 (United States)]. E-mail: nlabbe@utk.edu; Rials, Timothy G. [Forest Products Center, University of Tennessee, 2506 Jacob Drive, Knoxville, TN 37996-4570 (United States); Wullschleger, Stan D. [Environmental Sciences Division Oak Ridge National Laboratory, P.O. Box 2008 MS 6422, Oak Ridge TN 37831-6422 (United States)

2005-08-31

In this work, multivariate statistical analysis (MVA) techniques are coupled with laser-induced breakdown spectroscopy (LIBS) to identify preservative types (chromated copper arsenate, ammoniacal copper zinc or alkaline copper quat), and to predict elemental content in preservative-treated wood. The elemental composition of the samples was measured with a standard laboratory method of digestion followed by atomic absorption spectroscopy analysis. The elemental composition was then correlated with the LIBS spectra using projection to latent structures (PLS) models. The correlations for the different elements introduced by different treatments were very strong, with the correlation coefficients generally above 0.9. Additionally, principal component analysis (PCA) was used to differentiate the samples treated with different preservative formulations. The research has focused not only on demonstrating the application of LIBS as a tool for use in the forest products industry, but also considered sampling errors, limits of detection, reproducibility, and accuracy of measurements as they relate to multivariate analysis of this complex wood substrate.

Enhancement and stabilization of plasma using collinear long-short double-pulse laser-induced breakdown spectroscopy

Science.gov (United States)

Cui, Minchao; Deguchi, Yoshihiro; Wang, Zhenzhen; Fujita, Yuki; Liu, Renwei; Shiou, Fang-Jung; Zhao, Shengdun

2018-04-01

A collinear long-short dual-pulse laser-induced breakdown spectroscopy (DP-LIBS) method was employed to enhance and stabilize the laser-induced plasma from steel sample. The long-pulse-width laser beam with the pulse width of 60 μs was generated by a Nd: YAG laser which was operated at FR (free running) mode. The comparative experiments were carried out between single pulse LIBS (SP-LIBS) and long-short DP-LIBS. The recorded results showed that the emission intensities and the temperature of plasma were enhanced by long-short DP-LIBS. The plasma images showed that the plasma was bigger and had a longer lifetime in long-short DP-LIBS situation. Through the calculation of time-resolved plasma temperature and intensity ratio, it can be concluded that the plasma was stabilized by the long-pulse-width laser beam. The long-short DP-LIBS method also generated the stable plasma condition from the samples with different initial temperatures, which overcame the difficulties of LIBS in the online measurement for steel production line.

Mapping of the spatial distribution of silver nanoparticles in root tissues of Vicia faba by laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Krajcarová, L; Novotný, K; Kummerová, M; Dubová, J; Gloser, V; Kaiser, J

2017-10-01

The manuscript presents a procedure for optimal sample preparation and the mapping of the spatial distribution of metal ions and nanoparticles in plant roots using laser-induced breakdown spectroscopy (LIBS) in a double-pulse configuration (DP LIBS) in orthogonal reheating mode. Two Nd:YAG lasers were used; the first one was an ablation laser (UP-266 MACRO, New Wave, USA) with a wavelength of 266nm, and the second one (Brilliant, Quantel, France), with a fundamental wavelength of 1064nm, was used to reheat the microplasma. Seedlings of Vicia faba were cultivated for 7 days in CuSO 4 or AgNO 3 solutions with a concentration of 10µmoll -1 or in a solution of silver nanoparticles (AgNPs) with a concentration of 10µmoll -1 of total Ag, and in distilled water as a control. The total contents of the examined metals in the roots after sample mineralization as well as changes in the concentrations of the metals in the cultivation solutions were monitored by ICP-OES. Root samples embedded in the TissueTek medium and cut into 40µm thick cross sections using the Cryo-Cut Microtome proved to be best suited for an accurate LIBS analysis with a 50µm spatial resolution. 2D raster maps of elemental distribution were created for the emission lines of Cu(I) at 324.754nm and Ag(I) at 328.068nm. The limits of detection of DP LIBS for the root cross sections were estimated to be 4pg for Cu, 18pg for Ag, and 3pg for AgNPs. The results of Ag spatial distribution mapping indicated that unlike Ag + ions, AgNPs do not penetrate into the inner tissues of Vicia faba roots but stay in their outermost layers. The content of Ag in roots cultivated in the AgNP solution was one order of magnitude lower compared to roots cultivated in the metal ion solutions. The significantly smaller concentration of Ag in root tissues cultivated in the AgNP solution also supports the conclusion that the absorption and uptake of AgNPs by roots of Vicia faba is very slow. LIBS mapping of root sections

Novel estimation of the humification degree of soil organic matter by laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Ferreira, Edilene Cristina, E-mail: edilene@iq.unesp.br [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil); São Paulo State University—UNESP, Analytical Chemistry Department, P.O. Box 355, 14801-970 Rua Prof. Francisco Degni, 55, CEP 14800-900 Araraquara, SP (Brazil); Ferreira, Ednaldo José, E-mail: ednaldo.ferreira@embrapa.br [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil); Villas-Boas, Paulino Ribeiro, E-mail: paulino.villas-boas@embrapa.br [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil); Senesi, Giorgio Saverio, E-mail: giorgio.senesi@ba.imip.cnr.it [Institute of Inorganic Methodologies and Plasmas, CNR, Bari 70126 (Italy); Carvalho, Camila Miranda, E-mail: camilamc@gmail.com [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil); Physics Institute of São Carlos, University of São Paulo, IFSC-USP, Av. Trabalhador são-carlense, 400 Pq. Arnold Schimid, 13566-590 São Carlos, SP (Brazil); Romano, Renan Arnon, E-mail: renan.romano@gmail.com [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil); Physics Institute of São Carlos, University of São Paulo, IFSC-USP, Av. Trabalhador são-carlense, 400 Pq. Arnold Schimid, 13566-590 São Carlos, SP (Brazil); Martin-Neto, Ladislau, E-mail: ladislau.martin@embrapa.br [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil); and others

2014-09-01

Soil organic matter (SOM) constitutes an important reservoir of terrestrial carbon and can be considered an alternative for atmospheric carbon storage, contributing to global warming mitigation. Soil management can favor atmospheric carbon incorporation into SOM or its release from SOM to atmosphere. Thus, the evaluation of the humification degree (HD), which is an indication of the recalcitrance of SOM, can provide an estimation of the capacity of carbon sequestration by soils under various managements. The HD of SOM can be estimated by using various analytical techniques including fluorescence spectroscopy. In the present work, the potential of laser-induced breakdown spectroscopy (LIBS) to estimate the HD of SOM was evaluated for the first time. Intensities of emission lines of Al, Mg and Ca from LIBS spectra showing correlation with fluorescence emissions determined by laser-induced fluorescence spectroscopy (LIFS) reference technique were used to obtain a multivaried calibration model based on the k-nearest neighbor (k-NN) method. The values predicted by the proposed model (A-LIBS) showed strong correlation with LIFS results with a Pearson's coefficient of 0.87. The HD of SOM obtained after normalizing A-LIBS by total carbon in the sample showed a strong correlation to that determined by LIFS (0.94), thus suggesting the great potential of LIBS for this novel application. - Highlights: • Humification degree of soil organic matter (HD) • Importance of soil organic matter HD in keeping carbon in soil • Laser induced fluorescence spectroscopy (LIFS) for HD estimation (reference method) • New LIBS application to predict HD.

Analysis of pigments in polychromes by use of laser induced breakdown spectroscopy and Raman microscopy

Science.gov (United States)

Castillejo, M.; Martín, M.; Silva, D.; Stratoudaki, T.; Anglos, D.; Burgio, L.; Clark, R. J. H.

2000-09-01

Two laser-based analytical techniques, Laser Induced Breakdown Spectroscopy (LIBS) and Raman microscopy, have been used for the identification of pigments on a polychrome from the Rococo period. Detailed spectral data are presented from analyses performed on a fragment of a gilded altarpiece from the church of Escatrón, Zaragoza, Spain. LIBS measurements yielded elemental analytical data which suggest the presence of certain pigments and, in addition, provide information on the stratigraphy of the paint layers. Identification of most pigments and of the materials used in the preparation layer was performed by Raman microscopy.

Analyzing silver concentration in soil using laser-induced breakdown spectroscopy

Science.gov (United States)

Prasetyo, S.; Isnaeni; Zaitun; Mitchell, K.; Suliyanti, M. M.; Herbani, Y.

2018-03-01

Determination of concentration of heavy metal ions in soil, such as silver, is very important to study soil pollution levels. Several techniques have been developed to determine silver ion concentration in soil. In this paper, we utilized laser-induced breakdown spectroscopy (LIBS) to study silver concentration in soil. We used four different data analysis methods to calculate silver concentration. In this case, we prepared soil samples with different silver ion concentrations from 400 ppm to 1000 ppm. Our analysis was focused on the 843.15 nm silver atomic absorption line. We found that plasma intensity increased as silver concentration increased. Our findings were based on our analysis using four different analysis methods. We believe that these analysis methods are able to calculate silver concentration in soil using LIBS.

Determination of lanthanides in fossil samples using laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Anzano, J.M.; Lasheras, R.J.; Canudo, I.; Laguna, M.

2017-01-01

As being a fast, simple and relatively non-destructive analytical technique Laser-induced breakdown spectroscopy (LIBS) has a large variety of applications including the analysis of paleontological samples. In this work LIBS is employed for the quantitative determination of lanthanides (Ce, Dy, Er, Eu, Gd, Ho, La, Lu, Nd, Sm, Tb, Tm and Yb) in vertebrate fossil samples comprising teeth, disarticulated complete or fragmented bones, eggshell fragments, and coprolites of dinosaurs, mammals and crocodiles. For emission line data, standard AnalaR grade salts of lanthanides were used. The major components: iron, calcium, magnesium, silicon and aluminum in the samples were also determined. The analytical information may be helpful in studying the samples for their age, formation environment and other paleontological properties. (author)

Application of Laser Induced Breakdown Spectroscopy under Polar Conditions

Science.gov (United States)

Clausen, J. L.; Hark, R.; Bol'shakov, A.; Plumer, J.

2015-12-01

Over the past decade our research team has evaluated the use of commercial-off-the-shelf laser-induced breakdown spectroscopy (LIBS) for chemical analysis of snow and ice samples under polar conditions. One avenue of research explored LIBS suitability as a detector of paleo-climate proxy indicators (Ca, K, Mg, and Na) in ice as it relates to atmospheric circulation. LIBS results revealed detection of peaks for C and N, consistent with the presence of organic material, as well as major ions (Ca, K, Mg, and Na) and trace metals (Al, Cu, Fe, Mn, Ti). The detection of Ca, K, Mg, and Na confirmed that LIBS has sufficient sensitivity to be used as a tool for characterization of paleo-climate proxy indicators in ice-core samples. Techniques were developed for direct analysis of ice as well as indirect measurements of ice via melting and filtering. Pitfalls and issues of direct ice analysis using several cooling techniques to maintain ice integrity will be discussed. In addition, a new technique, laser ablation molecular isotopic spectroscopy (LAMIS) was applied to detection of hydrogen and oxygen isotopes in ice as isotopic analysis of ice is the main tool in paleoclimatology and glaciology studies. Our results demonstrated that spectra of hydroxyl isotopologues 16OH, 18OH, and 16OD can be recorded with a compact spectrograph to determine hydrogen and oxygen isotopes simultaneously. Quantitative isotopic calibration for ice analysis can be accomplished using multivariate chemometric regression as previously realized for water vapor. Analysis with LIBS and LAMIS required no special sample preparation and was about ten times faster than analysis using ICP-MS. Combination of the two techniques in one portable instrument for in-field analysis appears possible and would eliminate the logistical and cost issues associated with ice core management.

Characterization of coal fly ash components by laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Ctvrtnickova, Tereza; Mateo, Mari-Paz; Yanez, Armando; Nicolas, Gines

2009-01-01

The high sensitivity of laser-induced breakdown spectroscopy (LIBS) for the detection of most of the fly ash components enables the analysis of these residues produced during the combustion of coal. Fly ash consists of oxides (SiO 2 , Al 2 O 3 , Fe 2 O 3 , CaO...) and unburnt carbon which is the major determinant of combustion efficiency in coal fired boilers. For example, an excessive amount of residual carbon dispersed in the fly ash means a significant loss of energy (Styszko et al., 2004). Standard methods employed for the analysis of fly ash make not possible a control of boiler in real time. LIBS technique can significantly reduce the time of analysis, in some cases even an online detection can be performed. For this reason, some studies have been addressed in order to demonstrate the capability of the laser-induced breakdown spectroscopy technique for the detection of carbon content in high pressure conditions typical of thermal power plants (Noda et al., 2002) and for the monitoring of unburnt carbon for the boiler control in real time (Kurihara et al., 2003). In particular, the content of unburnt carbon is a valuable indicator for the control of fly ash quality and for the boiler combustion. Depending on this unburnt carbon content, fly ash can be disposed as an industrial waste or as a raw material for the production of concrete in the construction sector. In this study, analyses were performed on specimens of various forms of preparation. Pressed pellets were prepared with two different binders. Presented results concern the nature and amount of the binder used to pelletize the powder, and the laser-induced breakdown spectroscopy parameters and procedure required to draw calibration curves of elements from the fly ash. Analysis 'on tape' was performed in order to establish the experimental conditions for the future 'online analysis'.

Determination of Metals Present in Textile Dyes Using Laser-Induced Breakdown Spectroscopy and Cross-Validation Using Inductively Coupled Plasma/Atomic Emission Spectroscopy

Directory of Open Access Journals (Sweden)

K. Rehan

2017-01-01

Full Text Available Laser-induced breakdown spectroscopy (LIBS was used for the quantitative analysis of elements present in textile dyes at ambient pressure via the fundamental mode (1064 nm of a Nd:YAG pulsed laser. Three samples were collected for this purpose. Spectra of textile dyes were acquired using an HR spectrometer (LIBS2000+, Ocean Optics, Inc. having an optical resolution of 0.06 nm in the spectral range of 200 to 720 nm. Toxic metals like Cr, Cu, Fe, Ni, and Zn along with other elements like Al, Mg, Ca, and Na were revealed to exist in the samples. The %-age concentrations of the detected elements were measured by means of standard calibration curve method, intensities of every emission from every species, and calibration-free (CF LIBS approach. Only Sample 3 was found to contain heavy metals like Cr, Cu, and Ni above the prescribed limit. The results using LIBS were found to be in good agreement when compared to outcomes of inductively coupled plasma/atomic emission spectroscopy (ICP/AES.

Evaluation of the Nutritional Changes Caused by Huanglongbing (HLB) to Citrus Plants Using Laser-Induced Breakdown Spectroscopy.

Science.gov (United States)

Ranulfi, Anielle Coelho; Romano, Renan Arnon; Bebeachibuli Magalhães, Aida; Ferreira, Ednaldo José; Ribeiro Villas-Boas, Paulino; Marcondes Bastos Pereira Milori, Débora

2017-07-01

Huanglongbing (HLB) is the most recent and destructive bacterial disease of citrus and has no cure yet. A promising alternative to conventional methods is to use laser-induced breakdown spectroscopy (LIBS), a multi-elemental analytical technique, to identify the nutritional changes provoked by the disease to the citrus leaves and associate the mineral composition profile with its health status. The leaves were collected from adult citrus trees and identified by visual inspection as healthy, HLB-symptomatic, and HLB-asymptomatic. Laser-induced breakdown spectroscopy measurements were done in fresh leaves without sample preparation. Nutritional variations were evaluated using statistical tools, such as Student's t-test and analysis of variance applied to LIBS spectra, and the largest were found for Ca, Mg, and K. Considering the nutritional profile changes, a classifier induced by classification via regression combined with partial least squares regression was built resulting in an accuracy of 73% for distinguishing the three categories of leaves.

Standard Reference Line Combined with One-Point Calibration-Free Laser-Induced Breakdown Spectroscopy (CF-LIBS) to Quantitatively Analyze Stainless and Heat Resistant Steel.

Science.gov (United States)

Fu, Hongbo; Wang, Huadong; Jia, Junwei; Ni, Zhibo; Dong, Fengzhong

2018-01-01

Due to the influence of major elements' self-absorption, scarce observable spectral lines of trace elements, and relative efficiency correction of experimental system, accurate quantitative analysis with calibration-free laser-induced breakdown spectroscopy (CF-LIBS) is in fact not easy. In order to overcome these difficulties, standard reference line (SRL) combined with one-point calibration (OPC) is used to analyze six elements in three stainless-steel and five heat-resistant steel samples. The Stark broadening and Saha - Boltzmann plot of Fe are used to calculate the electron density and the plasma temperature, respectively. In the present work, we tested the original SRL method, the SRL with the OPC method, and intercept with the OPC method. The final calculation results show that the latter two methods can effectively improve the overall accuracy of quantitative analysis and the detection limits of trace elements.

Cluster analysis of polymers using laser-induced breakdown spectroscopy with K-means

Science.gov (United States)

Yangmin, GUO; Yun, TANG; Yu, DU; Shisong, TANG; Lianbo, GUO; Xiangyou, LI; Yongfeng, LU; Xiaoyan, ZENG

2018-06-01

Laser-induced breakdown spectroscopy (LIBS) combined with K-means algorithm was employed to automatically differentiate industrial polymers under atmospheric conditions. The unsupervised learning algorithm K-means were utilized for the clustering of LIBS dataset measured from twenty kinds of industrial polymers. To prevent the interference from metallic elements, three atomic emission lines (C I 247.86 nm , H I 656.3 nm, and O I 777.3 nm) and one molecular line C–N (0, 0) 388.3 nm were used. The cluster analysis results were obtained through an iterative process. The Davies–Bouldin index was employed to determine the initial number of clusters. The average relative standard deviation values of characteristic spectral lines were used as the iterative criterion. With the proposed approach, the classification accuracy for twenty kinds of industrial polymers achieved 99.6%. The results demonstrated that this approach has great potential for industrial polymers recycling by LIBS.

Identification of quantum dots labeled metallothionein by fast scanning laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Konecna, Marie; Novotny, Karel; Krizkova, Sona; Blazkova, Iva; Kopel, Pavel; Kaiser, Jozef; Hodek, Petr; Kizek, Rene

2014-01-01

The technique described in this paper allows detection of quantum dots (QDs) specifically deposited on the polystyrene surface by laser-induced breakdown spectroscopy (LIBS). Using LIBS, the distribution of QDs or their conjugates with biomolecules deposited on the surface can be observed, regardless of the fact if they exhibit fluorescence or not. QDs deposited on the specific surface of polystyrene microplate in the form of spots are detected by determination of the metal included in the QDs structure. Cd-containing QDs (CdS, CdTe) stabilized with mercaptopropionic (MPA) or mercaptosuccinic (MSA) acid, respectively, alone or in the form of conjugates with metallothionein (MT) biomolecule are determined by using the 508.58 nm Cd emission line. The observed absolute detection limit for Cd in CdTe QDs conjugates with MT in one spot was 3 ng Cd. Due to the high sensitivity of this technique, the immunoanalysis in combination with LIBS was also investigated. Cd spatial distribution in sandwich immunoassay was detected. - Highlights: • We describe determination of biomolecules labeled with quantum dots by LIBS. • LIBS and immunoassay are applied for the determination of metallothionein. • Metallothionein amount detected by LIBS is 10-times lower compared to ELISA

Identification of quantum dots labeled metallothionein by fast scanning laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Konecna, Marie [Central European Institute of Technology, Brno University of Technology, Technicka 3058/10, CZ-616 00 Brno (Czech Republic); Department of Chemistry and Biochemistry, Faculty of Agronomy, Mendel University in Brno, Zemedelska 1, CZ-613 00 Brno (Czech Republic); Novotny, Karel [Central European Institute of Technology, Masaryk University, Kamenice 753/5, CZ-625 00 Brno (Czech Republic); Krizkova, Sona [Central European Institute of Technology, Brno University of Technology, Technicka 3058/10, CZ-616 00 Brno (Czech Republic); Department of Chemistry and Biochemistry, Faculty of Agronomy, Mendel University in Brno, Zemedelska 1, CZ-613 00 Brno (Czech Republic); Blazkova, Iva [Department of Chemistry and Biochemistry, Faculty of Agronomy, Mendel University in Brno, Zemedelska 1, CZ-613 00 Brno (Czech Republic); Kopel, Pavel [Central European Institute of Technology, Brno University of Technology, Technicka 3058/10, CZ-616 00 Brno (Czech Republic); Department of Chemistry and Biochemistry, Faculty of Agronomy, Mendel University in Brno, Zemedelska 1, CZ-613 00 Brno (Czech Republic); Kaiser, Jozef [Central European Institute of Technology, Brno University of Technology, Technicka 3058/10, CZ-616 00 Brno (Czech Republic); Institute of Physical Engineering, Brno University of Technology, Technicka 2, CZ-616 69 Brno (Czech Republic); Hodek, Petr [Department of Biochemistry, Faculty of Science, Charles University in Prague, Hlavova 2030/8, CZ-128 00 Prague,Czech Republic (Czech Republic); Kizek, Rene [Central European Institute of Technology, Brno University of Technology, Technicka 3058/10, CZ-616 00 Brno (Czech Republic); Department of Chemistry and Biochemistry, Faculty of Agronomy, Mendel University in Brno, Zemedelska 1, CZ-613 00 Brno (Czech Republic); and others

2014-11-01

The technique described in this paper allows detection of quantum dots (QDs) specifically deposited on the polystyrene surface by laser-induced breakdown spectroscopy (LIBS). Using LIBS, the distribution of QDs or their conjugates with biomolecules deposited on the surface can be observed, regardless of the fact if they exhibit fluorescence or not. QDs deposited on the specific surface of polystyrene microplate in the form of spots are detected by determination of the metal included in the QDs structure. Cd-containing QDs (CdS, CdTe) stabilized with mercaptopropionic (MPA) or mercaptosuccinic (MSA) acid, respectively, alone or in the form of conjugates with metallothionein (MT) biomolecule are determined by using the 508.58 nm Cd emission line. The observed absolute detection limit for Cd in CdTe QDs conjugates with MT in one spot was 3 ng Cd. Due to the high sensitivity of this technique, the immunoanalysis in combination with LIBS was also investigated. Cd spatial distribution in sandwich immunoassay was detected. - Highlights: • We describe determination of biomolecules labeled with quantum dots by LIBS. • LIBS and immunoassay are applied for the determination of metallothionein. • Metallothionein amount detected by LIBS is 10-times lower compared to ELISA.

Dissociation dynamics of CH3I in electric spark induced breakdown revealed by time-resolved laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Wang, Yang; Liu, Wei-long; Song, Yun-fei; Duo, Li-ping; Liu, Yu-qiang; Yang, Yan-qiang

2015-01-01

Highlights: • Emission of electric spark dissociation of CH 3 I is similar to its fs LIBS. • We use fs laser induced breakdown as a simulation for electric spark dissociation. • The I 2 molecule formation is directly observed in the time-resolved LIBS. • Bimolecular collision of I ∗ and CH 3 I is responsible for the formation of I 2 . - Abstract: The electric discharge spark dissociation of gas CH 3 I is found to be similar to its femtosecond laser photodissociation. The almost identical spectra of the two processes show that their initial ionization conditions are very similar. The initial ionization followed by molecular fragmentation is proposed as the dissociation mechanism, in which the characteristic emissions of I + , CH 3 , CH 2 , CH, H, and I 2 are identified as the dissociation products. The emission band of 505 nm I 2 is clearly observed in the time-resolved laser induced breakdown spectroscopy (LIBS). The dynamic curve indicates that I 2 ∗ molecules are formed after the delay time of ∼4.7 ns. The formation of I 2 ∗ molecule results from the bimolecular collision of the highly excited iodine atom I ∗ ( 4 P) and CH 3 I molecule. This dynamical information can help understand the process of electric discharge spark dissociation of CH 3 I

The effect of nutrient media water purity on LIBS based identification of bacteria

Science.gov (United States)

Single pulse laser induced breakdown spectroscopy (LIBS) is used as the basis for discrimination between 3 genera of Gram-negative bacteria and 2 genera of gram-positive bacteria representing pathogenic threats commonly found in poultry processing rinse waters. Because LIBS-based discrimination reli...

Laser-induced breakdown spectroscopy for lambda quantification in a direct-injection engine

International Nuclear Information System (INIS)

Buschbeck, M.; Büchler, F.; Halfmann, T.; Arndt, S.

2012-01-01

We apply laser-induced breakdown spectroscopy (LIBS) to determine local lambda values (i.e. the normalized air-fuel mass ratio) at the ignition location λ ip in a direct-injection single-cylinder optical research engine. The technique enables us to determine variations of λ ip for different fuel injection strategies, as well as correlations between variations in λ ip and the combustion dynamics. In particular we observe, that fluctuations in λ ip are not the major cause of cycle-to-cycle variations in the combustion process. Moreover, our experiments identify insufficient lean λ ip values as a source of misfires in lean combustions. In a combination of LIBS with laser-induced fluorescence (LIF), we obtain additionally information about the two-dimensional λ distribution. These results demonstrate the potential of LIBS to monitor λ values during mixture formation in gasoline engines. - Highlights: ► Determination of λ values by means of LIBS in an optical gasoline engine. ► Evaluation of λ fluctuations for different fuel injection strategies. ► Investigation of the effect of λ upon combustion dynamics. ► Combination of LIBS and LIF to obtain two-dimensional λ distributions.

A review of the development of portable laser induced breakdown spectroscopy and its applications

Energy Technology Data Exchange (ETDEWEB)

Rakovský, J., E-mail: jozef.rakovsky@jh-inst.cas.cz [J. Heyrovský Institute of Physical Chemistry, Academy of Sciences of the Czech Republic, Dolejškova 3, 18223 Prague 8 (Czech Republic); Čermák, P. [Department of Experimental Physics, Faculty of Mathematics, Physics and Informatics, Comenius University, Mlynská dolina F2, 842 48 Bratislava (Slovakia); Musset, O. [Laboratoire interdisciplinaire Carnot de Bourgogne, UMR CNRS 6303, Université de Bourgogne, BP 47 870, F-21078 Dijon Cedex (France); Veis, P. [Department of Experimental Physics, Faculty of Mathematics, Physics and Informatics, Comenius University, Mlynská dolina F2, 842 48 Bratislava (Slovakia)

2014-11-01

In this review, we present person-transportable laser induced breakdown spectroscopy (LIBS) devices that have previously been developed and reported in the literature as well as their applications. They are compared with X-ray fluorescent (XRF) devices, which represent their strongest competition. Although LIBS devices have advantages over XRF devices, such as sensitivity to the light elements, high spatial resolution and the possibility to distinguish between different layers of the sample, there are also disadvantages and both are discussed here. Furthermore, the essential portable LIBS instrumentation (laser, spectrograph and detector) is presented, and published results related to new laser sources (diode-pumped solid-state, microchip and fiber lasers) used in LIBS are overviewed. Compared to conventional compact flashlamp pumped solid-state lasers, the new laser sources provide higher repetition rates, higher efficiency (less power consumption) and higher beam quality, resulting in higher fluences, even for lower energies, and could potentially increase the figure of merit of portable LIBS instruments. Compact spectrometers used in portable LIBS devices and their parts (spectrograph, detector) are also discussed. - Highlights: • Overview of portable LIBS devices transportable by a person • Discussion and new trends about portable LIBS instrumentation: laser, spectrograph and detector • Overview of applications of DPSS, microchip and fiber lasers in LIBS.

Remote in-situ laser-induced breakdown spectroscopy using optical fibers

Science.gov (United States)

Marquardt, Brian James

The following dissertation describes the development of methods for performing remote Laser-Induced Breakdown Spectroscopy (LIBS) using optical fibers. Studies were performed to determine the optimal excitation and collection parameters for remote LIBS measurements of glasses, soils and paint. A number of fiber-optic LIBS probes were developed and used to characterize various samples by plasma emission spectroscopy. A novel method for launching high-power laser pulses into optical fibers without causing catastrophic failure is introduced. A systematic study of a number of commercially available optical fibers was performed to determine which optical fibers were best suited for delivering high-power laser pulses. The general design of an all fiber-optic LIBS probe is described and applied to the determination of Pb in soil. A fiber-optic probe was developed for the microanalysis of solid samples remotely by LIBS, Raman spectroscopy and Raman imaging. The design of the probe allows for real-time sample imaging in-situ using coherent imaging fibers. This allows for precise atomic emission and Raman measurements to be performed remotely on samples in hostile or inaccessible environments. A novel technique was developed for collecting spectral plasma images using an acousto-optic tunable filter (AOTF). The spatial and temporal characteristics of the plasma were studied as a function of delay time. From the plasma images the distribution of Pb emission could be determined and fiber-optic designs could be optimized for signal collection. The performance of a two fiber LIBS probe is demonstrated for the determination of the amount of lead in samples of dry paint. It is shown that dry paint samples can be analyzed for their Pb content in-situ using a fiber-optic LIBS probe with detection limits well below the levels currently regulated by the Consumer Products Safety Commission. It is also shown that these measurements can be performed on both latex and enamel paints, and

Comparison of the Detection Characteristics of Trace Species Using Laser-Induced Breakdown Spectroscopy and Laser Breakdown Time-of-Flight Mass Spectrometry

Directory of Open Access Journals (Sweden)

Zhenzhen Wang

2015-03-01

Full Text Available The rapid and precise element measurement of trace species, such as mercury, iodine, strontium, cesium, etc. is imperative for various applications, especially for industrial needs. The elements mercury and iodine were measured by two detection methods for comparison of the corresponding detection features. A laser beam was focused to induce plasma. Emission and ion signals were detected using laser-induced breakdown spectroscopy (LIBS and laser breakdown time-of-flight mass spectrometry (LB-TOFMS. Multi-photon ionization and electron impact ionization in the plasma generation process can be controlled by the pressure and pulse width. The effect of electron impact ionization on continuum emission, coexisting molecular and atomic emissions became weakened in low pressure condition. When the pressure was less than 1 Pa, the plasma was induced by laser dissociation and multi-photon ionization in LB-TOFMS. According to the experimental results, the detection limits of mercury and iodine in N2 were 3.5 ppb and 60 ppb using low pressure LIBS. The mercury and iodine detection limits using LB-TOFMS were 1.2 ppb and 9.0 ppb, which were enhanced due to different detection features. The detection systems of LIBS and LB-TOFMS can be selected depending on the condition of each application.

The influence of laser-particle interaction in laser induced breakdown spectroscopy and laser ablation inductively coupled plasma spectrometry

International Nuclear Information System (INIS)

Lindner, Helmut; Loper, Kristofer H.; Hahn, David W.; Niemax, Kay

2011-01-01

Particles produced by previous laser shots may have significant influence on the analytical signal in laser-induced breakdown spectroscopy (LIBS) and laser ablation inductively coupled plasma (LA-ICP) spectrometry if they remain close to the position of laser sampling. The effects of these particles on the laser-induced breakdown event are demonstrated in several ways. LIBS-experiments were conducted in an ablation cell at atmospheric conditions in argon or air applying a dual-pulse arrangement with orthogonal pre-pulse, i.e., plasma breakdown in a gas generated by a focussed laser beam parallel and close to the sample surface followed by a delayed crossing laser pulse in orthogonal direction which actually ablates material from the sample and produces the LIBS plasma. The optical emission of the LIBS plasma as well as the absorption of the pre-pulse laser was measured. In the presence of particles in the focus of the pre-pulse laser, the plasma breakdown is affected and more energy of the pre-pulse laser is absorbed than without particles. As a result, the analyte line emission from the LIBS plasma of the second laser is enhanced. It is assumed that the enhancement is not only due to an increase of mass ablated by the second laser but also to better atomization and excitation conditions favored by a reduced gas density in the pre-pulse plasma. Higher laser pulse frequencies increase the probability of particle-laser interaction and, therefore, reduce the shot-to-shot line intensity variation as compared to lower particle loadings in the cell. Additional experiments using an aerosol chamber were performed to further quantify the laser absorption by the plasma in dependence on time both with and without the presence of particles. The overall implication of laser-particle interactions for LIBS and LA-ICP-MS/OES are discussed.

The influence of laser-particle interaction in laser induced breakdown spectroscopy and laser ablation inductively coupled plasma spectrometry

Science.gov (United States)

Lindner, Helmut; Loper, Kristofer H.; Hahn, David W.; Niemax, Kay

2011-02-01

Particles produced by previous laser shots may have significant influence on the analytical signal in laser-induced breakdown spectroscopy (LIBS) and laser ablation inductively coupled plasma (LA-ICP) spectrometry if they remain close to the position of laser sampling. The effects of these particles on the laser-induced breakdown event are demonstrated in several ways. LIBS-experiments were conducted in an ablation cell at atmospheric conditions in argon or air applying a dual-pulse arrangement with orthogonal pre-pulse, i.e., plasma breakdown in a gas generated by a focussed laser beam parallel and close to the sample surface followed by a delayed crossing laser pulse in orthogonal direction which actually ablates material from the sample and produces the LIBS plasma. The optical emission of the LIBS plasma as well as the absorption of the pre-pulse laser was measured. In the presence of particles in the focus of the pre-pulse laser, the plasma breakdown is affected and more energy of the pre-pulse laser is absorbed than without particles. As a result, the analyte line emission from the LIBS plasma of the second laser is enhanced. It is assumed that the enhancement is not only due to an increase of mass ablated by the second laser but also to better atomization and excitation conditions favored by a reduced gas density in the pre-pulse plasma. Higher laser pulse frequencies increase the probability of particle-laser interaction and, therefore, reduce the shot-to-shot line intensity variation as compared to lower particle loadings in the cell. Additional experiments using an aerosol chamber were performed to further quantify the laser absorption by the plasma in dependence on time both with and without the presence of particles. The overall implication of laser-particle interactions for LIBS and LA-ICP-MS/OES are discussed.

Use of laser induced breakdown spectroscopy in the determination of gem provenance: beryls

International Nuclear Information System (INIS)

McManus, Catherine E.; McMillan, Nancy J.; Harmon, Russell S.; Whitmore, Robert C.; De Lucia, Frank C. Jr.; Miziolek, Andrzej W.

2008-01-01

The provenance of gem stones has been of interest to geologists, gemologists, archeologists, and historians for centuries. Laser induced breakdown spectroscopy (LIBS) provides a minimally destructive tool for recording the rich chemical signatures of gem beryls (aquamarine, goshenite, heliodor, and morganite). Broadband LIBS spectra of 39 beryl (Be3Al2Si6O18) specimens from 11 pegmatite mines in New Hampshire, Connecticut, and Maine (USA) are used to assess the potential of using principal component analysis of LIBS spectra to determine specimen provenance. Using this technique, beryls from the three beryl-bearing zones in the Palermo no. 1 pegmatite (New Hampshire) can be recognized. However, the compositional variation within this single mine is comparable to that in beryls from all three states. Thus, a very large database with detailed location metadata will be required to routinely determine gem beryl provenance

High-resolution three-dimensional compositional imaging by double-pulse laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Schiavo, C.; Grifoni, E.; Legnaioli, S.; Lorenzetti, G.; Poggialini, F.; Pagnotta, S.; Palleschi, V.; Menichetti, L.

2016-01-01

In this paper we present a new instrument specifically realized for high-resolution three-dimensional compositional analysis and mapping of materials. The instrument is based on the coupling of a Double-Pulse Laser-Induced Breakdown Spectroscopy (LIBS) instrument with an optical microscope. The compositional mapping of the samples is obtained by scanning the laser beam across the surface of the sample, while the in depth analysis is performed by sending multiple laser pulses on the same point. Depths of analysis of several tens of microns can be obtained. The instrument presented has definite advantages with respect to Laser Ablation-ICP Mass Spectrometry in many applications related to material analysis, biomedicine and environmental diagnostics. An application to the diagnostics of industrial ceramics is presented, demonstrating the feasibility of Double-Pulse LIBS Imaging and its advantages with respect to conventional single-pulse LIBS imaging.

Analytical Methods to Distinguish the Positive and Negative Spectra of Mineral and Environmental Elements Using Deep Ablation Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Kim, Dongyoung; Yang, Jun-Ho; Choi, Soojin; Yoh, Jack J

2018-01-01

Environments affect mineral surfaces, and the surface contamination or alteration can provide potential information to understanding their regional environments. However, when investigating mineral surfaces, mineral and environmental elements appear mixed in data. This makes it difficult to determine their atomic compositions independently. In this research, we developed four analytical methods to distinguish mineral and environmental elements into positive and negative spectra based on depth profiling data using laser-induced breakdown spectroscopy (LIBS). The principle of the methods is to utilize how intensity varied with depth for creating a new spectrum. The methods were applied to five mineral samples exposed to four environmental conditions including seawater, crude oil, sulfuric acid, and air as control. The proposed methods are then validated by applying the resultant spectra to principal component analysis and data were classified by the environmental conditions and atomic compositions of mineral. By applying the methods, the atomic information of minerals and environmental conditions were successfully inferred in the resultant spectrum.

