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

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.

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 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)

Detection of Anomalies in Citrus Leaves Using Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Sankaran, Sindhuja; Ehsani, Reza; Morgan, Kelly T

2015-08-01

Nutrient assessment and management are important to maintain productivity in citrus orchards. In this study, laser-induced breakdown spectroscopy (LIBS) was applied for rapid and real-time detection of citrus anomalies. Laser-induced breakdown spectroscopy spectra were collected from citrus leaves with anomalies such as diseases (Huanglongbing, citrus canker) and nutrient deficiencies (iron, manganese, magnesium, zinc), and compared with those of healthy leaves. Baseline correction, wavelet multivariate denoising, and normalization techniques were applied to the LIBS spectra before analysis. After spectral pre-processing, features were extracted using principal component analysis and classified using two models, quadratic discriminant analysis and support vector machine (SVM). The SVM resulted in a high average classification accuracy of 97.5%, with high average canker classification accuracy (96.5%). LIBS peak analysis indicated that high intensities at 229.7, 247.9, 280.3, 393.5, 397.0, and 769.8 nm were observed of 11 peaks found in all the samples. Future studies using controlled experiments with variable nutrient applications are required for quantification of foliar nutrients by using LIBS-based sensing.

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

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.

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.

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

Czech Academy of Sciences Publication Activity Database

Procházka, D.; Mazura, M.; Samek, Ota; Rebrošová, K.; Pořízka, P.; Klus, J.; Procházková, P.; Novotný, J.; Novotný, K.; Kaiser, J.

2018-01-01

Roč. 139 (2018), s. 6-12 ISSN 0584-8547 R&D Projects: GA ČR(CZ) GA15-20645S; GA ČR(CZ) GA16-12477S; GA MŠk(CZ) LO1212; GA MŠk ED0017/01/01 Institutional support: RVO:68081731 Keywords : laser-induced breakdown spectroscopy * Raman spectroscopy * chemometrics * bacteria Impact factor: 3.241, year: 2016

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

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

Fs–ns double-pulse Laser Induced Breakdown Spectroscopy of copper-based-alloys: Generation and elemental analysis of nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Guarnaccio, A.; Parisi, G.P.; Mollica, D. [CNR-ISM, U.O.S. Tito Scalo, Zona Industriale, 85050 Tito Scalo, PZ (Italy); De Bonis, A. [CNR-ISM, U.O.S. Tito Scalo, Zona Industriale, 85050 Tito Scalo, PZ (Italy); Dipartimento di Scienze, Università degli Studi della Basilicata, Via dell' Ateneo Lucano 10, 85100 Potenza (Italy); Teghil, R. [Dipartimento di Scienze, Università degli Studi della Basilicata, Via dell' Ateneo Lucano 10, 85100 Potenza (Italy); Santagata, A. [CNR-ISM, U.O.S. Tito Scalo, Zona Industriale, 85050 Tito Scalo, PZ (Italy)

2014-11-01

Evolution of nanoparticles ejected during ultra-short (250 fs) laser ablation of certified copper alloys and relative calibration plots of a fs–ns double-pulse Laser Induced Breakdown Spectroscopy orthogonal configuration is presented. All work was performed in air at atmospheric pressure using certified copper-based-alloy samples irradiated by a fs laser beam and followed by a delayed perpendicular ns laser pulse. In order to evaluate possible compositional changes of the fs induced nanoparticles, it was necessary to consider, for all samples used, comparable features of the detected species. With this purpose the induced nanoparticles black-body-like emission evolution and their relative temperature decay have been studied. These data were exploited for defining the distance between the target surface and the successive ns laser beam to be used. The consequent calibration plots of minor constituents (i.e. Sn, Pb and Zn) of the certified copper-based-alloy samples have been reported by taking into account self-absorption effects. The resulting linear regression coefficients suggest that the method used, for monitoring and ruling the fs laser induced nanoparticles, could provide a valuable approach for establishing the occurrence of potential compositional changes of the detected species. All experimental data reveal that the fs laser induced nanoparticles can be used for providing a coherent composition of the starting target. In the meantime, the fs–ns double-pulse Laser Induced Breakdown Spectroscopy orthogonal configuration here used can be considered as an efficient technique for compositional determination of the nanoparticles ejected during ultra-short laser ablation processes. - Highlights: • Laser induced NP continuum black-body-like emission was used for T determination. • Invariable composition of generated NPs was assumed in the range of 20 μs. • Fs-ns DP-LIBS was employed for the compositional characterization of NPs. • NPs obtained by fs

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.

Laser-induced breakdown spectroscopy (LIBS): a new spectrochemical technique

International Nuclear Information System (INIS)

Radziemski, L.J.; Loree, T.R.; Cremers, D.A.

1982-01-01

We have used the breakdown spark from a focused laser beam to generate analytically useful emission spectra of minor constituents in air and other carrier gases. The medium was sampled directly. It was not necessary to reduce the sample to solution nor to introduce electrodes. The apparatus is particularly simple; a pulsed laser, spectrometer, and some method for time resolution. The latter is essential in laser-induced-breakdown spectroscopy (LIBS) because of the strong early continuum. High temperatures in the spark result in vaporization of small particles, dissociation of molecules, and excitation of atomic and ionic spectra, including species which are normally difficult to detect. In one application, we have monitored beryllium in air at conventrations below 1 μg/m 3 , which is below 1 ppB (w/w). In another we have monitored chlorine and fluorine atoms in real time. LIBS has the potential for real-time direct sampling of contaminants in situ

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.

A Simple LIBS (Laser-Induced Breakdown Spectroscopy) Laboratory Experiment to Introduce Undergraduates to Calibration Functions and Atomic Spectroscopy

Science.gov (United States)

Chinni, Rosemarie C.

2012-01-01

This laboratory experiment introduces students to a different type of atomic spectroscopy: laser-induced breakdown spectroscopy (LIBS). LIBS uses a laser-generated spark to excite the sample; once excited, the elemental emission is spectrally resolved and detected. The students use LIBS to analyze a series of standard synthetic silicate samples…

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.

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 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'.

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.

Standoff Detection of Explosives at 1 m using Laser Induced Breakdown Spectroscopy

Czech Academy of Sciences Publication Activity Database

Junjuri, R.; Myakalwar, A.K.; Gundawar, M.K.

2017-01-01

Roč. 67, č. 6 (2017), s. 623-630 ISSN 0011-748X Institutional support: RVO:67985882 Keywords : Laser induced breakdown spectroscopy * Multivariate analysis * Principal component analysis * Explosive detection Subject RIV: JB - Sensors, Measurment, Regulation OBOR OECD: Electrical and electronic engineering Impact factor: 0.500, year: 2016

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...

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

Laser-Induced Breakdown Spectroscopy (LIBS) for Monitoring the Formation of Hydroxyapatite Porous Layers

OpenAIRE

Sola, Daniel; Paulés, Daniel; Grima, Lorena; Anzano, Jesús

2017-01-01

Laser-induced breakdown spectroscopy (LIBS) is applied to characterize the formation of porous hydroxyapatite layers on the surface of 0.8CaSiO3-0.2Ca3(PO4)2 biocompatible eutectic glass immersed in simulated body fluid (SBF). Compositional and structural characterization analyses were also conducted by field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), and micro-Raman spectroscopy.

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…

Elemental analysis of halogens using molecular emission by laser-induced breakdown spectroscopy in air

Energy Technology Data Exchange (ETDEWEB)

Gaft, M.; Nagli, L.; Eliezer, N.; Groisman, Y. [Laser Distance Spectrometry, 9 Mota Gur St., Petah Tikva 49514 (Israel); Forni, O. [Université de Toulouse, UPS-OMP, IRAP, Toulouse (France); CNRS, IRAP, 9 Av. Colonel Roche, BP 44346, F-31028 Toulouse cedex 4 (France)

2014-08-01

Fluorine and chlorine do not produce atomic and ionic line spectra of sufficient intensity to permit their detection by laser-induced breakdown spectroscopy. They do, however, combine with alkali-earths and other elements to form molecules whose spectra may be easily identified, enabling detection in ambient conditions with much higher sensitivity than using F I and Cl I atomic lines. - Highlights: • We studied laser induced breakdown spectra of halogens with alkali-earth elements. • Emission and temporal behavior of CaF and CaCl molecules were determined. • Sensitivity of F and Cl detection by molecules and atoms was compared.

Laser-Induced Breakdown Spectroscopy (LIBS for Monitoring the Formation of Hydroxyapatite Porous Layers

Directory of Open Access Journals (Sweden)

Daniel Sola

2017-12-01

Full Text Available Laser-induced breakdown spectroscopy (LIBS is applied to characterize the formation of porous hydroxyapatite layers on the surface of 0.8CaSiO3-0.2Ca3(PO42 biocompatible eutectic glass immersed in simulated body fluid (SBF. Compositional and structural characterization analyses were also conducted by field emission scanning electron microscopy (FESEM, energy dispersive X-ray spectroscopy (EDX, and micro-Raman spectroscopy.

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.

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.

Long-wave, infrared laser-induced breakdown (LIBS) spectroscopy emissions from energetic materials.

Science.gov (United States)

Yang, Clayton S-C; Brown, Ei E; Hommerich, Uwe; Jin, Feng; Trivedi, Sudhir B; Samuels, Alan C; Snyder, A Peter

2012-12-01

Laser-induced breakdown spectroscopy (LIBS) has shown great promise for applications in chemical, biological, and explosives sensing and has significant potential for real-time standoff detection and analysis. In this study, LIBS emissions were obtained in the mid-infrared (MIR) and long-wave infrared (LWIR) spectral regions for potential applications in explosive material sensing. The IR spectroscopy region revealed vibrational and rotational signatures of functional groups in molecules and fragments thereof. The silicon-based detector for conventional ultraviolet-visible LIBS operations was replaced with a mercury-cadmium-telluride detector for MIR-LWIR spectral detection. The IR spectral signature region between 4 and 12 μm was mined for the appearance of MIR and LWIR-LIBS emissions directly indicative of oxygenated breakdown products as well as dissociated, and/or recombined sample molecular fragments. Distinct LWIR-LIBS emission signatures from dissociated-recombination sample molecular fragments between 4 and 12 μm are observed for the first time.

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

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.

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.

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...

Laser-induced breakdown spectroscopy for the real-time analysis of mixed waste samples containing Sr

International Nuclear Information System (INIS)

Barefield, J.E. II; Koskelo, A.C.; Multari, R.A.; Cremers, D.A.; Gamble, T.K.; Han, C.Y.

1995-01-01

In this report, the use of Laser-induced breakdown spectroscopy to analyze mixed waste samples containing Sr is discussed. The mixed waste samples investigated include vitrified waste glass and contaminated soil. Compared to traditional analysis techniques, the laser-based method is fast (i.e., analysis times on the order of minutes) and essentially waste free since little or no sample preparation is required. Detection limits on the order of pmm Sr were determined. Detection limits obtained using a fiber optic cable to deliver laser pulses to soil samples containing Cr, Zr, Pb, Be, Cu, and Ni will also be discussed

Prospects of real-time single-particle biological aerosol analysis: A comparison between laser-induced breakdown spectroscopy and aerosol time-of-flight mass spectrometry

International Nuclear Information System (INIS)

Beddows, D.C.S.; Telle, H.H.

2005-01-01

In this paper we discuss the prospects of real-time, in situ laser-induced breakdown spectroscopy applied for the identification and classification of bio-aerosols (including species of potential bio-hazard) within common urban aerosol mixtures. In particular, we address the issues associated with the picking out of bio-aerosols against common background aerosol particles, comparing laser-induced breakdown spectroscopy measurements with data from a mobile single-particle aerosol mass spectrometer (ATOFMS). The data from the latter provide statistical data over an extended period of time, highlighting the variation of the background composition. While single-particle bio-aerosols are detectable in principle, potential problems with small (∼ 1 μm size) bio-aerosols have been identified; constituents of the air mass other than background aerosols, e.g. gaseous CO 2 in conjunction with common background aerosols, may prevent unique recognition of the bio-particles. We discuss whether it is likely that laser-induced breakdown spectroscopy on its own can provide reliable, real-time identification of bio-aerosol in an urban environment, and it is suggested that more than one technique should be or would have to be used. A case for using a combination of laser-induced breakdown spectroscopy and Raman (and/or) laser-induced fluorescence spectroscopy is made

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.

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.

Development of microwave-enhanced spark-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Ikeda, Yuji; Moon, Ahsa; Kaneko, Masashi

2010-01-01

We propose microwave-enhanced spark-induced breakdown spectroscopy with the same measurement and analysis processes as in laser-induced breakdown spectroscopy, but with a different plasma generation mechanism. The size and lifetime of the plasma generated can contribute to increased measurement accuracy and expand its applicability to industrial measurement, such as an exhaust gas analyzer for automobile engine development and its regulation, which has been hard to operate by laser at an engineering evaluation site. The use of microwaves in this application helps lower the cost, reduce the system size, and increase the ease of operation to make it commercially viable. A microwave frequency of 2.45 GHz was used to enhance the volume and lifetime of the plasma at atmospheric condition even at elevated pressure.

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.

Applications of Laser-Induced Breakdown Spectroscopy (LIBS) in Molten Metal Processing

Science.gov (United States)

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

2017-10-01

In order for metals to meet the demand for critical applications in the automotive, aerospace, and defense industries, tight control over the composition and cleanliness of the metal must be achieved. The use of laser-induced breakdown spectroscopy (LIBS) for applications in metal processing has generated significant interest for its ability to perform quick analyses in situ. The fundamentals of LIBS, current techniques for deployment on molten metal, demonstrated capabilities, and possible avenues for development are reviewed and discussed.

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.

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.

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

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.

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.

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.

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.

Highly sensitive analysis of boron and lithium in aqueous solution using dual-pulse laser-induced breakdown spectroscopy.