Evaluation of laser induced breakdown spectroscopy for the determination of macronutrients in plant materials

Energy Technology Data Exchange (ETDEWEB)

Trevizan, Lilian Cristina [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario 303, 13416-000, Piracicaba-SP (Brazil)], E-mail: lilian@conectcor.com.br; Santos, Dario [Universidade Federal de Sao Paulo - UNIFESP, Rua Prof. Artur Riedel 275, 09972-270, Diadema-SP (Brazil); Elgul Samad, Ricardo; Dias Vieira, Nilson [Centro de Lasers e Aplicacoes, IPEN/CNEN-SP, Av. Prof. Lineu Prestes 2242, 05508-000, Sao Paulo-SP (Brazil); Seimi Nomura, Cassiana [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia 166, 09210-170, Santo Andre-SP (Brazil); Nunes, Lidiane Cristina [Departamento de Quimica, Universidade Federal de Sao Carlos, Rod. Washington Luis, km 235, 13565-905, Sao Carlos-SP (Brazil); Rufini, Iolanda Aparecida; Krug, Francisco Jose [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario 303, 13416-000, Piracicaba-SP (Brazil)

2008-10-15

Laser induced breakdown spectroscopy (LIBS) has become an analytical tool for the direct analysis of a large variety of materials in order to provide qualitative and/or quantitative information. However, there is a lack of information for LIBS analysis of agricultural and environmental samples. In this work a LIBS system has been evaluated for the determination of macronutrients (P, K, Ca, Mg) in pellets of vegetal reference materials. An experimental setup was designed by using a Nd:YAG laser operating at 1064 nm and an Echelle spectrometer with ICCD detector. The plasma temperature was estimated by Boltzmann plots and instrumental parameters such as delay time, lens-to-sample distance and pulse energy were evaluated. Certified reference materials as well as reference materials were used for analytical calibrations of P, K, Ca, and Mg. Most results of the direct analysis of plant samples by LIBS were in reasonable agreement with those obtained by ICP OES after wet acid decomposition.

Evaluation of laser induced breakdown spectroscopy for the determination of macronutrients in plant materials

International Nuclear Information System (INIS)

Trevizan, Lilian Cristina; Santos, Dario; Elgul Samad, Ricardo; Dias Vieira, Nilson; Seimi Nomura, Cassiana; Nunes, Lidiane Cristina; Rufini, Iolanda Aparecida; Krug, Francisco Jose

2008-01-01

Laser induced breakdown spectroscopy (LIBS) has become an analytical tool for the direct analysis of a large variety of materials in order to provide qualitative and/or quantitative information. However, there is a lack of information for LIBS analysis of agricultural and environmental samples. In this work a LIBS system has been evaluated for the determination of macronutrients (P, K, Ca, Mg) in pellets of vegetal reference materials. An experimental setup was designed by using a Nd:YAG laser operating at 1064 nm and an Echelle spectrometer with ICCD detector. The plasma temperature was estimated by Boltzmann plots and instrumental parameters such as delay time, lens-to-sample distance and pulse energy were evaluated. Certified reference materials as well as reference materials were used for analytical calibrations of P, K, Ca, and Mg. Most results of the direct analysis of plant samples by LIBS were in reasonable agreement with those obtained by ICP OES after wet acid decomposition

Analysis of human nails by laser-induced breakdown spectroscopy

Science.gov (United States)

Hosseinimakarem, Zahra; Tavassoli, Seyed Hassan

2011-05-01

Laser-induced breakdown spectroscopy (LIBS) is applied to analyze human fingernails using nanosecond laser pulses. Measurements on 45 nail samples are carried out and 14 key species are identified. The elements detected with the present system are: Al, C, Ca, Fe, H, K, Mg, N, Na, O, Si, Sr, Ti as well as CN molecule. Sixty three emission lines have been identified in the spectrum that are dominated by calcium lines. A discriminant function analysis is used to discriminate among different genders and age groups. This analysis demonstrates efficient discrimination among these groups. The mean concentration of each element is compared between different groups. Correlation between concentrations of elements in fingernails is calculated. A strong correlation is found between sodium and potassium while calcium and magnesium levels are inversely correlated. A case report on high levels of sodium and potassium in patients with hyperthyroidism is presented. It is shown that LIBS could be a promising technique for the analysis of nails and therefore identification of health problems.

Calibration-Free Laser-Induced Breakdown Spectroscopy (CF-LIBS) with Standard Reference Line for the Analysis of Stainless Steel.

Science.gov (United States)

Fu, Hongbo; Dong, Fengzhong; Wang, Huadong; Jia, Junwei; Ni, Zhibo

2017-08-01

In this work, calibration-free laser-induced breakdown spectroscopy (CF-LIBS) is used to analyze a certified stainless steel sample. Due to self-absorption of the spectral lines from the major element Fe and the sparse lines of trace elements, it is usually not easy to construct the Boltzmann plots of all species. A standard reference line method is proposed here to solve this difficulty under the assumption of local thermodynamic equilibrium so that the same temperature value for all elements present into the plasma can be considered. Based on the concentration and rich spectral lines of Fe, the Stark broadening of Fe(I) 381.584 nm and Saha-Boltzmann plots of this element are used to calculate the electron density and the plasma temperature, respectively. In order to determine the plasma temperature accurately, which is seriously affected by self-absorption, a pre-selection procedure for eliminating those spectral lines with strong self-absorption is employed. Then, one spectral line of each element is selected to calculate its corresponding concentration. The results from the standard reference lines with and without self-absorption of Fe are compared. This method allows us to measure trace element content and effectively avoid the adverse effects due to self-absorption.

Calibration strategies for the direct determination of Ca, K, and Mg in commercial samples of powdered milk and solid dietary supplements using laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Dos Santos Augusto, Amanda; Barsanelli, Paulo Lopes; Pereira, Fabiola Manhas Verbi; Pereira-Filho, Edenir Rodrigues

2017-04-01

This study describes the application of laser-induced breakdown spectroscopy (LIBS) for the direct determination of Ca, K and Mg in powdered milk and solid dietary supplements. The following two calibration strategies were applied: (i) use of the samples to calculate calibration models (milk) and (ii) use of sample mixtures (supplements) to obtain a calibration curve. In both cases, reference values obtained from inductively coupled plasma optical emission spectroscopy (ICP OES) after acid digestion were used. The emission line selection from LIBS spectra was accomplished by analysing the regression coefficients of partial least squares (PLS) regression models, and wavelengths of 534.947, 766.490 and 285.213nm were chosen for Ca, K and Mg, respectively. In the case of the determination of Ca in supplements, it was necessary to perform a dilution (10-fold) of the standards and samples to minimize matrix interference. The average accuracy for powdered milk ranged from 60% to 168% for Ca, 77% to 152% for K and 76% to 131% for Mg. In the case of dietary supplements, standard error of prediction (SEP) varied from 295 (Mg) to 3782mgkg -1 (Ca). The proposed method presented an analytical frequency of around 60 samples per hour and the step of sample manipulation was drastically reduced, with no generation of toxic chemical residues. Copyright © 2017 Elsevier Ltd. All rights reserved.

ERDA Paper: Quantitative Measurement of Chromium, Manganese, Rhenium, and Magnesium in Liquid by Laser-Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Keller, E.L.

2000-01-01

A technique is needed to measure Tc during the waste process at DOE Hanford site. Laser induced breakdown spectroscopy (LIBS), a laser-based, non-intrusive, and sensitive optical diagnostic technique for measuring the concentration of various atomic and molecular species in test media, has the potential to be an on-line monitor to monitor Tc in the effluent from the Tc removal column to track the technetium removal process. In this work, we evaluate the analytical figure of merit of LIBS system for the element that has similar properties to Tc

Study on the effect of beam propagation through atmospheric turbulence on standoff nanosecond laser induced breakdown spectroscopy measurements.

Science.gov (United States)

Laserna, J J; Reyes, R Fernández; González, R; Tobaria, L; Lucena, P

2009-06-08

We report on an experimental study of the effect of atmospheric turbulence on laser induced breakdown spectroscopy (LIBS) measurements. The characteristics of the atmosphere dictate specific performance constraints to this technology. Unlike classical laboratory LIBS systems where the distance to the sample is well known and characterized, LIBS systems working at several tens of meters to the target have specific atmospheric propagation conditions that cause the quality of the LIBS signals to be affected to a significant extent. Using a new LIBS based sensor system fitted with a nanosecond laser emitting at 1064 nm, propagation effects at distances of up to 120 m were investigated. The effects observed include wander and scintillation in the outgoing laser beam and in the return atomic emission signal. Plasmas were formed on aluminium targets. Average signal levels and signal fluctuations are measured so the effect of atmospheric turbulence on LIBS measurements is quantified.

Time-Resolved Spectroscopy Diagnostic of Laser-Induced Optical Breakdown

Directory of Open Access Journals (Sweden)

Christian G. Parigger

2010-01-01

Full Text Available Transient laser plasma is generated in laser-induced optical breakdown (LIOB. Here we report experiments conducted with 10.6-micron CO2 laser radiation, and with 1.064-micron fundamental, 0.532-micron frequency-doubled, 0.355-micron frequency-tripled Nd:YAG laser radiation. Characterization of laser induced plasma utilizes laser-induced breakdown spectroscopy (LIBS techniques. Atomic hydrogen Balmer series emissions show electron number density of 1017 cm−3 measured approximately 10 μs and 1 μs after optical breakdown for CO2 and Nd:YAG laser radiation, respectively. Recorded molecular recombination emission spectra of CN and C2 Swan bands indicate an equilibrium temperature in excess of 7000 Kelvin, inferred for these diatomic molecules. Reported are also graphite ablation experiments where we use unfocused laser radiation that is favorable for observation of neutral C3 emission due to reduced C3 cation formation. Our analysis is based on computation of diatomic molecular spectra that includes accurate determination of rotational line strengths, or Hönl-London factors.

Combined raman spectrometer/laser-induced breakdown spectrometer design concept

Science.gov (United States)

Bazalgette Courrèges-Lacoste, Gregory; Ahlers, Berit; Boslooper, Erik; Rull-Perez, Fernando; Maurice, Sylvestre

2017-11-01

Amongst the different instruments that have been preselected to be on-board the Pasteur payload on ExoMars is the Raman/ Laser Induced Breakdown Spectroscopy (LIBS) instrument. Raman spectroscopy and LIBS will be integrated into a single instrument sharing many hardware commonalities. An international team under the lead of TNO has been gathered to produce a design concept for a combined Raman Spectrometer/ LIBS Elegant Bread-Board (EBB). The instrument is based on a specifically designed extremely compact spectrometer with high resolution over a large wavelength range, suitable for both Raman spectroscopy and LIBS measurements. Low mass, size and resources are the main drivers of the instrument's design concept. The proposed design concept, realization and testing programme for the combined Raman/ LIBS EBB is presented as well as background information on Raman and LIBS.

Spectroscopic detection of health hazardous contaminants in lipstick using Laser Induced Breakdown Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Gondal, M.A., E-mail: magondal@kfupm.edu.sa [Physics Department and Center of Excellence in Nanotechnology, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Seddigi, Z.S. [Chemistry Department, Umm Al-Qura University, Makkah (Saudi Arabia); Nasr, M.M. [Natural Science Departments, Riyadh College of Dentistry and Pharmacy, P.O. Box 321815, Riyadh 11343 (Saudi Arabia); Gondal, B. [Plastic and Reconstructive Aesthetic Surgery, Whitfield Hospital, Waterford (Ireland)

2010-03-15

Laser Induced Breakdown Spectroscopy (LIBS) technique was applied to determine the concentrations of different toxic elements like lead, chromium, cadmium and zinc in four different lipstick brands sold at local markets in Saudi Arabia. These samples contain toxic elements like lead, cadmium and chromium which are carcinogen dermatitis, allergic and eczematous. Their extraction from human body takes over 40 years and accumulation in the body cause problems like disruption of nervous systems and kidney damage. They could trigger to systemic lupus erythematosus (SLE). In order to test the validity of our LIBS results, standard technique like (ICP-AES) was also applied. To the best of our knowledge, this is the first study where LIBS technique was applied for the measurement of toxic substances in lipsticks. The maximum concentration detected in four lipstick brands was much higher than the permissible safe limits for human use and could lead to serious health problems. It is worth mentioning that the lipstick is not a solid rather is in fluid state which is not trivial to analyze using LIBS technique. For this purpose, special treatment of the lipstick samples was necessary to analyze with our LIBS method.

Spectroscopic detection of health hazardous contaminants in lipstick using Laser Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Gondal, M.A.; Seddigi, Z.S.; Nasr, M.M.; Gondal, B.

2010-01-01

Laser Induced Breakdown Spectroscopy (LIBS) technique was applied to determine the concentrations of different toxic elements like lead, chromium, cadmium and zinc in four different lipstick brands sold at local markets in Saudi Arabia. These samples contain toxic elements like lead, cadmium and chromium which are carcinogen dermatitis, allergic and eczematous. Their extraction from human body takes over 40 years and accumulation in the body cause problems like disruption of nervous systems and kidney damage. They could trigger to systemic lupus erythematosus (SLE). In order to test the validity of our LIBS results, standard technique like (ICP-AES) was also applied. To the best of our knowledge, this is the first study where LIBS technique was applied for the measurement of toxic substances in lipsticks. The maximum concentration detected in four lipstick brands was much higher than the permissible safe limits for human use and could lead to serious health problems. It is worth mentioning that the lipstick is not a solid rather is in fluid state which is not trivial to analyze using LIBS technique. For this purpose, special treatment of the lipstick samples was necessary to analyze with our LIBS method.

Identification of vapor-phase chemical warfare agent simulants and rocket fuels using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Stearns, Jaime A.; McElman, Sarah E.; Dodd, James A.

2010-01-01

Application of laser-induced breakdown spectroscopy (LIBS) to the identification of security threats is a growing area of research. This work presents LIBS spectra of vapor-phase chemical warfare agent simulants and typical rocket fuels. A large dataset of spectra was acquired using a variety of gas mixtures and background pressures and processed using partial least squares analysis. The five compounds studied were identified with a 99% success rate by the best method. The temporal behavior of the emission lines as a function of chamber pressure and gas mixture was also investigated, revealing some interesting trends that merit further study.

Identification of vapor-phase chemical warfare agent simulants and rocket fuels using laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Stearns, Jaime A.; McElman, Sarah E.; Dodd, James A.

2010-05-01

Application of laser-induced breakdown spectroscopy (LIBS) to the identification of security threats is a growing area of research. This work presents LIBS spectra of vapor-phase chemical warfare agent simulants and typical rocket fuels. A large dataset of spectra was acquired using a variety of gas mixtures and background pressures and processed using partial least squares analysis. The five compounds studied were identified with a 99% success rate by the best method. The temporal behavior of the emission lines as a function of chamber pressure and gas mixture was also investigated, revealing some interesting trends that merit further study.

Applications of laser-induced breakdown spectroscopy in the aluminum electrolysis industry

Science.gov (United States)

Sun, Lanxiang; Yu, Haibin; Cong, Zhibo; Lu, Hui; Cao, Bin; Zeng, Peng; Dong, Wei; Li, Yang

2018-04-01

The industrial aluminum reduction cell is an electrochemistry reactor that operates under high temperatures and corrosive conditions. Monitoring the molten aluminum and electrolyte components is very important for controlling the chemical reaction process. Due to the lack of fast methods to monitor the components, controlling aluminum reduction cells is difficult. In this work, laser-induced breakdown spectroscopy (LIBS) was applied to aluminum electrolysis. A new method for calculating the molecular ratio, which is an important control parameter that represents the acidity of the electrolyte, was proposed. Experiments were first performed on solid electrolyte samples to test the performance of the proposed method. Using this method, the average relative standard deviation (RSD) of the molecular ratio measurement was 0.39%, and the average root mean square error (RMSE) was 0.0236. These results prove that LIBS can accurately measure the molecular ratio. Then, in situ measurements of the molten aluminum and electrolyte were performed in industrial aluminum induction cells using the developed LIBS equipment. The spectra of the molten electrolyte were successfully obtained and were consistent with the spectra of the solid electrolyte.

Time-resolved ultraviolet laser-induced breakdown spectroscopy for organic material analysis

Energy Technology Data Exchange (ETDEWEB)

Baudelet, Matthieu; Boueri, Myriam [Laboratoire de Spectrometrie Ionique et Moleculaire, Universite Claude Bernard Lyon 1, UMR CNRS 5579, 43, Bd. du 11 Novembre 1918, F-69622 Villeurbanne Cedex (France); Yu Jin [Laboratoire de Spectrometrie Ionique et Moleculaire, Universite Claude Bernard Lyon 1, UMR CNRS 5579, 43, Bd. du 11 Novembre 1918, F-69622 Villeurbanne Cedex (France)], E-mail: jin.yu@lasim.univ-lyon1.fr; Mao, Samuel S; Piscitelli, Vincent; Xianglei, Mao; Russo, Richard E [Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States)

2007-12-15

Ultraviolet pulses (266 nm) delivered by a quadrupled Nd:YAG laser were used to analyze organic samples with laser-induced breakdown spectroscopy (LIBS). We present characteristics of the spectra obtained from organic samples with special attentions on the emissions of organic elements, O and N, and molecular bonds CN. The choice of these atomic or molecular species is justified on one hand, by the importance of these species to specify organic or biological materials; and on the other hand by the possible interferences with ambient air when laser ablation takes place in the atmosphere. Time-resolved LIBS was used to determine the time-evolution of line intensity emitted from these species. We demonstrate different kinetic behaviors corresponding to different origins of emitters: native atomic or molecular species directly vaporized from the sample or those generated through dissociation or recombination due to interaction between laser-induced plasma and air molecules. Our results show the ability of time-resolved UV-LIBS for detection and identification of native atomic or molecular species from an organic sample.

Dehydrated Carbon Coupled with Laser-Induced Breakdown Spectrometry (LIBS) for the Determination of Heavy Metals in Solutions.

Science.gov (United States)

Niu, Guanghui; Shi, Qi; Xu, Mingjun; Lai, Hongjun; Lin, Qingyu; Liu, Kunping; Duan, Yixiang

2015-10-01

In this article, a novel and alternative method of laser-induced breakdown spectroscopy (LIBS) analysis for liquid sample is proposed, which involves the removal of metal ions from a liquid to a solid substrate using a cost-efficient adsorbent, dehydrated carbon, obtained using a dehydration reaction. Using this new technique, researchers can detect trace metal ions in solutions qualitatively and quantitatively, and the drawbacks of performing liquid analysis using LIBS can be avoided because the analysis is performed on a solid surface. To achieve better performance using this technique, we considered parameters potentially influencing both adsorption performance and LIBS analysis. The calibration curves were evaluated, and the limits of detection obtained for Cu(2+), Pb(2+), and Cr(3+) were 0.77, 0.065, and 0.46 mg/L, respectively, which are better than those in the previous studies. In addition, compared to other absorbents, the adsorbent used in this technique is much cheaper in cost, easier to obtain, and has fewer or no other elements other than C, H, and O that could result in spectral interference during analysis. We also used the recommended method to analyze spiked samples, obtaining satisfactory results. Thus, this new technique is helpful and promising for use in wastewater analysis and management.

Comparative measurements of mineral elements in milk powders with laser-induced breakdown spectroscopy and inductively coupled plasma atomic emission spectroscopy.

Science.gov (United States)

Lei, W Q; El Haddad, J; Motto-Ros, V; Gilon-Delepine, N; Stankova, A; Ma, Q L; Bai, X S; Zheng, L J; Zeng, H P; Yu, J

2011-07-01

Mineral elements contained in commercially available milk powders, including seven infant formulae and one adult milk, were analyzed with inductively coupled plasma atomic emission spectrometry (ICP-AES) and laser-induced breakdown spectroscopy (LIBS). The purpose of this work was, through a direct comparison of the analytical results, to provide an assessment of the performance of LIBS, and especially of the procedure of calibration-free LIBS (CF-LIBS), to deal with organic compounds such as milk powders. In our experiments, the matrix effect was clearly observed affecting the analytical results each time laser ablation was employed for sampling. Such effect was in addition directly observed by determining the physical parameters of the plasmas induced on the different samples. The CF-LIBS procedure was implemented to deduce the concentrations of Mg and K with Ca as the internal reference element. Quantitative analytical results with CF-LIBS were validated with ICP-AES measurements and nominal concentrations specified for commercial milks. The obtained good results with the CF-LIBS procedure demonstrate its capacity to take into account the difference in physical parameters of the plasma in the calculation of the concentrations of mineral elements, which allows a significant reduction of the matrix effect related to laser ablation. We finally discuss the way to optimize the implementation of the CF-LIBS procedure for the analysis of mineral elements in organic materials.

An artificial neural network approach to laser-induced breakdown spectroscopy quantitative analysis

International Nuclear Information System (INIS)

D’Andrea, Eleonora; Pagnotta, Stefano; Grifoni, Emanuela; Lorenzetti, Giulia; Legnaioli, Stefano; Palleschi, Vincenzo; Lazzerini, Beatrice

2014-01-01

The usual approach to laser-induced breakdown spectroscopy (LIBS) quantitative analysis is based on the use of calibration curves, suitably built using appropriate reference standards. More recently, statistical methods relying on the principles of artificial neural networks (ANN) are increasingly used. However, ANN analysis is often used as a ‘black box’ system and the peculiarities of the LIBS spectra are not exploited fully. An a priori exploration of the raw data contained in the LIBS spectra, carried out by a neural network to learn what are the significant areas of the spectrum to be used for a subsequent neural network delegated to the calibration, is able to throw light upon important information initially unknown, although already contained within the spectrum. This communication will demonstrate that an approach based on neural networks specially taylored for dealing with LIBS spectra would provide a viable, fast and robust method for LIBS quantitative analysis. This would allow the use of a relatively limited number of reference samples for the training of the network, with respect to the current approaches, and provide a fully automatizable approach for the analysis of a large number of samples. - Highlights: • A methodological approach to neural network analysis of LIBS spectra is proposed. • The architecture of the network and the number of inputs are optimized. • The method is tested on bronze samples already analyzed using a calibration-free LIBS approach. • The results are validated, compared and discussed

Quantitative mixture fraction measurements in combustion system via laser induced breakdown spectroscopy

KAUST Repository

Mansour, Mohy S.

2015-01-01

Laser induced breakdown spectroscopy (LIBS) technique has been applied to quantitative mixture fraction measurements in flames. The measured spectra of different mixtures of natural gas and air are used to obtain the calibration parameters for local elemental mass fraction measurements and hence calculate the mixture fraction. The results are compared with the mixture fraction calculations based on the ratios of the spectral lines of H/N elements, H/O elements and C/(N+O) and they show good agreement within the reaction zone of the flames. Some deviations are observed outside the reaction zone. The ability of LIBS technique as a tool for quantitative mixture fraction as well as elemental fraction measurements in reacting and non-reacting of turbulent flames is feasible. © 2014 Elsevier Ltd. All rights reserved.

Potential of Laser Induced Breakdown Spectroscopy for analyzing the quality of unroasted and ground coffee

Science.gov (United States)

Silva, Tiago Varão; Hubinger, Silviane Zanni; Gomes Neto, José Anchieta; Milori, Débora Marcondes Bastos Pereira; Ferreira, Ednaldo José; Ferreira, Edilene Cristina

2017-09-01

Coffee is an important commodity and a very popular beverage around the world. Its economic value as well as beverage quality are strongly dependent of the quality of beans. The presence of defective beans in coffee blends has caused a negative impact on the beverage Global Quality (GQ) assessed by cupping tests. The main defective beans observed in the productive chain has been those Blacks, Greens and Sours (BGS). Chemical composition of BGS has a damaging impact on beverage GQ. That is why analytical tools are needed for monitoring and controlling the GQ in coffee agro-industry. Near Infrared Spectroscopy (NIRS) has been successfully applied for assessment of coffee quality. Another potential technique for direct, clean and fast measurement of coffee GQ is Laser Induced Breakdown Spectroscopy (LIBS). Elements and diatomic molecules commonly present in organic compounds (structure) can be assessed by using LIBS. In this article is reported an evaluation of LIBS for the main interferents of GQ (BGS defects). Results confirm the great potential of LIBS for discriminating good beans from those with BGS defects by using emission lines of C, CN, C2 and N. Most importantly, some emission lines presented strong linear correlation (r > 0.9) with NIRS absorption bands assigned to proteins, lipids, sugar and carboxylic acids, suggesting LIBS potential to estimate these compounds in unroasted and ground coffee samples.

Detection and Classification of Live and Dead Escherichia coli by Laser-Induced Breakdown Spectroscopy

Science.gov (United States)

Sivakumar, P.; Fernández-Bravo, A.; Taleh, L.; Biddle, J.F.

2015-01-01

Abstract A common goal for astrobiology is to detect organic materials that may indicate the presence of life. However, organic materials alone may not be representative of currently living systems. Thus, it would be valuable to have a method with which to determine the health of living materials. Here, we present progress toward this goal by reporting on the application of laser-induced breakdown spectroscopy (LIBS) to study characteristics of live and dead cells using Escherichia coli (E. coli) strain K12 cells as a model organism since its growth and death in the laboratory are well understood. Our goal is to determine whether LIBS, in its femto- and/or nanosecond forms, could ascertain the state of a living organism. E. coli strain K12 cells were grown, collected, and exposed to one of two types of inactivation treatments: autoclaving and sonication. Cells were also kept alive as a control. We found that LIBS yields key information that allows for the discrimination of live and dead E. coli bacteria based on ionic shifts reflective of cell membrane integrity. Key Words: E. coli—Trace elements—Live and dead cells—Laser-induced breakdown spectroscopy—Atomic force microscopy. Astrobiology 15, 144–153. PMID:25683088

Laser induced breakdown spectroscopy of the uranium including calcium. Time resolved measurement spectroscopic analysis (Contract research)

International Nuclear Information System (INIS)

Akaoka, Katsuaki; Maruyama, Youichiro; Oba, Masaki; Miyabe, Masabumi; Otobe, Haruyoshi; Wakaida, Ikuo

2010-05-01

For the remote analysis of low DF TRU (Decontamination Factor Transuranic) fuel, Laser Breakdown Spectroscopy (LIBS) was applied to uranium oxide including a small amount of calcium oxide. The characteristics, such as spectrum intensity and plasma excitation temperature, were measured using time-resolved spectroscopy. As a result, in order to obtain the stable intensity of calcium spectrum for the uranium spectrum, it was found out that the optimum observation delay time of spectrum is 4 microseconds or more after laser irradiation. (author)

Evaluation of laser induced breakdown spectroscopy for cadmium determination in soils

International Nuclear Information System (INIS)

Santos, Dario; Nunes, Lidiane C.; Trevizan, Lilian C.; Godoi, Quienly; Leme, Flavio O.; Braga, Jez Willian B.; Krug, Francisco Jose

2009-01-01

Cadmium is known to be a toxic agent that accumulates in the living organisms and present high toxicity potential over lifetime. Efforts towards the development of methods for microanalysis of environmental samples, including the determination of this element by graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma optical emission spectrometry (ICP OES), and inductively coupled plasma-mass spectrometry (ICP-MS) techniques, have been increasing. Laser induced breakdown spectroscopy (LIBS) is an emerging technique dedicated to microanalysis and there is a lack of information dealing with the determination of cadmium. The aim of this work is to demonstrate the feasibility of LIBS for cadmium detection in soils. The experimental setup was designed using a laser Q-switched (Nd:YAG, 10 Hz, λ = 1064 nm) and the emission signals were collimated by lenses into an optical fiber coupled to a high-resolution intensified charge-coupled device (ICCD)-echelle spectrometer. Samples were cryogenically ground and thereafter pelletized before LIBS analysis. Best results were achieved by exploring a test portion (i.e. sampling spots) with larger surface area, which contributes to diminish the uncertainty due to element specific microheterogeneity. Calibration curves for cadmium determination were achieved using certified reference materials. The metrological figures of merit indicate that LIBS can be recommended for screening of cadmium contamination in soils.

Artificial neural network for on-site quantitative analysis of soils using laser induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

El Haddad, J. [Univ. Bordeaux, LOMA, UMR 5798, F-33400 Talence (France); CNRS, LOMA, UMR 5798, F-33400 Talence (France); Villot-Kadri, M.; Ismaël, A.; Gallou, G. [IVEA Solution, Centre Scientifique d' Orsay, Bât 503, 91400 Orsay (France); Michel, K.; Bruyère, D.; Laperche, V. [BRGM, Service Métrologie, Monitoring et Analyse, 3 avenue Claude Guillemin, B.P 36009, 45060 Orléans Cedex (France); Canioni, L. [Univ. Bordeaux, LOMA, UMR 5798, F-33400 Talence (France); CNRS, LOMA, UMR 5798, F-33400 Talence (France); Bousquet, B., E-mail: bruno.bousquet@u-bordeaux1.fr [Univ. Bordeaux, LOMA, UMR 5798, F-33400 Talence (France); CNRS, LOMA, UMR 5798, F-33400 Talence (France)

2013-01-01

Nowadays, due to environmental concerns, fast on-site quantitative analyses of soils are required. Laser induced breakdown spectroscopy is a serious candidate to address this challenge and is especially well suited for multi-elemental analysis of heavy metals. However, saturation and matrix effects prevent from a simple treatment of the LIBS data, namely through a regular calibration curve. This paper details the limits of this approach and consequently emphasizes the advantage of using artificial neural networks well suited for non-linear and multi-variate calibration. This advanced method of data analysis is evaluated in the case of real soil samples and on-site LIBS measurements. The selection of the LIBS data as input data of the network is particularly detailed and finally, resulting errors of prediction lower than 20% for aluminum, calcium, copper and iron demonstrate the good efficiency of the artificial neural networks for on-site quantitative LIBS of soils. - Highlights: ► We perform on-site quantitative LIBS analysis of soil samples. ► We demonstrate that univariate analysis is not convenient. ► We exploit artificial neural networks for LIBS analysis. ► Spectral lines other than the ones from the analyte must be introduced.

Artificial neural network for on-site quantitative analysis of soils using laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

El Haddad, J.; Villot-Kadri, M.; Ismaël, A.; Gallou, G.; Michel, K.; Bruyère, D.; Laperche, V.; Canioni, L.; Bousquet, B.

2013-01-01

Nowadays, due to environmental concerns, fast on-site quantitative analyses of soils are required. Laser induced breakdown spectroscopy is a serious candidate to address this challenge and is especially well suited for multi-elemental analysis of heavy metals. However, saturation and matrix effects prevent from a simple treatment of the LIBS data, namely through a regular calibration curve. This paper details the limits of this approach and consequently emphasizes the advantage of using artificial neural networks well suited for non-linear and multi-variate calibration. This advanced method of data analysis is evaluated in the case of real soil samples and on-site LIBS measurements. The selection of the LIBS data as input data of the network is particularly detailed and finally, resulting errors of prediction lower than 20% for aluminum, calcium, copper and iron demonstrate the good efficiency of the artificial neural networks for on-site quantitative LIBS of soils. - Highlights: ► We perform on-site quantitative LIBS analysis of soil samples. ► We demonstrate that univariate analysis is not convenient. ► We exploit artificial neural networks for LIBS analysis. ► Spectral lines other than the ones from the analyte must be introduced

Laser induced breakdown spectroscopy for analysis and characterization of degradation pathologies of Roman glasses

International Nuclear Information System (INIS)

Palomar, T.; Oujja, M.; García-Heras, M.; Villegas, M.A.; Castillejo, M.

2013-01-01

The feasibility and possibilities of laser induced breakdown spectroscopy (LIBS) in the full study of non-destructible historic glasses have been explored in the present work. Thirteen Roman glass samples, including seven entire glass beads, from the ancient town of Augusta Emerita (SW Spain) were characterized by LIBS in combination with other conventional techniques, such as scanning electron microscopy/energy dispersive X-ray spectrometry, X-ray fluorescence and ultraviolet–visible spectrophotometry. LIBS stratigraphic analysis, carried out by the application of successive laser pulses on the same spot, has been mainly targeted at characterizing particular features of non-destructible historic glasses, such as bulk chemical composition, surface degradation pathologies (dealkalinization layers and deposits), chromophores, and opacifying elements. The obtained data demonstrate that LIBS can be a useful and alternative technique for spectroscopic studies of historical glasses, especially for those conserved under burial conditions and when it deals with studying non-destructible samples. - Highlights: • Determination of chromophores and opacifiers in non-destructible glass by LIBS • Manganese is determined as principal component of dark deposits. • Antimony appears in all decorations while lead is only present in yellow ones. • Stratigraphic analysis enables the identification of dealkalinization layers

Laser induced breakdown spectroscopy for analysis and characterization of degradation pathologies of Roman glasses

Energy Technology Data Exchange (ETDEWEB)

Palomar, T. [Instituto de Historia, Centro de Ciencias Humanas y Sociales, CSIC, C/Albasanz 26-28, 28037 Madrid (Spain); Oujja, M., E-mail: m.oujja@iqfr.csic.es [Instituto de Química Física Rocasolano, CSIC, C/Serrano 119, 28006 Madrid (Spain); García-Heras, M.; Villegas, M.A. [Instituto de Historia, Centro de Ciencias Humanas y Sociales, CSIC, C/Albasanz 26-28, 28037 Madrid (Spain); Castillejo, M. [Instituto de Química Física Rocasolano, CSIC, C/Serrano 119, 28006 Madrid (Spain)

2013-09-01

The feasibility and possibilities of laser induced breakdown spectroscopy (LIBS) in the full study of non-destructible historic glasses have been explored in the present work. Thirteen Roman glass samples, including seven entire glass beads, from the ancient town of Augusta Emerita (SW Spain) were characterized by LIBS in combination with other conventional techniques, such as scanning electron microscopy/energy dispersive X-ray spectrometry, X-ray fluorescence and ultraviolet–visible spectrophotometry. LIBS stratigraphic analysis, carried out by the application of successive laser pulses on the same spot, has been mainly targeted at characterizing particular features of non-destructible historic glasses, such as bulk chemical composition, surface degradation pathologies (dealkalinization layers and deposits), chromophores, and opacifying elements. The obtained data demonstrate that LIBS can be a useful and alternative technique for spectroscopic studies of historical glasses, especially for those conserved under burial conditions and when it deals with studying non-destructible samples. - Highlights: • Determination of chromophores and opacifiers in non-destructible glass by LIBS • Manganese is determined as principal component of dark deposits. • Antimony appears in all decorations while lead is only present in yellow ones. • Stratigraphic analysis enables the identification of dealkalinization layers.

The detection of He in tungsten following ion implantation by laser-induced breakdown spectroscopy

Science.gov (United States)

Shaw, G.; Bannister, M.; Biewer, T. M.; Martin, M. Z.; Meyer, F.; Wirth, B. D.

2018-01-01

Laser-induced breakdown spectroscopy (LIBS) results are presented that provide depth-resolved identification of He implanted in polycrystalline tungsten (PC-W) targets by a 200 keV He+ ion beam, with a surface temperature of approximately 900 °C and a peak fluence of 1023 m-2. He retention, and the influence of He on deuterium and tritium recycling, permeation, and retention in PC-W plasma facing components are important questions for the divertor and plasma facing components in a fusion reactor, yet are difficult to quantify. The purpose of this work is to demonstrate the ability of LIBS to identify helium in tungsten; to investigate the sensitivity of laser parameters including, laser energy and gate delay, that directly influence the sensitivity and depth resolution of LIBS; and to perform a proof-of-principle experiment using LIBS to measure relative He intensities as a function of depth. The results presented demonstrate the potential not only to identify helium but also to develop a methodology to quantify gaseous impurity concentration in PC-W as a function of depth.

Analysis of material collected on swipes using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Chinni, Rosemarie; Cremers, David A.; Multari, Rosalie

2010-01-01

Laser-induced breakdown spectroscopy (LIBS) was evaluated to determine elements collected on swipes as surface contamination. A series of long laser plasmas formed along the swipe surface (Post-it paper) interrogated the collected contamination. LIBS detection limits, determined for the elements Ag, As, Ba, Be, Cd, Cr, Cu, Hg, Mn, Ni, Pb, Sr, and Zn on swipes (2 cm 2 area), ranged from 0.002 μg (Be) to 1.46 μg (Pb). The elements were introduced as constituents of synthetic silicate particles serving as a contaminant dust stimulant. The average predicted mass was within 16% of the actual mass on the swipe. The efficiency of collecting particles from surfaces including plastic, Formica, and Al metal was also evaluated. The ability to detect and differentiate two amino acids on a swipe from each other and from the swipe using chemometric modeling techniques was also demonstrated.

Investigation of archaeological metal artefacts by laser-induced breakdown spectroscopy (LIBS)

Science.gov (United States)

Tankova, V.; Malcheva, G.; Blagoev, K.; Leshtakov, L.

2018-03-01

In this work, laser-induced breakdown spectroscopy was applied to determining the elemental composition of a set of ancient bronze artefacts dated from the Late Bronze Age and Early Iron Age (14th – 10th century BC). We used a Nd:YAG laser at 1064 nm with pulse duration of 10 ns and energy of 10 mJ and determined the elemental composition of the bronze alloy that was used in manufacturing the samples under study. The concentrations of tin and lead in the bulk of the examined materials was estimated after generating calibration curves for a set of four standard samples. The preliminary results of the analysis will provide information on the artefacts provenance and on the production process.

A comparative study of the laser induce breakdown spectroscopy in single- and double-pulse laser geometry

International Nuclear Information System (INIS)

Sun Duixiong; Su Maogen; Dong Chenzhong; Wen Guanhong; Cao Xiangnian

2013-01-01

A time resolved laser induced breakdown spectroscopy technique (LIBS) was used for the investigation of emission signal enhancement on double-pulse LIBS. Two Q-switched Nd:YAG lasers at 1064 nm wavelength have been employed to generate laser-induced plasma on aluminium-based alloys. The plasma emission signals were recorded by spectrometer with ICCD detector. Spectral response calibration was performed by using deuterium and tungsten halogen lamps. Time evolution of the plasma temperature and electron density was investigated in SP and DP experiments. Based on the investigation of plasma parameters, the enhancements of emission line intensities were investigated, and the mechanisms of it were discussed. (author)

High resolution applications of laser-induced breakdown spectroscopy for environmental and forensic applications

International Nuclear Information System (INIS)

Martin, Madhavi Z.; Labbe, Nicole; Andre, Nicolas; Harris, Ronny; Ebinger, Michael; Wullschleger, Stan D.; Vass, Arpad A.

2007-01-01

Laser-induced breakdown spectroscopy (LIBS) has been used in the elemental analysis for a variety of environmental samples and as a proof of concept for a host of forensic applications. In the first application, LIBS was used for the rapid detection of carbon from a number of different soil types. In this application, a major breakthrough was achieved by using a multivariate analytical approach that has brought us closer towards a 'universal calibration curve'. In a second application, it has been demonstrated that LIBS in combination with multivariate analysis can be employed to analyze the chemical composition of annual tree growth rings and correlate them to external parameters such as changes in climate, forest fires, and disturbances involving human activity. The objectives of using this technology in fire scar determinations are: 1) To determine the characteristic spectra of wood exposed to forest fires and 2) To examine the viability of this technique for detecting fire occurrences in stems that did not develop fire scars. These examples demonstrate that LIBS-based techniques are inherently well suited for diverse environmental applications. LIBS was also applied to a variety of proof of concept forensic applications such as the analysis of cremains (human cremation remains) and elemental composition analysis of prosthetic implants

Multivariate methods for analysis of environmental reference materials using laser-induced breakdown spectroscopy

Directory of Open Access Journals (Sweden)

Shikha Awasthi

2017-06-01

Full Text Available Analysis of emission from laser-induced plasma has a unique capability for quantifying the major and minor elements present in any type of samples under optimal analysis conditions. Chemometric techniques are very effective and reliable tools for quantification of multiple components in complex matrices. The feasibility of laser-induced breakdown spectroscopy (LIBS in combination with multivariate analysis was investigated for the analysis of environmental reference materials (RMs. In the present work, different (Certified/Standard Reference Materials of soil and plant origin were analyzed using LIBS and the presence of Al, Ca, Mg, Fe, K, Mn and Si were identified in the LIBS spectra of these materials. Multivariate statistical methods (Partial Least Square Regression and Partial Least Square Discriminant Analysis were employed for quantitative analysis of the constituent elements using the LIBS spectral data. Calibration models were used to predict the concentrations of the different elements of test samples and subsequently, the concentrations were compared with certified concentrations to check the authenticity of models. The non-destructive analytical method namely Instrumental Neutron Activation Analysis (INAA using high flux reactor neutrons and high resolution gamma-ray spectrometry was also used for intercomparison of results of two RMs by LIBS.

RCRA materials analysis by laser-induced breakdown spectroscopy: Detection limits in soils

International Nuclear Information System (INIS)

Koskelo, A.; Cremers, D.A.

1994-01-01

The goal of the Technical Task Plan (TTP) that this report supports is research, development, testing and evaluation of a portable analyzer for RCRA and other metals. The instrumentation to be built will be used for field-screening of soils. Data quality is expected to be suitable for this purpose. The data presented in this report were acquired to demonstrate the detection limits for laser-induced breakdown spectroscopy (LIBS) of soils using instrument parameters suitable for fieldable instrumentation. The data are not expected to be the best achievable with the high pulse energies available in laboratory lasers. The report presents work to date on the detection limits for several elements in soils using LIBS. The elements targeted in the Technical Task Plan are antimony, arsenic, beryllium, cadmium, chromium, lead, selenium, and zirconium. Data for these elements are presented in this report. Also included are other data of interest to potential customers for the portable LIBS apparatus. These data are for barium, mercury, cesium and strontium. Data for uranium and thorium will be acquired during the tasks geared toward mixed waste characterization

Laser Induced Breakdown Spectroscopy Based on Single Beam Splitting and Geometric Configuration for Effective Signal Enhancement

Science.gov (United States)

Yang, Guang; Lin, Qingyu; Ding, Yu; Tian, Di; Duan, Yixiang

2015-01-01

A new laser induced breakdown spectroscopy (LIBS) based on single-beam-splitting (SBS) and proper optical geometric configuration has been initially explored in this work for effective signal enhancement. In order to improve the interaction efficiency of laser energy with the ablated material, a laser beam operated in pulse mode was divided into two streams to ablate/excite the target sample in different directions instead of the conventional one beam excitation in single pulse LIBS (SP-LIBS). In spatial configuration, the laser beam geometry plays an important role in the emission signal enhancement. Thus, an adjustable geometric configuration with variable incident angle between the two splitted laser beams was constructed for achieving maximum signal enhancement. With the optimized angles of 60° and 70° for Al and Cu atomic emission lines at 396.15 nm and 324.75 nm respectively, about 5.6- and 4.8-folds signal enhancements were achieved for aluminum alloy and copper alloy samples compared to SP-LIBS. Furthermore, the temporal analysis, in which the intensity of atomic lines in SP-LIBS decayed at least ten times faster than the SBS-LIBS, proved that the energy coupling efficiency of SBS-LIBS was significantly higher than that of SP-LIBS. PMID:25557721

A Laser Induced Breakdown Spectroscopy application based on Local Thermodynamic Equilibrium assumption for the elemental analysis of alexandrite gemstone and copper-based alloys

Energy Technology Data Exchange (ETDEWEB)

De Giacomo, A. [Department of Chemistry, University of Bari, Via Orabona 4, 70126 Bari (Italy); Institute of Inorganic Methodologies and Plasmas - CNR, U.O.S. Bari, Via Amendola 122/D, 70126 Bari (Italy); Dell' Aglio, M. [Institute of Inorganic Methodologies and Plasmas - CNR, U.O.S. Bari, Via Amendola 122/D, 70126 Bari (Italy); Gaudiuso, R., E-mail: rosalba.gaudiuso@ba.imip.cnr.it [Institute of Inorganic Methodologies and Plasmas - CNR, U.O.S. Bari, Via Amendola 122/D, 70126 Bari (Italy); Santagata, A. [Institute of Inorganic Methodologies and Plasmas - CNR, U.O.S. Potenza, Via S. Loja, Zona Ind., 85050 Tito Scalo (PZ) (Italy); Senesi, G.S. [Institute of Inorganic Methodologies and Plasmas - CNR, U.O.S. Bari, Via Amendola 122/D, 70126 Bari (Italy); Rossi, M.; Ghiara, M.R. [Department of Earth Sciences, University of Naples ' Federico II' , Via Mezzocannone 8, 80134 Naples (Italy); Capitelli, F. [Institute of Crystallography - CNR, Via Salaria Km 29.300, 00015 Monterotondo (Roma) (Italy); De Pascale, O. [Institute of Inorganic Methodologies and Plasmas - CNR, U.O.S. Bari, Via Amendola 122/D, 70126 Bari (Italy)

2012-04-04

Graphical abstract: Self-calibrated analytical techniques based on the approximation of Local Thermodynamic Equilibrium (LTE) have been employed for the analysis of gemstones and copper-based alloys by LIBS (Laser Induced Breakdown Spectroscopy), with a special focus on LTE conditions in laser induced plasmas. Highlights: Black-Right-Pointing-Pointer Discussion of Local Thermodynamic Equilibrium (LTE) condition in laser-induced plasmas. Black-Right-Pointing-Pointer LIBS enables elemental analysis with self-calibrated LTE-based methods. Black-Right-Pointing-Pointer Be detection in alexandrite gemstone is made possible by LIBS. - Abstract: Laser Induced Breakdown Spectroscopy (LIBS) is an appealing technique to study laser-induced plasmas (LIPs), both from the basic diagnostics point of view and for analytical applications. LIPs are complex dynamic systems, expanding at supersonic velocities and undergoing a transition between different plasma regimes. If the Local Thermodynamic Equilibrium (LTE) condition is valid for such plasmas, several analytical methods can be employed and fast quantitative analyses can be performed on a variety of samples. In the present paper, a discussion about LTE is carried out and an innovative application to the analysis of the alexandrite gemstone is presented. In addition, a study about the influence of plasma parameters on the performance of LTE-based methods is reported for bronze and brass targets.

Nanoparticle Enhanced Laser Induced Breakdown Spectroscopy: Effect of nanoparticles deposited on sample surface on laser ablation and plasma emission

International Nuclear Information System (INIS)

De Giacomo, A.; Gaudiuso, R.; Koral, C.; Dell'Aglio, M.; De Pascale, O.

2014-01-01

In this paper the use of metallic nanoparticles (NPs) for improving Laser Induced Breakdown Spectroscopy (LIBS) is discussed. In the case of conductors an emission signal enhancement up to 1–2 orders of magnitude was obtained depositing NPs on the sample surface by drying a micro-drop of colloidal solution. The basic mechanisms of Nanoparticle Enhanced LIBS (NELIBS) were studied and the main causes of this significantly large enhancement were found to be related to the effect of NPs on the laser ablation process, in terms of a faster and more efficient production of seed electrons with respect to conventional LIBS. The characteristics of NELIBS-produced plasma were investigated by emission spectroscopy and spectrally resolved images. In spite of similar plasma parameters, the NELIBS plasma was found to have larger emission volume and longer persistence than the LIBS one. A method to determine NP concentration and size was also proposed, which involved depositing NPs on non-interacting substrates, and proved the feasibility of LIBS as a fast detection tool for a preliminary characterization of NPs. - Highlights: • Effect of NPs on sample surface enables instantaneous field emission. • More efficient ablation • LIBS emission enhancement up to 1–2 orders of magnitude • Possibility of NP characterization in terms of concentration and size

Determination of Different Metals in Steel Waste Samples Using laser Induced Breakdown Spectroscopy

Directory of Open Access Journals (Sweden)

A. H. Bakry

2007-12-01

Full Text Available Elemental analysis of waste samples collected from steel products manufacturing plant (SPS located at industrial city of Jeddah, Saudi-Arabia has been carried out using Laser Induced Breakdown Spectroscopy (LIBS. The 1064 nm laser radiations from a Nd:YAG laser at an irradiance of 7.6  1010 W cm –2 were used. Atomic emission spectra of the elements present in the waste samples were recorded in the 200 – 620 nm region. Elements such as Fe, W, Ti, Al, Mg, Ca, S, Mn, and Na were detected in these samples. Quantitative determination of the elemental concentration was obtained for these metals against certified standard samples. Parametric dependences of LIBS signal intensity on incident laser energy and time delay between the laser pulse and data acquisition system were also carried out.

Determination of Heating Value of Estonian Oil Shale by Laser-Induced Breakdown Spectroscopy

Directory of Open Access Journals (Sweden)

M. Aints

2018-01-01

Full Text Available The laser-induced breakdown spectroscopy (LIBS combined with multivariate regression analysis of measured data were utilised for determination of the heating value and the chemical composition of pellets made from Estonian oil shale samples with different heating values. The study is the first where the oil shale heating value is determined on the basis of LIBS spectra. The method for selecting the optimal number of spectral lines for ordinary multivariate least squares regression model is presented. The correlation coefficient between the heating value predicted by the regression model, and that measured by calorimetric bomb, was R2=0.98. The standard deviation of prediction was 0.24 MJ/kg. Concentrations of oil shale components predicted by the regression model were compared with those measured by ordinary methods.

Online monitoring of corrosion behavior in molten metal using laser-induced breakdown spectroscopy

Science.gov (United States)

Zeng, Qiang; Pan, Congyuan; Li, Chaoyang; Fei, Teng; Ding, Xiaokang; Du, Xuewei; Wang, Qiuping

2018-04-01

The corrosion behavior of structure materials in direct contact with molten metals is widespread in metallurgical industry. The corrosion of casting equipment by molten metals is detrimental to the production process, and the corroded materials can also contaminate the metals being produced. Conventional methods for studying the corrosion behavior by molten metal are offline. This work explored the application of laser-induced breakdown spectroscopy (LIBS) for online monitoring of the corrosion behavior of molten metal. The compositional changes of molten aluminum in crucibles made of 304 stainless steel were obtained online at 1000 °C. Several offline techniques were combined to determine the corrosion mechanism, which was highly consistent with previous studies. Results proved that LIBS was an efficient method to study the corrosion mechanism of solid materials in molten metal.

Double pulse laser induced breakdown spectroscopy applied to natural and artificial materials from cultural heritages

International Nuclear Information System (INIS)

Brai, Maria; Gennaro, Gaetano; Schillaci, Tiziano; Tranchina, Luigi

2009-01-01

The laser-induced breakdown spectroscopy (LIBS) is an applied physical technique that has shown in recent years its great potential for rapid qualitative analysis of materials. Thanks to the possibility to implement a portable instrument that perform LIBS analysis, this technique is revealed to be particularly useful for in situ analysis in the field of cultural heritages. The purpose of this work is to evaluate the potentiality of LIBS technique in the field of cultural heritages, with respect to the chemical characterization of complex matrix as calcareous and refractory materials for further quantitative analyses on cultural heritages. X-Ray Fluorescence (XRF) analyses were used as reference. Calibration curves of certified materials used as standards were obtained by XRF analyses. The LIBS measurements were performed with a new mobile instrument called Modi (Mobile Double pulse Instrument for LIBS Analysis). The XRF analyses were performed with a portable instrument ArtTAX. LIBS and XRF measurement were performed on both reference materials and samples (bricks and mortars) sampled in the ancient Greek-Roman Theatre of Taormina. Although LIBS measurements performed on reference materials have shown non linear response to concentrations, and so we were not able to obtain quantitative results, an integrated study of XRF and LIBS signals permitted us to distinguish among chemical features and degradation state of measured building materials.

Double pulse laser induced breakdown spectroscopy applied to natural and artificial materials from cultural heritages

Energy Technology Data Exchange (ETDEWEB)

Brai, Maria; Gennaro, Gaetano [Dipartimento di Fisica e Tecnologie Relative, Universita di Palermo, Viale delle Scienze Ed.18, 90128 Palermo (Italy); Schillaci, Tiziano, E-mail: tschillaci@unipa.i [Dipartimento di Fisica e Tecnologie Relative, Universita di Palermo, Viale delle Scienze Ed.18, 90128 Palermo (Italy); Tranchina, Luigi [Dipartimento di Fisica e Tecnologie Relative, Universita di Palermo, Viale delle Scienze Ed.18, 90128 Palermo (Italy)

2009-10-15

The laser-induced breakdown spectroscopy (LIBS) is an applied physical technique that has shown in recent years its great potential for rapid qualitative analysis of materials. Thanks to the possibility to implement a portable instrument that perform LIBS analysis, this technique is revealed to be particularly useful for in situ analysis in the field of cultural heritages. The purpose of this work is to evaluate the potentiality of LIBS technique in the field of cultural heritages, with respect to the chemical characterization of complex matrix as calcareous and refractory materials for further quantitative analyses on cultural heritages. X-Ray Fluorescence (XRF) analyses were used as reference. Calibration curves of certified materials used as standards were obtained by XRF analyses. The LIBS measurements were performed with a new mobile instrument called Modi (Mobile Double pulse Instrument for LIBS Analysis). The XRF analyses were performed with a portable instrument ArtTAX. LIBS and XRF measurement were performed on both reference materials and samples (bricks and mortars) sampled in the ancient Greek-Roman Theatre of Taormina. Although LIBS measurements performed on reference materials have shown non linear response to concentrations, and so we were not able to obtain quantitative results, an integrated study of XRF and LIBS signals permitted us to distinguish among chemical features and degradation state of measured building materials.

Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Cabalin, L.M.; Gonzalez, A. [Department of Analytical Chemistry, University of Malaga, E-29071 Malaga (Spain); Ruiz, J. [Department of Applied Physics I, University of Malaga, E-29071 Malaga (Spain); Laserna, J.J., E-mail: laserna@uma.e [Department of Analytical Chemistry, University of Malaga, E-29071 Malaga (Spain)

2010-08-15

Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s{sup -1}. Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

Science.gov (United States)

Cabalín, L. M.; González, A.; Ruiz, J.; Laserna, J. J.

2010-08-01

Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s - 1 . Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Cabalin, L.M.; Gonzalez, A.; Ruiz, J.; Laserna, J.J.

2010-01-01

Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s -1 . Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

Roughness effects on the hydrogen signal in laser-induced breakdown spectroscopy

DEFF Research Database (Denmark)

Rapin, W.; Bousquet, B.; Lasue, J.

2017-01-01

On Mars, Laser-Induced Breakdown Spectroscopy (LIBS) as performed by the ChemCam instrument can be used to measure the hydrogen content of targets in situ, under a low pressure CO2 atmosphere. However, unexpected variations observed in the Martian dataset suggest an effect related to target...... to hydrogen, as other emission lines in the spectra are not affected. The increase of the signal could be related to an addition of hydrogen to the plasma due to interaction with the surrounding target surface, yet the exact physical process to explain such effect remains to be identified. More generally...

Fire debris analysis for forensic fire investigation using laser induced breakdown spectroscopy (LIBS)

Science.gov (United States)

Choi, Soojin; Yoh, Jack J.

2017-08-01

The possibility verification of the first attempt to apply LIBS to arson investigation was performed. LIBS has capabilities for real time in-situ analysis and depth profiling. It can provide valuable information about the fire debris that are complementary to the classification of original sample components and combustion residues. In this study, fire debris was analyzed to determine the ignition source and existence of a fire accelerant using LIBS spectra and depth profiling analysis. Fire debris chemical composition and carbon layer thickness determines the possible ignition source while the carbon layer thickness of combusted samples represents the degree of sample carbonization. When a sample is combusted with fire accelerants, a thicker carbon layer is formed because the burning rate is increased. Therefore, depth profiling can confirm the existence of combustion accelerants, which is evidence of arson. Also investigation of fire debris by depth profiling is still possible when a fire is extinguished with water from fire hose. Such data analysis and in-situ detection of forensic signals via the LIBS may assist fire investigation at crime scenes.

Laser-Induced Breakdown Spectroscopy Based Protein Assay for Cereal Samples.

Science.gov (United States)

Sezer, Banu; Bilge, Gonca; Boyaci, Ismail Hakki

2016-12-14

Protein content is an important quality parameter in terms of price, nutritional value, and labeling of various cereal samples. However, conventional analysis methods, namely, Kjeldahl and Dumas, have major drawbacks such as long analysis time, titration mistakes, and carrier gas dependence with high purity. For this reason, there is an urgent need for rapid, reliable, and environmentally friendly technologies for protein analysis. The present study aims to develop a new method for protein analysis in wheat flour and whole meal by using laser-induced breakdown spectroscopy (LIBS), which is a multielemental, fast, and simple spectroscopic method. Unlike the Kjeldahl and Dumas methods, it has potential to analyze a high number of samples in considerably short time. In the study, nitrogen peaks in LIBS spectra of wheat flour and whole meal samples with different protein contents were correlated with results of the standard Dumas method with the aid of chemometric methods. A calibration graph showed good linearity with the protein content between 7.9 and 20.9% and a 0.992 coefficient of determination (R 2 ). The limit of detection was calculated as 0.26%. The results indicated that LIBS is a promising and reliable method with its high sensitivity for routine protein analysis in wheat flour and whole meal samples.

Matrix effect on emission/current correlated analysis in laser-induced breakdown spectroscopy of liquid droplets

International Nuclear Information System (INIS)

Huang, J.-S.; Ke, C.-B.; Lin, K.-C.

2004-01-01

We have investigated influence of matrix salts on the liquid droplets by laser-induced breakdown spectroscopy (LIBS). An electrospray ionization technique coupled with LIBS is employed to generate the microdroplets of the Na sample solution with various matrix salts added. A sequence of single-shot time-resolved LIB emission signals is detected. The LIB signal intensity integrated within a gate linearly correlates with the plasma-induced current response obtained simultaneously on a single-shot basis. The slopes thus obtained increase with the sample concentration, but appear to be irrespective of different matrix salts, added up to a 2000 mg/l concentration. The matrix salts involved have the same K + cation but different anions. Given a laser radiation emitting at 355 nm with the energy fixed at 23±1 mJ, a limit of detection (LOD) of 1.0 mg/l may be achieved for the Na analysis. The current normalization might have probably taken into account the ablated amount of the sample and the plasma temperature. Accordingly, the LIB/current correlated analysis becomes efficient to suppress the signal fluctuation, improve the LOD determination, and concurrently correct the matrix effect

Detection of heavy metal Cd in polluted fresh leafy vegetables by laser-induced breakdown spectroscopy.

Science.gov (United States)

Yao, Mingyin; Yang, Hui; Huang, Lin; Chen, Tianbing; Rao, Gangfu; Liu, Muhua

2017-05-10

In seeking a novel method with the ability of green analysis in monitoring toxic heavy metals residue in fresh leafy vegetables, laser-induced breakdown spectroscopy (LIBS) was applied to prove its capability in performing this work. The spectra of fresh vegetable samples polluted in the lab were collected by optimized LIBS experimental setup, and the reference concentrations of cadmium (Cd) from samples were obtained by conventional atomic absorption spectroscopy after wet digestion. The direct calibration employing intensity of single Cd line and Cd concentration exposed the weakness of this calibration method. Furthermore, the accuracy of linear calibration can be improved a little by triple Cd lines as characteristic variables, especially after the spectra were pretreated. However, it is not enough in predicting Cd in samples. Therefore, partial least-squares regression (PLSR) was utilized to enhance the robustness of quantitative analysis. The results of the PLSR model showed that the prediction accuracy of the Cd target can meet the requirement of determination in food safety. This investigation presented that LIBS is a promising and emerging method in analyzing toxic compositions in agricultural products, especially combined with suitable chemometrics.

Laser induced breakdown spectroscopy for applications in nuclear industry

International Nuclear Information System (INIS)

Suri, B.M.

2010-01-01

There are several analytical techniques employing laser spectroscopy - each with its own distinctive potential. Laser Induced Breakdown Spectroscopy (LIBS) is one such technique which is attractive in view of its relative compactness and simplicity (in configuration), remote and online analysis (with no sample handling requirement) and high spatial resolution allowing compositional map or homogeneity analysis. In this technique, a high power pulsed (mostly nanosecond) laser is employed to irradiate the sample causing spark emission, characteristics of the sample composition, which is collected using suitable optics and analysed spectroscopically. Remote and online capability is derived from long distance delivery of laser beams and collection of emitted light by fibres or conventional optics. Since laser can be focused sharply on the target, it can facilitate compositional mapping. Beam Technology Development Group at BARC had initiated work on LIBS of nuclear materials several years ago. Recently the challenge of online monitoring of radioactive waste vitrification plant in a hot cell has been taken up. The theoretical and experimental work done by the group related to instrument development, plasma characterization, quantitative compositional analysis of ternary alloys and uranium vitrified glass samples (comprising more than dozen elements) are described. The future plans for setting up online glass homogeneity monitoring facility are also described. This should fulfill an important demand for optimization of vitrification process. Various other demands of nuclear industry are also reviewed

Improved accuracy in quantitative laser-induced breakdown spectroscopy using sub-models

Science.gov (United States)

Anderson, Ryan; Clegg, Samuel M.; Frydenvang, Jens; Wiens, Roger C.; McLennan, Scott M.; Morris, Richard V.; Ehlmann, Bethany L.; Dyar, M. Darby

2017-01-01

Accurate quantitative analysis of diverse geologic materials is one of the primary challenges faced by the Laser-Induced Breakdown Spectroscopy (LIBS)-based ChemCam instrument on the Mars Science Laboratory (MSL) rover. The SuperCam instrument on the Mars 2020 rover, as well as other LIBS instruments developed for geochemical analysis on Earth or other planets, will face the same challenge. Consequently, part of the ChemCam science team has focused on the development of improved multivariate analysis calibrations methods. Developing a single regression model capable of accurately determining the composition of very different target materials is difficult because the response of an element’s emission lines in LIBS spectra can vary with the concentration of other elements. We demonstrate a conceptually simple “sub-model” method for improving the accuracy of quantitative LIBS analysis of diverse target materials. The method is based on training several regression models on sets of targets with limited composition ranges and then “blending” these “sub-models” into a single final result. Tests of the sub-model method show improvement in test set root mean squared error of prediction (RMSEP) for almost all cases. The sub-model method, using partial least squares regression (PLS), is being used as part of the current ChemCam quantitative calibration, but the sub-model method is applicable to any multivariate regression method and may yield similar improvements.

Loading of deuterium and helium by Pilot-PSI plasma and their detection by in-situ LIBS

NARCIS (Netherlands)

Piip, K.; van der Meiden, H. J.; Bystrov, K.; Hämarik, L.; Karhunen, J.; Aints, M.; Laan, M.; Paris, P.; Seemen, H.; Hakola, A.; Brezinsek, S.

2017-01-01

Laser-induced breakdown spectroscopy (LIBS) is a promising method for quantifying the fuel content of the plasma-facing components of ITER both in between plasma discharges (in-situ) and after maintenance operations. The aim of the present study is to test the applicability of in-situ LIBS for

Ultra-short laser pulse ablation using shear-force feedback: Femtosecond laser induced breakdown spectroscopy feasibility study

International Nuclear Information System (INIS)

Samek, Ota; Kurowski, Andre; Kittel, Silke; Kukhlevsky, Sergei; Hergenroeder, Roland

2005-01-01

This work reports on a feasibility study of proximity ablation using femtosecond pulses. Ultra-short pulses were launched to a bare tapered optical fiber and delivered to the sample. The tip-sample distance was controlled by means of shear-force feedback. Consequently, ablation craters with submicrometer dimensions were obtained. Potential analytical applications for Laser Induced Breakdown Spectroscopy (LIBS) technique, such as e.g. inclusions in steel or bio cells, are suggested

Green-synthetized silver nanoparticles for Nanoparticle-Enhanced Laser Induced Breakdown Spectroscopy (NELIBS) using a mobile instrument

Science.gov (United States)

Poggialini, F.; Campanella, B.; Giannarelli, S.; Grifoni, E.; Legnaioli, S.; Lorenzetti, G.; Pagnotta, S.; Safi, A.; Palleschi, V.

2018-03-01

When compared to other analytical techniques, LIBS shows relatively low precision and, generally, high Limits of Detection (LODs). Until recently, the attempts in improving the LIBS performances have been based on the use of more stable/powerful lasers, high sensitivity detectors or controlled environmental parameters. This can hinder the competitiveness of LIBS by increasing the instrumental setup cost and the difficulty of operation. Sample treatment has proved to be a viable and simple way to increase the LIBS signal; in particular, the Nanoparticle-Enhanced Laser Induced Breakdown Spectroscopy (NELIBS) methodology uses a deposition of metal nanoparticles on the sample to greatly increase the emission of the LIBS plasma. In this work, we used a simple, fast, "green" and low-cost method to synthetize silver nanoparticles by using coffee extract as reducing agents for a silver nitrate solution. This allowed us to obtain nanoparticles of about 25 nm in diameter. We then explored the application of such nanoparticles to the NELIBS analysis of metallic samples with a mobile LIBS instrument. By adjusting the laser parameters and optimizing the sample preparation procedure, we obtained a NELIBS signal that is 4 times the LIBS one. This showed the potential of green-synthetized nanoparticle for NELIBS applications and suggests the possibility of an in-situ application of the technique.

Development of laser induced breakdown spectroscopy for studying erosion, deposition, and fuel retention in ASDEX Upgrade

Energy Technology Data Exchange (ETDEWEB)

Paris, Peeter; Piip, Kaarel [Institute of Physics, University of Tartu, Tartu (Estonia); Hakola, Antti [VTT Technical Research Centre of Finland, Espoo (Finland); Laan, Matti, E-mail: matti.laan@ut.ee [Institute of Physics, University of Tartu, Tartu (Estonia); Aints, Märt [Institute of Physics, University of Tartu, Tartu (Estonia); Koivuranta, Seppo; Likonen, Jari [VTT Technical Research Centre of Finland, Espoo (Finland); Lissovski, Aleksandr [Institute of Physics, University of Tartu, Tartu (Estonia); Mayer, Matej [Max-Planck-Institut für Plasmaphysik, Garching (Germany); Neu, Rudolf [Max-Planck-Institut für Plasmaphysik, Garching (Germany); Technische Universität München, Fachgebt Plasma-Material-Wechelwirkung, Garching (Germany); Rohde, Volker; Sugiyama, Kazuyoshi [Max-Planck-Institut für Plasmaphysik, Garching (Germany)

2015-10-15

Highlights: • LIBS development for in situ monitoring of first walls of fusion reactors. • Testing of samples extracted from the divertor tiles of ASDEX Upgrade. • Reliable detection of deuterium depth profiles. • A method of LIBS data processing which allows to find the elemental depth profiles. • Comparison of LIBS results with those of other surface characterization methods. - Abstract: The paper deals with the development of laser induced breakdown spectroscopy (LIBS) into an in situ method for studying erosion/deposition processes at the first walls of fusion reactors. To this end, samples extracted from the divertor tiles of ASDEX Upgrade after the 2009 plasma operations were analyzed using LIBS for their composition and the results were compared with other post mortem deposition data. Quantitative depth profiles for the elemental concentrations were extracted from LIBS spectra by applying a novel data processing method. In addition, both multiline and multispot averaging procedures were applied to reduce fluctuations in the data. The LIBS concentration profiles matched qualitatively with those given by secondary ion mass spectrometry and quantitatively with the ion-beam data. The deuterium content of the samples could be reliably determined if the surface densities were >10{sup 17} at/cm{sup 2}.

Establishment of the laser induced breakdown spectroscopy in a vacuum atmosphere for a accuracy improvement

International Nuclear Information System (INIS)

Kim, Seung Hyun; Kim, H. D.; Shin, H. S.

2009-06-01

This report describes the fundamentals of the Laser Induced Breakdown Spectroscopy(LIBS), and it describes the quantitative analysis method in the vacuum condition to obtain a high measurement accuracy. The LIBS system employs the following major components: a pulsed laser, a gas chamber, an emission spectrometer, a detector, and a computer. When the output from a pulsed laser is focused onto a small spot on a sample, an optically induced plasma, called a laser-induced plasma (LIP) is formed at the surface. The LIBS is a laser-based sensitive optical technique used to detect certain atomic and molecular species by monitoring the emission signals from a LIP. This report was described a fundamentals of the LIBS and current states of research. And, It was described a optimization of measurement condition and characteristic analysis of a LIP by measurement of the fundamental metals. The LIBS system shows about a 0.63 ∼ 5.82% measurement errors and calibration curve for the 'Cu, Cr and Ni'. It also shows about a 5% less of a measurement errors and calibration curve for a Nd and Sm. As a result, the LIBS accuracy for a part was little improved than preexistence by the optimized condition

[Quantitative analysis of Cu in water by collinear DP-LIBS].

Science.gov (United States)

Zheng, Mei-Lan; Yao, Ming-Yin; Chen, Tian-Bing; Lin, Yong-Zeng; Li, Wen-Bing; Liu, Mu-Hua

2014-07-01

The purpose of this research is to study the influence of double pulse laser induced breakdown spectroscopy (DP-LIBS) on the sensitivity of Cu in water. The water solution of Cu was tested by collinear DP-LIBS in this article. The results show that spectral intensity of Cu can be enhanced obviously by DP-LIBS, compared with single pulse laser induced breakdown spectroscopy (SP-LIBS). Besides, the experimental results were significantly impacted by delay time between laser pulse and spectrometer acquisition, delay time of double laser pulse and energy of laser pulse and so on. The paper determined the best conditions for DP-LIBS detecting Cu in water. The optimal acquisition delay time was 1 380 ns. The best laser pulse delay time was 25 ns. The most appropriate energy of double laser pulse was 100 mJ. Characteristic analysis of spectra of Cu at 324.7 and 327.4 nm was done for quantitative analysis. The detection limit was 3.5 microg x mL(-1) at 324.7 nm, and the detection limit was 4.84 microg x mL(-1) at 327.4 nm. The relative standard deviation of the two characteristic spectral lines was within 10%. The calibration curve of characteristic spectral line, established by 327.4 nm, was verified with 500 microg x mL(-1) sample. Concentration of the sample was 446 microg x mL(-1) calculated by the calibration curve. This research shows that the detection sensitivity of Cu in water can be improved by DP-LIBS. At the same time, it had high stability.

Validation of the solidifying soil process using laser-induced breakdown spectroscopy

Science.gov (United States)

Lin, Zhao-Xiang; Liu, Lin-Mei; Liu, Lu-Wen

2016-09-01

Although an Ionic Soil Stabilizer (ISS) has been widely used in landslide control, it is desirable to effectively monitor the stabilization process. With the application of laser-induced breakdown spectroscopy (LIBS), the ion contents of K, Ca, Na, Mg, Al, and Si in the permeable fluid are detected after the solidified soil samples have been permeated. The processes of the Ca ion exchange are analyzed at pressures of 2 and 3 atm, and it was determined that the cation exchanged faster as the pressure increased. The Ca ion exchanges were monitored for different stabilizer mixtures, and it was found that a ratio of 1:200 of ISS to soil is most effective. The investigated plasticity and liquidity indexes also showed that the 1:200 ratio delivers the best performance. The research work indicates that it is possible to evaluate the engineering performances of soil solidified by ISS in real time and online by LIBS.

Development of a mobile system based on laser-induced breakdown spectroscopy and dedicated to in situ analysis of polluted soils

International Nuclear Information System (INIS)

Bousquet, B.; Travaille, G.; Ismael, A.; Canioni, L.; Michel-Le Pierres, K.; Brasseur, E.; Roy, S.; Le Hecho, I.; Larregieu, M.; Tellier, S.; Potin-Gautier, M.; Boriachon, T.; Wazen, P.; Diard, A.; Belbeze, S.

2008-01-01

Principal Components Analysis (PCA) is successfully applied to the full laser-induced breakdown spectroscopy (LIBS) spectra of soil samples, defining classes according to the concentrations of the major elements. The large variability of the LIBS data is related to the heterogeneity of the samples and the representativeness of the data is finally discussed. Then, the development of a mobile LIBS system dedicated to the in-situ analysis of soils polluted by heavy metals is described. Based on the use of ten-meter long optical fibers, the mobile system allows deported measurements. Finally, the laser-assisted drying process studied by the use of a customized laser has not been retained to overcome the problem of moisture

Development of a mobile system based on laser-induced breakdown spectroscopy and dedicated to in situ analysis of polluted soils

Science.gov (United States)

Bousquet, B.; Travaillé, G.; Ismaël, A.; Canioni, L.; Michel-Le Pierrès, K.; Brasseur, E.; Roy, S.; le Hecho, I.; Larregieu, M.; Tellier, S.; Potin-Gautier, M.; Boriachon, T.; Wazen, P.; Diard, A.; Belbèze, S.

2008-10-01

Principal Components Analysis (PCA) is successfully applied to the full laser-induced breakdown spectroscopy (LIBS) spectra of soil samples, defining classes according to the concentrations of the major elements. The large variability of the LIBS data is related to the heterogeneity of the samples and the representativeness of the data is finally discussed. Then, the development of a mobile LIBS system dedicated to the in-situ analysis of soils polluted by heavy metals is described. Based on the use of ten-meter long optical fibers, the mobile system allows deported measurements. Finally, the laser-assisted drying process studied by the use of a customized laser has not been retained to overcome the problem of moisture.