Science.gov (United States)

Lee, Dong-Hyoung; Han, Sol-Chan; Kim, Tae-Hyeong; Yun, Jong-Il

2011-12-15

We have applied a dual-pulse laser-induced breakdown spectroscopy (DP-LIBS) to sensitively detect concentrations of boron and lithium in aqueous solution. Sequential laser pulses from two separate Q-switched Nd:YAG lasers at 532 nm wavelength have been employed to generate laser-induced plasma on a water jet. For achieving sensitive elemental detection, the optimal timing between two laser pulses was investigated. The optimum time delay between two laser pulses for the B atomic emission lines was found to be less than 3 μs and approximately 10 μs for the Li atomic emission line. Under these optimized conditions, the detection limit was attained in the range of 0.8 ppm for boron and 0.8 ppb for lithium. In particular, the sensitivity for detecting boron by excitation of laminar liquid jet was found to be excellent by nearly 2 orders of magnitude compared with 80 ppm reported in the literature. These sensitivities of laser-induced breakdown spectroscopy are very practical for the online elemental analysis of boric acid and lithium hydroxide serving as neutron absorber and pH controller in the primary coolant water of pressurized water reactors, respectively.

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.

A Simple Device for Lens-to-Sample Distance Adjustment in Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Cortez, Juliana; Farias Filho, Benedito B; Fontes, Laiane M; Pasquini, Celio; Raimundo, Ivo M; Pimentel, Maria Fernanda; de Souza Lins Borba, Flávia

2017-04-01

A simple device based on two commercial laser pointers is described to assist in the analysis of samples that present uneven surfaces and/or irregular shapes using laser-induced breakdown spectroscopy (LIBS). The device allows for easy positioning of the sample surface at a reproducible distance from the focusing lens that conveys the laser pulse to generate the micro-plasma in a LIBS system, with reproducibility better than ±0.2 mm. In this way, fluctuations in the fluence (J cm -2 ) are minimized and the LIBS analytical signals can be obtained with a better precision even when samples with irregular surfaces are probed.

Q-switched Nd:YAG/V:YAG microchip 1338 nm laser for laser-induced breakdown spectroscopy

Science.gov (United States)

Šulc, Jan; Jelínková, Helena; Nejezchleb, Karel; Škoda, Václav

2017-12-01

Q-switched microchip laser emitting radiation at wavelength 1338nm was tested as a radiation source for laser induced breakdown spectroscopy (LIBS). This laser used sandwich crystal which combined in one piece the cooling part (undoped YAG crystal 4mm long), the active laser part (Nd:YAG crystal 12mm long), and the saturable absorber (V:YAG crystal 0.7mm long). The diameter of this crystal was 5 mm. The microchip resonator consisted of dielectric mirrors directly deposited on the monolith crystal surfaces. The pump mirror (HT @ 808 nm, HR @ 1.3 ¹m) was placed on the undoped YAG part. The output coupler (R = 90% @ 1338 nm) was placed on the V:YAG part. The fibre-coupled 808nm pumping laser diode was operating in pulsed regime (rep. rate 250 Hz, pulse width 300 ¹s, pulse energy 6 mJ). Using this pumping, stable and high reproducible Q-switched pulses were generated at wavelength 1338 nm. Pulse length was 6.2 ns (FWHM) and the mean output power was 33mW. The single pulse energy and peak power was 0.13mJ and 21kW, respectively. Laser was operating in fundamental TEM00 mode. The laser radiation was focused on a tested sample using single plano-convex lens (focal length 75 mm). The focal spot radius was 40 ¹m. The corresponding peak-power density was 0.83GW/cm2. The laser induced break-down was successfully reached and corresponding laser-induced plasma spectra were recorded for set of metallic elements (Cu, Ag, Au, In, Zn, Al, Fe, Ni, Cr) and alloys (Sn-Pb solder, duralumin, stainless-steel, brass). To record the spectra, StellarNet BLACK-Comet concave grating CCD-based spectrometer was used without any special collimation optics. Thanks to used laser wavelength far from the detector sensitivity, no special filtering was needed to overcome the CCD dazzling. The constructed laser could significantly improve repletion-rate of up-to-date LIBS devices.

Temperature and Electron Density Determination on Laser-Induced Breakdown Spectroscopy (LIBS) Plasmas: A Physical Chemistry Experiment

Science.gov (United States)

Najarian, Maya L.; Chinni, Rosemarie C.

2013-01-01

This laboratory is designed for physical chemistry students to gain experience using laser-induced breakdown spectroscopy (LIBS) in understanding plasma diagnostics. LIBS uses a high-powered laser that is focused on the sample causing a plasma to form. The emission of this plasma is then spectrally resolved and detected. Temperature and electron…

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.

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 ...

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.

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.

Using laser-induced breakdown spectroscopy on vacuum alloys-production process for elements concentration analysis

Science.gov (United States)

Zhao, Tianzhuo; Fan, Zhongwei; Lian, Fuqiang; Liu, Yang; Lin, Weiran; Mo, Zeqiang; Nie, Shuzhen; Wang, Pu; Xiao, Hong; Li, Xin; Zhong, Qixiu; Zhang, Hongbo

2017-11-01

Laser-induced breakdown spectroscopy (LIBS) utilizing an echelle spectrograph-ICCD system is employed for on-line analysis of elements concentration in a vacuum induction melting workshop. Active temperature stabilization of echelle spectrometer is implemented specially for industrial environment applications. The measurement precision is further improved by monitoring laser parameters, such as pulse energy, spatial and temporal profiles, in real time, and post-selecting laser pulses with specific pulse energies. Experimental results show that major components of nickel-based alloys are stable, and can be well detected. By using internal standard method, calibration curves for chromium and aluminum are obtained for quantitative determination, with determination coefficient (relative standard deviation) to be 0.9559 (< 2.2%) and 0.9723 (< 2.8%), respectively.

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.

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.

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

Science.gov (United States)

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.

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.

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.

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.

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.

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

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

Aluminum alloy analysis using microchip-laser induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Freedman, Andrew [Center for Sensor Systems and Technologies, Aerodyne Research, Inc., 45 Manning Road Billerica, MA, 01821-3976 (United States)]. E-mail: af@aerodyne.com; Iannarilli, Frank J. [Center for Sensor Systems and Technologies, Aerodyne Research, Inc., 45 Manning Road Billerica, MA, 01821-3976 (United States); Wormhoudt, Joda C. [Center for Sensor Systems and Technologies, Aerodyne Research, Inc., 45 Manning Road Billerica, MA, 01821-3976 (United States)

2005-08-31

A laser induced breakdown spectroscopy-based apparatus for the analysis of aluminum alloys which employs a microchip laser and a handheld spectrometer with an ungated, non-intensified CCD array has been built and tested. The microchip laser, which emits low energy pulses (4-15 {mu}J) at high repetition rates (1-10 kHz) at 1064 nm, produces, when focused, an ablation crater with a radius on the order of only 10 {mu}m. The resulting emission is focused onto an optical fiber connected to 0.10 m focal length spectrometer with a spectral range of 275-413 nm. The apparatus was tested using 30 different aluminum alloy reference samples. Two techniques for constructing calibration curves from the data, peak integration and partial least squares regression, were quantitatively evaluated. Results for Fe, Mg, Mn, Ni, Si, and Zn indicated limits of detection (LOD) that ranged from 0.05 to 0.14 wt.% and overall measurement errors which varied from 0.06 to 0.18 wt.%. Higher limits of detection and overall error for Cu (> 0.3 wt.%) were attributed to analysis problems associated with the presence of optically thick lines and a spectral interference from Zn. Improvements in design and component sensitivity should increase overall performance by at least a factor of 2, allowing for dependable aluminum alloy classification.

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.

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.

Quantitative Analysis of Mg in Pipeline Dirt Based on Laser-Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Wang Shaolong; Wang Yangen; Chen Shanjun; Chen Qi

2015-01-01

In order to maintain the pipeline better and remove the dirt more effectively, it was necessary to analyze the contents of elements in dirt. Mg in soil outside of the pipe and the dirt inside of the pipe was quantitatively analyzed and compared by using the laser-induced breakdown spectroscopy (LIBS). Firstly, Mg was quantitatively analyzed on the basis of Mg I 285.213 nm by calibration curve for integrated intensity and peak intensity of the spectrum before and after subtracting noise, respectively. Then calibration curves on the basis of Mg II 279.553 nm and Mg II 280.270 nm were analyzed. The results indicated that it is better to use integrated intensity after subtracting noise of the spectrum line with high relative intensity to make the calibration curve. (paper)

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.

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.

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

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.

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...

Evaluation of Optical Depths and Self-Absorption of Strontium and Aluminum Emission Lines in Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Alfarraj, Bader A; Bhatt, Chet R; Yueh, Fang Yu; Singh, Jagdish P

2017-04-01

Laser-induced breakdown spectroscopy (LIBS) is a widely used laser spectroscopic technique in various fields, such as material science, forensic science, biological science, and the chemical and pharmaceutical industries. In most LIBS work, the analysis is performed using radiative transitions from atomic emissions. In this study, the plasma temperature and the product [Formula: see text] (the number density N and the absorption path length [Formula: see text]) were determined to evaluate the optical depths and the self-absorption of Sr and Al lines. A binary mixture of strontium nitrate and aluminum oxide was used as a sample, consisting of variety of different concentrations in powder form. Laser-induced breakdown spectroscopy spectra were collected by varying various parameters, such as laser energy, gate delay time, and gate width time to optimize the LIBS signals. Atomic emission from Sr and Al lines, as observed in the LIBS spectra of different sample compositions, was used to characterize the laser induced plasma and evaluate the optical depths and self-absorption of LIBS.

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.

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)

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

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.

Quantitative laser-induced breakdown spectroscopy of potassium for in-situ geochronology on Mars

Energy Technology Data Exchange (ETDEWEB)

Stipe, Christopher B., E-mail: stipec@seattleu.edu [Department of Mechanical Engineering, Seattle University, Seattle, WA 98122 (United States); Guevara, Edward; Brown, Jonathan [Department of Mechanical Engineering, Seattle University, Seattle, WA 98122 (United States); Rossman, George R. [Division of Geological and Planetary Sciences, California Institute of Technology, Pasadena, CA 91125 (United States)

2012-04-15

Laser-induced breakdown spectroscopy is explored for the development of an in-situ K-Ar geochronology instrument for Mars. Potassium concentrations in standard basaltic glasses and equivalent rock samples in their natural form are quantified using the potassium doublet at 766.49 and 769.90 nm. Measurement precision varies from 0.5 to 5.5 (% RSD) over the 3.63% to 0.025% potassium by weight for the standard samples, and little additional precision is achieved above 20 laser shots at 5 locations. For the glass standards, the quantification limits are 920 and 66 ppm for non-weighted and weighted calibration methods, respectively. For the basaltic rocks, the quantification limits are 2650 and 328 ppm for the non-weighted and weighted calibration methods, respectively. The heterogeneity of the rock samples leads to larger variations in potassium signal; however, normalizing the potassium peak by base area at 25 locations on the rock improved calibration accuracy. Including only errors in LIBS measurements, estimated age errors for the glasses range from approximately {+-} 30 Ma for 3000 Ma samples to {+-} 2 Ma for 100 Ma samples. For the basaltic rocks, the age errors are approximately {+-} 120 Ma for 3000 Ma samples and {+-} 8 Ma for 100 Ma samples. - Highlights: Black-Right-Pointing-Pointer Measurement of basaltic glasses and rocks by laser-induced breakdown spectroscopy. Black-Right-Pointing-Pointer Quantification of potassium for K-Ar dating. Black-Right-Pointing-Pointer Development of an instrument for in-situ geochronology on Mars. Black-Right-Pointing-Pointer Detection limit is 35 ppm, relative standard deviations range from 0.5% to 5.5%. Black-Right-Pointing-Pointer Estimated errors for the glass standards range from {+-} 30 Ma for 3000 Ma and {+-} 2 Ma for 100 Ma; estimated errors for the basaltic rocks range from {+-} 120 Ma for 3000 Ma and {+-} 8 Ma for 100 Ma.

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...

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

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)

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)

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.

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

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.

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.

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.

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.

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.

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.

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

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

Application of Handheld Laser-Induced Breakdown Spectroscopy (LIBS) to Geochemical Analysis.

Science.gov (United States)

Connors, Brendan; Somers, Andrew; Day, David

2016-05-01

While laser-induced breakdown spectroscopy (LIBS) has been in use for decades, only within the last two years has technology progressed to the point of enabling true handheld, self-contained instruments. Several instruments are now commercially available with a range of capabilities and features. In this paper, the SciAps Z-500 handheld LIBS instrument functionality and sub-systems are reviewed. Several assayed geochemical sample sets, including igneous rocks and soils, are investigated. Calibration data are presented for multiple elements of interest along with examples of elemental mapping in heterogeneous samples. Sample preparation and the data collection method from multiple locations and data analysis are discussed. © The Author(s) 2016.

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

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.

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.

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.

Remote metal analysis by laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Duckworth, A.

1996-01-01

This paper describes a new technique by which the composition of irradiated or inaccessible reactor components can be determined remotely. The technique uses very short duration, high energy laser pulses at a wavelength which can be transmitted down an optical fibre to ablate a tiny plasma from the surface of a metal component. Light from the plasma is collected by a second fibre and returned to a spectrometer where it is split into the characteristic emission wavelengths of the elements in the sample. Comparison of the emission line amplitude for a particular element with that of a chosen calibration line can be used to deduce the concentration of the element in the sample. The technique has been used successfully to differentiate between different highly radioactive control rod batches at Sizewell ''A'' and Hinkley Point ''A'' Power Stations. The material analysis accuracy is comparable with that obtained from electron microphobe analysis and other direct spectroscopic methods. However, by analysing the mild steel control rod casing material remotely, difficult sample removal becomes unneccessary and the integrity of the component remains essentially unaltered. In addition, removal of deposits or surface corrosion is incorporated very neatly into the process. These factors make remote laser induced breakdown spectroscopy an ideal tool for material analysis in the nuclear environment. (UK)

Remote metal analysis by laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Duckworth, A.

1996-01-01

This paper describes a new technique by which the composition of irradiated or inaccessible reactor components can be determined remotely. The technique uses very short duration, high energy laser pulses at a wavelength which can be transmitted down an optical fibre to ablate a tiny plasma from the surface of a metal component. Light from the plasma is collected by a second fibre and returned to a spectrometer where it is split into the characteristic emission wavelengths of the elements in the sample. Comparison of the emission line amplitude for a particular element with that of a chosen calibrationline can be used to deduce the concentration of the element in the sample. The technique has been used successfully to differentiate between highly radioactive control rod batches at Sizewell 'A' and Hinkley Point 'A Power Stations. The material analysis accuracy is comparable with that obtained from electron microprobe analysis and other direct spectroscopic methods. However, by analysing the mild steel control rod casing material remotely, difficult sample removal becomes unnecessary and the integrity of the component remains essentially unaltered. In addition, removal of deposits or surface corrosion is incorporated very neatly into the process. These factors make remote laser induced breakdown spectroscopy an ideal tool for material analysis in the nuclear environment. (Author)

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.