KARAKTERISASI SPEKTRUM UNSUR Cu UNTUK MENGHITUNG INTENSITAS EMISI ATOM FUNGSI WAKTU TUNDA DENGAN MENGGUNAKAN METODE LASER INDUCED BREAKDOWN SPECTROSCOPY (LIBS

Directory of Open Access Journals (Sweden)

Wulansari Efrilinda Diah

2013-08-01

Full Text Available Laser-Induced Breakdown Spectroscopy (LIBS is a spectroscopic method is highly reliable for atomic spectrochemical analysis both qualitatively and quantitatively. To achieve this, be aware of the detection parameters, one of which is a function of the atom emission intensity of detection delay time. In this study, plasma is generated by focusing the Nd-YAG laser (1064 nm, 7 ns on the surface of solid Cu sample with 99.99% purity level at 1 atm pressure air environment. Plasma emission spectrometer was arrested by elements of Cu + HR 2500 with specifications: (wavelength range 200-870 nm, resolution 0.1 nm (FWHM, 7 detector CCDs with a combined 14.336 pixels with variation detection delay time 0, 0.5, 1, 1.5, and 2 microseconds after the plasma formation and the energy varies the 60-160mJ. The data showed that the value of the Cu atom emission intensity 521.8 nm of the most highly visible on detection delay time decreased to 0.5 microseconds and detection delay time 2 microseconds. Based on these data it can be concluded that the characterization of the elements Cu to calculate the intensity was in the range of 100-140 mJ laser energy and time delay detection of 0.5 microseconds.

Monitoring of toxic elements present in sludge of industrial waste using CF-LIBS.

Science.gov (United States)

Kumar, Rohit; Rai, Awadhesh K; Alamelu, Devanathan; Aggarwal, Suresh K

2013-01-01

Industrial waste is one of the main causes of environmental pollution. Laser-induced breakdown spectroscopy (LIBS) was applied to detect the toxic metals in the sludge of industrial waste water. Sludge on filter paper was obtained after filtering the collected waste water samples from different sections of a water treatment plant situated in an industrial area of Kanpur City. The LIBS spectra of the sludge samples were recorded in the spectral range of 200 to 500 nm by focusing the laser light on sludge. Calibration-free laser-induced breakdown spectroscopy (CF-LIBS) technique was used for the quantitative measurement of toxic elements such as Cr and Pb present in the sample. We also used the traditional calibration curve approach to quantify these elements. The results obtained from CF-LIBS are in good agreement with the results from the calibration curve approach. Thus, our results demonstrate that CF-LIBS is an appropriate technique for quantitative analysis where reference/standard samples are not available to make the calibration curve. The results of the present experiment are alarming to the people living nearby areas of industrial activities, as the concentrations of toxic elements are quite high compared to the admissible limits of these substances.

Application and development of laser induced breakdown spectroscopy (LIBS) instrumentation for international safeguards

Energy Technology Data Exchange (ETDEWEB)

Barefield, II, James E.; Le, Loan; Lopez, Leon; Jolin, John L.; Clegg, Samuel M. [Chemical Diagnostic and Engineering and Physical Chemistry and Spectroscopy Los Alamos National Laboratory, Los Alamos, (United States)

2011-12-15

Advanced methodologies and improvements to current measurements techniques are needed to strengthen the effectiveness and efficiency of international safeguards. The primary tool employed by the IAEA to detect undeclared processes and activities at special nuclear material facilities and sites still is environmental sampling. This type of environmental sampling is both time consuming and costly since many samples must be collected, packaged, and shipped to an analytical laboratory for analysis that in some cases can take weeks to months to complete. Los Alamos National Laboratory is currently investigating potential uses of LIBS for safeguards applications, including(1) a user-friendly man-portable LIBS system to characterize samples in real to near-real time (typical analysis time are on the order of minutes) across a wide range of elements in the periodic table from hydrogen up to heavy elements like plutonium and uranium, (2) a LIBS system that can be deployed in harsh environments such as hot cells and glove boxes providing relative compositional analysis of process streams for example, ratios like Cm Division-Slash Pu and Cm Division-Slash / U, (3) an inspector field deployable system that can be used to analyze microscopic and single particle samples containing plutonium and uranium, and (4) a high resolution LIBS system that can be used to determine the isotopic composition of samples containing for example uranium and plutonium. In this paper, we will describe our current development and performance testing results for LIBS instrumentation both in a fixed lab and measurements in field deployable configurations.

Application of a compact diode pumped solid-state laser source for quantitative laser-induced breakdown spectroscopy analysis of steel

Science.gov (United States)

Tortschanoff, Andreas; Baumgart, Marcus; Kroupa, Gerhard

2017-12-01

Laser-induced breakdown spectroscopy (LIBS) technology holds the potential for onsite real-time measurements of steel products. However, for a mobile and robust LIBS measurement system, an adequate small and ruggedized laser source is a key requirement. In this contribution, we present tests with our compact high-power laser source, which, initially, was developed for ignition applications. The CTR HiPoLas® laser is a robust diode pumped solid-state laser with a passive Q-switch with dimensions of less than 10 cm3. The laser generates 2.5-ns pulses with 30 mJ at a maximum continuous repetition rate of about 30 Hz. Feasibility of LIBS experiments with the laser source was experimentally verified with steel samples. The results show that the laser with its current optical output parameters is very well-suited for LIBS measurements. We believe that the miniaturized laser presented here will enable very compact and robust portable high-performance LIBS systems.

Laser-induced breakdown spectroscopy measurements of uranium and thorium powders and uranium ore

Energy Technology Data Exchange (ETDEWEB)

Judge, Elizabeth J. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Barefield, James E., E-mail: jbarefield@lanl.gov [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Berg, John M. [Manufacturing Engineering and Technology Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Clegg, Samuel M.; Havrilla, George J.; Montoya, Velma M.; Le, Loan A.; Lopez, Leon N. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

2013-05-01

Laser-induced breakdown spectroscopy (LIBS) was used to analyze depleted uranium and thorium oxide powders and uranium ore as a potential rapid in situ analysis technique in nuclear production facilities, environmental sampling, and in-field forensic applications. Material such as pressed pellets and metals, has been extensively studied using LIBS due to the high density of the material and more stable laser-induced plasma formation. Powders, on the other hand, are difficult to analyze using LIBS since ejection and removal of the powder occur in the laser interaction region. The capability of analyzing powders is important in allowing for rapid analysis of suspicious materials, environmental samples, or trace contamination on surfaces since it most closely represents field samples (soil, small particles, debris etc.). The rapid, in situ analysis of samples, including nuclear materials, also reduces costs in sample collection, transportation, sample preparation, and analysis time. Here we demonstrate the detection of actinides in oxide powders and within a uranium ore sample as both pressed pellets and powders on carbon adhesive discs for spectral comparison. The acquired LIBS spectra for both forms of the samples differ in overall intensity but yield a similar distribution of atomic emission spectral lines. - Highlights: • LIBS analysis of mixed actinide samples: depleted uranium oxide and thorium oxide • LIBS analysis of actinide samples in powder form on carbon adhesive discs • Detection of uranium in a complex matrix (uranium ore) as a precursor to analyzing uranium in environmental samples.

Independent component analysis classification of laser induced breakdown spectroscopy spectra

International Nuclear Information System (INIS)

Forni, Olivier; Maurice, Sylvestre; Gasnault, Olivier; Wiens, Roger C.; Cousin, Agnès; Clegg, Samuel M.; Sirven, Jean-Baptiste; Lasue, Jérémie

2013-01-01

The ChemCam instrument on board Mars Science Laboratory (MSL) rover uses the laser-induced breakdown spectroscopy (LIBS) technique to remotely analyze Martian rocks. It retrieves spectra up to a distance of seven meters to quantify and to quantitatively analyze the sampled rocks. Like any field application, on-site measurements by LIBS are altered by diverse matrix effects which induce signal variations that are specific to the nature of the sample. Qualitative aspects remain to be studied, particularly LIBS sample identification to determine which samples are of interest for further analysis by ChemCam and other rover instruments. This can be performed with the help of different chemometric methods that model the spectra variance in order to identify a the rock from its spectrum. In this paper we test independent components analysis (ICA) rock classification by remote LIBS. We show that using measures of distance in ICA space, namely the Manhattan and the Mahalanobis distance, we can efficiently classify spectra of an unknown rock. The Mahalanobis distance gives overall better performances and is easier to manage than the Manhattan distance for which the determination of the cut-off distance is not easy. However these two techniques are complementary and their analytical performances will improve with time during MSL operations as the quantity of available Martian spectra will grow. The analysis accuracy and performances will benefit from a combination of the two approaches. - Highlights: • We use a novel independent component analysis method to classify LIBS spectra. • We demonstrate the usefulness of ICA. • We report the performances of the ICA classification. • We compare it to other classical classification schemes

Laser-induced breakdown spectroscopy applied to the characterization of rock by support vector machine combined with principal component analysis

International Nuclear Information System (INIS)

Yang Hong-Xing; Fu Hong-Bo; Wang Hua-Dong; Jia Jun-Wei; Dong Feng-Zhong; Sigrist, Markus W

2016-01-01

Laser-induced breakdown spectroscopy (LIBS) is a versatile tool for both qualitative and quantitative analysis. In this paper, LIBS combined with principal component analysis (PCA) and support vector machine (SVM) is applied to rock analysis. Fourteen emission lines including Fe, Mg, Ca, Al, Si, and Ti are selected as analysis lines. A good accuracy (91.38% for the real rock) is achieved by using SVM to analyze the spectroscopic peak area data which are processed by PCA. It can not only reduce the noise and dimensionality which contributes to improving the efficiency of the program, but also solve the problem of linear inseparability by combining PCA and SVM. By this method, the ability of LIBS to classify rock is validated. (paper)

Phosphate ore beneficiation via determination of phosphorus-to-silica ratios by Laser Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Asimellis, George; Giannoudakos, Aggelos; Kompitsas, Michael

2006-01-01

We report development and application of an in-situ applicable method to determine phosphate ore rock quality based on Laser-Induced Breakdown Spectroscopy (LIBS). This is an economically viable method for real-time evaluation of ore phosphate rocks in order to separate high-silica pebbles prior to deep beneficiation. This is achieved by monitoring relative emission line intensities from key probe elements via single laser ablation shots: the ratio of the phosphorous to silica line intensities (P/Si ratio) provides a simple and reliable indicator of ore rock quality. This is a unique LIBS application where no other current analytical spectroscopic method (ICP or XRF) can be applied. Method development is discussed, and results with actual ore samples are presented

Speciation analysis on Eu(3) in aqueous solution using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Hotokezaka, H.; Tanaka, S.; Nagasaki, S.

2001-01-01

Investigation of the chemical behaviour of lanthanides and actinides in the geosphere is important for the safety assessment of high-level radioactive waste disposal. However, determination of speciation for lanthanides and actinides is difficult, because it is too hard to distinguish between metal ion and colloidal metal in aqueous solution. Laser-induced breakdown spectroscopy (LIBS) can detect both ions and microparticles of metals in aqueous solution, especially, high sensitive to microparticles. In this study, we analysed Eu(III) ion and Eu 2 O 3 particle in aqueous solution by LIBS, and measured the hydrolysis behaviour of Eu(III) in aqueous solution. Furthermore, we tried to detect the plasma emission of Eu(III) ions sorbed on TiO 2 particles, and also tried to observe the adsorption behaviour of Eu(III) ions onto TiO 2 particles in aqueous solution. (authors)

Characterization of hard coatings produced by laser cladding using laser-induced breakdown spectroscopy technique

Science.gov (United States)

Varela, J. A.; Amado, J. M.; Tobar, M. J.; Mateo, M. P.; Yañez, A.; Nicolas, G.

2015-05-01

Protective coatings with a high abrasive wear resistance can be obtained from powders by laser cladding technique, in order to extend the service life of some industrial components. In this work, laser clad layers of self-fluxing NiCrBSi alloy powder mixed with WC powder have been produced on stainless steel substrates of austenitic type (AISI 304) in a first step and then chemically characterized by laser-induced breakdown spectroscopy (LIBS) technique. With the suitable laser processing parameters (mainly output power, beam scan speed and flow rate) and powders mixture proportions between WC ceramics and NiCrBSi alloys, dense pore free layers have been obtained on single tracks and on large areas with overlapped tracks. The results achieved by LIBS technique and applied for the first time to the analysis of laser clads provided the chemical composition of the tungsten carbides in metal alloy matrix. Different measurement modes (multiple point analyses, depth profiles and chemical maps) have been employed, demonstrating the usefulness of LIBS technique for the characterization of laser clads based on hardfacing alloys. The behavior of hardness can be explained by LIBS maps which evidenced the partial dilution of some WC spheres in the coating.

Understanding the signature of rock coatings in laser-induced breakdown spectroscopy data

Science.gov (United States)

Lanza, Nina L.; Ollila, Ann M.; Cousin, Agnes; Wiens, Roger C.; Clegg, Samuel M.; Mangold, Nicolas; Bridges, Nathan; Cooper, Daniel; Schmidt, Mariek E.; Berger, Jeffrey; Arvidson, Raymond E.; Melikechi, Noureddine; Newsom, Horton E.; Tokar, Robert; Hardgrove, Craig; Mezzacappa, Alissa; Jackson, Ryan S.; Clark, Benton C.; Forni, Olivier; Maurice, Sylvestre; Nachon, Marion; Anderson, Ryan B.; Blank, Jennifer; Deans, Matthew; Delapp, Dorothea; Léveillé, Richard; McInroy, Rhonda; Martinez, Ronald; Meslin, Pierre-Yves; Pinet, Patrick

2015-01-01

Surface compositional features on rocks such as coatings and weathering rinds provide important information about past aqueous environments and water–rock interactions. The search for these features represents an important aspect of the Curiosity rover mission. With its unique ability to do fine-scale chemical depth profiling, the ChemCam laser-induced breakdown spectroscopy instrument (LIBS) onboard Curiosity can be used to both identify and analyze rock surface alteration features. In this study we analyze a terrestrial manganese-rich rock varnish coating on a basalt rock in the laboratory with the ChemCam engineering model to determine the LIBS signature of a natural rock coating. Results show that there is a systematic decrease in peak heights for elements such as Mn that are abundant in the coating but not the rock. There is significant spatial variation in the relative abundance of coating elements detected by LIBS depending on where on the rock surface sampled; this is due to the variability in thickness and spatial discontinuities in the coating. Similar trends have been identified in some martian rock targets in ChemCam data, suggesting that these rocks may have coatings or weathering rinds on their surfaces.

Signal enhancement in collinear double-pulse laser-induced breakdown spectroscopy applied to different soils

Energy Technology Data Exchange (ETDEWEB)

Nicolodelli, Gustavo, E-mail: gunicolodelli@hotmail.com [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil); Senesi, Giorgio Saverio, E-mail: giorgio.senesi@imip.cnr.it [Institute of Inorganic Methodologies and Plasmas, CNR, Bari, 70126 Bari (Italy); Romano, Renan Arnon, E-mail: renan.romano@gmail.com [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil); Physics Institute of São Carlos, University of São Paulo, IFSC-USP, Av. Trabalhador são-carlense, 400 Pq. Arnold Schimid, 13566-590 São Carlos, SP (Brazil); Oliveira Perazzoli, Ivan Luiz de, E-mail: ivanperazzoli@hotmail.com [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil); Milori, Débora Marcondes Bastos Pereira, E-mail: debora.milori@embrapa.br [Embrapa Instrumentation, Rua XV de Novembro, 1452, CEP 13560-970 São Carlos, SP (Brazil)

2015-09-01

Laser-induced breakdown spectroscopy (LIBS) is a well-known consolidated analytical technique employed successfully for the qualitative and quantitative analysis of solid, liquid, gaseous and aerosol samples of very different nature and origin. Several techniques, such as dual-pulse excitation setup, have been used in order to improve LIBS's sensitivity. The purpose of this paper was to optimize the key parameters as excitation wavelength, delay time and interpulse, that influence the double pulse (DP) LIBS technique in the collinear beam geometry when applied to the analysis at atmospheric air pressure of soil samples of different origin and texture from extreme regions of Brazil. Additionally, a comparative study between conventional single pulse (SP) LIBS and DP LIBS was performed. An optimization of DP LIBS system, choosing the correct delay time between the two pulses, was performed allowing its use for different soil types and the use of different emission lines. In general, the collinear DP LIBS system improved the analytical performances of the technique by enhancing the intensity of emission lines of some elements up to about 5 times, when compared with conventional SP-LIBS, and reduced the continuum emission. Further, the IR laser provided the best performance in re-heating the plasma. - Highlights: • The correct choice of the delay time between the two pulses is crucial for the DP system. • An optimization of DP LIBS system was performed allowing its use for different soil and the use of different emission lines. • The DP LIBS system improved the analytical performances of the technique up to about 5 times, when compared with SP LIBS. • The IR laser provided the best performance in re-heating the plasma.

[Comparative investigation of underwater-LIBS using 532 and 1 064 nm lasers].

Science.gov (United States)

Song, Jiao-Jian; Tian, Ye; Lu, Yuan; Li, Ying; Zheng, Rong-Er

2014-11-01

With the hope of applying laser induced breakdown spectroscopy (LIBS) to the ocean applications, the laser energy at 532 and 1 064 nm wavelength with 3 and 40 mj respectively was used, which was near their breakdown threshold. Extensive experimental investigations of LIBS from CaCl2 water solution were carried out in this paper using different laser wavelengths of 532 and 1 064 nm. The obtained results show that compared with the 532 nm laser, the 1 064 nm laser can induce the plasma in water with higher emission intensity and longer lifetime, while the reproducibility of LIBS signal under 1 064 nm laser is poorer. On the other hand, due to the different attenuation ratios of 532 and 1 064 nm laser energies in water, the LIBS signal of 1 064 nm laser decreases a lot within the transmission distance range 2-5 cm, while LIBS signal of 532 nm remains the same, because that the wavelength of 532 nm lies in the "transmission window" of the water solution. This study will provide valuable design considerations for the development of LIBS-sea system in near future.

Identification of inks and structural characterization of contemporary artistic prints by laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Oujja, M.; Vila, A.; Rebollar, E.; Garcia, J.F.; Castillejo, M.

2005-01-01

Identification of the inks used in artistic prints and the order in which different ink layers have been applied on a paper substrate are important factors to complement the classical stylistic aspects for the authentication of this type of objects. Laser-induced breakdown spectroscopy (LIBS) is investigated to determine the chemical composition and structural distribution of the constituent materials of model prints made by applying one or two layers of several blue and black inks on an Arches paper substrate. By using suitable laser excitation conditions, identification of the inks was possible by virtue of emissions from key elements present in their composition. Analysis of successive spectra on the same spot allowed the identification of the order in which the inks were applied on the paper. The results show the potential of laser-induced breakdown spectroscopy for the chemical and structural characterization of artistic prints

LIBS coupled with ICP/OES for the spectral analysis of betel leaves

Science.gov (United States)

Rehan, I.; Rehan, K.; Sultana, S.; Khan, M. Z.; Muhammad, R.

2018-05-01

Laser-induced breakdown spectroscopy (LIBS) system was optimized and was applied for the elemental analysis and exposure of the heavy metals in betel leaves in air. Pulsed Nd:YAG (1064 nm) in conjunction with a suitable detector (LIBS 2000+, Ocean Optics, Inc) having the optical resolution of 0.06 nm was used to record the emission spectra from 200 to 720 nm. Elements like Al, Ba, Ca, Cr, Cu, P, Fe, K, Mg, Mn, Na, P, S, Sr, and Zn were found to be present in the samples. The abundances of observed elements were calculated through normalized calibration curve method, integrated intensity ratio method, and calibration free-LIBS approach. Quantitative analyses were accomplished under the assumption of local thermodynamic equilibrium (LTE) and optically thin plasma. LIBS findings were validated by comparing its results with the results obtained using a typical analytical technique of inductively coupled plasma-optical emission spectroscopy (ICP/OES). Limit of detection (LOD) of the LIBS system was also estimated for heavy metals.

All-fiber-coupled laser-induced breakdown spectroscopy sensor for hazardous materials analysis

Energy Technology Data Exchange (ETDEWEB)

Bohling, Christian [Institut fuer Physik und Physikalische Technologien, Technische Universitaet Clausthal, Leibnizstrasse 4, 38678 Clausthal-Zellerfeld (Germany); SECOPTA GmbH, Ostendstr. 25, 12459 Berlin (Germany)], E-mail: c.bohling@pe.tu-clausthal.de; Hohmann, Konrad [Institut fuer Physik und Physikalische Technologien, Technische Universitaet Clausthal, Leibnizstrasse 4, 38678 Clausthal-Zellerfeld (Germany)], E-mail: k.hohmann@pe.tu-clausthal.de; Scheel, Dirk [Systektum GmbH, Arnold-Sommerfeld-Str. 6, 38678 Clausthal-Zellerfeld (Germany)], E-mail: d.scheel@systektum.de; Bauer, Christoph [LaserAnwendungsCentrum (LAC) Technische Universitaet Clausthal, Arnold-Sommerfeld-Strasse 6, 38678 Clausthal-Zellerfeld (Germany)], E-mail: c.bauer@pe.tu-clausthal.de; Schippers, Wolfgang [Institut fuer Physik und Physikalische Technologien, Technische Universitaet Clausthal, Leibnizstrasse 4, 38678 Clausthal-Zellerfeld (Germany)], E-mail: w.schippers@pe.tu-clausthal.de; Burgmeier, Joerg [LaserAnwendungsCentrum (LAC) Technische Universitaet Clausthal, Arnold-Sommerfeld-Strasse 6, 38678 Clausthal-Zellerfeld (Germany)], E-mail: j.burgmeier@pe.tu-clausthal.de; Willer, Ulrike [Institut fuer Physik und Physikalische Technologien, Technische Universitaet Clausthal, Leibnizstrasse 4, 38678 Clausthal-Zellerfeld (Germany); LaserAnwendungsCentrum (LAC) Technische Universitaet Clausthal, Arnold-Sommerfeld-Strasse 6, 38678 Clausthal-Zellerfeld (Germany)], E-mail: u.willer@pe.tu-clausthal.de; Holl, Gerhard [Wehrwissenschaftliches Institut fuer Werk-, Explosiv- und Betriebsstoffe (WIWEB), Grosses Cent, 53913, Swisttal (Germany)], E-mail: gerhardholl@bwb.orgd; Schade, Wolfgang [Institut fuer Physik und Physikalische Technologien, Technische Universitaet Clausthal, Leibnizstrasse 4, 38678 Clausthal-Zellerfeld (Germany); LaserAnwendungsCentrum (LAC) Technische Universitaet Clausthal, Arnold-Sommerfeld-Strasse 6, 38678 Clausthal-Zellerfeld (Germany)], E-mail: w.schade@pe.tu-clausthal.de

2007-12-15

An all-fiber-coupled laser-induced breakdown spectroscopy (LIBS) sensor device is developed. A passively Q-switched Cr{sup 4+}Nd{sup 3+}:YAG microchip laser is amplified within an Yb fiber amplifier, thus generating high power laser pulses (pulse energy E{sub p} = 0.8 mJ, wavelength {lambda} = 1064 nm, repetition rate f{sub rep.} = 5 kHz, pulse duration t{sub p} = 1.2 ns). A passive (LMA) optical fiber is spliced to the active fiber of an Yb fiber amplifier for direct guiding of high power laser pulses to the sensor tip. In front of the sensor a plasma is generated on the surface to be analyzed. The plasma emission is collected by a set of optical fibers also integrated into the sensor tip. The spectrally resolved LIBS spectra are processed by application of principal component analysis (PCA) and analyzed together with the time-resolved spectra with neural networks. Such procedure allows accurate analysis of samples by LIBS even for materials with similar atomic composition. The system has been tested successfully during field measurements at the German Armed Forces test facility at Oberjettenberg. The LIBS sensor is not restricted to anti-personnel mine detection but has also the potential to be suitable for analysis of bulk explosives and surface contaminations with explosives, e.g. for the detection of improvised explosive devices (IEDs)

Portable laser-induced breakdown spectroscopy/diffuse reflectance hybrid spectrometer for analysis of inorganic pigments

Science.gov (United States)

Siozos, Panagiotis; Philippidis, Aggelos; Anglos, Demetrios

2017-11-01

A novel, portable spectrometer, combining two analytical techniques, laser-induced breakdown spectroscopy (LIBS) and diffuse reflectance spectroscopy, was developed with the aim to provide an enhanced instrumental and methodological approach with regard to the analysis of pigments in objects of cultural heritage. Technical details about the hybrid spectrometer and its operation are presented and examples are given relevant to the analysis of paint materials. Both LIBS and diffuse reflectance spectra in the visible and part of the near infrared, corresponding to several neat mineral pigment samples, were recorded and the complementary information was used to effectively distinguish different types of pigments even if they had similar colour or elemental composition. The spectrometer was also employed in the analysis of different paints on the surface of an ancient pottery sherd demonstrating the capabilities of the proposed hybrid diagnostic approach. Despite its instrumental simplicity and compact size, the spectrometer is capable of supporting analytical campaigns relevant to archaeological, historical or art historical investigations, particularly when quick data acquisition is required in the context of surveys of large numbers of objects and samples.

Evaluation of the standard normal variate method for Laser-Induced Breakdown Spectroscopy data treatment applied to the discrimination of painting layers

Science.gov (United States)

Syvilay, D.; Wilkie-Chancellier, N.; Trichereau, B.; Texier, A.; Martinez, L.; Serfaty, S.; Detalle, V.

2015-12-01

Nowadays, Laser-Induced Breakdown Spectroscopy (LIBS) is frequently used for in situ analyses to identify pigments from mural paintings. Nonetheless, in situ analyses require a robust instrumentation in order to face to hard experimental conditions. This may imply variation of fluencies and thus inducing variation of LIBS signal, which degrades spectra and then results. Usually, to overcome these experimental errors, LIBS signal is processed. Signal processing methods most commonly used are the baseline subtraction and the normalization by using a spectral line. However, the latter suggests that this chosen element is a constant component of the material, which may not be the case in paint layers organized in stratigraphic layers. For this reason, it is sometimes difficult to apply this normalization. In this study, another normalization will be carried out to throw off these signal variations. Standard normal variate (SNV) is a normalization designed for these conditions. It is sometimes implemented in Diffuse Reflectance Infrared Fourier Transform Spectroscopy and in Raman Spectroscopy but rarely in LIBS. The SNV transformation is not newly applied on LIBS data, but for the first time the effect of SNV on LIBS spectra was evaluated in details (energy of laser, shot by shot, quantification). The aim of this paper is the quick visualization of the different layers of a stratigraphic painting sample by simple data representations (3D or 2D) after SNV normalization. In this investigation, we showed the potential power of SNV transformation to overcome undesired LIBS signal variations but also its limit of application. This method appears as a promising way to normalize LIBS data, which may be interesting for in-situ depth analyses.

Use of Laser-Induced Breakdown Spectroscopy for the Detection of Glycemic Elements in Indian Medicinal Plants

Directory of Open Access Journals (Sweden)

Prashant Kumar Rai

2013-01-01

Full Text Available The demand for interdisciplinary research is increasing in the new millennium to help us understand complex problems and find solutions by integrating the knowledge from different disciplines. The present review is an excellent example of this and shows how unique combination of physics, chemistry, and biological techniques can be used for the evaluation of Indian medicinal herbs used for treating diabetes mellitus. Laser-induced breakdown spectroscopy (LIBS is a sensitive optical technique that is widely used for its simplicity and versatility. This review presents the most recent application of LIBS for detection of glycemic elements in medicinal plants. The characteristics of matrices, object analysis, use of laser system, and analytical performances with respect to Indian herbs are discussed.

Optimal conditions for taking spectra of coffee beans plasma spectroscopy induced by laser (LIBS)

International Nuclear Information System (INIS)

Diaz Guerrero, A. M.; Flores Reyes; Ponce Cabrera, L. V.

2016-01-01

Coffee beans, arabica and robusta, from Mexico (Chiapas and Veracruz), Colombia, Kenya and Sumatra were analyzed by Laser-induced breakdown spectroscopy (LIBS). The time delay and pulse energy were varied in order to find the optimal conditions for taking spectra in coffee beans; finding that the increased visibility of the peaks and the lowest electronic background is observed with 1 s and 450 mJ. Spectra were taken in different regions of grain area to confirm its homogeneous composition. It was found that the intensity of the signal Ca is much higher than that of K in African coffee, lower in the coffee of America, and much lower in the coffee from Asia. (Author)

Dispersive liquid-liquid microextraction for metals enrichment: a useful strategy for improving sensitivity of laser-induced breakdown spectroscopy in liquid samples analysis.

Science.gov (United States)

Aguirre, M A; Selva, E J; Hidalgo, M; Canals, A

2015-01-01

A rapid and efficient Dispersive Liquid-Liquid Microextraction (DLLME) followed by Laser-Induced Breakdown Spectroscopy detection (LIBS) was evaluated for simultaneous determination of Cr, Cu, Mn, Ni and Zn in water samples. Metals in the samples were extracted with tetrachloromethane as pyrrolidinedithiocarbamate (APDC) complexes, using vortex agitation to achieve dispersion of the extractant solvent. Several DLLME experimental factors affecting extraction efficiency were optimized with a multivariate approach. Under optimum DLLME conditions, DLLME-LIBS method was found to be of about 4.0-5.5 times more sensitive than LIBS, achieving limits of detection of about 3.7-5.6 times lower. To assess accuracy of the proposed DLLME-LIBS procedure, a certified reference material of estuarine water was analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.

Quantification of trace metals in infant formula premixes using laser-induced breakdown spectroscopy

Science.gov (United States)

Cama-Moncunill, Raquel; Casado-Gavalda, Maria P.; Cama-Moncunill, Xavier; Markiewicz-Keszycka, Maria; Dixit, Yash; Cullen, Patrick J.; Sullivan, Carl

2017-09-01

Infant formula is a human milk substitute generally based upon fortified cow milk components. In order to mimic the composition of breast milk, trace elements such as copper, iron and zinc are usually added in a single operation using a premix. The correct addition of premixes must be verified to ensure that the target levels in infant formulae are achieved. In this study, a laser-induced breakdown spectroscopy (LIBS) system was assessed as a fast validation tool for trace element premixes. LIBS is a promising emission spectroscopic technique for elemental analysis, which offers real-time analyses, little to no sample preparation and ease of use. LIBS was employed for copper and iron determinations of premix samples ranging approximately from 0 to 120 mg/kg Cu/1640 mg/kg Fe. LIBS spectra are affected by several parameters, hindering subsequent quantitative analyses. This work aimed at testing three matrix-matched calibration approaches (simple-linear regression, multi-linear regression and partial least squares regression (PLS)) as means for precision and accuracy enhancement of LIBS quantitative analysis. All calibration models were first developed using a training set and then validated with an independent test set. PLS yielded the best results. For instance, the PLS model for copper provided a coefficient of determination (R2) of 0.995 and a root mean square error of prediction (RMSEP) of 14 mg/kg. Furthermore, LIBS was employed to penetrate through the samples by repetitively measuring the same spot. Consequently, LIBS spectra can be obtained as a function of sample layers. This information was used to explore whether measuring deeper into the sample could reduce possible surface-contaminant effects and provide better quantifications.

Laser-induced breakdown spectroscopy used to detect endophyte-mediated accumulation of metals by tall fescue

Energy Technology Data Exchange (ETDEWEB)

Martin, Madhavi Z.; Stewart, Arthur J.; Gwinn, Kimberley D.; Waller, John C.

2010-05-01

Laser-induced breakdown spectroscopy (LIBS) was used to determine the impact of endophyte (Neotyphodium sp.) infection on elemental composition of tall fescue (Festuca arundinacea). Leaf material from endophyte-infected (E+) and endophyte-free (E-) tall fescue populations in established plots was examined. Leaf-tissue digestates were also tested for metals, by inductively coupled plasma (ICP) mass spectrometry (MS). Seven of eleven metals (Ca, Mg, Fe, Mn, Cu, Ni, and Zn) were measured by both techniques at concentrations great enough for a reliable comparison. Mg, Zn, and Cd, a toxic metal that can be present in forage, were readily detected by LIBS, even though Cd concentrations in the plants were below levels typically achieved using ICP MS detection. Implications of these results for research on forage analysis and phytoremediation are discussed.

Qualitative tissue differentiation by analysing the intensity ratios of atomic emission lines using laser induced breakdown spectroscopy (LIBS): prospects for a feedback mechanism for surgical laser systems.

Science.gov (United States)

Kanawade, Rajesh; Mahari, Fanuel; Klämpfl, Florian; Rohde, Maximilian; Knipfer, Christian; Tangermann-Gerk, Katja; Adler, Werner; Schmidt, Michael; Stelzle, Florian

2015-01-01

The research work presented in this paper focuses on qualitative tissue differentiation by monitoring the intensity ratios of atomic emissions using 'Laser Induced Breakdown Spectroscopy' (LIBS) on the plasma plume created during laser tissue ablation. The background of this study is to establish a real time feedback control mechanism for clinical laser surgery systems during the laser ablation process. Ex-vivo domestic pig tissue samples (muscle, fat, nerve and skin) were used in this experiment. Atomic emission intensity ratios were analyzed to find a characteristic spectral line for each tissue. The results showed characteristic elemental emission intensity ratios for the respective tissues. The spectral lines and intensity ratios of these specific elements varied among the different tissue types. The main goal of this study is to qualitatively and precisely identify different tissue types for tissue specific laser surgery. © 2015 The Authors. Journal of Biophotonics published by WILEY-VCH Verlag.

[Research on fast classification based on LIBS technology and principle component analyses].

Science.gov (United States)

Yu, Qi; Ma, Xiao-Hong; Wang, Rui; Zhao, Hua-Feng

2014-11-01

Laser-induced breakdown spectroscopy (LIBS) and the principle component analysis (PCA) were combined to study aluminum alloy classification in the present article. Classification experiments were done on thirteen different kinds of standard samples of aluminum alloy which belong to 4 different types, and the results suggested that the LIBS-PCA method can be used to aluminum alloy fast classification. PCA was used to analyze the spectrum data from LIBS experiments, three principle components were figured out that contribute the most, the principle component scores of the spectrums were calculated, and the scores of the spectrums data in three-dimensional coordinates were plotted. It was found that the spectrum sample points show clear convergence phenomenon according to the type of aluminum alloy they belong to. This result ensured the three principle components and the preliminary aluminum alloy type zoning. In order to verify its accuracy, 20 different aluminum alloy samples were used to do the same experiments to verify the aluminum alloy type zoning. The experimental result showed that the spectrum sample points all located in their corresponding area of the aluminum alloy type, and this proved the correctness of the earlier aluminum alloy standard sample type zoning method. Based on this, the identification of unknown type of aluminum alloy can be done. All the experimental results showed that the accuracy of principle component analyses method based on laser-induced breakdown spectroscopy is more than 97.14%, and it can classify the different type effectively. Compared to commonly used chemical methods, laser-induced breakdown spectroscopy can do the detection of the sample in situ and fast with little sample preparation, therefore, using the method of the combination of LIBS and PCA in the areas such as quality testing and on-line industrial controlling can save a lot of time and cost, and improve the efficiency of detection greatly.

Viability study of using the Laser-Induced Breakdown Spectroscopy technique for radioactive waste detection at IPEN-CNEN/SP, Brazil

International Nuclear Information System (INIS)

Tunes, Matheus A.; Schon, Claudio G.

2013-01-01

this work a viability study to apply the Laser-Induced Breakdown Spectroscopy (LIBS) technique for radioactive waste characterization was developed using a high power q-switched Nd:YAG rod-Laser, operating at 1064 nm with 9 ns of pulse-width and pulse-to-pulse energy around 10 to 20 mJ. When applied in a non-radioactive deionized water sample, our methodology exhibits a good potential to spectroscopy detection of Hydrogen species with resolution around 0.035 nm at full width at half maximum (FWHM). (author)

In situ Laser Induced Breakdown Spectroscopy as a tool to discriminate volcanic rocks and magmatic series, Iceland

Energy Technology Data Exchange (ETDEWEB)

Roux, C.P.M., E-mail: clement.roux@u-bourgogne.fr [Laboratoire interdisciplinaire Carnot de Bourgogne, UMR 6303 CNRS-Université de Bourgogne, BP 47 870, F-21078 Dijon Cedex (France); Rakovský, J.; Musset, O. [Laboratoire interdisciplinaire Carnot de Bourgogne, UMR 6303 CNRS-Université de Bourgogne, BP 47 870, F-21078 Dijon Cedex (France); Monna, F. [Laboratoire ARTéHIS, UMR 6298 CNRS-Université de Bourgogne, 6 Boulevard Gabriel, F-21000 Dijon (France); Buoncristiani, J.-F.; Pellenard, P.; Thomazo, C. [Laboratoire Biogéosciences, UMR 6282 CNRS-Université de Bourgogne, 6 Boulevard Gabriel, F-21000 Dijon (France)

2015-01-01

This study evaluates the potentialities of a lab-made pLIBS (portable Laser-Induced Breakdown Spectroscopy) to sort volcanic rocks belonging to various magmatic series. An in-situ chemical analysis of 19 atomic lines, including Al, Ba, Ca, Cr, Cu, Fe, Mg, Mn, Na, Si, Sr and Ti, from 21 sampled rocks was performed during a field exploration in Iceland. Iceland was chosen both for the various typologies of volcanic rocks and the rugged conditions in the field in order to test the sturdiness of the pLIPS. Elemental compositions were also measured using laboratory ICP-AES measurements on the same samples. Based on these latter results, which can be used to identify three different groups of volcanic rocks, a classification model was built in order to sort pLIBS data and to categorize unknown samples. Using a reliable statistical scheme applied to LIBS compositional data, the classification capability of the pLIBS system is clearly demonstrated (90–100% success rate). Although this prototype does not provide quantitative measurements, its use should be of particular interest for future geological field investigations. - Highlights: • Portable LIBS applied to field geology • Fast semi-quantitative geochemical analysis of volcanic rocks and magmatic series • Discriminant analysis and statistical treatments for LIBS compositional data.

Development of a Method for the Determination of Chromium and Cadmium in Tannery Wastewater Using Laser-Induced Breakdown Spectroscopy

Directory of Open Access Journals (Sweden)

Mahwish Bukhari

2012-01-01

Full Text Available This paper illustrates systematic development of a convenient analytical method for the determination of chromium and cadmium in tannery wastewater using laser-induced breakdown spectroscopy (LIBS. A new approach was developed by which liquid was converted into solid phase sample surface using absorption paper for subsequent LIBS analysis. The optimized values of LIBS parameters were 146.7 mJ for chromium and 89.5 mJ for cadmium (laser pulse energy, 4.5 μs (delay time, 70 mm (lens to sample surface distance, and 7 mm (light collection system to sample surface distance. Optimized values of LIBS parameters demonstrated strong spectrum lines for each metal keeping the background noise at minimum level. The new method of preparing metal standards on absorption papers exhibited calibration curves with good linearity with correlation coefficients, R2 in the range of 0.992 to 0.998. The developed method was tested on real tannery wastewater samples for determination of chromium and cadmium.

Influence of particle size and mineral phase in the analysis of iron ore slurries by Laser-Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Michaud, Daniel; Leclerc, Remi; Proulx, Eric

2007-01-01

Laser-Induced Breakdown Spectroscopy (LIBS) was applied to the analysis of iron ore concentrates. The objective was to determine the influence of particle size and mineral phase on the LIBS signal. The LIBS spectra of hematite and magnetite ore concentrates were qualitatively indistinguishable from each other but magnetite yielded systematically less than hematite. This behavior could be set into an empirical equation to correct the iron peak intensities according to the level of magnetite in the analyzed sample. Similarly, an increase of the LIBS signal was observed as the particle size of the ore samples decreased. Again, an equation could be written down to correct the intensity of either iron or silicon in response to a variation of the average particle size of the ore concentrate. Using these corrections, proper response of the silicon signal against the concentration of silica in the samples was restored. The observed dependence of the strength of the iron signal upon the mineral phase is attributed to oxidation of magnetite into hematite

Application of Laser Induced Breakdown Spectroscopy in Early Detection of Red Palm Weevil: (Rhynchophorus ferrugineus) Infestation in Date Palm

International Nuclear Information System (INIS)

Farooq, W. A.; Tawfik, Walid; Rasool, K. G.; Aldawood, A. S.

2015-01-01

The Kingdom of Saudi Arabia is one of the leading date producing countries. Unfortunately, this important fruit crop is under great threat from the red palm weevil (RPW) (Rhynchophorus ferrugineus), which is a highly invasive pest. Several techniques, including visual inspection, acoustic sensors, sniffer dogs, and pheromone traps have been tried to detect the early stages of a RPW infestation; however, each method has suffered certain logistical and implementation issues. We have applied laser induced breakdown spectroscopy (LIBS) for the early detection of RPW infestation. Through the analysis of the observed LIBS spectra of different infested and healthy samples, we have found presence of Ca, Mg, Na, C, K elements and OH, CN molecules. The spectra also reveal that with the population growth of the pest, the intensity of Mg and Ca atomic lines in LIBS spectra increases rapidly. Similar behavior is observed in the molecular lines of LIBS spectra. The obtained results indicate that the LIBS technique can be used for the early detection of RPW infestation without damaging the date palms. (paper)

Application of Laser Induced Breakdown Spectroscopy in Early Detection of Red Palm Weevil: (Rhynchophorus ferrugineus) Infestation in Date Palm

Science.gov (United States)

A. Farooq, W.; G. Rasool, K.; Walid, Tawfik; S. Aldawood, A.

2015-11-01

The Kingdom of Saudi Arabia is one of the leading date producing countries. Unfortunately, this important fruit crop is under great threat from the red palm weevil (RPW) (Rhynchophorus ferrugineus), which is a highly invasive pest. Several techniques, including visual inspection, acoustic sensors, sniffer dogs, and pheromone traps have been tried to detect the early stages of a RPW infestation; however, each method has suffered certain logistical and implementation issues. We have applied laser induced breakdown spectroscopy (LIBS) for the early detection of RPW infestation. Through the analysis of the observed LIBS spectra of different infested and healthy samples, we have found presence of Ca, Mg, Na, C, K elements and OH, CN molecules. The spectra also reveal that with the population growth of the pest, the intensity of Mg and Ca atomic lines in LIBS spectra increases rapidly. Similar behavior is observed in the molecular lines of LIBS spectra. The obtained results indicate that the LIBS technique can be used for the early detection of RPW infestation without damaging the date palms.

Validation studies on quick analysis of MOX fuel by combination of laser induced breakdown spectroscopy and ablation resonance absorption spectroscopy

International Nuclear Information System (INIS)

Wakaida, Ikuo; Akaoka, Katsuaki; Miyabe, Masabumi; Kato, Masaaki; Otobe, Haruyoshi; Ohoba, Hironori; Khumaeni, Ali

2014-01-01

Research and development of laser based quick analysis without chemical analysis and neutron measurement for next-generation Minor Actinide containing MOX fuel has been carried out, and the basic performances by using un-irradiated MOX fuel were demonstrated. The glove box had been re-constructed and specialized for laser spectroscopy, and the remote spectroscopy of MOX sample contained several concentrations of Pu was performed. In elemental analysis by Laser Induced Breakdown Spectroscopy (LIBS) with high resolution spectrometer, relative error of 2.9% at 30% Pu and the detection lower limit of 2500ppm in natural U oxide were demonstrated with the operation time of 5 min. In isotope ratio analysis by Ablation Resonance Absorption Spectroscopy, tunable semiconductor laser system was constructed, and the performances such as relative deviation less than 1% in the ratio of "2"4"0Pu/"2"3"9Pu and the sensitivity of 30-100ppm in natural U were also accomplished with laser operation time of 3 to 5min. As for an elemental analysis of the simulated liquid sample, ultra-thin laminate flow was experimented as LIBS target, and the sensitivity comparable to conventional ICP-AES was confirmed. Present study includes the result of the entrusted project by the Ministry of Education, Culture, Sports, Science and Technology of Japan (MEXT). (author)

Laser-induced Breakdown Spectroscopy: A New Approach for Nanoparticle's Mapping and Quantification in Organ Tissue

Science.gov (United States)

Sancey, Lucie; Motto-Ros, Vincent; Kotb, Shady; Wang, Xiaochun; Lux, François; Panczer, Gérard; Yu, Jin; Tillement, Olivier

2014-01-01

Emission spectroscopy of laser-induced plasma was applied to elemental analysis of biological samples. Laser-induced breakdown spectroscopy (LIBS) performed on thin sections of rodent tissues: kidneys and tumor, allows the detection of inorganic elements such as (i) Na, Ca, Cu, Mg, P, and Fe, naturally present in the body and (ii) Si and Gd, detected after the injection of gadolinium-based nanoparticles. The animals were euthanized 1 to 24 hr after intravenous injection of particles. A two-dimensional scan of the sample, performed using a motorized micrometric 3D-stage, allowed the infrared laser beam exploring the surface with a lateral resolution less than 100 μm. Quantitative chemical images of Gd element inside the organ were obtained with sub-mM sensitivity. LIBS offers a simple and robust method to study the distribution of inorganic materials without any specific labeling. Moreover, the compatibility of the setup with standard optical microscopy emphasizes its potential to provide multiple images of the same biological tissue with different types of response: elemental, molecular, or cellular. PMID:24962015

Development of laser-based technology for the routine first wall diagnostic on the tokamak EAST: LIBS and LIAS

Science.gov (United States)

Hu, Z.; Gierse, N.; Li, C.; Liu, P.; Zhao, D.; Sun, L.; Oelmann, J.; Nicolai, D.; Wu, D.; Wu, J.; Mao, H.; Ding, F.; Brezinsek, S.; Liang, Y.; Ding, H.; Luo, G.; Linsmeier, C.; EAST Team

2017-12-01

A laser based method combined with spectroscopy, such as laser-induced breakdown spectroscopy (LIBS) and laser-induced ablation spectroscopy (LIAS), is a promising technology for plasma-wall interaction studies. In this work, we report the development of in situ laser-based diagnostics (LIBS and LIAS) for the assessment of static and dynamic fuel retention on the first wall without removing the tiles between and during plasma discharges in the Experimental Advanced Superconducting Tokamak (EAST). The fuel retention on the first wall was measured after different wall conditioning methods and daily plasma discharges by in situ LIBS. The result indicates that the LIBS can be a useful tool to predict the wall condition in EAST. With the successful commissioning of a refined timing system for LIAS, an in situ approach to investigate fuel retention is proposed.

Using LIBS Method in Safeguards

International Nuclear Information System (INIS)

Kovacs-Szeles, E.; Almasi, I.

2015-01-01

Laser-Induced Breakdown Spectroscopy (LIBS) is a type of atomic emission spectroscopic technique which is capable to detect almost all the elements from the periodic table in different sample types (solid, liquid or gas). Other advantage of the technique is that a LIBS analysis is much faster than a conventional laboratory technique. Beside the easy usability and fastness of the system the main advantages of the technique is that portable systems are also available. Using a so-called ''backpack'' version in-field analysis can be carried out. Therefore, LIBS is a more and more popular technique also e.g., in the nuclear analytics due to its several advantages. It is also tested for Safeguards purposes as a novel technology. In this work development and test of a portable LIBS system is discussed in detail. Detector system with higher resolution and specific software for evaluation of uranium isotope composition has been developed. Different kind of uranium fuel pellets with various enrichments was analyzed as test samples. Concerning the test measurements the developed LIBS instrument was found well-applicable for analysis of Safeguards samples and determination of higher enrichment of uranium in-field. The method is rapid and simple enough for short in-field sample analysis. (author)

Combined Raman spectrometer/laser-induced breakdown spectrometer for the next ESA mission to Mars

Science.gov (United States)

Bazalgette Courrèges-Lacoste, Grégory; Ahlers, Berit; Pérez, Fernando Rull

2007-12-01

Among the different instruments that have been pre-selected to be on-board the Pasteur payload on ExoMars is the Raman/ laser induced breakdown spectroscopy (LIBS) instrument. Raman spectroscopy and LIBS will be integrated into a single instrument sharing many hardware commonalities. An international team under the lead of TNO has been gathered to produce a design concept for a combined Raman spectrometer/LIBS elegant bread-board (EBB). The instrument is based on a specially designed, extremely compact, spectrometer with high resolution over a large wavelength range, suitable for both Raman spectroscopy and LIBS measurements. Low mass, size and power consumption are the main drivers of the instrument's design concept. In this paper, science objectives for the combined instrument are detailed. Background information on Raman spectroscopy and LIBS are presented, focussing on the synergy of these two techniques. In the last section, the instrument concept resulting from the assessment of the feasibility of the combined Raman/LIBS EBB is presented.

Detection of tire tread particles using laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Prochazka, David, E-mail: prochazka.d@fme.vutbr.cz [Brno University of Technology, Institute of Physical Engineering, Technická 2, 616 00 Brno (Czech Republic); Brno University of Technology, Central European Institute of Technology, Technická 3058/10, CZ-616 00 Brno (Czech Republic); Bilík, Martin [Brno University of Technology, Institute of Forensic Engineering, Údolní 244/53, 602 00 Brno (Czech Republic); Prochazková, Petra [Masaryk University, Faculty of Science, Department of Chemistry, Kamenice 735/5, 625 00 Brno (Czech Republic); Klus, Jakub; Pořízka, Pavel; Novotný, Jan [Brno University of Technology, Central European Institute of Technology, Technická 3058/10, CZ-616 00 Brno (Czech Republic); Novotný, Karel [Masaryk University, Faculty of Science, Department of Chemistry, Kamenice 735/5, 625 00 Brno (Czech Republic); Brno University of Technology, Central European Institute of Technology, Technická 3058/10, CZ-616 00 Brno (Czech Republic); Ticová, Barbora [Masaryk University, Faculty of Science, Department of Chemistry, Kamenice 735/5, 625 00 Brno (Czech Republic); Bradáč, Albert; Semela, Marek [Brno University of Technology, Institute of Forensic Engineering, Údolní 244/53, 602 00 Brno (Czech Republic); and others

2015-06-01

The objective of this paper is a study of the potential of laser induced breakdown spectroscopy (LIBS) for detection of tire tread particles. Tire tread particles may represent pollutants; simultaneously, it is potentially possible to exploit detection of tire tread particles for identification of optically imperceptible braking tracks at locations of road accidents. The paper describes the general composition of tire treads and selection of an element suitable for detection using the LIBS method. Subsequently, the applicable spectral line is selected considering interferences with lines of elements that might be present together with the detected particles, and optimization of measurement parameters such as incident laser energy, gate delay and gate width is performed. In order to eliminate the matrix effect, measurements were performed using 4 types of tires manufactured by 3 different producers. An adhesive tape was used as a sample carrier. The most suitable adhesive tape was selected from 5 commonly available tapes, on the basis of their respective LIBS spectra. Calibration standards, i.e. an adhesive tape with different area content of tire tread particles, were prepared for the selected tire. A calibration line was created on the basis of the aforementioned calibration standards. The linear section of this line was used for determination of the detection limit value applicable to the selected tire. Considering the insignificant influence of matrix of various types of tires, it is possible to make a simple recalculation of the detection limit value on the basis of zinc content in a specific tire. - Highlights: • LIBS experimental measurement parameters for tire tread particles were optimize. • Calibration curve was prepared. • Limit of detection was determined.

Detection of tire tread particles using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Prochazka, David; Bilík, Martin; Prochazková, Petra; Klus, Jakub; Pořízka, Pavel; Novotný, Jan; Novotný, Karel; Ticová, Barbora; Bradáč, Albert; Semela, Marek

2015-01-01

The objective of this paper is a study of the potential of laser induced breakdown spectroscopy (LIBS) for detection of tire tread particles. Tire tread particles may represent pollutants; simultaneously, it is potentially possible to exploit detection of tire tread particles for identification of optically imperceptible braking tracks at locations of road accidents. The paper describes the general composition of tire treads and selection of an element suitable for detection using the LIBS method. Subsequently, the applicable spectral line is selected considering interferences with lines of elements that might be present together with the detected particles, and optimization of measurement parameters such as incident laser energy, gate delay and gate width is performed. In order to eliminate the matrix effect, measurements were performed using 4 types of tires manufactured by 3 different producers. An adhesive tape was used as a sample carrier. The most suitable adhesive tape was selected from 5 commonly available tapes, on the basis of their respective LIBS spectra. Calibration standards, i.e. an adhesive tape with different area content of tire tread particles, were prepared for the selected tire. A calibration line was created on the basis of the aforementioned calibration standards. The linear section of this line was used for determination of the detection limit value applicable to the selected tire. Considering the insignificant influence of matrix of various types of tires, it is possible to make a simple recalculation of the detection limit value on the basis of zinc content in a specific tire. - Highlights: • LIBS experimental measurement parameters for tire tread particles were optimize. • Calibration curve was prepared. • Limit of detection was determined

Detection sensitivity of laser-induced breakdown spectroscopy for Cr II in liquid samples

International Nuclear Information System (INIS)

Rai, Nilesh K.; Rai, Awadhesh K.; Kumar, Akshaya; Thakur, Surya N.

2008-01-01

The performance of laser-induced breakdown spectroscopy (LIBS) has been evaluated for detection of toxic metals such as Cr in water. Pure aqueous solutions (unitary matrix) with variable Cr concentration were used to construct calibration curves and to estimate the LIBS limit of detection (LOD). The calibration curves for Cr in a binary matrix (Cr plus Cd) and a tertiary matrix (Cr plus Cd and Co) were used to evaluate the matrix effect on the LOD. The LOD for Cr was found to be 1.1, 1.5, and 2.0 ppm (parts in 10 6 ) in a unitary, binary, and tertiary matrix, respectively. Once calibrated, the system was utilized for the detection and quantification of the Cr in tannery wastewater collected from different locations in the industrial area of Kanpur, India, where Cr concentrations were determined to be far higher than the U.S. Environmental Protection Agency safe drinking water limit of 0.05 ppm

Multi-elemental imaging of paraffin-embedded human samples by laser-induced breakdown spectroscopy

Science.gov (United States)

Moncayo, S.; Trichard, F.; Busser, B.; Sabatier-Vincent, M.; Pelascini, F.; Pinel, N.; Templier, I.; Charles, J.; Sancey, L.; Motto-Ros, V.

2017-07-01

Chemical elements play central roles for physiological homeostasis in human cells, and their dysregulation might lead to a certain number of pathologies. Novel imaging techniques that improve the work of pathologists for tissue analysis and diagnostics are continuously sought. We report the use of Laser-Induced Breakdown Spectroscopy (LIBS) to perform multi-elemental images of human paraffin-embedded skin samples on the entire biopsy scale in a complementary and compatible way with microscope histopathological examination. A specific instrumental configuration is proposed in order to detect most of the elements of medical interest (i.e. P, Al, Mg, Na, Zn, Si, Fe, and Cu). As an example of medical application, we selected and analysed skin biopsies, including healthy skin tissue, cutaneous metastasis of melanoma, Merkel-cell carcinoma and squamous cell carcinoma. Clear distinctions in the distribution of chemical elements are observed from the different samples investigated. This study demonstrates the high complementarity of LIBS elemental imaging with conventional histopathology, opening new opportunities for any medical application involving metals.

Optimal emission enhancement in orthogonal double-pulse laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Sanginés, R.; Contreras, V.; Sobral, H.; Robledo-Martinez, A.

2015-01-01

Orthogonal double-pulse (DP) laser-induced breakdown spectroscopy (LIBS) was performed using reheating and pre-ablative configurations. The ablation pulse power density was varied by two orders of magnitude and the DP experiments were carried out for a wide range of interpulse delays. For both DP-LIBS schemes, the signal enhancement was evaluated with respect to the corresponding single-pulse (SP) LIBS as a function of the interpulse delay. The reheating scheme shows a sharp maximum signal enhancement of up to 200-fold for low ablative power densities (0.4 GW cm −2 ); however, for power densities larger than 10 GW cm −2 this configuration did not improve the SP outcome. On the other hand, a more uniform signal enhancement of about 4–6 was obtained for the pre-ablative scheme nearly independently of the used ablative power density. In terms of the signal-to-noise ratio (SNR) the pre-ablative scheme shows a monotonic increment with the ablative power density. Whereas the reheating configuration reaches a maximum at 2.2 GW cm −2 , its enhancement effect collapses markedly for fluencies above 10 GW cm −2 . - Highlights: • Comparison of reheating and pre-ablative double-pulse LIBS was done using a wide range of ablation power densities. • Experimental parameters that could achieve optimal signal-to-noise ratio were investigated. • A reheating scheme is better for low-ablation power densities. • A pre-ablative configuration is better for high-ablation power densities

Rapid long-wave infrared laser-induced breakdown spectroscopy measurements using a mercury-cadmium-telluride linear array detection system.

Science.gov (United States)

Yang, Clayton S-C; Brown, Eiei; Kumi-Barimah, Eric; Hommerich, Uwe; Jin, Feng; Jia, Yingqing; Trivedi, Sudhir; D'souza, Arvind I; Decuir, Eric A; Wijewarnasuriya, Priyalal S; Samuels, Alan C

2015-11-20

In this work, we develop a mercury-cadmium-telluride linear array detection system that is capable of rapidly capturing (∼1-5  s) a broad spectrum of atomic and molecular laser-induced breakdown spectroscopy (LIBS) emissions in the long-wave infrared (LWIR) region (∼5.6-10  μm). Similar to the conventional UV-Vis LIBS, a broadband emission spectrum of condensed phase samples covering the whole 5.6-10 μm region can be acquired from just a single laser-induced microplasma or averaging a few single laser-induced microplasmas. Atomic and molecular signature emission spectra of solid inorganic and organic tablets and thin liquid films deposited on a rough asphalt surface are observed. This setup is capable of rapidly probing samples "as is" without the need of elaborate sample preparation and also offers the possibility of a simultaneous UV-Vis and LWIR LIBS measurement.

Characterization of cinematographic films by Laser Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Gaspard, S.; Oujja, M.; Rebollar, E.; Abrusci, C.; Catalina, F.; Castillejo, M.

2007-01-01

The emulsion-coated transparent plastic-base film has been the main carrier for production and preservation of motion picture contents since the 19th century. The knowledge of the composition of black and white silver gelatine cinematographic films is of great importance for the characterization of the photographic process and for identifying the optimum conditions for conservation. A cinematographic film is a multi-component system that consists of a layer of photographic emulsion overcoating a polymeric support (plasticized cellulose triacetate) and a protective transparent cross-linked gelatine layer coating the emulsion. In the present work, Laser Induced Breakdown Spectroscopy (LIBS) is used to characterize the composition of the materials of cinematographic films. LIB spectra of film samples and of different individual film components, polymeric support and reference gelatines, were acquired in vacuum by excitation at 266 nm (Q-switched Nd:YAG laser, 6 ns, 10 Hz). In the cinematographic film, silver lines from the light-sensitive silver halide salts of the photographic emulsion are accompanied by iron, lead, chrome and phosphorus lines. Iron and lead are constituents of film developers, chrome is included in the composition of the hardening agents and phosphorus has its origin in the plasticizer used in the polymeric support. By applying successive pulses on the same spot of the film sample, it was possible to observe through stratigraphic analysis the different layers composition. Additionally, the results obtained reveal the analytical capacity of LIBS for the study and classification of the different gelatine types and qualities used for the protecting layer and the photographic emulsion

Detection of boron in simulated corrosion products by using a laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Song, K.; Yeon, J-W.; Jung, S-H.; Hwang, J.; Jung, E-C.

2010-01-01

In nuclear power plants, many methods for detection of coolant leakage have been developed and employed for the safe operation. However, these methods have many limitations for analyzing and dealing with the corrosion products due to the high radioactivity. LIBS (Laser-induced breakdown spectroscopy) offer a remote and on-site elemental analysis including the boron in the corrosion products with no sample preparation. In this study, we investigated the feasibility of detecting boron and analyzing an elemental composition of boron-containing iron oxides with the LIBS, in order to develop a coolant leakage detection system. First, we prepared five different boron-containing iron oxides and the element ratios were determined by using ICP-AES (inductive coupled plasma-atomic emission spectrometer). After this, the laser induced emission spectra of these iron oxides were obtained by using a 266 nm Nd:YAG laser. The B/Fe ratios of the oxides were determined by comparing the intensities of the B emission peak at 249.844 nm with those of the Fe peak at 250.217 nm as an internal reference. It was confirmed that the B contents in the oxides could be analyzed over 0.1 wt% by the laser induced breakdown spectroscopic technique. (author)

Raman, Infrared, and Laser-Induced Breakdown Spectroscopy Identification of Particles in Raw Materials.

Science.gov (United States)

Lee, Kathryn; Lankers, Markus; Valet, Oliver

2018-02-01

Raw materials need to be of a certain quality with respect to physical and chemical composition. They also need to have no contaminants, including particles, because these could indicate raw material impurities or contaminate the product. Particle identification allows determination of process conditions that caused them and whether the quality of the final product is acceptable. Particles may appear to the eye to be very different things than they actually are. They may be coated with the raw material and may consist of several components; therefore, chemical and elemental analyses are required for accuracy in proper identification and definitive information about their source. Thus, microscope versions of Raman spectroscopy, laser-induced breakdown spectroscopy (LIBS), and infrared (IR) spectroscopy are excellent tools for identifying particles in materials. Those tools are fast and accurate, and can provide chemical and elemental composition as well as images that can aid identification. The micro-analysis capabilities allow for easy analysis of different portions of samples so that multiple components can be identified and sample preparation can be reduced or eliminated. The differences in sensitivities of Raman and IR spectroscopies to different functional groups as well as the elemental analysis provided by LIBS and the image analysis provided by the microscopy makes these complementary techniques and provides the advantage of identifying various chemical components. Proper spectral searching techniques and interpretation of the results are important for interpretation and identification of trace contaminants.

Combined raman/laser-induced breakdown spectrometer: space and non-space applications

NARCIS (Netherlands)

Sandtke, M.; Laan, E.C.; Ahlers, B.

2010-01-01

TNO has developed the combination of two spectroscopic analysis methods in one instrument. Raman spectroscopy and Laser-induced Breakdown Spectroscopy (LIBS) were brought together for an instrument to be flown on the ExoMars mission from the European Space Agency (ESA) to investigate the Martian

Application of Laser Induced Breakdown Spectroscopy to the identification of emeralds from different synthetic processes

International Nuclear Information System (INIS)

Agrosì, G.; Tempesta, G.; Scandale, E.; Legnaioli, S.; Lorenzetti, G.; Pagnotta, S.; Palleschi, V.; Mangone, A.; Lezzerini, M.

2014-01-01

Laser Induced Breakdown Spectroscopy can provide a useful contribution in mineralogical field in which the quantitative chemical analyses (including the evaluation of light elements) can play a key role in the studies on the origin of the emeralds. In particular, the chemical analyses permit to determine those trace elements, known as fingerprints, that can be useful to study their provenance. This technique, not requiring sample preparation results particularly suitable for gemstones, that obviously must be studied in a non-destructive way. In this paper, the LIBS technique was applied to distinguish synthetic emeralds grown by Biron hydrothermal method from those grown by Chatham flux method. The analyses performed by collinear double-pulse LIBS give a signal enhancement useful for the quantitative chemical analyses while guaranteeing a minimal sample damage. In this way it was obtained a considerable improvement on the detection limit of the trace elements, whose determination is essential for determining the origin of emerald gemstone. The trace elements V, Cr, and Fe and their relative amounts allowed the correct attribution of the manufacturer. Two different methods for quantitative analyses were used for this study: the standard Calibration-Free LIBS (CF-LIBS) method and its recent evolution, the One Point Calibration LIBS (OPC-LIBS). This is the first approach to the evaluation of the emerald origin by means of the LIBS technique. - Highlights: • A LIBS method for discrimination between synthetic emeralds is presented. • Only one standard of known composition is needed for the analysis. • A set of two kind of synthetic emeralds has been analyzed. • The cromophoric elements Cr, V and Fe amounts have been used to determine the origin of emerald gemstone

Application of Laser Induced Breakdown Spectroscopy to the identification of emeralds from different synthetic processes

Energy Technology Data Exchange (ETDEWEB)

Agrosì, G. [Department of Scienze della Terra e Geoambientali, University of Bari, Bari (Italy); Tempesta, G., E-mail: gioacchino.tempesta@uniba.it [Department of Scienze della Terra e Geoambientali, University of Bari, Bari (Italy); Scandale, E. [Department of Scienze della Terra e Geoambientali, University of Bari, Bari (Italy); Legnaioli, S.; Lorenzetti, G.; Pagnotta, S.; Palleschi, V. [Institute of Chemistry of Organometallic Compounds, CNR, Pisa (Italy); Mangone, A. [Department of Chemistry, University of Bari, Bari (Italy); Lezzerini, M. [Department of Earth Sciences, University of Pisa, Pisa (Italy)

2014-12-01

Laser Induced Breakdown Spectroscopy can provide a useful contribution in mineralogical field in which the quantitative chemical analyses (including the evaluation of light elements) can play a key role in the studies on the origin of the emeralds. In particular, the chemical analyses permit to determine those trace elements, known as fingerprints, that can be useful to study their provenance. This technique, not requiring sample preparation results particularly suitable for gemstones, that obviously must be studied in a non-destructive way. In this paper, the LIBS technique was applied to distinguish synthetic emeralds grown by Biron hydrothermal method from those grown by Chatham flux method. The analyses performed by collinear double-pulse LIBS give a signal enhancement useful for the quantitative chemical analyses while guaranteeing a minimal sample damage. In this way it was obtained a considerable improvement on the detection limit of the trace elements, whose determination is essential for determining the origin of emerald gemstone. The trace elements V, Cr, and Fe and their relative amounts allowed the correct attribution of the manufacturer. Two different methods for quantitative analyses were used for this study: the standard Calibration-Free LIBS (CF-LIBS) method and its recent evolution, the One Point Calibration LIBS (OPC-LIBS). This is the first approach to the evaluation of the emerald origin by means of the LIBS technique. - Highlights: • A LIBS method for discrimination between synthetic emeralds is presented. • Only one standard of known composition is needed for the analysis. • A set of two kind of synthetic emeralds has been analyzed. • The cromophoric elements Cr, V and Fe amounts have been used to determine the origin of emerald gemstone.

Determination of a brass alloy concentration composition using calibration-free laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Achouri, M.; Baba-Hamed, T.; Beldjilali, S. A., E-mail: sidahmed.beldjilali@univ-usto.dz; Belasri, A. [Université des Sciences et de la Technologie d’Oran Mohamed Boudiaf USTO-MB, LPPMCA (Algeria)

2015-09-15

Laser-induced breakdown spectroscopy (LIBS) is a technique that can provide qualitative and quantitative measurements of the characteristics of irradiated metals. In the present work, we have calculated the parameters of the plasma produced from a brass alloy sample under the action of a pulsed Nd: YAG laser operating at 1064 nm. The emission lines of copper atoms (Cu I), zinc atoms (Zn I), and lead atoms (Pb I), which are elements of a brass alloy composition, were used to investigate the parameters of the brass plasma. The spectral profiles of Cu, Zn, and Pb lines have been used to extract the electron temperature and density of the brass alloy plasma. The characteristics of Cu, Zn, and Pb were determined quantatively by the calibration-free LIBS (CF-LIBS) method considering for accurate analysis that the laser-induced ablated plasma is optically thin in local thermodynamic equilibrium conditions and the plasma ablation is stoichiometric. The Boltzmann plot method was used to evaluate the plasma temperature, and the Stark broadened profiles were used to determine the electron density. An algorithm based on the experimentally measured values of the intensity of spectral lines and the basic laws of plasma physics was developed for the determination of Cu, Zn, and Pb concentrations in the brass sample. The concentrations C{sub CF-LIBS} calculated by CF-LIBS and the certified concentrations C{sub certified} were very close.

An investigation of Laser Induced Breakdown Spectroscopy for use as a control in the laser removal of rock from fossils found at the Malapa hominin site, South Africa

CSIR Research Space (South Africa)

Roberts, DE

2012-07-01

Full Text Available Laser Induced Breakdown Spectroscopy (LIBS) was used to study the spectra from fossils and surrounding rock recovered from the Cradle of Mankind site at Malapa, South Africa. The objective was to find a suitable spectral line(s), specific to fossils...

Development of Laser-Induced Breakdown Spectroscopy Technologies for Nuclear Safeguards and Forensic Applications

International Nuclear Information System (INIS)

Chen, S.; El-Jaby, A.; Doucet, F.; Bouchard, P.; Sabsabi, M.

2015-01-01

Under the IAEA Task A1855, the Canadian Safeguards Support Program (CSSP) undertook the development of laser-induced breakdown spectroscopy (LIBS) technologies for safeguards applications. Collaboration between the Canadian Nuclear Safety Commission (CNSC), the National Research Council Canada, and the IAEA has demonstrated that the LIBS technique combined with chemometrics can determine the origins of yellowcake, identify maraging steels, aluminium alloys, and magnesium alloys, among other materials involved in the nuclear industry; and determine heavy water content as well as the isotope ratios of other actinides. As part of the task, the CSSP has developed a portable LIBS system to enable inspectors to characterize specific nuclear and non-nuclear material during complementary access and inspections. This device was recently tested by the IAEA in both Vienna and Siebersdorf for various metals and uranium bearing materials. The laser source proved to be stable and the chemometrics software was able to identify various materials. The device is ready for further in-depth testing. The chemometrics algorithm that has been developed for LIBS can also be adapted to nuclear forensics for the querying database. Multi-stage pattern recognition algorithms can reliably identify unknown materials among database populations (e.g., identify origins of yellowcake). Further work in this field is being undertaken as part of the CNSC's National Nuclear Forensics Library (NNFL) development activities for the Canadian National Nuclear Forensics Capability Project (CNNFCP). The paper will provide an overview of the LIBS techniques being developed for safeguards and forensic applications, and of progress in integrating all components into a compact unit. (author)

Surface characterization of carbon fiber reinforced polymers by picosecond laser induced breakdown spectroscopy

Science.gov (United States)

Ledesma, Rodolfo; Palmieri, Frank; Connell, John; Yost, William; Fitz-Gerald, James

2018-02-01

Adhesive bonding of composite materials requires reliable monitoring and detection of surface contaminants as part of a vigorous quality control process to assure robust and durable bonded structures. Surface treatment and effective monitoring prior to bonding are essential in order to obtain a surface which is free from contaminants that may lead to inferior bond quality. In this study, the focus is to advance the laser induced breakdown spectroscopy (LIBS) technique by using pulse energies below 100 μJ (μLIBS) for the detection of low levels of silicone contaminants in carbon fiber reinforced polymer (CFRP) composites. Various CFRP surface conditions were investigated by LIBS using ∼10 ps, 355 nm laser pulses with pulse energies below 30 μJ. Time-resolved analysis was conducted to optimize the gate delay and gate width for the detection of the C I emission line at 247.9 nm to monitor the epoxy resin matrix of CFRP composites and the Si I emission line at 288.2 nm for detection of silicone contaminants in CFRP. To study the surface sensitivity to silicone contamination, CFRP surfaces were coated with polydimethylsiloxane (PDMS), the active ingredient in many mold release agents. The presence of PDMS was studied by inspecting the Si I emission lines at 251.6 nm and 288.2 nm. The measured PDMS areal densities ranged from 0.15 to 2 μg/cm2. LIBS measurements were performed before and after laser surface ablation. The results demonstrate the successful detection of PDMS thin layers on CFRP using picosecond μLIBS.

A study of association between fingernail elements and osteoporosis by laser-induced breakdown spectroscopy

Science.gov (United States)

Bahreini, Maryam; Hosseinimakarem, Zahra; Hassan Tavassoli, Seyed

2012-09-01

Laser induced breakdown spectroscopy (LIBS) is used to investigate the possible effect of osteoporosis on the elemental composition of fingernails. Also, the ability to classify healthy, osteopenic, and osteoporotic subjects based on their fingernail spectra has been examined. 46 atomic and ionic emission lines belonging to 13 elements, which are dominated by calcium and magnesium, have been identified. Measurements are carried out on fingernail clippings of 99 subjects including 27 healthy, 47 osteopenic, and 25 osteoporotic subjects. The Pearson correlations between spectral intensities of different elements of fingernail and age and bone mineral densities (BMDs) in nail samples are calculated. Correlations between line intensities of some elements such as sodium and potassium, calcium and iron, magnesium and silicon and also between some fingernail elements, BMD, and age are observed. Although some of these correlations are weak, some information about mineral metabolism can be deduced from them. Discrimination between nail samples of healthy, osteopenic, and osteoporotic subjects is shown to be somehow possible by a discriminant function analysis using 46 atomic emission lines of the LIBS spectra as input variables. The results of this study provide some evidences for association between osteoporosis and elemental composition of fingernails measured by LIBS.

Standoff Sensing Technology Based on Laser-Induced Breakdown Spectroscopy: Advanced Targeting, Surveillance and Reconnaissance in Security and Architectural Heritage Applications

OpenAIRE

Gaona Fernández, María Inmaculada

2014-01-01

Due to the ability to perform simultaneous, multi-element and real-time analysis without pretreatment and doing from a distance, laser induced breakdown spectroscopy (LIBS) in standoff mode is now considered a cutting-edge analytical technology. All these features have allowed its application in various fields such as security, environment, cultural heritage protection and space exploration, among the more outstanding. Nonetheless, the fact of working to long distances involves greater dif...