Gallium Content in PuO2 Using Laser Induced Breakdown Spectroscopy (LIBS)

International Nuclear Information System (INIS)

Smith, C.A.; Martinez, M.A.; Veirs, D.K.

1999-01-01

Laser Induced Breakdown Spectroscopy (LIBS) has been applied to the semi-quantitative analysis of gallium in plutonium oxide at the Los Alamos Plutonium Facility. The oxide samples were generated by the Thermally Induced Gallium Removal (TIGR) process, a pretreatment step prior to MOX fuel processing. The TIGR process uses PuO 2 containing 1 wt% gallium (nominal) as feed material. Following the TIGR process, gallium content was analyzed by LIBS and also by conventional wet chemical analysis (ICP-MS). Although the data range was insufficient to obtain an adequate calibration, general agreement between the two techniques was good. LIBS was found to have a useful analytical range of 34-400 ppm for Ga in PuO 2

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

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

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.

Linear correlation for identification of materials by laser induced breakdown spectroscopy: Improvement via spectral filtering and masking

Energy Technology Data Exchange (ETDEWEB)

Gornushkin, I.B., E-mail: igor.gornushkin@bam.d [BAM Federal Institute for Materials Research and Testing, Berlin (Germany); Panne, U. [BAM Federal Institute for Materials Research and Testing, Berlin (Germany); Winefordner, J.D. [University of Florida, Gainesville, Florida (United States)

2009-10-15

The purpose of this work is to improve the performance of a linear correlation method used for material identification in laser induced breakdown spectroscopy. The improved correlation procedure is proposed based on the selection and use of only essential spectral information and ignoring empty spectral fragments. The method is tested on glass samples of forensic interest. The 100% identification capability of the new method is demonstrated in contrast to the traditional approach where the identification rate falls below 100% for many samples.

Nanoparticle-Enhanced Laser Induced Breakdown Spectroscopy for the noninvasive analysis of transparent samples and gemstones.

Science.gov (United States)

Koral, C; Dell'Aglio, M; Gaudiuso, R; Alrifai, R; Torelli, M; De Giacomo, A

2018-05-15

In this paper, Nanoparticle-Enhanced Laser Induced Breakdown Spectroscopy is applied to transparent samples and gemstones with the aim to overcome the laser induced damage on the sample. We propose to deposit a layer of AuNPs on the sample surface by drying a colloidal solution before ablating the sample with a 532 nm pulsed laser beam. This procedure ensures that the most significant fraction of the beam, being in resonance with the AuNP surface plasmon, is mainly absorbed by the NP layer, which in turn results the breakdown to be induced on NPs rather than on the sample itself. The fast explosion of the NPs and the plasma induction allow the ablation and the transfer in the plasma phase of the portion of sample surface where the NPs were placed. The employed AuNPs are prepared in milliQ water without the use of any chemical stabilizers by Pulsed Laser Ablation in Liquids (PLAL), in order to obtain a strict control of composition and impurities, and to limit possible spectral interferences (except from Au emission lines). Therefore with this technique it is possible to obtain, together with the emission signal of Au (coming from atomized NPs), the emission spectrum of the sample, by limiting or avoiding the direct interaction of the laser pulse with the sample itself. This approach is extremely useful for the elemental analysis by laser ablation of high refractive index samples, where the laser pulse on an untreated surface can otherwise penetrate inside the sample, generate breakdown events below the superficial layer, and consequently cause cracks and other damage. The results obtained with NELIBS on high refractive index samples like glasses, tourmaline, aquamarine and ruby are very promising, and demonstrate the potentiality of this approach for precious gemstones analysis. Copyright © 2018 Elsevier B.V. All rights reserved.

Accuracy Enhancement of Raman Spectroscopy Using Complementary Laser-Induced Breakdown Spectroscopy (LIBS) with Geologically Mixed Samples.

Science.gov (United States)

Choi, Soojin; Kim, Dongyoung; Yang, Junho; Yoh, Jack J

2017-04-01

Quantitative Raman analysis was carried out with geologically mixed samples that have various matrices. In order to compensate the matrix effect in Raman shift, laser-induced breakdown spectroscopy (LIBS) analysis was performed. Raman spectroscopy revealed the geological materials contained in the mixed samples. However, the analysis of a mixture containing different matrices was inaccurate due to the weak signal of the Raman shift, interference, and the strong matrix effect. On the other hand, the LIBS quantitative analysis of atomic carbon and calcium in mixed samples showed high accuracy. In the case of the calcite and gypsum mixture, the coefficient of determination of atomic carbon using LIBS was 0.99, while the signal using Raman was less than 0.9. Therefore, the geological composition of the mixed samples is first obtained using Raman and the LIBS-based quantitative analysis is then applied to the Raman outcome in order to construct highly accurate univariate calibration curves. The study also focuses on a method to overcome matrix effects through the two complementary spectroscopic techniques of Raman spectroscopy and 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...

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

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.

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....

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.

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

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

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 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.

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.

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)

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

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.

Mid-infrared, long wave infrared (4-12 μm) molecular emission signatures from pharmaceuticals using laser-induced breakdown spectroscopy (LIBS).

Science.gov (United States)

Yang, Clayton S-C; Brown, Ei E; Kumi-Barimah, Eric; Hommerich, Uwe H; Jin, Feng; Trivedi, Sudhir B; Samuels, Alan C; Snyder, A Peter

2014-01-01

In an effort to augment the atomic emission spectra of conventional laser-induced breakdown spectroscopy (LIBS) and to provide an increase in selectivity, mid-wave to long-wave infrared (IR), LIBS studies were performed on several organic pharmaceuticals. Laser-induced breakdown spectroscopy signature molecular emissions of target organic compounds are observed for the first time in the IR fingerprint spectral region between 4-12 μm. The IR emission spectra of select organic pharmaceuticals closely correlate with their respective standard Fourier transform infrared spectra. Intact and/or fragment sample molecular species evidently survive the LIBS event. The combination of atomic emission signatures derived from conventional ultraviolet-visible-near-infrared LIBS with fingerprints of intact molecular entities determined from IR LIBS promises to be a powerful tool for chemical detection.

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

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

Quantitative analysis by laser-induced breakdown spectroscopy based on generalized curves of growth

Energy Technology Data Exchange (ETDEWEB)

Aragón, C., E-mail: carlos.aragon@unavarra.es; Aguilera, J.A.

2015-08-01

A method for quantitative elemental analysis by laser-induced breakdown spectroscopy (LIBS) is proposed. The method (Cσ-LIBS) is based on Cσ graphs, generalized curves of growth which allow including several lines of various elements at different concentrations. A so-called homogeneous double (HD) model of the laser-induced plasma is used, defined by an integration over a single-region of the radiative transfer equation, combined with a separated treatment for neutral atoms (z = 0) and singly-charged ions (z = 1) in Cσ graphs and characteristic parameters. The procedure includes a criterion, based on a model limit, for eliminating data which, due to a high line intensity or concentration, are not well described by the HD model. An initial procedure provides a set of parameters (βA){sup z}, (ηNl){sup z}, T{sup z} and N{sub e}{sup z} (z = 0, 1) which characterize the plasma and the LIBS system. After characterization, two different analytical procedures, resulting in relative and absolute concentrations, may be applied. To test the method, fused glass samples prepared from certified slags and pure compounds are analyzed. We determine concentrations of Ca, Mn, Mg, V, Ti, Si and Al relative to Fe in three samples prepared from slags, and absolute concentrations of Fe, Ca and Mn in three samples prepared from Fe{sub 2}O{sub 3}, CaCO{sub 3} and Mn{sub 2}O{sub 3}. The accuracy obtained is 3.2% on the average for relative concentrations and 9.2% for absolute concentrations. - Highlights: • Method for quantitative analysis by LIBS, based on Csigma graphs • Conventional calibration is replaced with characterization of the LIBS system. • All elements are determined from measurement of one or two Csigma graphs. • The method is tested with fused glass disks prepared from slags and pure compounds. • Accurate results for relative (3.2%) and absolute concentrations (9.2%)

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

Real-time monitoring of airborne beryllium, at OSHA limit levels, by time-resolved laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Radziemski, L.J.; Loree, T.R.; Cremers, D.A.

1982-01-01

Real-time detection of beryllium particulate is being investigated by the new technique of laser-induced breakdown spectroscopy. For beryllium detection we monitor the 313.1-nm feature of once ionized beryllium (Be II). Numerous publications describe the technique, our beryllium results, and other applications. Here we summarize the important points and describe our experiments with beryllium

The use of laser-induced breakdown spectroscopy for the determination of fluorine concentration in glass ionomer cement

Czech Academy of Sciences Publication Activity Database

Kratochvíl, T.; Pouzar, M.; Novotný, K.; Havránek, Vladimír; Černohorský, T.; Zvolská, M.

2013-01-01

Roč. 88, OCT (2013), s. 26-31 ISSN 0584-8547 Grant - others:GA ČR(CZ) GAP207/11/0555 Institutional support: RVO:61389005 Keywords : Fluorine * GIC * Laser-induced breakdown spectroscopy * Quantitative analysis Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 3.150, year: 2013 http://www.sciencedirect.com/science/article/pii/S0584854713002243#

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.

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)

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

Science.gov (United States)

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.

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.

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.

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)

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....

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.

Analysis of copper contamination in transformer insulating material with nanosecond- and femtosecond-laser-induced breakdown spectroscopy

Science.gov (United States)

Aparna, N.; Vasa, N. J.; Sarathi, R.

2018-06-01

This work examines the oil-impregnated pressboard insulation of high-voltage power transformers, for the determination of copper contamination. Nanosecond- and femtosecond-laser-induced breakdown spectroscopy revealed atomic copper lines and molecular copper monoxide bands due to copper sulphide diffusion. X-ray diffraction studies also indicated the presence of CuO emission. Elemental and molecular mapping compared transformer insulating material ageing in different media—air, N2, He and vacuum.

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

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.

Laser-Induced Breakdown Spectroscopy to high-resolution analysis of ion distribution in cement-bound solid; Laser-induzierte Breakdown Spektroskopie (LIBS) zur hochaufloesenden Analyse der Ionenverteilung in zementgebundenen Feststoffen

Energy Technology Data Exchange (ETDEWEB)

Molkenthin, Andre

2009-06-03

The Laser-Induced Breakdown Spectroscopy allows imaging and quantitative analysis of the ion distribution of all relevant elements on the surface of mineral building materials. The measuring system has been characterised by investigations on specimens of hardened cement paste, mortar and concrete. Transport and accumulation processes are visualised. Besides, results are introduced for the peripheral zone close to the surface and the extraction is shown. (orig.) [German] Die Laser-induzierte Breakdown Spektroskopie ermoeglicht eine bildgebende und quantitative Analyse der Ionenverteilung aller massgeblichen Elemente auf mineralischen Baustoffoberflaechen. Das Messsystem wurde durch verfahrenspezifische Untersuchungen an Proben aus Zementstein, -moerteln und Betonen charakterisiert, Transport- und Anlagerungsprozesse wurden visuell dargestellt. Zudem werden Ergebnisse fuer den Ionenhaushalt in der ungestoerten oberflaechenahen Randzone sowie bei deren Auslaugung bzw. Anreicherung vorgestellt.

Real-time qualitative study of forsterite crystal - Melt lithium distribution by laser-induced breakdown spectroscopy

Science.gov (United States)

Lebedev, V. F.; Makarchuk, P. S.; Stepanov, D. N.

2017-11-01

A factor of lithium distribution between single-crystal forsterite (Cr,Li:Mg2SiO4) and its melt are studied by laser-induced breakdown spectroscopy. Lithium content in the crystalline phase is found to achieve a saturation at relatively low Li concentration in the melt (about 0.02%wt.). An algorithm and software are developed for real-time analysis of the studied spectra of lithium trace amounts at wide variation of the plasma radiation intensity. The analyzed plasma spectra processing method is based on the calculation of lithium emission part in the total emission of the target plasma for each recorded spectrum followed by the error estimation for the series of measurements in the normal distribution approximation.

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

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.)

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)

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.

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.

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.

Studies of Basalt Through Laser Induced Breakdown Spectroscopy (LIBS for the Manufacturing of Lapilli Blocks

Directory of Open Access Journals (Sweden)

Ismael De la Viuda-Pérez

2016-10-01

Full Text Available Basaltic samples selected from different areas of Tenerife were analyzed by applying laser induced breakdown spectroscopy (LIBS, Raman spectroscopy and X Ray Diffraction (XRD in order to identify the basic chemical composition and mineralogy. The basic composition obtained from the analysis was: O, F, Na, K, Mg, Al Si, Ca, Ti and Fe. Raman spectroscopic and XRD analyses indicated a basaltic mineralogy which is consistent with the basic composition results obtained from LIBS. The results of the analyses carried out using portable instrumentation proved the suitability of the LIBS, specially combined with the Raman spectroscopy for their application in the mineralogical-chemical identification in the areas where basalts and lapilli are extracted for construction works in Tenerife.

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.

Laser-induced breakdown spectroscopy in gases using ungated detection in combination with polarization filtering and online background correction

International Nuclear Information System (INIS)

Kiefer, J; Tröger, J W; Seeger, T; Leipertz, A; Li, B; Li, Z S; Aldén, M

2010-01-01

Quantitative and fast analysis of gas mixtures is an important task in the field of chemical, security and environmental analysis. In this paper we present a diagnostic approach based on laser-induced breakdown spectroscopy (LIBS). A polarization filter in the signal collection system enables sufficient suppression of elastically scattered light which otherwise reduces the dynamic range of the measurement. Running the detector with a doubled repetition rate as compared to the laser online background correction is obtained. Quantitative measurements of molecular air components in synthetic, ambient and expiration air are performed and demonstrate the potential of the method. The detection limits for elemental oxygen and hydrogen are in the order of 15 ppm and 10 ppm, respectively

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.

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.

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

Science.gov (United States)

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.