X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy analysis of Roman silver denarii

Energy Technology Data Exchange (ETDEWEB)

Pardini, L. [Istituto di Chimica dei Composti Organometallici del CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); El Hassan, A. [National Institute for Laser- Enhanced Sciences (NILES), Cairo University Giza (Egypt); Ferretti, M. [Istituto per le Tecnologie Applicate ai Beni Culturali, Area della Ricerca del CNR di Montelibretti Roma (Italy); Foresta, A.; Legnaioli, S.; Lorenzetti, G. [Istituto di Chimica dei Composti Organometallici del CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); Nebbia, E. [Universita degli Studi di Torino (Italy); Catalli, F. [Monetiere di Firenze, Museo Archeologico Nazionale Firenze (Italy); Harith, M.A. [National Institute for Laser- Enhanced Sciences (NILES), Cairo University Giza (Egypt); Diaz Pace, D. [Institute of Physics ' Arroyo Seco' , Faculty of Science, Tandil (Argentina); Anabitarte Garcia, F. [Photonics Engineering Group, University of Cantabria, Santander (Spain); Scuotto, M. [Dipartimento di Scienze Archeologiche, Via Galvani 1, 56126 Pisa (Italy); Palleschi, V., E-mail: vincenzo.palleschi@cnr.it [Istituto di Chimica dei Composti Organometallici del CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); Dipartimento di Scienze Archeologiche, Via Galvani 1, 56126 Pisa (Italy)

2012-08-15

In this paper we present the results of a study performed on a large collection of silver Roman republican denarii, encompassing about two centuries of history. The joint use of Laser-Induced Breakdown Spectroscopy (LIBS) and X-Ray Fluorescence (XRF) spectroscopy allowed for an accurate determination of the coins' elemental composition; the measurements, performed mostly in situ at the 'Monetiere' in Florence, revealed a striking connection between the 'quality' of the silver alloy and some crucial contemporary events. This finding was used to classify a group of denarii whose dating was otherwise impossible. The comparison with other contemporary denarii disproves a recent theory on the origin of the so called 'serrated' denarii (denarii showing notched chisel marks on the edge of the coin). - Highlights: Black-Right-Pointing-Pointer We studied a large collection of Roman republican silver denarii. Black-Right-Pointing-Pointer XRF and LIBS allowed to determine the precious metal content of the coins. Black-Right-Pointing-Pointer A correlation of the 'quality' of the alloy with some contemporary events was found. Black-Right-Pointing-Pointer The study allowed to controvert a recent theory on the so called 'serrated' denarii.

Multivariate calibration in Laser-Induced Breakdown Spectroscopy quantitative analysis: The dangers of a 'black box' approach and how to avoid them

Science.gov (United States)

Safi, A.; Campanella, B.; Grifoni, E.; Legnaioli, S.; Lorenzetti, G.; Pagnotta, S.; Poggialini, F.; Ripoll-Seguer, L.; Hidalgo, M.; Palleschi, V.

2018-06-01

The introduction of multivariate calibration curve approach in Laser-Induced Breakdown Spectroscopy (LIBS) quantitative analysis has led to a general improvement of the LIBS analytical performances, since a multivariate approach allows to exploit the redundancy of elemental information that are typically present in a LIBS spectrum. Software packages implementing multivariate methods are available in the most diffused commercial and open source analytical programs; in most of the cases, the multivariate algorithms are robust against noise and operate in unsupervised mode. The reverse of the coin of the availability and ease of use of such packages is the (perceived) difficulty in assessing the reliability of the results obtained which often leads to the consideration of the multivariate algorithms as 'black boxes' whose inner mechanism is supposed to remain hidden to the user. In this paper, we will discuss the dangers of a 'black box' approach in LIBS multivariate analysis, and will discuss how to overcome them using the chemical-physical knowledge that is at the base of any LIBS quantitative analysis.

Laser-induced breakdown spectroscopy measurement of a small fraction of rhenium in bulk tungsten

Science.gov (United States)

Nishijima, D.; Ueda, Y.; Doerner, R. P.; Baldwin, M. J.; Ibano, K.

2018-03-01

Laser-induced breakdown spectroscopy (LIBS) of bulk rhenium (Re) and tungsten (W)-Re alloy has been performed using a Q-switched Nd:YAG laser (wavelength = 1064 nm, pulse width ∼4-6 ns, laser energy = 115 mJ). It is found that the electron temperature, Te, of laser-induced Re plasma is lower than that of W plasma, and that Te of W-Re plasma is in between Re and W plasmas. This indicates that material properties affect Te in a laser-induced plasma. For analysis of W-3.3%Re alloy, only the strongest visible Re I 488.9 nm line is found to be used because of the strong enough intensity without contamination with W lines. Using the calibration-free LIBS method, the atomic fraction of Re, cRe, is evaluated as a function of the ambient Ar gas pressure, PAr. At PAr 10 Torr due to spectral overlapping of the Re I 488.9 nm line by an Ar II 488.9 nm line.

Determination of the postmortem interval by Laser Induced Breakdown Spectroscopy using swine skeletal muscles

International Nuclear Information System (INIS)

Marín-Roldan, A.; Manzoor, S.; Moncayo, S.; Navarro-Villoslada, F.; Izquierdo-Hornillos, R.C.; Caceres, J.O.

2013-01-01

Skin and muscle samples are useful to discriminate individuals as well as their postmortem interval (PMI) in crime scenes and natural or caused disasters. In this study, a simple and fast method based on Laser Induced Breakdown Spectroscopy (LIBS) has been developed to estimate PMI using swine skeletal muscle samples. Environmental conditions (moisture, temperature, fauna, etc.) having strong influence on the PMI determination were considered. Time-dependent changes in the emission intensity ratio for Mg, Na, Hα and K were observed, as a result of the variations in their concentration due to chemical reactions in tissues and were correlated with PMI. This relationship, which has not been reported previously in the forensic literature, offers a simple and potentially valuable means of estimating the PMI. - Highlights: • LIBS has been applied for Postmortem Interval estimation. • Environmental and sample storage conditions have been considered. • Significant correlation of elemental emission intensity with PMI has been observed. • Pig skeletal muscle samples have been used

Determination of the postmortem interval by Laser Induced Breakdown Spectroscopy using swine skeletal muscles

Energy Technology Data Exchange (ETDEWEB)

Marín-Roldan, A.; Manzoor, S.; Moncayo, S.; Navarro-Villoslada, F.; Izquierdo-Hornillos, R.C.; Caceres, J.O., E-mail: jcaceres@quim.ucm.es

2013-10-01

Skin and muscle samples are useful to discriminate individuals as well as their postmortem interval (PMI) in crime scenes and natural or caused disasters. In this study, a simple and fast method based on Laser Induced Breakdown Spectroscopy (LIBS) has been developed to estimate PMI using swine skeletal muscle samples. Environmental conditions (moisture, temperature, fauna, etc.) having strong influence on the PMI determination were considered. Time-dependent changes in the emission intensity ratio for Mg, Na, Hα and K were observed, as a result of the variations in their concentration due to chemical reactions in tissues and were correlated with PMI. This relationship, which has not been reported previously in the forensic literature, offers a simple and potentially valuable means of estimating the PMI. - Highlights: • LIBS has been applied for Postmortem Interval estimation. • Environmental and sample storage conditions have been considered. • Significant correlation of elemental emission intensity with PMI has been observed. • Pig skeletal muscle samples have been used.

Remote quantitative analysis of cerium through a shielding window by stand-off laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Gong, Yongdeuk; Choi, Daewoong; Han, Bo-Young; Yoo, Jonghyun; Han, Song-Hee; Lee, Yonghoon

2014-01-01

Highlights: • Remote LIBS analysis of cerium in the samples located behind a shielding window. • Effects of a shielding window on the remote LIBS analysis were investigated. • Multivariate analysis improves the calibration quality. - Abstract: Laser-Induced Breakdown Spectroscopy (LIBS) has been considered in many applications in nuclear industry. LIBS can be an ideal technique for analyzing the inaccessible nuclear materials typically located behind a shielding window. We report the effect of optical transmittance of the shielding window on the analytical performances of stand-off LIBS for the preliminary surrogate sample of demonstration pyrochemical process, a mixture of cerium oxide (CeO 2 ) and potassium chloride (KCl). A pulsed laser beam was focused on the surface of the sample located 1.45 m away from the stand-off LIBS device. The laser-induced plasma emission was collected through a Schmidt–Cassegrain telescope. LIBS spectra were obtained in an open path and through the shielding window. Univariate calibration curves were obtained using the integrated area of partially resolved Ce I and II lines. The limits of detection (LOD) for Ce were estimated to be 0.046 and 0.061 wt.% for the open-path and through-window analysis, respectively. We found that the through-window LOD is mainly influenced by the optical transmittance of the shielding window and therefore, the through-window LOD can be predicted from the open-path LOD and the optical transmittance of the shielding window. Also, multivariate calibration using partial least squares regression was successfully applied. The quality of calibration could be improved by the multivariate analysis

Remote quantitative analysis of cerium through a shielding window by stand-off laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Gong, Yongdeuk [Department of Chemistry, Mokpo National University, Jeonnam 534-729 (Korea, Republic of); Choi, Daewoong [Department of Chemistry, Mokpo National University, Jeonnam 534-729 (Korea, Republic of); Korea Atomic Energy Research Institute, P.O. Box 255, Yuseong, Daejeon 305-353 (Korea, Republic of); Han, Bo-Young, E-mail: byhan@kaeri.re.kr [Korea Atomic Energy Research Institute, P.O. Box 255, Yuseong, Daejeon 305-353 (Korea, Republic of); Yoo, Jonghyun [Applied Spectra, 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Han, Song-Hee [Division of Maritime Transportation System, Mokpo National Maritime University, Jeonnam 530-729 (Korea, Republic of); Lee, Yonghoon, E-mail: yhlee@mokpo.ac.kr [Department of Chemistry, Mokpo National University, Jeonnam 534-729 (Korea, Republic of)

2014-10-15

Highlights: • Remote LIBS analysis of cerium in the samples located behind a shielding window. • Effects of a shielding window on the remote LIBS analysis were investigated. • Multivariate analysis improves the calibration quality. - Abstract: Laser-Induced Breakdown Spectroscopy (LIBS) has been considered in many applications in nuclear industry. LIBS can be an ideal technique for analyzing the inaccessible nuclear materials typically located behind a shielding window. We report the effect of optical transmittance of the shielding window on the analytical performances of stand-off LIBS for the preliminary surrogate sample of demonstration pyrochemical process, a mixture of cerium oxide (CeO{sub 2}) and potassium chloride (KCl). A pulsed laser beam was focused on the surface of the sample located 1.45 m away from the stand-off LIBS device. The laser-induced plasma emission was collected through a Schmidt–Cassegrain telescope. LIBS spectra were obtained in an open path and through the shielding window. Univariate calibration curves were obtained using the integrated area of partially resolved Ce I and II lines. The limits of detection (LOD) for Ce were estimated to be 0.046 and 0.061 wt.% for the open-path and through-window analysis, respectively. We found that the through-window LOD is mainly influenced by the optical transmittance of the shielding window and therefore, the through-window LOD can be predicted from the open-path LOD and the optical transmittance of the shielding window. Also, multivariate calibration using partial least squares regression was successfully applied. The quality of calibration could be improved by the multivariate analysis.

Application of laser-induced breakdown spectroscopy to the analysis of algal biomass for industrial biotechnology

Science.gov (United States)

Pořízka, P.; Prochazka, D.; Pilát, Z.; Krajcarová, L.; Kaiser, J.; Malina, R.; Novotný, J.; Zemánek, P.; Ježek, J.; Šerý, M.; Bernatová, S.; Krzyžánek, V.; Dobranská, K.; Novotný, K.; Trtílek, M.; Samek, O.

2012-08-01

We report on the application of laser-induced breakdown spectroscopy (LIBS) to the determination of elements distinctive in terms of their biological significance (such as potassium, magnesium, calcium, and sodium) and to the monitoring of accumulation of potentially toxic heavy metal ions in living microorganisms (algae), in order to trace e.g. the influence of environmental exposure and other cultivation and biological factors having an impact on them. Algae cells were suspended in liquid media or presented in a form of adherent cell mass on a surface (biofilm) and, consequently, characterized using their spectra. In our feasibility study we used three different experimental arrangements employing double-pulse LIBS technique in order to improve on analytical selectivity and sensitivity for potential industrial biotechnology applications, e.g. for monitoring of mass production of commercial biofuels, utilization in the food industry and control of the removal of heavy metal ions from industrial waste waters.

Controlled laser cleaning of artworks via low resolution LIBS and linear correlation analysis

NARCIS (Netherlands)

Lentjes, M.; Dickmann, Klaus; Meijer, J.; Ostendof, A.; Hoult, A.; Lu, Y.

2005-01-01

Based on a fibre optic miniature spectrometer (spectral range 200-1100 nm, λ-resolution 2 nm) we have built up a LIBS-system (Laser Induced Breakdown Spectroscopy) for online monitoring during laser cleaning of artworks. This system is unsuitable for high resolved elemental identification but is

Laser-induced breakdown spectroscopy for in situ qualitative and quantitative analysis of mineral ores

International Nuclear Information System (INIS)

Pořízka, P.; Demidov, A.; Kaiser, J.; Keivanian, J.; Gornushkin, I.; Panne, U.; Riedel, J.

2014-01-01

In this work, the potential of laser-induced breakdown spectroscopy (LIBS) for discrimination and analysis of geological materials was examined. The research was focused on classification of mineral ores using their LIBS spectra prior to quantitative determination of copper. Quantitative analysis is not a trivial task in LIBS measurement because intensities of emission lines in laser-induced plasmas (LIP) are strongly affected by the sample matrix (matrix effect). To circumvent this effect, typically matrix-matched standards are used to obtain matrix-dependent calibration curves. If the sample set consists of a mixture of different matrices, even in this approach, the corresponding matrix has to be known prior to the downstream data analysis. For this categorization, the multielemental character of LIBS spectra can be of help. In this contribution, a principal component analysis (PCA) was employed on the measured data set to discriminate individual rocks as individual matrices against each other according to their overall elemental composition. Twenty-seven igneous rock samples were analyzed in the form of fine dust, classified and subsequently quantitatively analyzed. Two different LIBS setups in two laboratories were used to prove the reproducibility of classification and quantification. A superposition of partial calibration plots constructed from the individual clustered data displayed a large improvement in precision and accuracy compared to the calibration plot constructed from all ore samples. The classification of mineral samples with complex matrices can thus be recommended prior to LIBS system calibration and quantitative analysis. - Highlights: • Twenty seven igneous rocks were measured on different LIBS systems. • Principal component analysis (PCA) was employed for classification. • The necessity of the classification of the rock (ore) samples prior to the quantification analysis is stressed. • Classification based on the whole LIP spectra and

Laser-induced breakdown spectroscopy for in situ qualitative and quantitative analysis of mineral ores

Energy Technology Data Exchange (ETDEWEB)

Pořízka, P. [BAM, Federal Institute for Materials Research and Testing, Richard Willstätter-Straße 11, D-12489 Berlin (Germany); Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technická 2896/2, 61669 Brno (Czech Republic); Demidov, A. [BAM, Federal Institute for Materials Research and Testing, Richard Willstätter-Straße 11, D-12489 Berlin (Germany); Kaiser, J. [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technická 2896/2, 61669 Brno (Czech Republic); Keivanian, J. [Institute for Mining, Technical University Clausthal, Erzstraße 18, 38678 Clausthal-Zellerfeld (Germany); Gornushkin, I. [BAM, Federal Institute for Materials Research and Testing, Richard Willstätter-Straße 11, D-12489 Berlin (Germany); Panne, U. [BAM, Federal Institute for Materials Research and Testing, Richard Willstätter-Straße 11, D-12489 Berlin (Germany); Chemistry Department, Humboldt Univerisät zu Berlin, Brook-Taylor-Straße 2, D-12489 Berlin (Germany); Riedel, J., E-mail: jens.riedel@bam.de [BAM, Federal Institute for Materials Research and Testing, Richard Willstätter-Straße 11, D-12489 Berlin (Germany)

2014-11-01

In this work, the potential of laser-induced breakdown spectroscopy (LIBS) for discrimination and analysis of geological materials was examined. The research was focused on classification of mineral ores using their LIBS spectra prior to quantitative determination of copper. Quantitative analysis is not a trivial task in LIBS measurement because intensities of emission lines in laser-induced plasmas (LIP) are strongly affected by the sample matrix (matrix effect). To circumvent this effect, typically matrix-matched standards are used to obtain matrix-dependent calibration curves. If the sample set consists of a mixture of different matrices, even in this approach, the corresponding matrix has to be known prior to the downstream data analysis. For this categorization, the multielemental character of LIBS spectra can be of help. In this contribution, a principal component analysis (PCA) was employed on the measured data set to discriminate individual rocks as individual matrices against each other according to their overall elemental composition. Twenty-seven igneous rock samples were analyzed in the form of fine dust, classified and subsequently quantitatively analyzed. Two different LIBS setups in two laboratories were used to prove the reproducibility of classification and quantification. A superposition of partial calibration plots constructed from the individual clustered data displayed a large improvement in precision and accuracy compared to the calibration plot constructed from all ore samples. The classification of mineral samples with complex matrices can thus be recommended prior to LIBS system calibration and quantitative analysis. - Highlights: • Twenty seven igneous rocks were measured on different LIBS systems. • Principal component analysis (PCA) was employed for classification. • The necessity of the classification of the rock (ore) samples prior to the quantification analysis is stressed. • Classification based on the whole LIP spectra and

Rapid quantitative analysis of elemental composition and depth profile of Cu(In,Ga)Se{sub 2} thin solar cell film using laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

In, Jung-Hwan; Kim, Chan-Kyu; Lee, Seok-Hee; Choi, Jang-Hee; Jeong, Sungho, E-mail: shjeong@gist.ac.kr

2015-03-31

Laser-induced breakdown spectroscopy (LIBS) is reported as a method for rapid quantitative analysis of elemental composition and depth profile of Cu(In,Ga)Se{sub 2} (CIGS) thin film. A calibration model considering compositional grading over depth was developed and verified with test samples. The results from eight test samples showed that the average concentration of Cu, In, Ga and Se could be predicted with a root mean square error of below 1% and a relative standard deviation of also below 1%. The depth profile of each constituent element of CIGS predicted by LIBS was close to those by Auger electron spectroscopy and secondary ion mass spectrometry. The average ablation depth per pulse during depth profiling was about 100 nm. - Highlights: • LIBS was adopted for quantitative analysis of CIGS thin film. • A calibration model considering compositional grading over depth was developed. • Concentration prediction of CIGS thin film was accurate and precise. • Quantitative depth profiling by LIBS was compared with those by AES and SIMS.

Secondary plasma formation after single pulse laser ablation underwater and its advantages for laser induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Gavrilović, M R; Cvejić, M; Lazic, V; Jovićević, S

2016-06-07

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.

Spectroscopy of laser-produced plasmas

Indian Academy of Sciences (India)

It is a well-known fact that laser-induced breakdown spectroscopy (LIBS) has emerged as one of the best analytical techniques for multi-elemental compositional analysis of samples. We report assembling and optimization of LIBS set up using high resolution and broad-range echelle spectrograph coupled to an intensified ...

New insights on the Dronino iron meteorite by double-pulse micro-Laser-Induced Breakdown Spectroscopy

Science.gov (United States)

Tempesta, Gioacchino; Senesi, Giorgio S.; Manzari, Paola; Agrosì, Giovanna

2018-06-01

Two fragments of an iron meteorite shower named Dronino were characterized by a novel technique, i.e. Double-Pulse micro-Laser Induced Breakdown Spectroscopy (DP-μLIBS) combined with optical microscope. This technique allowed to perform a fast and detailed analysis of the chemical composition of the fragments and permitted to determine their composition, the alteration state differences and the cooling rate of the meteorite. Qualitative analysis indicated the presence of Fe, Ni and Co in both fragments, whereas the elements Al, Ca, Mg, Si and, for the first time Li, were detected only in one fragment and were related to its post-falling alteration and contamination by weathering processes. Quantitative analysis data obtained using the calibration-free (CF) - LIBS method showed a good agreement with those obtained by traditional methods generally applied to meteorite analysis, i.e. Electron Dispersion Spectroscopy - Scanning Electron Microscopy (EDS-SEM), also performed in this study, and Electron Probe Microanalysis (EMPA) (literature data). The local and coupled variability of Ni and Co (increase of Ni and decrease of Co) determined for the unaltered portions exhibiting plessite texture, suggested the occurrence of solid state diffusion processes under a slow cooling rate for the Dronino meteorite.

Laser-induced breakdown spectroscopy: Extending its application to soil pH measurements

Energy Technology Data Exchange (ETDEWEB)

Ferreira, Edilene Cristina, E-mail: edilene@iq.unesp.br [São Paulo State University – UNESP, Analytical Chemistry Department, Rua Prof. Francisco Degni 55, CEP 14800-060, Araraquara, SP (Brazil); Gomes Neto, José A. [São Paulo State University – UNESP, Analytical Chemistry Department, Rua Prof. Francisco Degni 55, CEP 14800-060, Araraquara, SP (Brazil); Milori, Débora M.B.P.; Ferreira, Ednaldo José [Embrapa Agricultural Instrumentation, Rua XV de Novembro 1452, CEP 13560-970, São Carlos, SP (Brazil); Anzano, Jesús Manuel [Laser Laboratory & Environment, Faculty of Sciences, University of Zaragoza, C/. Pedro Cerbuna 12, 50009, Zaragoza (Spain)

2015-08-01

Acid–base equilibria are involved in almost all the processes that occur in soil. The bioavailability of nutrients for plants, for instance, depends on the solubilization of mineral nutrients in the soil solution, which is a pH-dependent process. The determination of pH in soil solutions is usually carried out by potentiometry using a glass membrane electrode, after extracting some of the soil components with water or CaCl{sub 2} solution. The present work describes a simple method for determining the pH of soil, using laser-induced breakdown spectroscopy (LIBS). Sixty samples presenting different textural composition and pH (previously determined by potentiometry) were employed. The samples were divided into a calibration set with fifty samples and a validation set with ten samples. LIBS spectra were recorded for each pelleted sample using laser pulse energy of 115 mJ. The intensities of thirty-two emission lines for Al, Ca, H, and O were used to fit a partial least squares (PLS) model. The model was validated by prediction of the pH of the validation set samples, which showed good agreement with the reference values. The prediction mean absolute error was 0.3 pH units and the root mean square error of the prediction was 0.4. These results highlight the potential of LIBS for use in other applications beyond elemental composition determinations. For soil analysis, the proposed method offers the possibility of determining pH, in addition to nutrients and contaminants, using a single LIBS measurement. - Highlights: • Physical, chemical, and biological properties of soil are influenced by pH. • The pH of mineral soils is normally determined in slurries of water and soil sample by potentiometric measurements. • The association of LIBS elemental emissions with multivariate strategies of analysis has become LIBS a powerful technique. • LIBS was unprecedentedly applied for direct pH determination in different kinds of soil sample. • The clean and fast proposed

Infrared (1-12 μm) atomic and molecular emission signatures from energetic materials using laser-induced breakdown spectroscopy

Science.gov (United States)

Kumi Barimah, E.; Hömmerich, U.; Brown, E.; Yang, C. S.-C.; Trivedi, S. B.; Jin, F.; Wijewarnasuriya, P. S.; Samuels, A. C.; Snyder, A. P.

2013-05-01

Laser-induced breakdown spectroscopy (LIBS) is a powerful analytical technique to detect the elemental composition of solids, liquids, and gases in real time. For example, recent advances in UV-VIS LIBS have shown great promise for applications in chemical, biological, and explosive sensing. The extension of conventional UVVIS LIBS to the near-IR (NIR), mid-IR (MIR) and long wave infrared (LWIR) regions (~1-12 μm) offers the potential to provide additional information due to IR atomic and molecular signatures. In this work, a Q-switched Nd: YAG laser operating at 1064 nm was employed as the excitation source and focused onto several chlorate and nitrate compounds including KClO3, NaClO3, KNO3, and NaNO3 to produce intense plasma at the target surface. IR LIBS studies on background air, KCl , and NaCl were also included for comparison. All potassium and sodium containing samples revealed narrow-band, atomic-like emissions assigned to transitions of neutral alkali-metal atoms in accordance with the NIST atomic spectra database. In addition, first evidence of broad-band molecular LIBS signatures from chlorate and nitrate compounds were observed at ~10 μm and ~7.3 μm, respectively. The observed molecular emissions showed strong correlation with FTIR absorption spectra of the investigated materials.

IMPLEMENTACIÓN DE TÉCNICAS ESPECTROQUÍMICAS EN LA INVESTIGACIÓN ZOOARQUEOLÓGICA. CUANTIFICACIÓN DE ESTRONCIO UTILIZANDO LASER INDUCED BREAKDOWN SPECTROSCOPY (LIBS/ Implementation of spectrochemical techniques in zooarchaeological research...

Directory of Open Access Journals (Sweden)

Gabriela Srur

2012-11-01

Full Text Available Los estudios químicos sobre restos zooarqueológicos se vienen desarrollando con mayor intensidad en las últimas décadas, especialmente aquellos dedicados a la identificación de huellas químicas o diversos tipos de isótopos y sus relaciones. El objetivo de este trabajo es el de presentar dos procedimientos utilizados para la caracterización química de huesos en base a datos espectrométricos obtenidos mediante la técnica LIBS (Laser Induced Breakdown Spectroscopy. El primero denominado Adición Estándar, consiste en un procedimiento destructivo, con un grado de error estimable, mientras que el segundo, Reemplazo de la Matriz Ósea, constituye un método no invasivo y con un grado de error relativamente bajo. Con esto se espera lograr el desarrollo de un corpus metodológico y analítico que permita caracterizar de un modo eficiente y económico las huellas químicas de diverso material arqueofaunístico. En este sentido se intenta lograr una caracterización química de huesos arqueológicos con el fin de dar respuesta a cuestiones relacionadas tanto a la alimentación como a la movilidad de los animales en el pasado. Abstract Chemical studies on zooarchaeological remains have been most extensively developed in recent decades, especially those focused on the identification of chemical fingerprints or types of isotopes and their relationships. This paper aims at showing two procedures used for chemical characterization of bones on the basis of spectrometric data obtained by LIBS technique (Laser Induced Breakdown Spectroscopy. One called Standard Addition, a destructive procedure, with a high error degree; the other called Bone Matrix Replacement, a noninvasive method with a relatively low error degree. We expect to gather a methodological and analytical corpus to characterize, efficiently and inexpensively, the chemical fingerprints of diverse archaeofaunal material. Hence, we intend to achieve chemical characterization of

Study of different concentric rings inside gallstones with LIBS.

Science.gov (United States)

Pathak, Ashok Kumar; Singh, Vivek Kumar; Rai, Nilesh Kumar; Rai, Awadhesh Kumar; Rai, Pradeep Kumar; Rai, Pramod Kumar; Rai, Suman; Baruah, G D

2011-07-01

Gallstones obtained from patients from the north-east region of India (Assam) were studied using laser-induced breakdown spectroscopy (LIBS) technique. LIBS spectra of the different layers (in cross-section) of the gallstones were recorded in the spectral region 200-900 nm. Several elements, including calcium, magnesium, manganese, copper, silicon, phosphorus, iron, sodium and potassium, were detected in the gallstones. Lighter elements, including carbon, hydrogen, nitrogen and oxygen were also detected, which demonstrates the superiority of the LIBS technique over other existing analytical techniques. The LIBS technique was applied to investigate the evolution of C(2) swan bands and CN violet bands in the LIBS spectra of the gallstones in air and an argon atmosphere. The different layers (dark and light layers) of the gallstones were discriminated on the basis of the presence and intensities of the spectral lines for carbon, hydrogen, nitrogen, oxygen and copper. An attempt was also made to correlate the presence of major and minor elements in the gallstones with the common diet of the population of Assam.

Evaluation of self-absorption coefficients of aluminum emission lines in laser-induced breakdown spectroscopy measurements

International Nuclear Information System (INIS)

El Sherbini, A.M.; El Sherbini, Th.M.; Hegazy, H.; Cristoforetti, G.; Legnaioli, S.; Palleschi, V.; Pardini, L.; Salvetti, A.; Tognoni, E.

2005-01-01

In quantitative Laser Induced Breakdown Spectroscopy (LIBS) measurements it is essential to account for the effect of self-absorption on the emission lines intensity. In order to quantify this effect, in this paper we propose a simple method for evaluating the ratio between the actual measured line intensity and the intensity expected in absence of self-absorption and, if necessary, correcting the effect of self-absorption on line intensity. The method, based on a homogeneous plasma model, is applicable when the plasma electron density is known and in particular to lines whose Stark broadening parameter is available

Development of a compact vertical-cavity surface-emitting laser end-pumped actively Q-switched laser for laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Li, Shuo; Chen, Rongzhang; Nelsen, Bryan; Chen, Kevin, E-mail: pec9@pitt.edu [Department of Electrical and Computer Engineering, University of Pittsburgh, Pittsburgh, Pennsylvania 15260 (United States); Liu, Lei; Huang, Xi; Lu, Yongfeng [Department of Electrical and Computer Engineering, University of Nebraska-Lincoln, Lincoln, Nebraska 68588 (United States)

2016-03-15

This paper reports the development of a compact and portable actively Q-switched Nd:YAG laser and its applications in laser-induced breakdown spectroscopy (LIBS). The laser was end-pumped by a vertical-cavity surface-emitting laser (VCSEL). The cavity lases at a wavelength of 1064 nm and produced pulses of 16 ns with a maximum pulse energy of 12.9 mJ. The laser exhibits a reliable performance in terms of pulse-to-pulse stability and timing jitter. The LIBS experiments were carried out using this laser on NIST standard alloy samples. Shot-to-shot LIBS signal stability, crater profile, time evolution of emission spectra, plasma electron density and temperature, and limits of detection were studied and reported in this paper. The test results demonstrate that the VCSEL-pumped solid-state laser is an effective and compact laser tool for laser remote sensing applications.

Qualitative evaluation of maternal milk and commercial infant formulas via LIBS.

Science.gov (United States)

Abdel-Salam, Z; Al Sharnoubi, J; Harith, M A

2013-10-15

This study focuses on the use of laser-induced breakdown spectroscopy (LIBS) for the evaluation of the nutrients in maternal milk and some commercially available infant formulas. The results of such evaluation are vital for adequate and healthy feeding for babies during lactation period. Laser-induced breakdown spectroscopy offers special advantages in comparison to the other conventional analytical techniques. Specifically, LIBS is a straightforward technique that can be used in situ to provide qualitative analytical information in few minutes for the samples under investigation without preparation processes. The samples studied in the current work were maternal milk samples collected during the first 3 months of lactation (not colostrum milk) and samples from six different types of commercially available infant formulas. The samples' elemental composition has been compared with respect to the relative abundance of the elements of nutrition importance, namely Mg, Ca, Na, and Fe using their spectral emission lines in the relevant LIBS spectra. In addition, CN and C2 molecular emission bands in the same spectra have been studied as indicators of proteins content in the samples. The obtained analytical results demonstrate the higher elemental contents of the maternal milk compared with the commercial formulas samples. Similar results have been obtained as for the proteins content. It has been also shown that calcium and proteins have similar relative concentration trends in the studied samples. This work demonstrates the feasibility of adopting LIBS as a fast, safe, less costly technique evaluating qualitatively the nutrients content of both maternal and commercial milk samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of Trace Available Heavy Metals in Soil Using Laser-Induced Breakdown Spectroscopy Assisted with Phase Transformation Method.

Science.gov (United States)

Yi, Rongxing; Yang, Xinyan; Zhou, Ran; Li, Jiaming; Yu, Huiwu; Hao, Zhongqi; Guo, Lianbo; Li, Xiangyou; Lu, Yongfeng; Zeng, Xiaoyan

2018-05-18

To detect available heavy metals in soil using laser-induced breakdown spectroscopy (LIBS) and improve its poor detection sensitivity, a simple and low cost sample pretreatment method named solid-liquid-solid transformation was proposed. By this method, available heavy metals were extracted from soil through ultrasonic vibration and centrifuging and then deposited on a glass slide. Utilization of this solid-liquid-solid transformation method, available Cd and Pb elements in soil were detected successfully. The results show that the regression coefficients of calibration curves for soil analyses reach to more than 0.98. The limits of detection could reach to 0.067 and 0.94 ppm for available Cd and Pb elements in soil under optimized conditions, respectively, which are much better than those obtained by conventional LIBS.

Discrimination of lymphoma using laser-induced breakdown spectroscopy conducted on whole blood samples

Science.gov (United States)

Chen, Xue; Li, Xiaohui; Yang, Sibo; Yu, Xin; Liu, Aichun

2018-01-01

Lymphoma is a significant cancer that affects the human lymphatic and hematopoietic systems. In this work, discrimination of lymphoma using laser-induced breakdown spectroscopy (LIBS) conducted on whole blood samples is presented. The whole blood samples collected from lymphoma patients and healthy controls are deposited onto standard quantitative filter papers and ablated with a 1064 nm Q-switched Nd:YAG laser. 16 atomic and ionic emission lines of calcium (Ca), iron (Fe), magnesium (Mg), potassium (K) and sodium (Na) are selected to discriminate the cancer disease. Chemometric methods, including principal component analysis (PCA), linear discriminant analysis (LDA) classification, and k nearest neighbor (kNN) classification are used to build the discrimination models. Both LDA and kNN models have achieved very good discrimination performances for lymphoma, with an accuracy of over 99.7%, a sensitivity of over 0.996, and a specificity of over 0.997. These results demonstrate that the whole-blood-based LIBS technique in combination with chemometric methods can serve as a fast, less invasive, and accurate method for detection and discrimination of human malignancies. PMID:29541503

Simultaneous Determination of Trace Lead and Chromium in Water Using Laser-Induced Breakdown Spectroscopy and Paper Substrate

International Nuclear Information System (INIS)

Yu Youli; Zhou Weidong; Qian Huiguo; Su Xuejiao; Ren Ke

2014-01-01

Toxic metals such as lead and chromium in aqueous solutions have been analyzed simultaneously by laser-induced breakdown spectroscopy (LIBS), in which the ordinary printing paper is used as a liquid absorber which was immerged into Pb(NO 3 ) 2 and Cr(NO 3 ) 3 aqueous solution to enrich the heavy metals. This method overcomes the drawbacks of splashing and low sensitivity in ordinary LIBS analysis of water, in which a laser beam is directly focused on a liquid surface. A good signal intensity and reproducibility has been demonstrated. The Pb 405.78 nm and Cr 427.48 nm spectral lines are used as the analytical lines. The variation of line intensity with immersion time was investigated. The calibration curve for quantitative measurement of Pb and Cr in water was established, and the detection limits are 0.033 mg/L and 0.026 mg/L respectively, which is about 2–3 orders of magnitude better than that in the ordinary LIBS analysis of heavy metal in solution. (plasma technology)

A Comparison of Multivariate and Pre-Processing Methods for Quantitative Laser-Induced Breakdown Spectroscopy of Geologic Samples

Science.gov (United States)

Anderson, R. B.; Morris, R. V.; Clegg, S. M.; Bell, J. F., III; Humphries, S. D.; Wiens, R. C.

2011-01-01

The ChemCam instrument selected for the Curiosity rover is capable of remote laser-induced breakdown spectroscopy (LIBS).[1] We used a remote LIBS instrument similar to ChemCam to analyze 197 geologic slab samples and 32 pressed-powder geostandards. The slab samples are well-characterized and have been used to validate the calibration of previous instruments on Mars missions, including CRISM [2], OMEGA [3], the MER Pancam [4], Mini-TES [5], and Moessbauer [6] instruments and the Phoenix SSI [7]. The resulting dataset was used to compare multivariate methods for quantitative LIBS and to determine the effect of grain size on calculations. Three multivariate methods - partial least squares (PLS), multilayer perceptron artificial neural networks (MLP ANNs) and cascade correlation (CC) ANNs - were used to generate models and extract the quantitative composition of unknown samples. PLS can be used to predict one element (PLS1) or multiple elements (PLS2) at a time, as can the neural network methods. Although MLP and CC ANNs were successful in some cases, PLS generally produced the most accurate and precise results.

Direct spectral analysis and determination of high content of carcinogenic bromine in bread using UV pulsed laser induced breakdown spectroscopy.

Science.gov (United States)

Mehder, A O; Gondal, Mohammed A; Dastageer, Mohamed A; Habibullah, Yusuf B; Iqbal, Mohammed A; Oloore, Luqman E; Gondal, Bilal

2016-01-01

Laser induced breakdown spectroscopy (LIBS) was applied for the detection of carcinogenic elements like bromine in four representative brands of loaf bread samples and the measured bromine concentrations were 352, 157, 451, and 311 ppm, using Br I (827.2 nm) atomic transition line as the finger print atomic transition. Our LIBS system is equipped with a pulsed laser of wavelength 266 nm with energy 25 mJ pulse(-1), 8 ns pulse duration, 20 Hz repetition rate, and a gated ICCD camera. The LIBS system was calibrated with the standards of known concentrations in the sample (bread) matrix and such plot is linear in 20-500 ppm range. The capability of our system in terms of limit of detection and relative accuracy with respect to the standard inductively coupled plasma mass spectrometry (ICPMS) technique was evaluated and these values were 5.09 ppm and 0.01-0.05, respectively, which ensures the applicability of our system for Br trace level detection, and LIBS results are in excellent agreement with that of ICPMS results.

Laser-induced breakdown spectroscopy analysis of asbestos

International Nuclear Information System (INIS)

Caneve, L.; Colao, F.; Fabbri, F.; Fantoni, R.; Spizzichino, V.; Striber, J.

2005-01-01

Laser-induced breakdown spectroscopy was applied to test the possibility of detecting and identifying asbestos in different samples in view of the perspective at field operation without sample preparation which is peculiar to this technique. Several like-resin materials were first investigated by laser-induced breakdown spectroscopy, in order to find an asbestos container assuring safe laboratory operation during the material characterization aimed to identify indicators suitable for a quick identification on field. Successively, spectra of asbestos samples of both in serpentine and amphibole forms were measured and the variability in elemental composition was calculated from the emission spectra. Ratios of intensities of characteristic elements were tested as indicators for asbestos recognition. Laser-induced breakdown spectroscopy results were compared with those obtained by analyzing the same asbestos samples with a scanning electron microscopy equipped with an energy dispersive X-ray spectroscopy, a good correlation was found for Mg/Si and Fe/Si, thus showing the capability of laser-induced breakdown spectroscopy as a diagnostic tool for this category of materials. In particular, it was demonstrated that the method based on two indicators derived from laser-induced breakdown spectroscopy intensity ratios allows to discriminate between asbestos and cements in single shot measurements suitable to field operation

Spectroscopic analysis of high protein nigella seeds (Kalonji) using laser-induced breakdown spectroscopy and inductively coupled plasma/optical emission spectroscopy

Science.gov (United States)

Rehan, Imran; Khan, M. Zubair; Ali, Irfan; Rehan, Kamran; Sultana, Sabiha; Shah, Sher

2018-03-01

The spectroscopic analysis of high protein nigella seeds (also called Kalonji) was performed using pulsed nanosecond laser-induced breakdown spectroscopy (LIBS) at 532 nm. The emission spectrum of Kalonji recorded with an LIBS spectrometer exposed the presence of various elements like Al, B, Ba, Ca, Cr, K, P, Mg, Mn, Na, Ni, S, Si, Cu, Fe, Ti, Sn, Sr, and Zn. The plasma parameters (electron temperature and electron density) were estimated using Ca-I spectral lines and their behavior were studied against laser irradiance. The electron temperature and electron density was observed to show an increasing trend in the range of 5802-7849 K, and (1.2-3.9) × 1017 cm- 3, respectively, in the studied irradiance range of (1.2-12.6) × 109 W/cm2. Furthermore, the effect of varying laser energy on the integrated signal intensities was also studied. The quantitative analysis of the detected elements was performed via the calibration curves drawn for all the observed elements through typical samples made in the known concentration in the Kalonji matrix, and by setting the concentration of P as the calibration. The validity of our LIBS findings was verified via comparison of the results with the concentration of every element find in Kalonji using the standard analytical tool like ICP/OES. The results acquired using LIBS and ICP/OES were found in fine harmony. Moreover, limit of detection was measured for toxic metals only.

Quantification of gold and silver in minerals by laser-induced breakdown spectroscopy

Science.gov (United States)

Díaz, Daniel; Hahn, David W.; Molina, Alejandro

2017-10-01

The performance of laser-induced breakdown spectroscopy (LIBS) to identify and quantify gold and silver in ore samples was evaluated. Ores from a gold-producing mine and samples artificially doped with Au and Ag solutions to previously defined concentrations (surrogates) were prepared as 50-mm pellets prior to LIBS analysis. Silver detection and intensity measurement was straightforward for concentrations from 0.4 to 43 μg/g and from 1.1 to 375 μg/g in ore and surrogate samples, respectively. Au emission lines were not found after ensemble average or accumulation of 100-single shot LIBS spectra of ore samples containing up to 9.5 μg/g Au. However, the Au signal was present in the spectra of surrogate samples, for which a detection limit of about 0.8 μg/g was determined. When the number of sampling shots in ore samples increased, various single shot spectra registered Au emission lines. The number of spectra containing Au emission lines increased with the number of single shots. Those results, as well as scanning electron microscopy analysis of ore samples, suggest that the discrete analyte distribution as well as the inherent discrete characteristics associated to LIBS made the presence of gold in the LIBS spark an unlikely occurrence. The particle sampling rates (the percentage of laser pulses expected to sample at least one particle) were estimated for gold concentrations of 1.1 and 10.0 μg/g as 0.04% and 0.32%, respectively. A Monte Carlo simulation indicated that > 100 gold-containing particles should be sampled to accurately represent the discrete character of gold in the ore. Sampling 100 such particles requires > 105 laser pulses over a single pellet. Despite the fact that this rather large number of shots makes difficult to conduct conditional analysis on pellets, for some samples that withstood 5000 shots, gold quantification in ores was successfully achieved at concentrations as low as 1 μg/g. Results are encouraging and illustrate the applicability

Remote imaging laser-induced breakdown spectroscopy and laser-induced fluorescence spectroscopy using nanosecond pulses from a mobile lidar system.

Science.gov (United States)

Grönlund, Rasmus; Lundqvist, Mats; Svanberg, Sune

2006-08-01

A mobile lidar system was used in remote imaging laser-induced breakdown spectroscopy (LIBS) and laser-induced fluorescence (LIF) experiments. Also, computer-controlled remote ablation of a chosen area was demonstrated, relevant to cleaning of cultural heritage items. Nanosecond frequency-tripled Nd:YAG laser pulses at 355 nm were employed in experiments with a stand-off distance of 60 meters using pulse energies of up to 170 mJ. By coaxial transmission and common folding of the transmission and reception optical paths using a large computer-controlled mirror, full elemental imaging capability was achieved on composite targets. Different spectral identification algorithms were compared in producing thematic data based on plasma or fluorescence light.

Determination of Cd, Cr and Pb in phosphate fertilizers by laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Nunes, Lidiane Cristina; Gustinelli Arantes de Carvalho, Gabriel [NAPTISA Research Support Center “Technology and Innovation for a Sustainable Agriculture”, Center for Nuclear Energy in Agriculture, University of São Paulo, Av. Centenário 303, 13416-000, Piracicaba SP (Brazil); Santos, Dario [Federal University of São Paulo, R. Prof. Artur Riedel 275, 09972-270, Diadema SP (Brazil); Krug, Francisco José, E-mail: fjkrug@cena.usp.br [NAPTISA Research Support Center “Technology and Innovation for a Sustainable Agriculture”, Center for Nuclear Energy in Agriculture, University of São Paulo, Av. Centenário 303, 13416-000, Piracicaba SP (Brazil)

2014-07-01

A validated method for quantitative determination of Cd, Cr, and Pb in phosphate fertilizers by laser-induced breakdown spectroscopy (LIBS) is presented. Laboratory samples were comminuted and homogenized by cryogenic or planetary ball milling, pressed into pellets and analyzed by LIBS. The experimental setup was designed by using a Q-switched Nd:YAG at 1064 nm with 10 Hz repetition rate, and the intensity signals from Cd II 214.441 nm, Cr II 267.716 nm and Pb II 220.353 nm emission lines were measured by using a spectrometer furnished with an intensified charge-coupled device. LIBS parameters (laser fluence, lens-to-sample distance, delay time, integration time gate, number of sites and number of laser pulses per site) were chosen after univariate experiments with a pellet of NIST SRM 695 (Trace Elements in Multi-Nutrient Fertilizer). Calibration and validation were carried out with 30 fertilizer samples from single superphosphate, triple superphosphate, monoammonium phosphate, and NPK mixtures. Good results were obtained by using 30 pulses of 50 J cm{sup −2} (750 μm spot size), 2.0 μs delay time and 5.0 μs integration time gate. No significant differences between Cd, Cr, and Pb mass fractions determined by the proposed LIBS method and by ICP OES after microwave-assisted acid digestion (AOAC 2006.03 Official Method) were found at 95% confidence level. The limits of detection of 1 mg kg{sup −1} Cd, 2 mg kg{sup −1} Cr and 15 mg kg{sup −1} Pb and the precision (coefficients of variation of results ranging from 2% to 15%) indicate that the proposed LIBS method can be recommended for the determination of these analytes in phosphate fertilizers. - Highlights: • First LIBS application for quantitative Cd, Cr and Pb determination in fertilizers. • LIBS method was validated for analysis of phosphate fertilizers pressed pellets. • LIBS sample throughput is remarkably better than already existing methods.

A Novel and Effective Multivariate Method for Compositional Analysis using Laser Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Wang, W; Qi, H; Ayhan, B; Kwan, C; Vance, S

2014-01-01

Compositional analysis is important to interrogate spectral samples for direct analysis of materials in agriculture, environment and archaeology, etc. In this paper, multi-variate analysis (MVA) techniques are coupled with laser induced breakdown spectroscopy (LIBS) to estimate quantitative elemental compositions and determine the type of the sample. In particular, we present a new multivariate analysis method for composition analysis, referred to as s pectral unmixing . The LIBS spectrum of a testing sample is considered as a linear mixture with more than one constituent signatures that correspond to various chemical elements. The signature library is derived from regression analysis using training samples or is manually set up with the information from an elemental LIBS spectral database. A calibration step is used to make all the signatures in library to be homogeneous with the testing sample so as to avoid inhomogeneous signatures that might be caused by different sampling conditions. To demonstrate the feasibility of the proposed method, we compare it with the traditional partial least squares (PLS) method and the univariate method using a standard soil data set with elemental concentration measured a priori. The experimental results show that the proposed method holds great potential for reliable and effective elemental concentration estimation

Evaluation of laser-induced breakdown spectroscopy analysis potential for addressing radiological threats from a distance

International Nuclear Information System (INIS)

Gaona, I.; Serrano, J.; Moros, J.; Laserna, J.J.

2014-01-01

Although radioactive materials are nowadays valuable tools in nearly all fields of modern science and technology, the dangers stemming from the uncontrolled use of ionizing radiation are more than evident. Since preparedness is a key issue to face the risks of a radiation dispersal event, development of rapid and efficient monitoring technologies to control the contamination caused by radioactive materials is of crucial interest. Laser-induced breakdown spectroscopy (LIBS) exhibits appealing features for this application. This research focuses on the assessment of LIBS potential for the in-situ fingerprinting and identification of radioactive material surrogates from a safe distance. LIBS selectivity and sensitivity to detect a variety of radioactive surrogates, namely 59 Co, 88 Sr, 130 Ba, 133 Cs, 193 Ir and 238 U, on the surface of common urban materials at a distance of 30 m have been evaluated. The performance of the technique for nuclear forensics has been also studied on different model scenarios. Findings have revealed the difficulties to detect and to identify the analytes depending on the surface being interrogated. However, as demonstrated, LIBS shows potential enough for prompt and accurate gathering of essential evidence at a number of sites after the release, either accidental or intentional, of radioactive material. The capability of standoff analysis confers to LIBS unique advantages in terms of fast and safe inspection of forensic scenarios. The identity of the radioactive surrogates is easily assigned from a distance and the sensitivity to their detection is in the range of a few hundreds of ng per square centimeter. - Highlights: • Distant identification of radioactive surrogates on urban surfaces has been proved. • LIBS sensitivity to distant detection of radioactive surrogates has been checked. • Influences of the atmosphere on emission signals have been ascertained. • Usage of standoff LIBS for identifying forensic evidences has been

Evaluation of laser-induced breakdown spectroscopy analysis potential for addressing radiological threats from a distance

Energy Technology Data Exchange (ETDEWEB)

Gaona, I.; Serrano, J.; Moros, J.; Laserna, J.J., E-mail: laserna@uma.es

2014-06-01

Although radioactive materials are nowadays valuable tools in nearly all fields of modern science and technology, the dangers stemming from the uncontrolled use of ionizing radiation are more than evident. Since preparedness is a key issue to face the risks of a radiation dispersal event, development of rapid and efficient monitoring technologies to control the contamination caused by radioactive materials is of crucial interest. Laser-induced breakdown spectroscopy (LIBS) exhibits appealing features for this application. This research focuses on the assessment of LIBS potential for the in-situ fingerprinting and identification of radioactive material surrogates from a safe distance. LIBS selectivity and sensitivity to detect a variety of radioactive surrogates, namely {sup 59}Co, {sup 88}Sr, {sup 130}Ba, {sup 133}Cs, {sup 193}Ir and {sup 238}U, on the surface of common urban materials at a distance of 30 m have been evaluated. The performance of the technique for nuclear forensics has been also studied on different model scenarios. Findings have revealed the difficulties to detect and to identify the analytes depending on the surface being interrogated. However, as demonstrated, LIBS shows potential enough for prompt and accurate gathering of essential evidence at a number of sites after the release, either accidental or intentional, of radioactive material. The capability of standoff analysis confers to LIBS unique advantages in terms of fast and safe inspection of forensic scenarios. The identity of the radioactive surrogates is easily assigned from a distance and the sensitivity to their detection is in the range of a few hundreds of ng per square centimeter. - Highlights: • Distant identification of radioactive surrogates on urban surfaces has been proved. • LIBS sensitivity to distant detection of radioactive surrogates has been checked. • Influences of the atmosphere on emission signals have been ascertained. • Usage of standoff LIBS for identifying

Evaluation of the laser-induced breakdown spectroscopy technique for determination of the chemical composition of copper concentrates

International Nuclear Information System (INIS)

Łazarek, Łukasz; Antończak, Arkadiusz J.; Wójcik, Michał R.; Drzymała, Jan; Abramski, Krzysztof M.

2014-01-01

Laser-induced breakdown spectroscopy (LIBS), like many other spectroscopic techniques, is a comparative method. Typically, in qualitative analysis, synthetic certified standard with a well-known elemental composition is used to calibrate the system. Nevertheless, in all laser-induced techniques, such calibration can affect the accuracy through differences in the overall composition of the chosen standard. There are also some intermediate factors, which can cause imprecision in measurements, such as optical absorption, surface structure and thermal conductivity. In this work the calibration performed for the LIBS technique utilizes pellets made directly from the tested materials (old well-characterized samples). This choice produces a considerable improvement in the accuracy of the method. This technique was adopted for the determination of trace elements in industrial copper concentrates, standardized by conventional atomic absorption spectroscopy with a flame atomizer. A series of copper flotation concentrate samples was analyzed for three elements: silver, cobalt and vanadium. We also proposed a method of post-processing the measurement data to minimize matrix effects and permit reliable analysis. It has been shown that the described technique can be used in qualitative and quantitative analyses of complex inorganic materials, such as copper flotation concentrates. It was noted that the final validation of such methodology is limited mainly by the accuracy of the characterization of the standards. - Highlights: • A laser-induced breakdown spectroscopy technique is introduced for composition monitoring in industrial copper concentrates. • Calibration samples consisted of pellets produced from the tested materials. • The proposed method of post-processing significantly minimizes matrix effects. • The possible uses of this technique are limited mainly by accurate characterization of the standard samples

Evaluation of the laser-induced breakdown spectroscopy technique for determination of the chemical composition of copper concentrates

Energy Technology Data Exchange (ETDEWEB)

Łazarek, Łukasz, E-mail: lukasz.lazarek@pwr.wroc.pl [Laser and Fiber Electronics Group, Faculty of Electronics, Wroclaw University of Technology, Wyb. Wyspianskiego 27, 50-370 Wroclaw (Poland); Antończak, Arkadiusz J.; Wójcik, Michał R. [Laser and Fiber Electronics Group, Faculty of Electronics, Wroclaw University of Technology, Wyb. Wyspianskiego 27, 50-370 Wroclaw (Poland); Drzymała, Jan [Faculty of Geoengineering, Mining and Geology, Wroclaw University of Technology, Wyb. Wyspianskiego 27, 50-370 Wroclaw (Poland); Abramski, Krzysztof M. [Laser and Fiber Electronics Group, Faculty of Electronics, Wroclaw University of Technology, Wyb. Wyspianskiego 27, 50-370 Wroclaw (Poland)

2014-07-01

Laser-induced breakdown spectroscopy (LIBS), like many other spectroscopic techniques, is a comparative method. Typically, in qualitative analysis, synthetic certified standard with a well-known elemental composition is used to calibrate the system. Nevertheless, in all laser-induced techniques, such calibration can affect the accuracy through differences in the overall composition of the chosen standard. There are also some intermediate factors, which can cause imprecision in measurements, such as optical absorption, surface structure and thermal conductivity. In this work the calibration performed for the LIBS technique utilizes pellets made directly from the tested materials (old well-characterized samples). This choice produces a considerable improvement in the accuracy of the method. This technique was adopted for the determination of trace elements in industrial copper concentrates, standardized by conventional atomic absorption spectroscopy with a flame atomizer. A series of copper flotation concentrate samples was analyzed for three elements: silver, cobalt and vanadium. We also proposed a method of post-processing the measurement data to minimize matrix effects and permit reliable analysis. It has been shown that the described technique can be used in qualitative and quantitative analyses of complex inorganic materials, such as copper flotation concentrates. It was noted that the final validation of such methodology is limited mainly by the accuracy of the characterization of the standards. - Highlights: • A laser-induced breakdown spectroscopy technique is introduced for composition monitoring in industrial copper concentrates. • Calibration samples consisted of pellets produced from the tested materials. • The proposed method of post-processing significantly minimizes matrix effects. • The possible uses of this technique are limited mainly by accurate characterization of the standard samples.

Mapping of lead, magnesium and copper accumulation in plant tissues by laser-induced breakdown spectroscopy and laser-ablation inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Kaiser, J. [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technicka 2896/2, 616 69 Brno (Czech Republic)], E-mail: kaiser@fme.vutbr.cz; Galiova, M.; Novotny, K.; Cervenka, R. [Department of Chemistry, Faculty of Science, Masaryk University, Kotlarska 2, 611 37 Brno (Czech Republic); Reale, L. [Faculty of Sciences, University of L' Aquila, Via Vetoio (Coppito 1), 67010 L' Aquila (Italy); Novotny, J.; Liska, M.; Samek, O. [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technicka 2896/2, 616 69 Brno (Czech Republic); Kanicky, V.; Hrdlicka, A. [Department of Chemistry, Faculty of Science, Masaryk University, Kotlarska 2, 611 37 Brno (Czech Republic); Stejskal, K.; Adam, V.; Kizek, R. [Department of Chemistry and Biochemistry, Faculty of Agronomy, Mendel University of Agriculture and Forestry, Zemedelska 1, 613 00 Brno (Czech Republic)

2009-01-15

Laser-Induced Breakdown Spectroscopy (LIBS) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) were utilized for mapping the accumulation of Pb, Mg and Cu with a resolution up to 200 {mu}m in a up to cm x cm area of sunflower (Helianthus annuus L.) leaves. The results obtained by LIBS and LA-ICP-MS are compared with the outcomes from Atomic Absorption Spectrometry (AAS) and Thin-Layer Chromatography (TLC). It is shown that laser-ablation based analytical methods can substitute or supplement these techniques mainly in the cases when a fast multi-elemental mapping of a large sample area is needed.

Novel high-density packaging of solid state diode pumped eye-safe laser for LIBS

Science.gov (United States)

Bares, Kim; Torgerson, Justin; McNeil, Laine; Maine, Patrick; Patterson, Steve

2018-02-01

Laser-Induced Breakdown Spectroscopy (LIBS) has proven to be a useful research tool for material analysis for decades. However, because of the amount of energy required in a few nanosecond pulse to generate a stable and reliable LIBS signal, the lasers are often large and inefficient, relegating their implementation to research facilities, factory floors, and assembly lines. Small portable LIBS systems are now possible without having to compromise on energy needs by leveraging off of advances in high-density packaging of electronics, opto-mechanics, and highly efficient laser resonator architecture. This paper explores the integration of these techniques to achieve a mJ class eye-safe LIBS laser source, while retaining a small, light-weight package suitable for handheld systems.

Detection and evaluation of uranium in different minerals by gamma spectrometry and laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Sergani, F.M.; Khedr, M.A.; Harith, M.A.; El Mongy, S.A.

2004-01-01

Analysis, detection and evaluation of source nuclear materials (e.g. uranium) in different minerals by sensitive techniques are a vital objective for uranium exploration, nuclear materials extraction, processing and verification. In this work, uranium in different geological formations was determined using gamma spectrometry and laser induced breakdown spectroscopy (LIBS). The investigated samples were collected from different regions distributed all over Egypt. The samples were then prepared for non-destructive analysis. A hyper pure germanium detector was used to measure the emitted gamma rays of uranium and its daughters in the samples. The concentrations of uranium in ppm (μg/g) in the investigated samples are given and discussed in this work. The highest uranium concentration (4354.9 ppm) was found in uranophane samples of Gattar rocks. In Laser induced breakdown spectroscopy (LIBS) technique, plasma was formed by irradiating the rock surface with focused Q-switched Nd:Yag laser pulses of 7 ns pulse duration at the fundamental wavelength (1064 nm). Atoms and ions originating from the rock surface are excited and ionized in the laser produced hot plasma (∝10 000 K). The plasma emission spectral line is characteristic of the elements present in the plasma and allows identification of the uranium in the uranophane mineral. The strong atomic line at 424.2 nm is used for the qualitative identification of uranium. It can be mentioned that the elevated levels of uranium in some of the investigated uranophane samples are of great economic feasibility to be extracted. (orig.)

On the elemental analysis of different cigarette brands using laser induced breakdown spectroscopy and laser-ablation time of flight mass spectrometry

Science.gov (United States)

Ahmed, Nasar; Umar, Zeshan A.; Ahmed, Rizwan; Aslam Baig, M.

2017-10-01

We present qualitative and quantitative analysis of the trace elements present in different brands of tobacco available in Pakistan using laser induced breakdown spectroscopy (LIBS) and Laser ablation Time of Flight Mass Spectrometer (LA-TOFMS). The compositional analysis using the calibration free LIBS technique is based on the observed emission spectra of the laser produced plasma plume whereas the elemental composition analysis using LA-TOFMS is based on the mass spectra of the ions produced by laser ablation. The optical emission spectra of these samples contain spectral lines of calcium, magnesium, sodium, potassium, silicon, strontium, barium, lithium and aluminum with varying intensities. The corresponding mass spectra of the elements were detected in LA-TOF-MS with their composition concentration. The analysis of different brands of cigarettes demonstrates that LIBS coupled with a LA-TOF-MS is a powerful technique for the elemental analysis of the trace elements in any solid sample.

Study of archaeological coins of different dynasties using libs coupled with multivariate analysis

Science.gov (United States)

Awasthi, Shikha; Kumar, Rohit; Rai, G. K.; Rai, A. K.

2016-04-01

Laser Induced Breakdown Spectroscopy (LIBS) is an atomic emission spectroscopic technique having unique capability of an in-situ monitoring tool for detection and quantification of elements present in different artifacts. Archaeological coins collected form G.R. Sharma Memorial Museum; University of Allahabad, India has been analyzed using LIBS technique. These coins were obtained from excavation of Kausambi, Uttar Pradesh, India. LIBS system assembled in the laboratory (laser Nd:YAG 532 nm, 4 ns pulse width FWHM with Ocean Optics LIBS 2000+ spectrometer) is employed for spectral acquisition. The spectral lines of Ag, Cu, Ca, Sn, Si, Fe and Mg are identified in the LIBS spectra of different coins. LIBS along with Multivariate Analysis play an effective role for classification and contribution of spectral lines in different coins. The discrimination between five coins with Archaeological interest has been carried out using Principal Component Analysis (PCA). The results show the potential relevancy of the methodology used in the elemental identification and classification of artifacts with high accuracy and robustness.

Detection of early caries by laser-induced breakdown spectroscopy

Science.gov (United States)

Sasazawa, Shuhei; Kakino, Satoko; Matsuura, Yuji

2015-07-01

To improve sensitivity of dental caries detection by laser-induced breakdown spectroscopy (LIBS) analysis, it is proposed to utilize emission peaks in the ultraviolet. We newly focused on zinc whose emission peaks exist in ultraviolet because zinc exists at high concentration in the outer layer of enamel. It was shown that by using ratios between heights of an emission peak of Zn and that of Ca, the detection sensitivity and stability are largely improved. It was also shown that early caries are differentiated from healthy part by properly setting a threshold in the detected ratios. The proposed caries detection system can be applied to dental laser systems such as ones based on Er:YAG-lasers. When ablating early caries part by laser light, the system notices the dentist that the ablation of caries part is finished. We also show the intensity of emission peaks of zinc decreased with ablation with Er:YAG laser light.

Laser-induced breakdown spectroscopy - An emerging chemical sensor technology for real-time field-portable, geochemical, mineralogical, and environmental applications

International Nuclear Information System (INIS)

Harmon, Russell S.; DeLucia, Frank C.; McManus, Catherine E.; McMillan, Nancy J.; Jenkins, Thomas F.; Walsh, Marianne E.; Miziolek, Andrzej

2006-01-01

Laser induced breakdown spectroscopy (LIBS) is a simple spark spectrochemical sensor technology in which a laser beam is directed at a sample surface to create a high-temperature microplasma and a detector used to collect the spectrum of light emission and record its intensity at specific wavelengths. LIBS is an emerging chemical sensor technology undergoing rapid advancement in instrumentation capability and in areas of application. Attributes of a LIBS sensor system include: (i) small size and weight; (ii) technologically mature, inherently rugged, and affordable components; (iii) real-time response; (iv) in situ analysis with no sample preparation required; (v) a high sensitivity to low atomic weight elements which are difficult to determine by other field-portable sensor techniques, and (vi) point sensing or standoff detection. Recent developments in broadband LIBS provide the capability for detection at very high resolution (0.1 nm) of all elements in any unknown target material because all chemical elements emit in the 200-980 nm spectral region. This progress portends a unique potential for the development of a rugged and reliable field-portable chemical sensor that has the potential to be utilized in variety of geochemical, mineralogical, and environmental applications

Nondestructive Determination of Cu Residue in Orange Peel by Laser Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Hu Huiqin; Huang Lin; Liu Muhua; Chen Tianbing; Yang Ping; Yao Mingyin

2015-01-01

Laser induced breakdown spectroscopy (LIBS) is an emerging tool with rapid, nondestructive, green characteristics in qualitative or quantitative analyses of composition in materials. But LIBS has its shortcomings in detect limit and sensitivity. In this work, heavy metal Cu in Gannan Navel Orange, which is one of famous fruits from Jiangxi of China, was analyzed. In view of LIBS's limit, it is difficult to determinate heavy metals in natural fruits. In this work, nine orange samples were pretreated in 50-500 μg/mL Cu solution, respectively. Another one orange sample was chosen as a control group without any pollution treatment. Previous researchers observed that the content of heavy metals is much higher in peel than in pulp. So, the content in pulp can be reflected by detecting peel. The real concentrations of Cu in peels were acquired by atomic absorption spectrophotometer (AAS). A calibration model of Cu I 324.7 and Cu I 327.4 was constructed between LIBS intensity and AAS concentration by six samples. The correlation coefficient of the two models is also 0.95. All of the samples were used to verify the accuracy of the model. The results show that the relative error (RE) between predicted and real concentration is less than 6.5%, and Cu I 324.7 line has smaller RE than Cu I 327.4. The analysis demonstrated that different characteristic lines decided different accuracy. The results prove the feasibility of detecting heavy metals in fruits by LIBS. But the results are limited in treated samples. The next work will focus on direct analysis of heavy metals in natural fruits without any pretreatment. This work is helpful to explore the distribution of heavy metals between pulp and peel. (paper)

Nondestructive Determination of Cu Residue in Orange Peel by Laser Induced Breakdown Spectroscopy

Science.gov (United States)

Hu, Huiqin; Huang, Lin; Liu, Muhua; Chen, Tianbing; Yang, Ping; Yao, Mingyin

2015-08-01

Laser induced breakdown spectroscopy (LIBS) is an emerging tool with rapid, nondestructive, green characteristics in qualitative or quantitative analyses of composition in materials. But LIBS has its shortcomings in detect limit and sensitivity. In this work, heavy metal Cu in Gannan Navel Orange, which is one of famous fruits from Jiangxi of China, was analyzed. In view of LIBS's limit, it is difficult to determinate heavy metals in natural fruits. In this work, nine orange samples were pretreated in 50-500 μg/mL Cu solution, respectively. Another one orange sample was chosen as a control group without any pollution treatment. Previous researchers observed that the content of heavy metals is much higher in peel than in pulp. So, the content in pulp can be reflected by detecting peel. The real concentrations of Cu in peels were acquired by atomic absorption spectrophotometer (AAS). A calibration model of Cu I 324.7 and Cu I 327.4 was constructed between LIBS intensity and AAS concentration by six samples. The correlation coefficient of the two models is also 0.95. All of the samples were used to verify the accuracy of the model. The results show that the relative error (RE) between predicted and real concentration is less than 6.5%, and Cu I 324.7 line has smaller RE than Cu I 327.4. The analysis demonstrated that different characteristic lines decided different accuracy. The results prove the feasibility of detecting heavy metals in fruits by LIBS. But the results are limited in treated samples. The next work will focus on direct analysis of heavy metals in natural fruits without any pretreatment. This work is helpful to explore the distribution of heavy metals between pulp and peel. supported by National Natural Science Foundation of China (No. 31460419) and Major Project of Science and Technology of Jiangxi, China (No. 20143ACB21013)

LIBS Sensor for Sub-surface CO2 Leak Detection in Carbon Sequestration

Directory of Open Access Journals (Sweden)

Jinesh JAIN

2017-07-01

Full Text Available Monitoring carbon sequestration poses numerous challenges to the sensor community. For example, the subsurface environment is notoriously harsh, with large potential mechanical, thermal, and chemical stresses, making long-term stability and survival a challenge to any potential in situ monitoring method. Laser induced breakdown spectroscopy (LIBS has been demonstrated as a promising technology for chemical monitoring of harsh environments and hard to reach places. LIBS has a real- time monitoring capability and can be used for the elemental and isotopic analysis of solid, liquid, and gas samples. The flexibility of the probe design and the use of fiber- optics has made LIBS particularly suited for remote measurements. The paper focuses on developing a LIBS instrument for downhole high-pressure, high-temperature brine experiments, where CO2 leakage could result in changes in the trace mineral composition of an aquifer. The progress in fabricating a compact, robust, and simple LIBS sensor for widespread subsurface leak detection is presented.

Chemical analysis of industrial scale deposits by combined use of correlation coefficients with emission line detection of laser induced breakdown spectroscopy spectra

International Nuclear Information System (INIS)

Siozos, P.; Philippidis, A.; Hadjistefanou, M.; Gounarakis, C.; Anglos, D.

2013-01-01

Laser-induced breakdown spectroscopy (LIBS) was used to determine the mineral composition of various industrial scale samples. The aim of the study has been to investigate the capacity of LIBS to provide a fast, reliable analytical tool for carrying out routine analysis of inorganic scales, potentially on site, as a means to facilitate decision making concerning scale removal procedures. LIBS spectra collected in the range of 200–660 nm conveyed information about the metal content of the minerals. Via a straightforward analysis based on linear correlation of LIBS spectra it was possible to successfully discriminate scale samples into three main groups, Fe-rich, Ca-rich and Ba-rich, on the basis of correlation coefficients. By combining correlation coefficients with spectral data collected in the NIR, 860–960 nm, where sulfur emissions are detected, it became further possible to discriminate sulfates from carbonates as confirmed by independent analysis based on Raman spectroscopy. It is emphasized that the proposed LIBS-based method successfully identifies the major mineral or minerals present in the samples classifying the scales into relevant groups hence enabling process engineers to select appropriate scale dissolution strategies. - Highlights: • LIBS was used to determine the mineral composition of industrial scale samples. • Three groups of inorganic scales were identified: Ca rich, Ba rich and Fe rich. • A method that combines correlation coefficients and line detection is proposed. • The method successfully identifies the main mineral, or minerals, in the samples. • The results were compared with results obtained by use of Raman analysis

Laser-Induced Breakdown Spectroscopy for Rapid Discrimination of Heavy-Metal-Contaminated Seafood Tegillarca granosa

Directory of Open Access Journals (Sweden)

Guoli Ji

2017-11-01

Full Text Available Tegillarca granosa samples contaminated artificially by three kinds of toxic heavy metals including zinc (Zn, cadmium (Cd, and lead (Pb were attempted to be distinguished using laser-induced breakdown spectroscopy (LIBS technology and pattern recognition methods in this study. The measured spectra were firstly processed by a wavelet transform algorithm (WTA, then the generated characteristic information was subsequently expressed by an information gain algorithm (IGA. As a result, 30 variables obtained were used as input variables for three classifiers: partial least square discriminant analysis (PLS-DA, support vector machine (SVM, and random forest (RF, among which the RF model exhibited the best performance, with 93.3% discrimination accuracy among those classifiers. Besides, the extracted characteristic information was used to reconstruct the original spectra by inverse WTA, and the corresponding attribution of the reconstructed spectra was then discussed. This work indicates that the healthy shellfish samples of Tegillarca granosa could be distinguished from the toxic heavy-metal-contaminated ones by pattern recognition analysis combined with LIBS technology, which only requires minimal pretreatments.

Laser-induced breakdown spectroscopy and chemometrics for classification of toys relying on toxic elements

International Nuclear Information System (INIS)

Godoi, Quienly; Leme, Flavio O.; Trevizan, Lilian C.; Pereira Filho, Edenir R.; Rufini, Iolanda A.; Santos, Dario; Krug, Francisco J.

2011-01-01

Quality control of toys for avoiding children exposure to potentially toxic elements is of utmost relevance and it is a common requirement in national and/or international norms for health and safety reasons. Laser-induced breakdown spectroscopy (LIBS) was recently evaluated at authors' laboratory for direct analysis of plastic toys and one of the main difficulties for the determination of Cd, Cr and Pb was the variety of mixtures and types of polymers. As most norms rely on migration (lixiviation) protocols, chemometric classification models from LIBS spectra were tested for sampling toys that present potential risk of Cd, Cr and Pb contamination. The classification models were generated from the emission spectra of 51 polymeric toys and by using Partial Least Squares - Discriminant Analysis (PLS-DA), Soft Independent Modeling of Class Analogy (SIMCA) and K-Nearest Neighbor (KNN). The classification models and validations were carried out with 40 and 11 test samples, respectively. Best results were obtained when KNN was used, with corrected predictions varying from 95% for Cd to 100% for Cr and Pb.

Preliminary results of in situ laser-induced breakdown spectroscopy for the first wall diagnostics on EAST

Science.gov (United States)

Hu, Zhenhua; Li, Cong; Xiao, Qingmei; Liu, Ping; Fang, Ding; Mao, Hongmin; Wu, Jing; Zhao, Dongye; Ding, Hongbin; Luo, Guang-Nan; EAST Team

2017-02-01

Post-mortem methods cannot fulfill the requirement of monitoring the lifetime of the plasma facing components (PFC) and measuring the tritium inventory for the safety evaluation. Laser-induced breakdown spectroscopy (LIBS) is proposed as a promising method for the in situ study of fuel retention and impurity deposition in a tokamak. In this study, an in situ LIBS system was successfully established on EAST to investigate fuel retention and impurity deposition on the first wall without the need of removal tiles between plasma discharges. Spectral lines of D, H and impurities (Mo, Li, Si, … ) in laser-induced plasma were observed and identified within the wavelength range of 500-700 nm. Qualitative measurements such as thickness of the deposition layers, element depth profile and fuel retention on the wall are obtained by means of in situ LIBS. The results demonstrated the potential applications of LIBS for in situ characterization of fuel retention and co-deposition on the first wall of EAST. Supported by the National Magnetic Confinement Fusion Science Program of China (Nos. 2013GB105002, 2015GB109001, and 2013GB109005), National Natural Science Foundation of China (Nos. 11575243, 11605238, 11605023), Chinesisch-Deutsches Forschungs Project (GZ765), and Korea Research Council of Fundamental Science and Technology (KRCF) under the international collaboration & research in Asian countries (PG1314).

Measurement of Irradiated Pyroprocessing Samples via Laser Induced Breakdown Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Phongikaroon, Supathorn [Virginia Commonwealth Univ., Richmond, VA (United States)

2016-10-31

The primary objective of this research is to develop an applied technology and provide an assessment to remotely measure and analyze the real time or near real time concentrations of used nuclear fuel (UNF) dissolute in electrorefiners. Here, Laser-Induced Breakdown Spectroscopy (LIBS), in UNF pyroprocessing facilities will be investigated. LIBS is an elemental analysis method, which is based on the emission from plasma generated by focusing a laser beam into the medium. This technology has been reported to be applicable in the media of solids, liquids (includes molten metals), and gases for detecting elements of special nuclear materials. The advantages of applying the technology for pyroprocessing facilities are: (i) Rapid real-time elemental analysis|one measurement/laser pulse, or average spectra from multiple laser pulses for greater accuracy in < 2 minutes; (ii) Direct detection of elements and impurities in the system with low detection limits|element specific, ranging from 2-1000 ppm for most elements; and (iii) Near non-destructive elemental analysis method (about 1 g material). One important challenge to overcome is achieving high-resolution spectral analysis to quantitatively analyze all important fission products and actinides. Another important challenge is related to accessibility of molten salt, which is heated in a heavily insulated, remotely operated furnace in a high radiation environment with an argon atmosphere.