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)

Discrimination between authentic and false tax stamps from liquor bottles using laser-induced breakdown spectroscopy and chemometrics

International Nuclear Information System (INIS)

Gonzaga, Fabiano Barbieri; Rocha, Werickson Fortunato de Carvalho; Correa, Deleon Nascimento

2015-01-01

This work describes the preliminary application of a compact and low-cost laser-induced breakdown spectroscopy (LIBS) instrument for falsification detection of tax stamps used in alcoholic beverages. The new instrument was based on a diode-pumped passively Q-switched Nd:YLF microchip laser and a mini-spectrometer containing a Czerny–Turner polichromator coupled to a non-intensified, non-gated, and non-cooled 2048 pixel linear sensor array (200 to 850 nm spectral range). Twenty-three tax stamp samples were analyzed by firing laser pulses within two different regions of each sample: a hologram and a blank paper region. For each acquired spectrum, the emitted radiation was integrated for 3000 ms under the continuous application of laser pulses at 100 Hz (integration of 300 plasmas). Principal component analysis (PCA) or hierarchical cluster analysis (HCA) of all emission spectra from the hologram or blank paper region revealed two well-defined groups of authentic and false samples. Moreover, for the hologram data, three subgroups of false samples were found. Additionally, partial least squares discriminant analysis (PLS-DA) was successfully applied for the detection of the false tax stamps using all emission spectra from hologram or blank paper region. The discrimination between the samples was mostly ascribed to different levels of calcium concentration in the samples. - Highlights: • Compact and low-cost laser-induced breakdown spectrometer • Analysis of tax stamps used in alcoholic beverages • Detection of false tax stamps using the LIBS spectra and chemometrics • Falsification detection ascribed to different levels of calcium concentration

Discrimination between authentic and false tax stamps from liquor bottles using laser-induced breakdown spectroscopy and chemometrics

Energy Technology Data Exchange (ETDEWEB)

Gonzaga, Fabiano Barbieri, E-mail: fbgonzaga@inmetro.gov.br [Chemical Metrology Division, National Institute of Metrology, Quality and Technology (INMETRO), Av. Nossa Senhora das Graças, 50, Xerém, 25250-020 Duque de Caxias, RJ (Brazil); Rocha, Werickson Fortunato de Carvalho [Chemical Metrology Division, National Institute of Metrology, Quality and Technology (INMETRO), Av. Nossa Senhora das Graças, 50, Xerém, 25250-020 Duque de Caxias, RJ (Brazil); Correa, Deleon Nascimento [Technical–Scientific Police Superintendency, Criminalistic Institute Dr. Octávio Eduardo de Brito Alvarenga—IC-SPTC-SP, 05507-060 São Paulo, SP (Brazil)

2015-07-01

This work describes the preliminary application of a compact and low-cost laser-induced breakdown spectroscopy (LIBS) instrument for falsification detection of tax stamps used in alcoholic beverages. The new instrument was based on a diode-pumped passively Q-switched Nd:YLF microchip laser and a mini-spectrometer containing a Czerny–Turner polichromator coupled to a non-intensified, non-gated, and non-cooled 2048 pixel linear sensor array (200 to 850 nm spectral range). Twenty-three tax stamp samples were analyzed by firing laser pulses within two different regions of each sample: a hologram and a blank paper region. For each acquired spectrum, the emitted radiation was integrated for 3000 ms under the continuous application of laser pulses at 100 Hz (integration of 300 plasmas). Principal component analysis (PCA) or hierarchical cluster analysis (HCA) of all emission spectra from the hologram or blank paper region revealed two well-defined groups of authentic and false samples. Moreover, for the hologram data, three subgroups of false samples were found. Additionally, partial least squares discriminant analysis (PLS-DA) was successfully applied for the detection of the false tax stamps using all emission spectra from hologram or blank paper region. The discrimination between the samples was mostly ascribed to different levels of calcium concentration in the samples. - Highlights: • Compact and low-cost laser-induced breakdown spectrometer • Analysis of tax stamps used in alcoholic beverages • Detection of false tax stamps using the LIBS spectra and chemometrics • Falsification detection ascribed to different levels of calcium concentration.

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

Sensitive elemental detection using microwave-assisted laser-induced breakdown imaging

Science.gov (United States)

Iqbal, Adeel; Sun, Zhiwei; Wall, Matthew; Alwahabi, Zeyad T.

2017-10-01

This study reports a sensitive spectroscopic method for quantitative elemental detection by manipulating the temporal and spatial parameters of laser-induced plasma. The method was tested for indium detection in solid samples, in which laser ablation was used to generate a tiny plasma. The lifetime of the laser-induced plasma can be extended to hundreds of microseconds using microwave injection to remobilize the electrons. In this novel method, temporal integrated signal of indium emission was significantly enhanced. Meanwhile, the projected detectable area of the excited indium atoms was also significantly improved using an interference-, instead of diffraction-, based technique, achieved by directly imaging microwave-enhanced plasma through a novel narrow-bandpass filter, exactly centered at the indium emission line. Quantitative laser-induce breakdown spectroscopy was also recorded simultaneously with the new imaging method. The intensities recorded from both methods exhibit very good mutual linear relationship. The detection intensity was improved to 14-folds because of the combined improvements in the plasma lifetime and the area of detection.

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.

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 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.

Microanalysis of tool steel and glass with laser-induced breakdown spectroscopy

Science.gov (United States)

Loebe, Klaus; Uhl, Arnold; Lucht, Hartmut

2003-10-01

A laser microscope system for the microanalytical characterization of complex materials is described. The universal measuring principle of laser-induced breakdown spectroscopy (LIBS) in combination with echelle optics permits a fast simultaneous multielement analysis with a possible spatial resolution below 10 pm. The developed system features completely UV-transparent optics for the laser-microscope coupling and the emission beam path and enables parallel signal detection within the wavelength range of 200-800 nm with a spectral resolution of a few picometers. Investigations of glass defects and tool steels were performed. The characterization of a glass defect in a tumbler by a micro-LIBS line scan, with use of a 266-nm diode-pumped Nd:YAG laser for excitation, is possible by simple comparison of plasma spectra of the defect and the surrounding area. Variations in the main elemental composition as well as impurities by trace elements are detected at the same time. Through measurement of the calibration samples with the known concentration of the corresponding element, a correlation between the intensity of spectral lines and the element concentration was also achieved. The change of elemental composition at the transient stellite solder of tool steels has been determined by an area scan. The two-dimensional pictures show abrupt changes of the element distribution along the solder edge and allow fundamental researches of dynamic modifications (e.g., diffusion) in steel.

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.

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.

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.

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.

Numerical and experimental depth profile analyses of coated and attached layers by laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Ardakani, H. Afkhami [Laser and Plasma Research Institute, Shahid Beheshti University, G. C., Evin, Tehran (Iran, Islamic Republic of); Tavassoli, S.H., E-mail: h-tavassoli@sbu.ac.i [Laser and Plasma Research Institute, Shahid Beheshti University, G. C., Evin, Tehran (Iran, Islamic Republic of)

2010-03-15

Laser-induced breakdown spectroscopy (LIBS) is applied for depth profile analysis of different thicknesses of copper foils attached on steel and aluminum substrates. In order to account interfacial effects, depth profile analysis of copper coated on steel is also carried out. Experiments are done at ambient air and at two different wavelengths of 266 and 1064 nm of a Nd:YAG laser with pulse durations of 5 ns. A three-dimensional model of multi-pulse laser ablation is introduced on the base of normal evaporation mechanism and the simulation results are compared with the experiments. A normalized concentration (C{sup N}) is introduced for determination of interface position and results are compared with the usually used normalized intensity (I{sup N}). The effect of coating thickness on average ablation rate and resolution of depth profiling are examined. There is a correlation coefficient higher than 0.95 between the model and experimental depth profiles based on the C{sup N} method. Depth profile analysis on the base of C{sup N} method shows a better depth resolution in comparison with I{sup N} method .Increase in the layer thickness, leads to a decrease in the ablation rate.

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

Science.gov (United States)

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.

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.

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.

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

Development of a coal quality analyzer for application to power plants based on laser-induced breakdown spectroscopy

Science.gov (United States)

Zhang, Lei; Gong, Yao; Li, Yufang; Wang, Xin; Fan, Juanjuan; Dong, Lei; Ma, Weiguang; Yin, Wangbao; Jia, Suotang

2015-11-01

It is vitally important for a power plant to determine the coal property rapidly to optimize the combustion process. In this work, a fully software-controlled laser-induced breakdown spectroscopy (LIBS) based coal quality analyzer comprising a LIBS apparatus, a sampling equipment, and a control module, has been designed for possible application to power plants for offering rapid and precise coal quality analysis results. A closed-loop feedback pulsed laser energy stabilization technology is proposed to stabilize the Nd: YAG laser output energy to a preset interval by using the detected laser energy signal so as to enhance the measurement stability and applied in a month-long monitoring experiment. The results show that the laser energy stability has been greatly reduced from ± 5.2% to ± 1.3%. In order to indicate the complex relationship between the concentrations of the analyte of interest and the corresponding plasma spectra, the support vector regression (SVR) is employed as a non-linear regression method. It is shown that this SVR method combined with principal component analysis (PCA) enables a significant improvement in cross-validation accuracy by using the calibration set of coal samples. The root mean square error for prediction of ash content, volatile matter content, and calorific value decreases from 2.74% to 1.82%, 1.69% to 1.22%, and 1.23 MJ/kg to 0.85 MJ/kg, respectively. Meanwhile, the corresponding average relative error of the predicted samples is reduced from 8.3% to 5.48%, 5.83% to 4.42%, and 5.4% to 3.68%, respectively. The enhanced levels of accuracy obtained with the SVR combined with PCA based calibration models open up avenues for prospective prediction in coal properties.

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.

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

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.

Effective laser-induced breakdown spectroscopy (LIBS) detection using double pulse at optimum configuration.

Science.gov (United States)

Choi, Soo Jin; Yoh, Jack J

2011-08-01

A short laser pulse is irradiated on a sample to create a highly energetic plasma that emits light of a specific peak wavelength according to the material. By identifying different peaks for the analyzed samples, their chemical composition can be rapidly determined. The characteristics of the laser-induced breakdown spectroscopy (LIBS) plasma are strongly dependent on the ambient conditions. Research aimed at enhancing LIBS intensity is of great benefit in advancing LIBS for the exploration of harsh environments. By using double-pulse LIBS, the signal intensity of Al and Ca lines was enhanced by five times compared to the single-pulse signal. Also, the angles of the target and detector are adjusted to simulate samples of arbitrary shape. We verified that there exists an optimal angle at which specific elements of a test sample may be detected with stronger signal intensity. We provide several optimum configurations for the LIBS system for maximizing the signal intensity for the analysis of a nonstandard aluminum sample.

Laser-induced breakdown spectroscopy analysis of the copper added to gadolinium (Contract research)

International Nuclear Information System (INIS)

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

2008-11-01

For applying Laser-induced breakdown Spectroscopy (LIBS) to the analysis of nuclear fuel materials, it is very important to investigate the analytical method to identify the emission spectrum and its intensity on impurities intermingled within complex emission spectra of matrix elements such as uranium (U) and plutonium (Pu). Experiments using gadolinium (Gd) as simulated sample, in which several 100 ppm of copper (Cu) was contained, were performed and the analytical performance was estimated. The spectrum was decomposed into each peak of some spectra component on Gd and Cu. And the result, intensity of Cu component intermingled in Gd was determined quantitatively. In order to evaluate the linearity in the impurity analysis, the experiments with various concentration of Cu were carried out. The detection limit was determined to be about 70 ppm from the equivalent noise level which was estimated from the standard deviation in wavelength. The results curried out under the other laser conditions (intensity and wavelength) ware also evaluated. (author)

Time-resolved spectroscopy of laser-induced breakdown in water

Science.gov (United States)

Thomas, Robert J.; Hammer, Daniel X.; Noojin, Gary D.; Stolarski, David J.; Rockwell, Benjamin A.; Roach, William P.

1996-05-01

Laser pulses of 60-ps and 80-ps at a wavelength of 532-nm and 1064-nm respectively were used to produce laser induced breakdown in triple-distilled water. The resulting luminescent flash from the plasma was captured with an imaging spectrograph coupled to a streak camera with a 5-ps time resolution. The wavelength range was 350 to 900-nm. We present the resulting experimental data which gives plasma duration and time-resolved spectral information. Plasma temperature is also computed from the data. All parameters are presented at a pulse energy of 1-mJ and are compared with time-integrated spectra at the same pulse duration and at 5 to 7-ns pulse duration in a similar energy range.

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.

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.

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.

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.

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.

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.

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...

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

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.

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)

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.

Feasibility of laser-induced breakdown spectroscopy (LIBS) for classification of sea salts.

Science.gov (United States)

Tan, Man Minh; Cui, Sheng; Yoo, Jonghyun; Han, Song-Hee; Ham, Kyung-Sik; Nam, Sang-Ho; Lee, Yonghoon

2012-03-01

We have investigated the feasibility of laser-induced breakdown spectroscopy (LIBS) as a fast, reliable classification tool for sea salts. For 11 kinds of sea salts, potassium (K), magnesium (Mg), calcium (Ca), and aluminum (Al), concentrations were measured by inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and the LIBS spectra were recorded in the narrow wavelength region between 760 and 800 nm where K (I), Mg (I), Ca (II), Al (I), and cyanide (CN) band emissions are observed. The ICP-AES measurements revealed that the K, Mg, Ca, and Al concentrations varied significantly with the provenance of each salt. The relative intensities of the K (I), Mg (I), Ca (II), and Al (I) peaks observed in the LIBS spectra are consistent with the results using ICP-AES. The principal component analysis of the LIBS spectra provided the score plot with quite a high degree of clustering. This indicates that classification of sea salts by chemometric analysis of LIBS spectra is very promising. Classification models were developed by partial least squares discriminant analysis (PLS-DA) and evaluated. In addition, the Al (I) peaks enabled us to discriminate between different production methods of the salts. © 2012 Society for Applied Spectroscopy

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.

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.

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.

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.

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.

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.

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.

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)

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.

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.

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.