Analysis of LiSn alloy at several depths using LIBS

Energy Technology Data Exchange (ETDEWEB)

Suchoňová, M., E-mail: maria.suchonova@fmph.uniba.sk [Dept. of Experimental Physics, Faculty of Mathematics Physics and Informatics, Comenius University in Bratislava, Mlynská dolina F2, 842 48 Bratislava (Slovakia); Krištof, J.; Pribula, M. [Dept. of Experimental Physics, Faculty of Mathematics Physics and Informatics, Comenius University in Bratislava, Mlynská dolina F2, 842 48 Bratislava (Slovakia); Veis, M. [Dept. of Inorganic Chemistry, Faculty of Natural Science, Comenius University, Mlynská dolina, Ilkovičova 6, 842 15 Bratislava 4 (Slovakia); Tabarés, F.L. [Fusion Department, Ciemat, Av Complutense 40, 28040 Madrid (Spain); Veis, P., E-mail: pavel.veis@fmph.uniba.sk [Dept. of Experimental Physics, Faculty of Mathematics Physics and Informatics, Comenius University in Bratislava, Mlynská dolina F2, 842 48 Bratislava (Slovakia)

2017-04-15

The difference between the composition of the surface and the inner part of the LiSn sample was studied using Calibration Free Laser Induced Breakdown Spectroscopy (CF-LIBS) method. The sample was analysed under the low pressure (1330 Pa) in Ar atmosphere. The spectra were record using Echelle spectrometer (Mechelle ME5000). Gate delay and gate width was optimised and set to 300 ns. In order to analyse depth profile the LIBS spectra was recorded after each laser shot. The electron density analysed by laser induced plasma was determined separately for each laser shot, which means for each ablated layer of investigated sample. The difference between the individual shots taken at distinct sites of the sample are shown. The CF-LIBS method was used to determine the elemental composition near the surface and in the central part of the LiSn sample.

Compositional analysis of Hispanic Terra Sigillata by laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Lopez, A.J.; Nicolas, G.; Mateo, M.P.; Pinon, V.; Tobar, M.J.; Ramil, A.

2005-01-01

Laser induced breakdown spectroscopy (LIBS) has been applied for the analysis of Roman pottery Hispanic Terra Sigillata dating back to the 1st-5th century A.C. from two important ceramic production centers in Spain. For each sample, several examinations were performed on slip and body providing data necessary to draw depth profiles of the contents of various elements. In all the cases investigated, the amount of some elements such as calcium and iron and the presence of other ones such as silicon and aluminum showed the differences existing between slip and body in these ancient ceramics in relation with their region and period of production. In addition, complementary analyses were carried out with scanning electron microscopy linked with energy dispersive X-ray microanalysis (SEM/EDX) to measure the thickness of slip and to obtain verification of chemical results

Laser-induced breakdown spectroscopy-based investigation and classification of pharmaceutical tablets using multivariate chemometric analysis

Science.gov (United States)

Myakalwar, Ashwin Kumar; Sreedhar, S.; Barman, Ishan; Dingari, Narahara Chari; Rao, S. Venugopal; Kiran, P. Prem; Tewari, Surya P.; Kumar, G. Manoj

2012-01-01

We report the effectiveness of laser-induced breakdown spectroscopy (LIBS) in probing the content of pharmaceutical tablets and also investigate its feasibility for routine classification. This method is particularly beneficial in applications where its exquisite chemical specificity and suitability for remote and on site characterization significantly improves the speed and accuracy of quality control and assurance process. Our experiments reveal that in addition to the presence of carbon, hydrogen, nitrogen and oxygen, which can be primarily attributed to the active pharmaceutical ingredients, specific inorganic atoms were also present in all the tablets. Initial attempts at classification by a ratiometric approach using oxygen to nitrogen compositional values yielded an optimal value (at 746.83 nm) with the least relative standard deviation but nevertheless failed to provide an acceptable classification. To overcome this bottleneck in the detection process, two chemometric algorithms, i.e. principal component analysis (PCA) and soft independent modeling of class analogy (SIMCA), were implemented to exploit the multivariate nature of the LIBS data demonstrating that LIBS has the potential to differentiate and discriminate among pharmaceutical tablets. We report excellent prospective classification accuracy using supervised classification via the SIMCA algorithm, demonstrating its potential for future applications in process analytical technology, especially for fast on-line process control monitoring applications in the pharmaceutical industry. PMID:22099648

Trace element quantification of lead based roof sheets of historical monuments by Laser Induced Breakdown Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Syvilay, D., E-mail: delphine.syvilay@culture.gouv.fr [LRMH USR 3224, 29 rue de Paris, 77420 Champs-sur-Marne (France); Texier, A. [LRMH USR 3224, 29 rue de Paris, 77420 Champs-sur-Marne (France); Arles, A.; Gratuze, B. [IRAMAT, 3D, rue de la Férollerie, 45071 Orléans Cedex 2 (France); Wilkie-Chancellier, N.; Martinez, L.; Serfaty, S. [SATIE, UMR CNRS 8029, Université de Cergy-Pontoise, ENS Cachan, 95000 Cergy-Pontoise Cedex (France); Detalle, V. [LRMH USR 3224, 29 rue de Paris, 77420 Champs-sur-Marne (France)

2015-01-01

The aim of this paper is to identify the different periods of construction or restoration of the lead roof of a historic monument. Trace elements in a lead matrix can be a signature of the metallurgical processes, allowing identification of a specific time period for the production of the lead used to build the roof. The ability of LIBS (Laser Induced Breakdown Spectroscopy) to detect such trace elements in a lead matrix is therefore explored and checked by comparing its results with LA-ICP-MS as a reference method (Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry). Concentrations of 263 samples were compared between LIBS and LA-ICP-MS data and their correlation was evaluated. Another way to compare their results is also suggested by combining PCA (Principal Component Analysis) and GIS (Geographic Information System). As a result statistical mappings were created, highlighting metallurgical groups of samples across the roof of the building. This innovative approach links concentration and spatial location resulting in an easily interpretable graphical presentation of the data. The results of both spectrometry methods lead to similar conclusions with distinctive areas of different lead compositions and by extension different lead dating across the roof. But since LIBS is portable we can conclude that it is a suitable and reliable instrument for in-situ applications on historic monuments. - Highlights: • Quantification of trace elements (Ag, Bi, Cu and Sn) in a lead matrix by LIBS and LA-ICP-MS • Low limit of detection for Ag, Bi, Cu and Sn by using LIBS portable instrumentation • Set up a specific data processing combining PCA and GIS for cultural heritage application • Comparison of LIBS and LA-ICP-MS results with 263 samples • 488 samples analyzed by LIBS.

Analysis of laser-induced breakdown spectroscopy spectra: The case for extreme value statistics

International Nuclear Information System (INIS)

Michel, Anna P.M.; Chave, Alan D.

2007-01-01

In most instances, laser-induced breakdown spectroscopy (LIBS) spectra are obtained through analog accumulation of multiple shots in the spectrometer CCD. The average acquired in the CCD at a given wavelength is assumed to be a good representation of the population mean, which in turn is implicitly regarded to be the best estimator for the central value of the distribution of the spectrum at the same wavelength. Multiple analog accumulated spectra are taken and then in turn averaged wavelength-by-wavelength to represent the final spectrum. In this paper, the statistics of single-shot and analog accumulated LIBS spectra of both solids and liquids were examined to evaluate whether the spectrum averaging approach is statistically defensible. At a given wavelength, LIBS spectra are typically drawn from a Frechet extreme value distribution, and hence the mean of an ensemble of LIBS spectra is not necessarily an optimal summary statistic. Under circumstances that are broadly general, the sample mean for LIBS data is statistically inconsistent and the central limit theorem does not apply. This result appears to be due to very high shot-to-shot plasma variability in which a very small number of spectra are high in intensity while the majority are very weak, yielding the extreme value form of the distribution. The extreme value behavior persists when individual shots are analog accumulated. An optimal estimator in a well-defined sense for the spectral average at a given wavelength follows from the maximum likelihood method for the extreme value distribution. Example spectra taken with both an Echelle and a Czerny-Turner spectrometer are processed with this scheme to create smooth, high signal-to-noise summary spectra. Plasma imaging was used in an attempt to visually understand the observed variability and to validate the use of extreme value statistics. The data processing approach presented in this paper is statistically reliable and should be used for accurate

Evaluation of a compact spectrograph for in-situ and stand-off Laser-Induced Breakdown Spectroscopy analyses of geological samples on Mars missions

International Nuclear Information System (INIS)

Salle, Beatrice; Cremers, David A.; Maurice, Sylvestre; Wiens, Roger C.; Fichet, Pascal

2005-01-01

Laser-induced Breakdown Spectroscopy (LIBS) is actively under development for future use on surface probes to Mars. The analytical method can be deployed for in-situ and/or stand-off analysis with the latter embodiment providing the greatest advantages compared to previous and current elemental analysis methods used for planetary surface analysis. For this application, LIBS must be thoroughly investigated in terms of analytical capabilities and flight-rated instruments must be developed. Because of the low pressure of the predominantly CO 2 atmosphere on Mars, studies are needed to understand analytical requirements and to determine performance under these conditions. Stand-off analysis demands the most stringent requirements on instrumentation. Therefore, it must be determined if the high performance components that are normally used in a typical LIBS laboratory setup, which are generally not optimized for small size and weight, are essential to obtain the maximum scientific return from a mission. A key component of a LIBS apparatus is the detection system consisting of a spectrograph and a detector. Here we present an evaluation of one design of a compact spectrograph (Ocean Optics HR2000) for in-situ and stand-off LIBS analyses of geological samples under Mars atmospheric conditions

Quantitative estimation of carbonation and chloride penetration in reinforced concrete by laser-induced breakdown spectroscopy

Science.gov (United States)

Eto, Shuzo; Matsuo, Toyofumi; Matsumura, Takuro; Fujii, Takashi; Tanaka, Masayoshi Y.

2014-11-01

The penetration profile of chlorine in a reinforced concrete (RC) specimen was determined by laser-induced breakdown spectroscopy (LIBS). The concrete core was prepared from RC beams with cracking damage induced by bending load and salt water spraying. LIBS was performed using a specimen that was obtained by splitting the concrete core, and the line scan of laser pulses gave the two-dimensional emission intensity profiles of 100 × 80 mm2 within one hour. The two-dimensional profile of the emission intensity suggests that the presence of the crack had less effect on the emission intensity when the measurement interval was larger than the crack width. The chlorine emission spectrum was measured without using the buffer gas, which is usually used for chlorine measurement, by collinear double-pulse LIBS. The apparent diffusion coefficient, which is one of the most important parameters for chloride penetration in concrete, was estimated using the depth profile of chlorine emission intensity and Fick's law. The carbonation depth was estimated on the basis of the relationship between carbon and calcium emission intensities. When the carbon emission intensity was statistically higher than the calcium emission intensity at the measurement point, we determined that the point was carbonated. The estimation results were consistent with the spraying test results using phenolphthalein solution. These results suggest that the quantitative estimation by LIBS of carbonation depth and chloride penetration can be performed simultaneously.

Comparative study on fast classification of brick samples by combination of principal component analysis and linear discriminant analysis using stand-off and table-top laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Vítková, Gabriela [Department of Chemistry, Faculty of Science, Masaryk University, Kamenice 5/A14, 625 00 Brno (Czech Republic); Prokeš, Lubomír [Department of Chemistry, Faculty of Science, Masaryk University, Kamenice 5/A14, 625 00 Brno (Czech Republic); Department of Physical Electronics, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); CEPLANT, R and D Center for Low-Cost Plasma and Nanotechnology Surface Modifications, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Novotný, Karel [Department of Chemistry, Faculty of Science, Masaryk University, Kamenice 5/A14, 625 00 Brno (Czech Republic); CEITEC — Central European Institute of Technology, Masaryk University, Kamenice 5, 625 00 Brno (Czech Republic); Pořízka, Pavel [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technická 2896/2, 616 69 Brno (Czech Republic); Novotný, Jan [CEITEC — Central European Institute of Technology, Brno University of Technology, Technická 3058/10, 616 00 Brno (Czech Republic); Všianský, Dalibor [Department of Geological Sciences, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Čelko, Ladislav [CEITEC — Central European Institute of Technology, Brno University of Technology, Technická 3058/10, 616 00 Brno (Czech Republic); and others

2014-11-01

Focusing on historical aspect, during archeological excavation or restoration works of buildings or different structures built from bricks it is important to determine, preferably in-situ and in real-time, the locality of bricks origin. Fast classification of bricks on the base of Laser-Induced Breakdown Spectroscopy (LIBS) spectra is possible using multivariate statistical methods. Combination of principal component analysis (PCA) and linear discriminant analysis (LDA) was applied in this case. LIBS was used to classify altogether the 29 brick samples from 7 different localities. Realizing comparative study using two different LIBS setups — stand-off and table-top it is shown that stand-off LIBS has a big potential for archeological in-field measurements. - Highlights: • Comparison of two potentially field-deployable LIBS setups is introduced. • The aim is classification of LIBS spectra of brick samples into several localities. • LDA filled with PCA scores is proposed as an effective classification method. • An influence of brick firing temperature on LIBS spectra is discovered and examined.

Determination of plasma temperature and electron density in river sediment plasma using calibration-free laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Austria, Elmer S. Jr.; Lamorena-Lim, Rheo B.

2015-01-01

Calibration-free laser-induced breakdown spectroscopy (CF-LIBS) technique is an approach used to quantitatively measure elemental composition of samples without the use of standard reference materials (SRMs). Due to the unavailability of most SRMs for specific samples, the CF-LIBS approach is steadily becoming more prevalent. CF-LIBS also minimizes interferences from the sample matrix by accounting spectral line intensifies of different elements. The first part of the CF-LIBS algorithm is the calculation of plasma temperature and electron density of the sample while the second part deals with the self-absorption correction and quantitative elemental analysis. In this study, the precursor parameters for the algorithm - plasma temperature and electron density - were measured through the neutral atom and ion line emissions of Fe and Cu in the time window of 0.1 to 10 μs. Plasma from river sediment samples were produced by a 1064 nm nanosecond pulsed Nd:YAG laser at atmospheric pressure. The plasma temperature and electron density were calculated from the Boltzmann plot and Saha-Boltzmann equation methods, respectively. These precursor parameters can be used in calculating the time window wherein the plasma is optically thin at local thermodynamic equilibrium (LTE) and for quantitative multi-elemental analysis. (author)

Identifikasi Unsur Radioaktif Pada Batako Ringan Aerasi Citicon Dengan Metode Laser Induced Breakdown Spectroscopy (LIBS

Directory of Open Access Journals (Sweden)

Wahyulianti Wahyulianti

2016-02-01

Full Text Available Research has been done to identify the radioactive elements in the Citicon aerated lightweight concrete block sample. In this research used a Citicon aerated lightweight concrete block as a sample with 1 cm x 3 cm in size and identification process used LIBS method. Radioactive elements identified in Citicon aerated lightweight concrete block the LIBS method were Th, Ra, and K. The number of photon emission intensity at the wavelength of each element is 396.710 nm, 620.033 nm, and 766.497 nm respectively by 62.33 a.u, 1.67 a.u, and 72.75 a.u.

Discrimination of forensic trace evidence using laser induced breakdown spectroscopy

Science.gov (United States)

Bridge, Candice Mae

Elemental analysis in forensic laboratories can be tedious and many trace evidence items are not analyzed to determine their elemental composition. Presently, scanning electron microscopy-energy dispersive x-ray spectroscopy (SEM-EDS) is the primary analytical tool for determining the elemental composition of trace evidence items. However, due to the time it takes to obtain the required vacuum and the limited number of samples that can be analyzed at any one time, SEM-EDS can be impractical for a high volume of evidence items. An alternative instrument that can be used for this type of analysis is laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). While LA-ICP-MS is a very precise and quantitative analytical method that determines elemental composition based on isotopic mass measurements; however, the instrumentation is relatively expensive and therefore is budgetarily prohibitive for many forensic laboratories. It is the purpose of this research to evaluate an inexpensive instrument that can potentially provide rapid elemental analysis for many forensic laboratories. Laser induced breakdown spectroscopy (LIBS) is an analytical method that meets these requirements and offers information about the elemental composition based on ionic, atomic and diatomic molecular emissions.

New ways for the quantification by the laser-induced plasma spectroscopy; Neue Wege zur Quantifizierung mit der laserinduzierten Plasmaspektroskopie (LIBS)

Energy Technology Data Exchange (ETDEWEB)

Mueller, Maike

2010-04-27

Laser Induced Breakdown Spectroscopy (LIBS) is capable of a fast and multielement analysis of various samples types and matrices which makes the method particularly attractive for industrial process analysis. However, for LIBS to become well accepted as an analytical method some issues in calibration and understanding of the underlying transient plasma processes have to be solved. The objective of this work was to identify influential instrumental parameters and plasma conditions in order to improve the overall quantitative performance of LIBS. As the spectral sensitivity and signal-to-noise ratio of the detector represents a decisive element for the application of LIBS in an industrial environment, two detectors, an ICCD and CCD camera, were compared. In combination with a high-resolution echelle spectrograph, the superior or at least equivalent efficiency of the non-intensified CCD was experimentally demonstrated and supported by corresponding plasma simulations. Further investigations of the plasma expansion under different atmospheric conditions revealed that the geometry of observing the expanding plasma influences the sensitivity and reproducibility of the measurements considerably. The diagnostics of self-absorbed spectral lines and their use for calibration purposes were studied with a mirror-based duplication method and a statistical line shape analysis employing linear correlation. The linear correlation approach displayed good performance for identifying the on-set of self absorption in comparison to the duplication method. As matrixmatched reference materials are essential to validate laser ablation methods, two novel preparations of individual calibration standards based on a copper-and polyacrylamide matrix were tested for their applicability to LIBS. (orig.)

Optimization of laser-induced breakdown spectroscopy for coal powder analysis with different particle flow diameters

Energy Technology Data Exchange (ETDEWEB)

Yao, Shunchun, E-mail: epscyao@scut.edu.cn [School of Electric Power, South China University of Technology, Guangzhou, Guangdong 510640 (China); State Key Laboratory of Pulsed Power Laser Technology, Electronic Engineering Institute, Hefei 230037 (China); Xu, Jialong; Dong, Xuan; Zhang, Bo; Zheng, Jianping [School of Electric Power, South China University of Technology, Guangzhou, Guangdong 510640 (China); Lu, Jidong, E-mail: jdlu@scut.edu.cn [School of Electric Power, South China University of Technology, Guangzhou, Guangdong 510640 (China)

2015-08-01

The on-line measurement of coal is extremely useful for emission control and combustion process optimization in coal-fired plant. Laser-induced breakdown spectroscopy was employed to directly analyze coal particle flow. A set of tapered tubes were proposed for beam-focusing the coal particle flow to different diameters. For optimizing the measurement of coal particle flow, the characteristics of laser-induced plasma, including optical breakdown, the relative standard deviation of repeated measurement, partial breakdown spectra ratio and line intensity, were carefully analyzed. The comparison of the plasma characteristics among coal particle flow with different diameters showed that air breakdown and the random change in plasma position relative to the collection optics could significantly influence on the line intensity and the reproducibility of measurement. It is demonstrated that the tapered tube with a diameter of 5.5 mm was particularly useful to enrich the coal particles in laser focus spot as well as to reduce the influence of air breakdown and random changes of plasma in the experiment. - Highlights: • Tapered tube was designed for beam-focusing the coal particle flow as well as enriching the particles in laser focus spot. • The characteristics of laser-induced plasma of coal particle flow were investigated carefully. • An appropriate diameter of coal particle flow was proven to benefit for improving the performance of LIBS measurement.

Analysis of carbon and nitrogen signatures with laser-induced breakdown spectroscopy; the quest for organics under Mars-like conditions

Science.gov (United States)

Dequaire, T.; Meslin, P.-Y.; Beck, P.; Jaber, M.; Cousin, A.; Rapin, W.; Lasne, J.; Gasnault, O.; Maurice, S.; Buch, A.; Szopa, C.; Coll, P.

2017-05-01

Organic matter has been continuously delivered by meteorites and comets to Mars since its formation, and possibly formed in situ by abiogenic and/or biogenic processes. This organic matter may be preserved from the harsh oxidizing environment of Mars in specific locations. Together with water, organic molecules are necessary to the emergence of life as we know it. Since the first martian landers, scientists have been searching for organics and until today, only one positive detection has been made by a Gas Chromatography Mass Spectrometer (GCMS) instrument onboard the Curiosity rover. In this article we investigate a complementary approach to guide the search for organic matter using ChemCam, the first Laser-Induced Breakdown Spectroscopy (LIBS) instrument on Mars. This experimental study focuses on the analysis of carbon and nitrogen LIBS signatures in organoclay samples and allows the determination of the critical level (Lc) and limit of detection (LoD) of these elements with LIBS under Mars-like conditions, giving new insights into the search of organic matter on Mars.

Calibration curves for commercial copper and aluminum alloys using handheld laser-induced breakdown spectroscopy

Science.gov (United States)

Bennett, B. N.; Martin, M. Z.; Leonard, D. N.; Garlea, E.

2018-03-01

Handheld laser-induced breakdown spectroscopy (HH LIBS) was used to study the elemental composition of four copper alloys and four aluminum alloys to produce calibration curves. The HH LIBS instrument used is a SciAps Z-500, commercially available, that contains a class-1 solid-state laser with an output wavelength of 1532 nm, laser energy of 5 mJ/pulse, and a pulse duration of 5 ns. Test samples were solid specimens comprising copper and aluminum alloys and data were collected from the samples' surface at three different locations, employing a 12-point-grid pattern for each data set. All three data sets of the spectra were averaged, and the intensity, corrected by subtraction of background, was used to produce the elemental calibration curves. Calibration curves are presented for the matrix elements, copper and aluminum, as well as several minor elements. The surface damage produced by the laser was examined by microscopy. The alloys were tested in air and in a glovebox to evaluate the instrument's ability to identify the constituents within materials under different environmental conditions. The main objective of using this HH LIBS technology is to determine its capability to fingerprint the presence of certain elements related to subpercent level within materials in real time and in situ, as a starting point for undertaking future complex material characterization work.

Geometrical effects in data collection and processing for calibration-free laser-induced breakdown spectroscopy

Science.gov (United States)

Shabanov, S. V.; Gornushkin, I. B.

2018-01-01

Data processing in the calibration-free laser-induced breakdown spectroscopy (LIBS) is usually based on the solution of the radiative transfer equation along a particular line of sight through a plasma plume. The LIBS data processing is generalized to the case when the spectral data are collected from large portions of the plume. It is shown that by adjusting the optical depth and width of the lines the spectra obtained by collecting light from an entire spherical homogeneous plasma plume can be least-square fitted to a spectrum obtained by collecting the radiation just along a plume diameter with a relative error of 10-11 or smaller (for the optical depth not exceeding 0.3) so that a mismatch of geometries of data processing and data collection cannot be detected by fitting. Despite the existence of such a perfect least-square fit, the errors in the line optical depth and width found by a data processing with an inappropriate geometry can be large. It is shown with analytic and numerical examples that the corresponding relative errors in the found elemental number densities and concentrations may be as high as 50% and 20%, respectively. Safe for a few found exceptions, these errors are impossible to eliminate from LIBS data processing unless a proper solution of the radiative transfer equation corresponding to the ray tracing in the spectral data collection is used.

Laser-induced breakdown spectroscopy to monitor ion cyclotron range of frequency wall cleaning Li/D co-deposition in EAST tokamak

Energy Technology Data Exchange (ETDEWEB)

Liu, P.; Wu, D.; Sun, L.Y.; Zhao, D.Y.; Hai, R.; Li, C. [Key Laboratory of Materials Modification by Laser, Ion and Electron Beams, Chinese Ministry of Education, School of Physics and Optical Electronic Technology, Dalian University of Technology, Dalian, 116024 (China); Ding, H., E-mail: hding@dlut.edu.cn [Key Laboratory of Materials Modification by Laser, Ion and Electron Beams, Chinese Ministry of Education, School of Physics and Optical Electronic Technology, Dalian University of Technology, Dalian, 116024 (China); Hu, Z.H.; Wang, L.; Hu, J.S.; Chen, J.L.; Luo, G.N. [Institute of Plasma Physics, Chinese Academy of Sciences, P.O. Box 1126, Hefei, Anhui 230031 (China)

2017-05-15

Highlights: • LIBS was applied to EAST for monitoring the cleaning performance of the first wall using He-ICRF cleaning. • The cleaning performance is effective under helium ambient gas and some measurements have been obtained. • The results also indicate that the influence of magnetic field on LIBS signal is much stronger in helium ambient gas. • The effect of delay time and laser fluence on the LIBS signal has been investigated. - Abstract: In this paper, laser-induced breakdown spectroscopy (LIBS) under magnetic field condition has been studied in laboratory and EAST tokamak. The experimental results reveal that in helium ambient gas, the magnetic field significantly enhances the LIBS signal intensity (∼3 times). The effect of time delay and laser fluence on the intensity of LIBS has been investigated for optimizing the signal to background ratio (S/B). The developed LIBS approach has been applied to monitor the cleaning performance of the first wall in the fusion device of EAST using the ion cyclotron range of frequency (ICRF). The experimental results demonstrate that the cleaning performance for Li/D co-deposition layer is effective under helium ambient gas. The removing rate of Li on the surface of W tile is faster than that on Mo tile in He-ICRF cleaning and the D/(D + H) ratio on Mo tile is higher by ∼1.2 times than that on W tile. This work would indicate the feasibility of using LIBS to monitor the wall cleaning processes in EAST tokamak.

Effects of laser wavelengths and pulse energy ratio on the emission enhancement in dual pulse LIBS

International Nuclear Information System (INIS)

Ahmed, Rizwan; Iqbal, Javed; Baig, M Aslam

2015-01-01

We present new studies on the effects of laser wavelengths, pulse energy ratio and interpulse delay between two laser pulses in the collinear dual pulse configuration of laser-induced breakdown spectroscopy (LIBS) on an iron sample in air using the fundamental (1064 nm) and the second harmonics (532 nm) of Nd:YAG lasers. In the dual pulse LIBS, an optimum value of interpulse delay with an appropriate combination of laser wavelengths, and laser pulse energy ratio, yields a 30 times signal intensity enhancement in the neutral iron lines as compared with single pulse LIBS. A comparison in the spatial variations of electron temperature along the axis of the plume expansion in single and double pulse LIBS has also been studied. (letter)

Laser-induced breakdown spectroscopy (LIBS) for detection of ammonium nitrate in soils

Science.gov (United States)

Díaz, Daniel; Hahn, David W.; Molina, Alejandro

2009-05-01

The extensive use of improvised explosive devices (IED) by irregular armed groups in Colombia has posed a threat, not only to the Colombian regular army but to the civilian population. It is expected that in future years, after an eventual cease fire, humanitarian missions for IED clearance will be fundamental to secure safe transit of people and goods, particularly in Colombian rural areas. The clandestine nature of IEDs preparation in Colombia yielded a rather diverse nature of these irregular weapons. Although, some have metal parts such as nails and shrapnel, others are metal-free devices in which detonation is obtained by chemical means. Despite this variability in IEDs design, one thing that is common in IEDs preparation is the use of significant amounts of ANFO (ammonium nitrate (AN), fuel oil (FO)) in their construction. The goal of this work was to identify AN and FO in soils using LIBS. Experiments showed the ability of LIBS to identify the presence of AN based on Hα (656.3 nm) and Hβ (486.1 nm) emission lines. It was not possible to identify FO mixed with soils in the spectral windows studied. FO caused a reduction on spark intensity on the samples. This would represent a challenge for identification of chemical compounds in wet soils. Potential interferences with fertilizers are discussed as well.

Double pulse laser induced breakdown spectroscopy: A potential tool for the analysis of contaminants and macro/micronutrients in organic mineral fertilizers.

Science.gov (United States)

Nicolodelli, Gustavo; Senesi, Giorgio Saverio; de Oliveira Perazzoli, Ivan Luiz; Marangoni, Bruno Spolon; De Melo Benites, Vinícius; Milori, Débora Marcondes Bastos Pereira

2016-09-15

Organic fertilizers are obtained from waste of plant or animal origin. One of the advantages of organic fertilizers is that, from the composting, it recycles waste-organic of urban and agriculture origin, whose disposal would cause environmental impacts. Fast and accurate analysis of both major and minor/trace elements contained in organic mineral and inorganic fertilizers of new generation have promoted the application of modern analytical techniques. In particular, laser induced breakdown spectroscopy (LIBS) is showing to be a very promising, quick and practical technique to detect and measure contaminants and nutrients in fertilizers. Although, this technique presents some limitations, such as a low sensitivity, if compared to other spectroscopic techniques, the use of double pulse (DP) LIBS is an alternative to the conventional LIBS in single pulse (SP). The macronutrients (Ca, Mg, K, P), micronutrients (Cu, Fe, Na, Mn, Zn) and contaminant (Cr) in fertilizer using LIBS in SP and DP configurations were evaluated. A comparative study for both configurations was performed using optimized key parameters for improving LIBS performance. The limit of detection (LOD) values obtained by DP LIBS increased up to seven times as compared to SP LIBS. In general, the marked improvement obtained when using DP system in the simultaneous LIBS quantitative determination for fertilizers analysis could be ascribed to the larger ablated mass of the sample. The results presented in this study show the promising potential of the DP LIBS technique for a qualitative analysis in fertilizers, without requiring sample preparation with chemical reagents. Copyright © 2016 Elsevier B.V. All rights reserved.

Applications of ultra-short pulsed laser ablation: thin films deposition and fs/ns dual-pulse laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Teghil, R; De Bonis, A; Galasso, A; Santagata, A; Albano, G; Villani, P; Spera, D; Parisi, G P

2008-01-01

In this paper, we report a survey of two of the large number of possible practical applications of the laser ablation performed by an ultra-short pulse laser, namely pulsed laser deposition (PLD) and fs/ns dual-pulse laser-induced breakdown spectroscopy (DP-LIBS). These applications differ from those using just longer pulsed lasers as a consequence of the distinctive characteristics of the plasma produced by ultra-short laser beams. The most important feature of this plasma is the large presence of particles with nanometric size which plays a fundamental role in both applications.

Classification of Explosive Residues on Organic Substrates Using Laser Induced Breakdown Spectroscopy

Science.gov (United States)

2013-04-01

Army Research Laboratory (ARL), we have been using laser induced breakdown spectro - scopy (LIBS), an optical spectroscopic technique that determines the...LX200GPS) was fitted with UV -coated optics to provide full broadband ( UV - VIS-NIR) capability. A custom-made three-channel gated CCD spectrometer (Ocean...Chem. 82, 1389–1400 (2010). 8. F. C. De Lucia, Jr., R. S. Harmon, K. L. McNesby, R. J. Winkel, Jr., and A. W. Miziolek, “Laser-induced breakdown spectro

Use of the vacuum ultraviolet spectral region for laser-induced breakdown spectroscopy-based Martian geology and exploration

International Nuclear Information System (INIS)

Radziemski, Leon; Cremers, David A.; Benelli, Katharine; Khoo, Cynthia; Harris, Ronny D.

2005-01-01

Several elements important to planetary geology (e.g. Br, C, Cl, P, S) and the human exploration of Mars (e.g. toxic elements such as As) have strong emission lines in the purge and vacuum ultraviolet (VUV) spectral region (100-200 nm). This spectral region has not been extensively studied for space applications using geological samples. We studied emissions from the laser-induced breakdown spectroscopy (LIBS) plasma in this region using a sample chamber filled with 7 torr (930 Pa) of CO 2 to simulate the Martian atmosphere. Pressures down to 0.02 torr were also used to evaluate the effect of the residual CO 2 on the spectra and to begin investigating the use of VUV-LIBS for airless bodies such as asteroids and the Moon. Spectra were recorded using a 0.3-m vacuum spectrometer with an intensified CCD (ICCD) camera. The effects of time delay and laser energy on LIBS detection at reduced pressure were examined. The effect of ambient CO 2 on the detection of C in soil was also evaluated. Lines useful for the spectrochemical analysis of As, Br, C, Cl, P, and S were determined and calibration curves were prepared for these elements. Although LIBS is being developed for stand-off analysis at many meters distance, the experiments reported here were aimed at in-situ (close-up) analysis

Characterization of deuterium retention and co-deposition of fuel with lithium on the divertor tile of EAST using laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Li, Cong; Zhao, Dongye; Hu, Zhenhua; Wu, Xingwei; Luo, Guang-Nan; Hu, Jiansheng; Ding, Hongbin

2015-01-01

A laser induced breakdown spectroscopy (LIBS) system has been developed to measure and monitor the composition evolution on plasma facing materials (PFMs) of Experimental Advanced Superconducting Tokamak (EAST). As a necessity and important proof of principle experiment, LIBS analysis has been performed for lithium–deuterium co-deposition layer diagnosis of EAST divertor tiles in lab experiments. The distribution of deuterium retention has been obtained from the depth of 0.5–4 μm in the divertor tiles. The deuterium/hydrogen concentration ratio was estimated as 0.17 ± 0.02 in lithium–deuterium co-deposition layer. Moreover, the depth profile behaviors of lithium and deuterium indicate that the deuterium retention in divertor tile came from lithium–deuterium co-deposition processes during deuterium discharge in EAST. This work would improve the understanding of deuterium retention and lithium–deuterium co-deposition mechanism and give a guidance to optimize the LIBS system which will be a unique and useful diagnostic approach in EAST 2014-campaign

Recognition of explosives fingerprints on objects for courier services using machine learning methods and laser-induced breakdown spectroscopy.

Science.gov (United States)

Moros, J; Serrano, J; Gallego, F J; Macías, J; Laserna, J J

2013-06-15

During recent years laser-induced breakdown spectroscopy (LIBS) has been considered one of the techniques with larger ability for trace detection of explosives. However, despite of the high sensitivity exhibited for this application, LIBS suffers from a limited selectivity due to difficulties in assigning the molecular origin of the spectral emissions observed. This circumstance makes the recognition of fingerprints a latent challenging problem. In the present manuscript the sorting of six explosives (chloratite, ammonal, DNT, TNT, RDX and PETN) against a broad list of potential harmless interferents (butter, fuel oil, hand cream, olive oil, …), all of them in the form of fingerprints deposited on the surfaces of objects for courier services, has been carried out. When LIBS information is processed through a multi-stage architecture algorithm built from a suitable combination of 3 learning classifiers, an unknown fingerprint may be labeled into a particular class. Neural network classifiers trained by the Levenberg-Marquardt rule were decided within 3D scatter plots projected onto the subspace of the most useful features extracted from the LIBS spectra. Experimental results demonstrate that the presented algorithm sorts fingerprints according to their hazardous character, although its spectral information is virtually identical in appearance, with rates of false negatives and false positives not beyond of 10%. These reported achievements mean a step forward in the technology readiness level of LIBS for this complex application related to defense, homeland security and force protection. Copyright © 2013 Elsevier B.V. All rights reserved.

Identification and measurement of dirt composition of manufactured steel plates using laser-induced breakdown spectroscopy.

Science.gov (United States)

Orzi, Daniel J O; Bilmes, Gabriel M

2004-12-01

Laser-induced breakdown spectroscopy (LIBS) was used for the characterization of the main components of the surface residual dirt produced in cold-rolled steel plates as a consequence of the manufacturing stages. At laser fluences between 0.05 J/cm(2) manufacturing process carbon residuals can also be found. By measuring light emission from the lambda = 495.9 nm line of Fe(I) after laser ablation, we developed a real-time on-line method for the determination of the concentration of iron particles present in the surface dirt. The obtained results open new possibilities in the design of real-time instruments for industrial applications as a quality control of products and processes.

Study of early laser-induced plasma dynamics: Transient electron density gradients via Thomson scattering and Stark Broadening, and the implications on laser-induced breakdown spectroscopy measurements

International Nuclear Information System (INIS)

Diwakar, P.K.; Hahn, D.W.

2008-01-01

To further develop laser-induced breakdown spectroscopy (LIBS) as an analytical technique, it is necessary to better understand the fundamental processes and mechanisms taking place during the plasma evolution. This paper addresses the very early plasma dynamics (first 100 ns) using direct plasma imaging, light scattering, and transmission measurements from a synchronized 532-nm probe laser pulse. During the first 50 ns following breakdown, significant Thomson scattering was observed while the probe laser interacted with the laser-induced plasma. The Thomson scattering was observed to peak 15-25 ns following plasma initiation and then decay rapidly, thereby revealing the highly transient nature of the free electron density and plasma equilibrium immediately following breakdown. Such an intense free electron density gradient is suggestive of a non-equilibrium, free electron wave generated by the initial breakdown and growth processes. Additional probe beam transmission measurements and electron density measurements via Stark broadening of the 500.1-nm nitrogen ion line corroborate the Thomson scattering observations. In concert, the data support the finding of a highly transient plasma that deviates from local thermodynamic equilibrium (LTE) conditions during the first tens of nanoseconds of plasma lifetime. The implications of this early plasma transient behavior are discussed in the context of plasma-analyte interactions and the role on LIBS measurements

A novel baseline correction method using convex optimization framework in laser-induced breakdown spectroscopy quantitative analysis

Science.gov (United States)

Yi, Cancan; Lv, Yong; Xiao, Han; Ke, Ke; Yu, Xun

2017-12-01