Optical breakdown threshold investigation of 1064 nm laser induced air plasmas

International Nuclear Information System (INIS)

Thiyagarajan, Magesh; Thompson, Shane

2012-01-01

We present the theoretical and experimental measurements and analysis of the optical breakdown threshold for dry air by 1064 nm infrared laser radiation and the significance of the multiphoton and collisional cascade ionization process on the breakdown threshold measurements over pressures range from 10 to 2000 Torr. Theoretical estimates of the breakdown threshold laser intensities and electric fields are obtained using two distinct theories namely multiphoton and collisional cascade ionization theories. The theoretical estimates are validated by experimental measurements and analysis of laser induced breakdown processes in dry air at a wavelength of 1064 nm by focusing 450 mJ max, 6 ns, 75 MW max high-power 1064 nm IR laser radiation onto a 20 μm radius spot size that produces laser intensities up to 3 - 6 TW/cm 2 , sufficient for air ionization over the pressures of interest ranging from 10 to 2000 Torr. Analysis of the measured breakdown threshold laser intensities and electric fields are carried out in relation with classical and quantum theoretical ionization processes, operating pressures. Comparative analysis of the laser air breakdown results at 1064 nm with corresponding results of a shorter laser wavelength (193 nm) [M. Thiyagarajan and J. E. Scharer, IEEE Trans. Plasma Sci. 36, 2512 (2008)] and a longer microwave wavelength (10 8 nm) [A. D. MacDonald, Microwave Breakdown in Gases (Wiley, New York, 1966)]. A universal scaling analysis of the breakdown threshold measurements provided a direct comparison of breakdown threshold values over a wide range of frequencies ranging from microwave to ultraviolet frequencies. Comparison of 1064 nm laser induced effective field intensities for air breakdown measurements with data calculated based on the collisional cascade and multiphoton breakdown theories is used successfully to determine the scaled collisional microwave portion. The measured breakdown threshold of 1064 nm laser intensities are then scaled to

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.

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 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.

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.

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

Science.gov (United States)

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.

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.

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

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)

Space-resolved analysis of trace elements in fresh vegetables using ultraviolet nanosecond laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Juve, Vincent; Portelli, Richard; Boueri, Myriam; Baudelet, Matthieu; Yu Jin

2008-01-01

Laser-induced breakdown spectroscopy (LIBS) has been applied to analyze trace elements contained in fresh vegetables. A quadrupled Nd:YAG laser is used in the experiments for ablation. Analyzed samples come from local markets and represent frequently consumed vegetables. For a typical root vegetable, such as potato, spectral analysis of the plasma emission reveals more than 400 lines emitted by 27 elements and 2 molecules, C 2 and CN. Among these species, one can find trace as well as ultra-trace elements. A space-resolved analysis of several trace elements with strong emissions is then applied to typical root, stem and fruit vegetables. The results from this study demonstrate the potential of an interesting tool for botanical and agricultural studies as well for food quality/safety and environment pollution assessment and control

Micro-Crater Laser Induced Breakdown Spectroscopy--an Analytical approach in metals samples

Energy Technology Data Exchange (ETDEWEB)

Piscitelli, Vincent [UCV- Laboratorio de Espectroscopia Laser, Caracas (Venezuela); Lawrence Berkeley National laboratory, Berkeley, US (United States); Gonzalez, Jhanis; Xianglei, Mao; Russo, Richard [Lawrence Berkeley National laboratory, Berkeley, US (United States); Fernandez, Alberto [UCV- Laboratorio de Espectroscopia Laser, Caracas (Venezuela)

2008-04-15

The laser ablation has been increasing its popularity like as technique of chemical analysis. This is due to its great potentiality in the analysis of solid samples. On the way to contributing to the development of the technique, we in this work studied the laser induced breakdown spectroscopy (LIBS) in conditions of micro ablation for future studies of coverings and micro crates analysis. Craters between 2 and 7 micrometers of diameter were made using an Nd-YAG nanosecond laser in their fundamental emission of 1064 nm. In order to create these craters we use an objective lens of long distance work and 0.45 of numerical aperture. The atomic emission versus the energy of the laser and its effect on the size of craters was study. We found that below 3 micrometers although there was evidence of material removal by the formation of a crater, it was no detectable atomic emission for our instruments. In order to try to understand this, curves of size of crater versus plasma temperature using the Boltzmann distribution graphs taking the Copper emission lines in the visible region were made. In addition calibration curves for Copper and aluminum were made in two different matrices; one of it was a Cu/Zn alloy and the other a Zinc Matrix. The atomic lines Cu I (521.78 nm) and Al I (396.15 nm) was used. From the Calibration curve the analytical limit of detection and other analytical parameters were obtained.

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 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.

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.

Automatic variable selection method and a comparison for quantitative analysis in laser-induced breakdown spectroscopy

Science.gov (United States)

Duan, Fajie; Fu, Xiao; Jiang, Jiajia; Huang, Tingting; Ma, Ling; Zhang, Cong

2018-05-01

In this work, an automatic variable selection method for quantitative analysis of soil samples using laser-induced breakdown spectroscopy (LIBS) is proposed, which is based on full spectrum correction (FSC) and modified iterative predictor weighting-partial least squares (mIPW-PLS). The method features automatic selection without artificial processes. To illustrate the feasibility and effectiveness of the method, a comparison with genetic algorithm (GA) and successive projections algorithm (SPA) for different elements (copper, barium and chromium) detection in soil was implemented. The experimental results showed that all the three methods could accomplish variable selection effectively, among which FSC-mIPW-PLS required significantly shorter computation time (12 s approximately for 40,000 initial variables) than the others. Moreover, improved quantification models were got with variable selection approaches. The root mean square errors of prediction (RMSEP) of models utilizing the new method were 27.47 (copper), 37.15 (barium) and 39.70 (chromium) mg/kg, which showed comparable prediction effect with GA and SPA.

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

International Nuclear Information System (INIS)

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

2009-01-01

Laser induced breakdown spectroscopy (LIBS) has been evaluated for the determination of micronutrients (B, Cu, Fe, Mn and Zn) in pellets of plant materials, using NIST, BCR and GBW biological certified reference materials for analytical calibration. Pellets of approximately 2 mm thick and 15 mm diameter were prepared by transferring 0.5 g of powdered material to a 15 mm die set and applying 8.0 tons cm -2 . An experimental setup was designed by using a Nd:YAG laser operating at 1064 nm (200 mJ per pulse, 10 Hz) and an Echelle spectrometer with ICCD detector. Repeatability precision varied from 4 to 30% from measurements obtained in 10 different positions (8 laser shots per test portion) in the same sample pellet. Limits of detection were appropriate for routine analysis of plant materials and were 2.2 mg kg -1 B, 3.0 mg kg -1 Cu, 3.6 mg kg -1 Fe, 1.8 mg kg -1 Mn and 1.2 mg kg -1 Zn. Analysis of different plant samples were carried out by LIBS and results were compared with those obtained by ICP OES after wet acid decomposition.

Influence of Er:YAG and Nd:YAG wavelengths on laser-induced breakdown spectroscopy measurements under air or helium atmosphere

International Nuclear Information System (INIS)

Detalle, Vincent; Sabsabi, Mohamad; St-Onge, Louis; Hamel, Andre; Heon, Rene

2003-01-01

Laser-induced breakdown spectroscopy (LIBS) is widely dependent on the conditions of its implementation in terms of laser characteristics (wavelength, energy, and pulse duration), focusing conditions, and surrounding gas. In this study two wavelengths, 1.06 and 2.94 μm, obtained with Nd:YAG and Er:YAG lasers, respectively, were used for LIBS analysis of aluminum alloy samples in two conditions of surrounding gas. The influence of the laser wavelength on the laser-produced plasma was studied for the same irradiance by use of air or helium as a buffer gas at atmospheric pressure. We used measurements of light emission to determine the temporally resolved space-averaged electron density and plasma temperature in the laser-induced plasma. We also examined the effect of laser wavelength in two different ambient conditions in terms of spectrochemical analysis by LIBS. The results indicate that the effect of the surrounding gas depends on the laser wavelength and the use of an Er:YAG laser could increase linearity by limiting the leveling in the calibration curve for some elements in aluminum alloys. There is also a significant difference between the plasma induced by the two lasers in terms of electron density and plasma temperature

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

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.

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.

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.

Effect of pulse repetition rate and number of pulses in the analysis of polypropylene and high density polyethylene by nanosecond infrared laser induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Leme, Flavio O. [Laboratorio de Quimica Analitica ' Henrique Bergamin Filho' , Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario 303, 13416-000 Piracicaba, SP (Brazil); Godoi, Quienly [Laboratorio de Quimica Analitica ' Henrique Bergamin Filho' , Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario 303, 13416-000 Piracicaba, SP (Brazil); Departamento de Quimica, Universidade Federal de Sao Carlos, Rod. Washington Luis, km 235, 13565-905 Sao Carlos, SP (Brazil); Kiyataka, Paulo H.M. [Centro de Tecnologia de Embalagens, Instituto de Tecnologia de Alimentos, Av. Brasil 2880, 13070-178 Campinas, SP (Brazil); Santos, Dario [Departamento de Ciencias Exatas e da Terra, Universidade Federal de Sao Paulo, Rua Prof. Artur Riedel 275, 09972-270 Diadema, SP (Brazil); Agnelli, Jose A.M. [Departamento de Engenharia de Materiais, Universidade Federal de Sao Carlos, Rod. Washington Luis, km 235, 13565-905 Sao Carlos, SP (Brazil); and others

2012-02-01

Pulse repetition rates and the number of laser pulses are among the most important parameters that do affect the analysis of solid materials by laser induced breakdown spectroscopy, and the knowledge of their effects is of fundamental importance for suggesting analytical strategies when dealing with laser ablation processes of polymers. In this contribution, the influence of these parameters in the ablated mass and in the features of craters was evaluated in polypropylene and high density polyethylene plates containing pigment-based PbCrO{sub 4}. Surface characterization and craters profile were carried out by perfilometry and scanning electron microscopy. Area, volume and profile of craters were obtained using Taylor Map software. A laser induced breakdown spectroscopy system consisted of a Q-Switched Nd:YAG laser (1064 nm, 5 ns) and an Echelle spectrometer equipped with ICCD detector were used. The evaluated operating conditions consisted of 10, 25 and 50 laser pulses at 1, 5 and 10 Hz, 250 mJ/pulse (85 J cm{sup -2}), 2 {mu}s delay time and 6 {mu}s integration time gate. Differences in the topographical features among craters of both polymers were observed. The decrease in the repetition rate resulted in irregular craters and formation of edges, especially in polypropylene sample. The differences in the topographical features and ablated masses were attributed to the influence of the degree of crystallinity, crystalline melting temperature and glass transition temperature in the ablation process of the high density polyethylene and polypropylene. It was also observed that the intensities of chromium and lead emission signals obtained at 10 Hz were two times higher than at 5 Hz by keeping the number of laser pulses constant.

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

Fiber-optic laser-induced breakdown spectroscopy of zirconium metal in air: Special features of the plasma produced by a long-pulse laser

Science.gov (United States)

Matsumoto, Ayumu; Ohba, Hironori; Toshimitsu, Masaaki; Akaoka, Katsuaki; Ruas, Alexandre; Sakka, Tetsuo; Wakaida, Ikuo

2018-04-01

The decommissioning of the Tokyo Electric Power Company (TEPCO) Fukushima Daiichi Nuclear Power Plant is an essential issue in nuclear R&D. Fiber-optic laser-induced breakdown spectroscopy (Fiber-optic LIBS) could be used for in-situ elemental analysis of the inside of the damaged reactors. To improve the performances under difficult conditions, using a long-pulse laser can be an efficient alternative. In this work, the emission spectra of zirconium metal in air obtained for a normal-pulse laser (6 ns) and a long-pulse laser (100 ns) (wavelength: 1064 nm, pulse energy: 12.5 mJ, spot diameter: 0.35 mm) are compared to investigate the fundamental aspects of fiber-optic LIBS with the long-pulse laser. The spectral features are considerably different: when the long-pulse laser is used, the atomic and molecular emission is remarkably enhanced. The enhancement of the atomic emission at the near infrared (NIR) region would lead to the observation of emission lines with minimum overlapping. To understand the differences in the spectra induced respectively from the normal-pulse laser and the long-pulse laser, photodiode signals, time-resolved spectra, plasma parameters, emission from the ambient air, and emission regions are investigated, showing the particular characteristics of the plasma produced by the long-pulse laser.

Feasibility of Trace Alcohol Congener Detection and Identification Using Laser-Induced Breakdown Spectroscopy

International Nuclear Information System (INIS)

Zhang Jialiang; Wang Shangmin; Zhao Lixian; Liu Liying; Wang Dezhen

2014-01-01

In this paper, a feasible scheme is reported for the detection and identification of trace alcohol congeners that have identical elemental composition using laser-induced breakdown spectroscopy (LIBS). In the scheme, an intensive pulsed laser is used to break down trace alcohol samples and the optical emission spectra of the induced plasma are collected for the detection and identification of alcohol molecules. In order to prepare trace alcohol samples, pure ethanol or methanol is bubbled by argon carrier gas and then mixed into matrix gases. The key issue for the scheme is to constitute indices from the LIBS data of the alcohol samples. Two indices are found to be suitable for alcohol detection and identification. One is the emission intensity ratio (denoted as H/C) of the hydrogen line (653.3 nm) to the carbon line (247.9 nm) for identification and the other is the ratio of the carbon line (as C/Ar) or the hydrogen line (as H/Ar) to the argon lines (866.7 nm) for quantitative detection. The calibration experiment result shows that the index H/C is specific for alcohol congeners while almost being independent of alcohol concentration. In detail, the H/C keeps a specific constant of 34 and 23 respectively for ethanol and methanol. In the meanwhile, the C/Ar and H/Ar indices respond almost linearly to the alcohol concentration below 1300 ppm, and are therefore competent for concentration measurement. With the indices, trace alcohol concentration measurement achieves a limit of 140 ppm using a laser pulse energy of 300 mJ. (plasma technology)

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.

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

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

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.

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).

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.

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

Determination of silicon in plant materials by laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Souza, Paulino Florêncio de [Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000, Piracicaba, SP (Brazil); Centro de Tecnologia Canavieira, PO Box 162, 13400-970 Piracicaba, SP (Brazil); Santos, Dário [Departamento de Ciências Exatas e da Terra, Universidade Federal de São Paulo, Rua Prof. Artur Riedel, 275, 09972-270, Diadema, SP (Brazil); Gustinelli Arantes de Carvalho, Gabriel; Nunes, Lidiane Cristina [Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000, Piracicaba, SP (Brazil); Silva Gomes, Marcos da [Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000, Piracicaba, SP (Brazil); Departamento de Química, Universidade Federal de São Carlos, 13565-905 São Carlos, SP (Brazil); Guerra, Marcelo Braga Bueno [Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000, Piracicaba, SP (Brazil); Krug, Francisco José, E-mail: fjkrug@cena.usp.br [Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000, Piracicaba, SP (Brazil)

2013-05-01

In spite of the importance of Si for improving the productivity of many important crops, such as those from the Poaceae family (e.g. sugar cane, maize, wheat, rice), its quantitative determination in plants is seldom carried out and restricted to few laboratories in the world. There is a survey of methods in the literature, but most of them are either laborious or difficult to validate in view of the low availability of reference materials with a certified Si mass fraction. The aim of this study is to propose a method for the direct determination of Si in pellets of plant materials by laser-induced breakdown spectroscopy (LIBS). The experimental setup was designed by using a Q-switched Nd:YAG laser at 1064 nm (5 ns, 10 Hz) and the emission signals were collected by lenses into an optical fiber coupled to an Echelle spectrometer equipped with an intensified charge-coupled device. Experiments were carried out with leaves from 24 sugar cane varieties, with mass fractions varying from ca. 2 to 10 g kg{sup −1} Si. Pellets prepared from cryogenically ground leaves were used as test samples for both method development and validation of the calibration model. Best results were obtained when the test samples were interrogated with laser fluence of 50 J cm{sup −2} (750 μm spot size) and measurements carried out at Si I 212.412 nm emission line. The results obtained by LIBS were compared with those from inductively coupled plasma optical emission spectrometry after oven-induced alkaline digestion, and no significant differences were observed after applying the Student's t-test at 95% confidence level. The trueness of the proposed LIBS method was also confirmed from the analysis of CRM GBW 07603 (Bush branches and leaves). - Highlights: • This is the first application of LIBS for determination of Si in plant materials. • Data indicate that the method is appropriate for Si diagnosis in routine analysis. • Silicon can be simultaneously determined with macro- and

Determination of silicon in plant materials by laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Souza, Paulino Florêncio de; Santos, Dário; Gustinelli Arantes de Carvalho, Gabriel; Nunes, Lidiane Cristina; Silva Gomes, Marcos da; Guerra, Marcelo Braga Bueno; Krug, Francisco José

2013-01-01

In spite of the importance of Si for improving the productivity of many important crops, such as those from the Poaceae family (e.g. sugar cane, maize, wheat, rice), its quantitative determination in plants is seldom carried out and restricted to few laboratories in the world. There is a survey of methods in the literature, but most of them are either laborious or difficult to validate in view of the low availability of reference materials with a certified Si mass fraction. The aim of this study is to propose a method for the direct determination of Si in pellets of plant materials by laser-induced breakdown spectroscopy (LIBS). The experimental setup was designed by using a Q-switched Nd:YAG laser at 1064 nm (5 ns, 10 Hz) and the emission signals were collected by lenses into an optical fiber coupled to an Echelle spectrometer equipped with an intensified charge-coupled device. Experiments were carried out with leaves from 24 sugar cane varieties, with mass fractions varying from ca. 2 to 10 g kg −1 Si. Pellets prepared from cryogenically ground leaves were used as test samples for both method development and validation of the calibration model. Best results were obtained when the test samples were interrogated with laser fluence of 50 J cm −2 (750 μm spot size) and measurements carried out at Si I 212.412 nm emission line. The results obtained by LIBS were compared with those from inductively coupled plasma optical emission spectrometry after oven-induced alkaline digestion, and no significant differences were observed after applying the Student's t-test at 95% confidence level. The trueness of the proposed LIBS method was also confirmed from the analysis of CRM GBW 07603 (Bush branches and leaves). - Highlights: • This is the first application of LIBS for determination of Si in plant materials. • Data indicate that the method is appropriate for Si diagnosis in routine analysis. • Silicon can be simultaneously determined with macro- and micronutrients

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

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.

Influence of Ambient Gas on Laser-Induced Breakdown Spectroscopy of Uranium Metal

International Nuclear Information System (INIS)

Zhang Dacheng; Ma Xinwen; Wang Shulong; Zhu Xiaolong

2015-01-01

Laser-induced breakdown spectroscopy (LIBS) is regarded as a suitable method for the remote analysis of materials in any phase, even in an environment with high radiation levels. In the present work we used the third harmonic pulse of a Nd:YAG laser for ablation of uranium metal and measured the plasma emission with a fiber-optic spectrometer. The LIBS spectra of uranium metal and their features in different ambient gases (i.e., argon, neon, oxygen, and nitrogen) at atmospheric pressure were studied. Strong continuum spectrum and several hundreds of emission lines from UI and UII were observed. It is found that the continuum spectrum observed in uranium not only comes from bremsstrahlung emission but is also due to the complex spectrum of uranium. The influence of ambient gas and the gas flow rate for ablation of uranium metal was investigated. The experimental results indicate that the intensity of the uranium lines was enhanced in argon and nitrogen. However, the intensity of uranium lines was decreased in oxygen due to the generation of UO and other oxides. The results also showed that the highest intensity of uranium lines were obtained in argon gas with a gas flow rate above 2.5 L/min. The enhanced mechanism in ambient gas and the influence of the gas flow rate were analyzed in this work. (paper)

Evaluation of minor element concentrations in potatoes using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Beldjilali, S.; Borivent, D.; Mercadier, L.; Mothe, E.; Clair, G.; Hermann, J.

2010-01-01

We have performed spectroscopic analysis of the plasma generated by Nd:YAG laser irradiation of flesh and skin of fresh potatoes. From the spectra recorded with an Echelle spectrometer 11 minor elements have been identified. Their relative concentrations were estimated by comparing the measured spectra to the spectral radiance computed for a plasma in local thermal equilibrium. According the moderate plasma temperature of about 6500 K at the time of spectroscopic observation, the electrons are essentially generated by the ionization of the minor metal atoms, making plasma modeling possible although the organic elements may be out of equilibrium. Among the spectral lines selected for the analysis, the Na I 588.99 and 589.59 nm doublet was found to be partially self-absorbed allowing us to estimate the number density of sodium atoms. The value was found to agree with the number density predicted by the plasma model. As a result, the relative concentrations of the detected minor elements have been estimated for both the flesh and skin of the potatoes. Among these, aluminum and silicon were found to have relatively large mass fractions in the potato skin whereas their presence was not detected in the flesh. The present study shows that laser-induced breakdown spectroscopy is a promising tool to measure the elemental composition of fresh vegetables without any sample preparation.

Laser induced breakdown spectroscopy in water | Boudjemai ...

African Journals Online (AJOL)

Sparks were generated in water by the focused beam of a Q-switched Nd:YAG laser Na and Cu aqueous solutions exhibited fluorescence signal on the decaying edge of plasma emission at their respective characteristic resonance lines. Potential of the laser plasma spectroscopy for in-situ pollution monitoring in natural ...

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.

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.

Development and Validation of a Laser Induced Breakdown Spectrometry Method for Cancer Detection and Characterization

International Nuclear Information System (INIS)

Otieno, E.A.

2015-01-01

Laser Induced Breakdown Spectroscopy (LIBS) is a type of atomic emission spectroscopy which employs a highly energetic laser pulse to simultaneously prepare the sample and excite the species. The simplest calibration technique is based on the use of standard calibration curves. The phenomenon of self-absorption may be considered as a factor of linearity deviation in conventional calibration. Chemometrics has the ability to extract underlying phenomena from complex data with the help of multivariate techniques such as SIMCA, ICA, PCA, SVM and ANNs. The techniques are also capable of capturing information about correlated trends in a given dataset. It has been reported that in normal liver the zinc concentration is about 78ug/g, wet weight and the primary liver cancer itself is about 18ug/g

Influence of Lead on the Interpretation of Bone Samples with Laser-Induced Breakdown Spectroscopy

Directory of Open Access Journals (Sweden)

Abdolhamed Shahedi

2016-01-01

Full Text Available This study is devoted to tracing and identifying the elements available in bone sample using Laser-Induced Breakdown Spectroscopy (LIBS. The bone samples were prepared from the thigh of laboratory rats, which consumed 325.29 g/mol lead acetate having 4 mM concentration in specified time duration. About 76 atomic lines have been analyzed and we found that the dominant elements are Ca I, Ca II, Mg I, Mg II, Fe I, and Fe II. Temperature curve and bar graph were drawn to compare bone elements of group B which consumed lead with normal group, group A, in the same laboratory conditions. Plasma parameters including plasma temperature and electron density were determined by considering Local Thermodynamic Equilibrium (LTE condition in the plasma. An inverse relationship has been detected between lead absorption and elements like Calcium and Magnesium absorption comparing elemental values for both the groups.

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

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

Determination of hazardous ingredients in personal care products using laser-induced breakdown spectroscopy

Science.gov (United States)

Abrar, M.; Iqbal, T.; Fahad, M.; Andleeb, M.; Farooq, Z.; Afsheen, S.

2018-05-01

In the present work, the laser-induced breakdown spectroscopy technique is applied to explore the concentration of toxic elements present in cosmetic materials. The elemental analysis of chromium (Cr), magnesium (Mg), cadmium (Cd) and lead (Pb) are selected as major elements and manganese (Mn), sodium (Na), potassium (P), sulfur (S), silicon (Si) and titanium (Ti) as minor elements in cosmetic products. In this technique, a plasma plume is generated by using an Nd:YAG Laser of 532 nm wavelength and spectral lines for the respective samples are observed. Four different samples of cosmetic products are selected, i.e. two samples for lipstick and two for eyeshadow. The observed spectral lines of all major and minor elements are used to calculate their concentration in all samples through the intensity ratio method. Among selected lipstick and eyeshadow samples, one sample is branded, and one is collected from the local market. It is observed that chromium, magnesium and lead have strong spectral lines and consequently show high concentration. The calculated concentrations are then compared to permissible limits set by the Food and Drug Administration with regard to the cosmetics industry. The concentration of these toxic elements in selected local cosmetic samples exceeds the safe permissible limit for human use and could lead to serious health problems.

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.

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.

Local Thermodynamic Equilibrium in Laser-Induced Breakdown Spectroscopy: Beyond the McWhirter criterion

International Nuclear Information System (INIS)

Cristoforetti, G.; De Giacomo, A.; Dell'Aglio, M.; Legnaioli, S.; Tognoni, E.; Palleschi, V.; Omenetto, N.

2010-01-01

In the Laser-Induced Breakdown Spectroscopy (LIBS) technique, the existence of Local Thermodynamic Equilibrium (LTE) is the essential requisite for meaningful application of theoretical Boltzmann-Maxwell and Saha-Eggert expressions that relate fundamental plasma parameters and concentration of analyte species. The most popular criterion reported in the literature dealing with plasma diagnostics, and usually invoked as a proof of the existence of LTE in the plasma, is the McWhirter criterion [R.W.P. McWhirter, in: Eds. R.H. Huddlestone, S.L. Leonard, Plasma Diagnostic Techniques, Academic Press, New York, 1965, pp. 201-264]. However, as pointed out in several papers, this criterion is known to be a necessary but not a sufficient condition to insure LTE. The considerations reported here are meant to briefly review the theoretical analysis underlying the concept of thermodynamic equilibrium and the derivation of the McWhirter criterion, and to critically discuss its application to a transient and non-homogeneous plasma, like that created by a laser pulse on solid targets. Specific examples are given of theoretical expressions involving relaxation times and diffusion coefficients, as well as a discussion of different experimental approaches involving space and time-resolved measurements that could be used to complement a positive result of the calculation of the minimum electron number density required for LTE using the McWhirter formula. It is argued that these approaches will allow a more complete assessment of the existence of LTE and therefore permit a better quantitative result. It is suggested that the mere use of the McWhirter criterion to assess the existence of LTE in laser-induced plasmas should be discontinued.

Quantitative analysis of toxic metals lead and cadmium in water jet by laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Cheri, M. Sadegh; Tavassoli, S. H.

2011-03-20

Laser-induced breakdown spectroscopy (LIBS) has been applied to the analysis of toxic metals Pb and Cd in Pb(NO{sub 3}){sub 2} and Cd(NO{sub 3}){sub 2}.4H{sub 2}O aqueous solutions, respectively. The plasma is generated by focusing a nanosecond Nd:YAG ({lambda}=1064 nm) laser on the surface of liquid in the homemade liquid jet configuration. With an assumption of local thermodynamic equilibrium (LTE), calibration curves of Pb and Cd were obtained at different delay times between 1 to 5 {mu}s. The temporal behavior of limit of detections (LOD) was investigated and it is shown that the minimum LODs for Pb and Cd are 4 and 68 parts in 10{sup 6} (ppm), respectively. In order to demonstrate the correctness of the LTE assumption, plasma parameters including plasma temperature and electron density are evaluated, and it is shown that the LTE condition is satisfied at all delay times.

Vibrational emission analysis of the CN molecules in laser-induced breakdown spectroscopy of organic compounds

Energy Technology Data Exchange (ETDEWEB)

Fernández-Bravo, Ángel; Delgado, Tomás; Lucena, Patricia; Laserna, J. Javier, E-mail: laserna@uma.es

2013-11-01

Laser-induced breakdown spectroscopy (LIBS) of organic materials is based on the analysis of atomic and ionic emission lines and on a few molecular bands, the most important being the CN violet system and the C{sub 2} Swan system. This paper is focused in molecular emission of LIBS plasmas based on the CN (B{sup 2}Σ–X{sup 2}Σ) band, one of the strongest emissions appearing in all carbon materials when analyzed in air atmosphere. An analysis of this band with sufficient spectral resolution provides a great deal of information on the molecule, which has revealed that valuable information can be obtained from the plume chemistry and dynamics affecting the excitation mechanisms of the molecules. The vibrational emission of this molecular band has been investigated to establish the dependence of this emission on the molecular structure of the materials. The paper shows that excitation/emission phenomena of molecular species observed in the plume depend strongly on the time interval selected and on the irradiance deposited on the sample surface. Precise time resolved LIBS measurements are needed for the observation of distinctive CN emission. For the organic compounds studied, larger differences in the behavior of the vibrational emission occur at early stages after plasma ignition. Since molecular emission is generally more complex than that involving atomic emission, local plasma conditions as well as plume chemistry may induce changes in vibrational emission of molecules. As a consequence, alterations in the distribution of the emissions occur in terms of relative intensities, being sensitive to the molecular structure of every single material. - Highlights: • Vibrational emission of CN species in laser-induced plasmas has been investigated. • Distribution of vibrational emission of CN has been found to be time dependent. • Laser irradiance affects the vibrational distribution of the CN molecules. • Plume chemistry controls the excitation mechanisms of CN

Quantitative analysis of manganese concentration in manganese-doped glasses by laser-induced breakdown spectroscopy using a nanosecond ultraviolet Nd:YAG laser

International Nuclear Information System (INIS)

Unnikrishnan, V.K.; Nayak, Rajesh; Kartha, V.B.; Santhosh, C.; Sonavane, M.S.; Yeotikar, R.G.; Gupta, G.P.; Suri, B.M.

2012-01-01

Laser-induced breakdown spectroscopy (LIBS) has been well recognized as a simple, fast and direct analytical technique for the analysis 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. During the last two decades, LIBS has attracted a lot of attention, leading to an ever increasing list of applications, both in laboratory and in industry. In this work, the quantitative analysis of manganese in manganese-doped glass samples in air at atmospheric pressure has been carried out by the LIBS system assembled and optimized in the laboratory. The plasma is generated using a nanosecond ultraviolet Nd:YAG laser with an irradiance of 1x10 9 W/cm 2 on the sample surface. The spatially integrated plasma light emission was collected and imaged on to the spectrograph slit using an optical-fibre-based collection system. An Echelle spectrograph-ICCD system (Andor Mechelle ME5000-DH734-18U-03PS150) was used to record the emission spectrum. The spectrograph with an Echelle grating covers 200-975 nm spectral range in a single shot with a good wavelength resolution (0.05 nm). The detector was gated in synchronization with the laser pulse to get maximum signal-to-background (S/B) ratio. The detector gate width of 2 μs and the detector gate delay of 2 μs were chosen for recording the plasma emission signals, discriminating the continuum radiation which is intense at initial delay time less than 300 ns and decreases at later time

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.

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.

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

A spectrum standardization approach for laser-induced breakdown spectroscopy measurements

Energy Technology Data Exchange (ETDEWEB)

Wang Zhe, E-mail: zhewang@mail.tsinghua.edu.cn; Li Lizhi; West, Logan; Li Zheng, E-mail: lz-dte@tsinghua.edu.cn; Ni Weidou

2012-02-15

This paper follows and completes a previous presentation of a spectrum normalization method for laser-induced breakdown spectroscopy (LIBS) measurements by converting the experimentally recorded line intensity at varying operational conditions to the intensity that would be obtained under a 'standard state' condition, characterized by a standard plasma temperature, electron number density, and total number density of the interested species. At first, for each laser shot and corresponding spectrum, the line intensities of the interested species are converted to the intensity at a fixed plasma temperature and electron number density, but with varying total number density. Under this state, if the influence of changing plasma morphology is neglected, the sum of multiple spectral line intensities for the measured element is proportional to the total number density of the specific element. Therefore, the fluctuation of the total number density, or the variation of ablation mass, can be compensated for by applying the proportional relationship. The application of this method to Cu in 29 brass alloy samples, showed an improvement over the commonly applied normalization method with regard to measurement precision and accuracy. The average relative standard deviation (RSD) value, average value of the error bar, R{sup 2}, root mean square error of prediction (RMSEP), and average value of the maximum relative error were: 5.29%, 0.68%, 0.98, 2.72%, 16.97%, respectively, while the above parameter values for normalization with the whole spectrum area were: 8.61%, 1.37%, 0.95, 3.28%, 29.19%, respectively. - Highlights: Black-Right-Pointing-Pointer Intensity converted into an ideal standard plasma state for uncertainty reduction. Black-Right-Pointing-Pointer Ablated mass fluctuations compensated by variation of sum of multiple intensities. Black-Right-Pointing-Pointer A spectrum standardization model established. Black-Right-Pointing-Pointer Results in both uncertainty

Comparative analysis of automotive paints by laser induced breakdown spectroscopy and nonparametric permutation tests

International Nuclear Information System (INIS)

McIntee, Erin; Viglino, Emilie; Rinke, Caitlin; Kumor, Stephanie; Ni Liqiang; Sigman, Michael E.

2010-01-01

Laser-induced breakdown spectroscopy (LIBS) has been investigated for the discrimination of automobile paint samples. Paint samples from automobiles of different makes, models, and years were collected and separated into sets based on the color, presence or absence of effect pigments and the number of paint layers. Twelve LIBS spectra were obtained for each paint sample, each an average of a five single shot 'drill down' spectra from consecutive laser ablations in the same spot on the sample. Analyses by a nonparametric permutation test and a parametric Wald test were performed to determine the extent of discrimination within each set of paint samples. The discrimination power and Type I error were assessed for each data analysis method. Conversion of the spectral intensity to a log-scale (base 10) resulted in a higher overall discrimination power while observing the same significance level. Working on the log-scale, the nonparametric permutation tests gave an overall 89.83% discrimination power with a size of Type I error being 4.44% at the nominal significance level of 5%. White paint samples, as a group, were the most difficult to differentiate with the power being only 86.56% followed by 95.83% for black paint samples. Parametric analysis of the data set produced lower discrimination (85.17%) with 3.33% Type I errors, which is not recommended for both theoretical and practical considerations. The nonparametric testing method is applicable across many analytical comparisons, with the specific application described here being the pairwise comparison of automotive paint 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

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.

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.

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.

Time-resolved resonance fluorescence spectroscopy for study of chemical reactions in laser-induced plasmas.

Science.gov (United States)

Liu, Lei; Deng, Leimin; Fan, Lisha; Huang, Xi; Lu, Yao; Shen, Xiaokang; Jiang, Lan; Silvain, Jean-François; Lu, Yongfeng

2017-10-30

Identification of chemical intermediates and study of chemical reaction pathways and mechanisms in laser-induced plasmas are important for laser-ablated applications. Laser-induced breakdown spectroscopy (LIBS), as a promising spectroscopic technique, is efficient for elemental analyses but can only provide limited information about chemical products in laser-induced plasmas. In this work, time-resolved resonance fluorescence spectroscopy was studied as a promising tool for the study of chemical reactions in laser-induced plasmas. Resonance fluorescence excitation of diatomic aluminum monoxide (AlO) and triatomic dialuminum monoxide (Al 2 O) was used to identify these chemical intermediates. Time-resolved fluorescence spectra of AlO and Al 2 O were used to observe the temporal evolution in laser-induced Al plasmas and to study their formation in the Al-O 2 chemistry in air.

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.

Influences on the Emissions of Bacterial Plasmas Generated through Nanosecond Laser-Induced Breakdown Spectroscopy

Science.gov (United States)

Malenfant, Dylan J.

In the past decade, laser-induced breakdown spectroscopy has been shown to provide compositional data that can be used for discrimination between bacterial specimens at the strain level. This work demonstrates the viability of this technique in a clinical setting. Studies were conducted to investigate the impact of emissions generated by a nitrocellulose filter paper background on the classification of four species: E. coli, S. epidermidis, M. smegmatis, and P. aeruginosa. Limits of detection were determined as 48+/-12 kCFU per ablation event for new mounting procedures using standard diagnostic laboratory techniques, and a device for centrifuge filtration was designed for sampling from low-titer bacterial suspensions. Plasma emissions from samples grown at biological levels of magnesium, zinc, and glucose were shown not to deviate from controls. A limit of detection for environmental zinc was found to be 11 ppm. Discrimination with heat-killed samples was demonstrated, providing a sterile diagnostic environment.

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

Science.gov (United States)

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.

Evaluation of the laser-induced breakdown spectroscopy technique for determination of the chemical composition of copper concentrates

Science.gov (United States)

Łazarek, Łukasz; Antończak, Arkadiusz J.; Wójcik, Michał R.; Drzymała, Jan; Abramski, Krzysztof M.

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.

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

Science.gov (United States)

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).

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.

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

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.

Exploring laser-induced breakdown spectroscopy for nuclear materials analysis and in-situ applications

Science.gov (United States)

Martin, Madhavi Z.; Allman, Steve; Brice, Deanne J.; Martin, Rodger C.; Andre, Nicolas O.

2012-08-01

Laser-induced breakdown spectroscopy (LIBS) has been used to determine the limits of detection of strontium (Sr) and cesium (Cs), common nuclear fission products. Additionally, detection limits were determined for cerium (Ce), often used as a surrogate for radioactive plutonium in laboratory studies. Results were obtained using a laboratory instrument with a Nd:YAG laser at fundamental wavelength of 1064 nm, frequency doubled to 532 nm with energy of 50 mJ/pulse. The data was compared for different concentrations of Sr and Ce dispersed in a CaCO3 (white) and carbon (black) matrix. We have addressed the sampling errors, limits of detection, reproducibility, and accuracy of measurements as they relate to multivariate analysis in pellets that were doped with the different elements at various concentrations. These results demonstrate that LIBS technique is inherently well suited for in situ analysis of nuclear materials in hot cells. Three key advantages are evident: (1) small samples (mg) can be evaluated; (2) nuclear materials can be analyzed with minimal sample preparation; and (3) samples can be remotely analyzed very rapidly (ms-seconds). Our studies also show that the methods can be made quantitative. Very robust multivariate models have been used to provide quantitative measurement and statistical evaluation of complex materials derived from our previous research on wood and soil samples.

Identification and discrimination of Pseudomonas aeruginosa bacteria grown in blood and bile by laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Rehse, Steven J.; Diedrich, Jonathan; Palchaudhuri, Sunil

2007-01-01

Pseudomonas aeruginosa bacteria colonies have been analyzed by laser-induced breakdown spectroscopy using nanosecond laser pulses. LIBS spectra were obtained after transferring the bacteria from a nutrient-rich culture medium to a nutrient-free agar plate for laser ablation. To study the dependence of the LIBS spectrum on growth and environmental conditions, colonies were cultured on three different nutrient media: a trypticase soy agar (TSA) plate, a blood agar plate, and a medium chosen deliberately to induce bacteria membrane changes, a MacConkey agar plate containing bile salts. Nineteen atomic and ionic emission lines in the LIBS spectrum, which was dominated by inorganic elements such as calcium, magnesium and sodium, were used to identify and classify the bacteria. A discriminant function analysis was used to discriminate between the P. aeruginosa bacteria and two strains of E. coli: a non-pathogenic environmental strain and the pathogenic strain enterohemorrhagic E. coli 0157:H7 (EHEC). Nearly identical spectra were obtained from P. aeruginosa grown on the TSA plate and the blood agar plate, while the bacteria grown on the MacConkey plate exhibited easily distinguishable differences from the other two. All P. aeruginosa samples, independent of initial growth conditions, were readily discriminated from the two E. coli strains

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)

Temporal dependence of the enhancement of material removal in femtosecond-nanosecond dual-pulse laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Scaffidi, Jon; Pearman, William; Carter, J. Chance; Colston, Bill W. Jr.; Angel, S. Michael

2004-01-01

Despite the large neutral atomic and ionic emission enhancements that have been noted in collinear and orthogonal dual-pulse laser-induced breakdown spectroscopy, the source or sources of these significant signal and signal-to-noise ratio improvements have yet to be explained. In the research reported herein, the combination of a femtosecond preablative air spark and a nanosecond ablative pulse yields eightfold and tenfold material removal improvement for brass and aluminum, respectively, but neutral atomic emission is enhanced by only a factor of 3-4. Additionally, temporal correlation between enhancement of material removal and of atomic emission is quite poor, suggesting that the atomic-emission enhancements noted in the femtosecond-nanosecond pulse configuration result in large part from some source other than simple improvement in material removal

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.

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.

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.

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

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.

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.

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.

Spectroscopic analysis of femtosecond laser-induced gas breakdown

International Nuclear Information System (INIS)

Hermann, J.; Bruneau, S.; Sentis, M.

2004-01-01

The plasma generated by the interaction of a femtosecond laser pulse with gas has been analyzed using time- and space-resolved emission spectroscopy. The laser beam has been focused with a microscope objective into different gases (air, Ar, He) at pressures ranging from 10 2 to 10 5 Pa. From the analysis of spectral line emission from ions and neutral atoms, the plasma parameters and the plasma composition have been determined as a function of time and space. Furthermore, the generation of fast electrons and/or VUV radiation by the femtosecond laser interaction with the gas was brought to the fore. From the time- and space-evolution of the plasma parameters, a rough estimation of initial values of electron density and refraction index in the focal volume has been performed. These results are compared to analysis of the laser beam transmitted by the plasma. The latter show that only a small fraction of the laser energy is absorbed by the plasma while the spatial distribution of the transmitted laser beam is strongly perturbed by the plasma, which acts like a defocusing lens. However, in ambient helium, the plasma defocusing is weak due to the high ionization potential of helium. The understanding of femtosecond laser-induced gas breakdown is useful for process optimization in femtosecond laser applications like micromachining or surface microanalysis, etc

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.

Calibration-free quantitative elemental analysis of meteor plasma using reference laser-induced breakdown spectroscopy of meteorite samples

Science.gov (United States)

Ferus, Martin; Koukal, Jakub; Lenža, Libor; Srba, Jiří; Kubelík, Petr; Laitl, Vojtěch; Zanozina, Ekaterina M.; Váňa, Pavel; Kaiserová, Tereza; Knížek, Antonín; Rimmer, Paul; Chatzitheodoridis, Elias; Civiš, Svatopluk

2018-03-01

Aims: We aim to analyse real-time Perseid and Leonid meteor spectra using a novel calibration-free (CF) method, which is usually applied in the laboratory for laser-induced breakdown spectroscopic (LIBS) chemical analysis. Methods: Reference laser ablation spectra of specimens of chondritic meteorites were measured in situ simultaneously with a high-resolution laboratory echelle spectrograph and a spectral camera for meteor observation. Laboratory data were subsequently evaluated via the CF method and compared with real meteor emission spectra. Additionally, spectral features related to airglow plasma were compared with the spectra of laser-induced breakdown and electric discharge in the air. Results: We show that this method can be applied in the evaluation of meteor spectral data observed in real time. Specifically, CF analysis can be used to determine the chemical composition of meteor plasma, which, in the case of the Perseid and Leonid meteors analysed in this study, corresponds to that of the C-group of chondrites.

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.

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.

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 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.

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.

Comparison of brass alloys composition by laser-induced breakdown spectroscopy and self-organizing maps

Energy Technology Data Exchange (ETDEWEB)

Pagnotta, Stefano; Grifoni, Emanuela; Legnaioli, Stefano [Applied and Laser Spectroscopy Laboratory, ICCOM-CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); Lezzerini, Marco [Department of Earth Sciences, University of Pisa, Via S. Maria 53, 56126 Pisa (Italy); Lorenzetti, Giulia [Applied and Laser Spectroscopy Laboratory, ICCOM-CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); Palleschi, Vincenzo, E-mail: vincenzo.palleschi@cnr.it [Applied and Laser Spectroscopy Laboratory, ICCOM-CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); Department of Civilizations and Forms of Knowledge, University of Pisa, Via L. Galvani 1, 56126 Pisa (Italy)

2015-01-01

In this paper we face the problem of assessing similarities in the composition of different metallic alloys, using the laser-induced breakdown spectroscopy technique. The possibility of determining the degree of similarity through the use of artificial neural networks and self-organizing maps is discussed. As an example, we present a case study involving the comparison of two historical brass samples, very similar in their composition. The results of the paper can be extended to many other situations, not necessarily associated with cultural heritage and archeological studies, where objects with similar composition have to be compared. - Highlights: • A method for assessing the similarity of materials analyzed by LIBS is proposed. • Two very similar fragments of historical brass were analyzed. • Using a simple artificial neural network the composition of the two alloys was determined. • The composition of the two brass alloys was the same within the experimental error. • Using self-organizing maps, the probability of the alloys to have the same composition was assessed.

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.

Comparison of brass alloys composition by laser-induced breakdown spectroscopy and self-organizing maps

International Nuclear Information System (INIS)

Pagnotta, Stefano; Grifoni, Emanuela; Legnaioli, Stefano; Lezzerini, Marco; Lorenzetti, Giulia; Palleschi, Vincenzo

2015-01-01

In this paper we face the problem of assessing similarities in the composition of different metallic alloys, using the laser-induced breakdown spectroscopy technique. The possibility of determining the degree of similarity through the use of artificial neural networks and self-organizing maps is discussed. As an example, we present a case study involving the comparison of two historical brass samples, very similar in their composition. The results of the paper can be extended to many other situations, not necessarily associated with cultural heritage and archeological studies, where objects with similar composition have to be compared. - Highlights: • A method for assessing the similarity of materials analyzed by LIBS is proposed. • Two very similar fragments of historical brass were analyzed. • Using a simple artificial neural network the composition of the two alloys was determined. • The composition of the two brass alloys was the same within the experimental error. • Using self-organizing maps, the probability of the alloys to have the same composition was assessed

Wavelength dependence on the forensic analysis of glass by nanosecond 266 nm and 1064 nm laser induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Cahoon, Erica M.; Almirall, Jose R.

2010-05-01

Laser induced breakdown spectroscopy can be used for the chemical characterization of glass to provide evidence of an association between a fragment found at a crime scene to a source of glass of known origin. Two different laser irradiances, 266 nm and 1064 nm, were used to conduct qualitative and quantitative analysis of glass standards. Single-pulse and double-pulse configurations and lens-to-sample-distance settings were optimized to yield the best laser-glass coupling. Laser energy and acquisition timing delays were also optimized to result in the highest signal-to-noise ratio corresponding to the highest precision and accuracy. The crater morphology was examined and the mass removed was calculated for both the 266 nm and 1064 nm irradiations. The analytical figures of merit suggest that the 266 nm and 1064 nm wavelengths are capable of good performance for the forensic chemical characterization of glass. The results presented here suggest that the 266 nm laser produces a better laser-glass matrix coupling, resulting in a better stoichiometric representation of the glass sample. The 266 nm irradiance is therefore recommended for the forensic analysis and comparison of glass samples.

Wavelength dependence on the forensic analysis of glass by nanosecond 266 nm and 1064 nm laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Cahoon, Erica M.; Almirall, Jose R.

2010-01-01

Laser induced breakdown spectroscopy can be used for the chemical characterization of glass to provide evidence of an association between a fragment found at a crime scene to a source of glass of known origin. Two different laser irradiances, 266 nm and 1064 nm, were used to conduct qualitative and quantitative analysis of glass standards. Single-pulse and double-pulse configurations and lens-to-sample-distance settings were optimized to yield the best laser-glass coupling. Laser energy and acquisition timing delays were also optimized to result in the highest signal-to-noise ratio corresponding to the highest precision and accuracy. The crater morphology was examined and the mass removed was calculated for both the 266 nm and 1064 nm irradiations. The analytical figures of merit suggest that the 266 nm and 1064 nm wavelengths are capable of good performance for the forensic chemical characterization of glass. The results presented here suggest that the 266 nm laser produces a better laser-glass matrix coupling, resulting in a better stoichiometric representation of the glass sample. The 266 nm irradiance is therefore recommended for the forensic analysis and comparison of glass samples.

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.

The effect of sequential dual-gas testing on laser-induced breakdown spectroscopy-based discrimination: Application to brass samples and bacterial strains

International Nuclear Information System (INIS)

Rehse, Steven J.; Mohaidat, Qassem I.

2009-01-01

Four Cu-Zn brass alloys with different stoichiometries and compositions have been analyzed by laser-induced breakdown spectroscopy (LIBS) using nanosecond laser pulses. The intensities of 15 emission lines of copper, zinc, lead, carbon, and aluminum (as well as the environmental contaminants sodium and calcium) were normalized and analyzed with a discriminant function analysis (DFA) to rapidly categorize the samples by alloy. The alloys were tested sequentially in two different noble gases (argon and helium) to enhance discrimination between them. When emission intensities from samples tested sequentially in both gases were combined to form a single 30-spectral line 'fingerprint' of the alloy, an overall 100% correct identification was achieved. This was a modest improvement over using emission intensities acquired in argon gas alone. A similar study was performed to demonstrate an enhanced discrimination between two strains of Escherichia coli (a Gram-negative bacterium) and a Gram-positive bacterium. When emission intensities from bacteria sequentially ablated in two different gas environments were combined, the DFA achieved a 100% categorization accuracy. This result showed the benefit of sequentially testing highly similar samples in two different ambient gases to enhance discrimination between the samples.

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.

Sensitive detection of chlorine in iron oxide by single pulse and dual pulse laser-induced breakdown spectroscopy

Science.gov (United States)

Pedarnig, J. D.; Haslinger, M. J.; Bodea, M. A.; Huber, N.; Wolfmeir, H.; Heitz, J.

2014-11-01

The halogen chlorine is hard to detect in laser-induced breakdown spectroscopy (LIBS) mainly due to its high excited state energies of 9.2 and 10.4 eV for the most intense emission lines at 134.72 nm and 837.59 nm, respectively. We report on sensitive detection of Cl in industrial iron oxide Fe2O3 powder by single-pulse (SP) and dual-pulse (DP) LIBS measurements in the near infrared range in air. In compacted powder measured by SP excitation (Nd:YAG laser, 532 nm) Cl was detected with limit of detection LOD = 440 ppm and limit of quantitation LOQ = 720 ppm. Orthogonal DP LIBS was studied on pressed Fe2O3 pellets and Fe3O4 ceramics. The transmission of laser-induced plasma for orthogonal Nd:YAG 1064 nm and ArF 193 nm laser pulses showed a significant dependence on interpulse delay time (ipd) and laser wavelength (λL). The UV pulses (λL = 193 nm) were moderately absorbed in the plasma and the Cl I emission line intensity was enhanced while IR pulses (λL = 1064 nm) were not absorbed and Cl signals were not enhanced at ipd = 3 μs. The UV laser enhancement of Cl signals is attributed to the much higher signal/background ratio for orthogonal DP excitation compared to SP excitation and to the increased plasma temperature and electron number density. This enabled measurement at a very short delay time of td ≥ 0.1 μs with respect to the re-excitation pulse and detection of the very rapidly decaying Cl emission with higher efficiency.

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.

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.

Quantitative Potassium Measurements with Laser-Induced Breakdown Spectroscopy Using Low-Energy Lasers: Application to In Situ K-Ar Geochronology for Planetary Exploration.

Science.gov (United States)

Cho, Yuichiro; Horiuchi, Misa; Shibasaki, Kazuo; Kameda, Shingo; Sugita, Seiji

2017-08-01

In situ radiogenic isotope measurements to obtain the absolute age of geologic events on planets are of great scientific value. In particular, K-Ar isochrons are useful because of their relatively high technical readiness and high accuracy. Because this isochron method involves spot-by-spot K measurements using laser-induced breakdown spectroscopy (LIBS) and simultaneous Ar measurements with mass spectrometry, LIBS measurements are conducted under a high vacuum condition in which emission intensity decreases significantly. Furthermore, using a laser power used in previous planetary missions is preferable to examine the technical feasibility of this approach. However, there have been few LIBS measurements for K under such conditions. In this study, we measured K contents in rock samples using 30 mJ and 15 mJ energy lasers under a vacuum condition (10 -3  Pa) to assess the feasibility of in situ K-Ar dating with lasers comparable to those used in NASA's Curiosity and Mars 2020 missions. We obtained various calibration curves for K using internal normalization with the oxygen line at 777 nm and continuum emission from the laser-induced plasma. Experimental results indicate that when K 2 O laser energy, with a detection limit of 88 ppm and 20% of error at 2400 ppm of K 2 O. Futhermore, the calibration curve based on the K 769 nm line intensity normalized with continuum emission yielded the best result for the 15 mJ laser, giving a detection limit of 140 ppm and 20% error at 3400 ppm K 2 O. Error assessments using obtained calibration models indicate that a 4 Ga rock with 3000 ppm K 2 O would be measured with 8% (30 mJ) and 10% (15 mJ) of precision in age when combined with mass spectrometry of 40 Ar with 10% of uncertainty. These results strongly suggest that high precision in situ isochron K-Ar dating is feasible with a laser used in previous and upcoming Mars rover missions.

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)

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.

Blackbody Emission from Laser Breakdown in High-Pressure Gases

Science.gov (United States)

Bataller, A.; Plateau, G. R.; Kappus, B.; Putterman, S.

2014-08-01

Laser induced breakdown of pressurized gases is used to generate plasmas under conditions where the atomic density and temperature are similar to those found in sonoluminescing bubbles. Calibrated streak spectroscopy reveals that a blackbody persists well after the exciting femtosecond laser pulse has turned off. Deviation from Saha's equation of state and an accompanying large reduction in ionization potential are observed at unexpectedly low atomic densities—in parallel with sonoluminescence. In laser breakdown, energy input proceeds via excitation of electrons whereas in sonoluminescence it is initiated via the atoms. The similar responses indicate that these systems are revealing the thermodynamics and transport of a strongly coupled plasma.

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.

Computational fluid-dynamic model of laser-induced breakdown in air

International Nuclear Information System (INIS)

Dors, Ivan G.; Parigger, Christian G.

2003-01-01

Temperature and pressure profiles are computed by the use of a two-dimensional, axially symmetric, time-accurate computational fluid-dynamic model for nominal 10-ns optical breakdown laser pulses. The computational model includes a kinetics mechanism that implements plasma equilibrium kinetics in ionized regions and nonequilibrium, multistep, finite-rate reactions in nonionized regions. Fluid-physics phenomena following laser-induced breakdown are recorded with high-speed shadowgraph techniques. The predicted fluid phenomena are shown by direct comparison with experimental records to agree with the flow patterns that are characteristic of laser spark decay

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.

Tuning excitation laser wavelength for secondary resonance in low-intensity phase-selective laser-induced breakdown spectroscopy for in-situ analytical measurement of nanoaerosols

Science.gov (United States)

Xiong, Gang; Li, Shuiqing; Tse, Stephen D.

2018-02-01

In recent years, a novel low-intensity phase-selective laser-induced breakdown spectroscopy (PS-LIBS) technique has been developed for unique elemental-composition identification of aerosolized nanoparticles, where only the solid-phase nanoparticles break down, forming nanoplasmas, without any surrounding gas-phase breakdown. Additional work has demonstrated that PS-LIBS emissions can be greatly enhanced with secondary resonant excitation by matching the excitation laser wavelength with an atomic transition line in the formed nanoplasma, thereby achieving low limits of detection. In this work, a tunable dye laser is employed to investigate the effects of excitation wavelength and irradiance on in-situ PS-LIBS measurements of TiO2 nanoaerosols. The enhancement factor by resonant excitation can be 220 times greater than that for non-resonant cases under similar conditions. Moreover, the emitted spectra are unique for the selected resonant transition lines for a given element, suggesting the potential to make precise phase-selective and analyte-selective measurements of nanoparticles in a multicomponent multiphase system. The enhancement factor by resonant excitation is highly sensitive to excitation laser wavelength, with narrow excitation spectral windows, i.e., 0.012 to 0.023 nm (FWHM, full width at half maximum) for Ti (I) neutral atomic lines, and 0.051 to 0.139 nm (FWHM) for Ti (II) single-ionized atomic lines. Boltzmann analysis of the emission intensities, temporal response of emissions, and emission dependence on excitation irradiance are investigated to understand aspects of the generated nanoplasmas such as temperature, local thermodynamic equilibrium (LTE), and excitation mechanism.

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).

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.

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.

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

For laser-induced breakdown spectroscopy (LIBS) quantitative analysis technique, baseline correction is an essential part for the LIBS data preprocessing. As the widely existing cases, the phenomenon of baseline drift is generated by the fluctuation of laser energy, inhomogeneity of sample surfaces and the background noise, which has aroused the interest of many researchers. Most of the prevalent algorithms usually need to preset some key parameters, such as the suitable spline function and the fitting order, thus do not have adaptability. Based on the characteristics of LIBS, such as the sparsity of spectral peaks and the low-pass filtered feature of baseline, a novel baseline correction and spectral data denoising method is studied in this paper. The improved technology utilizes convex optimization scheme to form a non-parametric baseline correction model. Meanwhile, asymmetric punish function is conducted to enhance signal-noise ratio (SNR) of the LIBS signal and improve reconstruction precision. Furthermore, an efficient iterative algorithm is applied to the optimization process, so as to ensure the convergence of this algorithm. To validate the proposed method, the concentration analysis of Chromium (Cr),Manganese (Mn) and Nickel (Ni) contained in 23 certified high alloy steel samples is assessed by using quantitative models with Partial Least Squares (PLS) and Support Vector Machine (SVM). Because there is no prior knowledge of sample composition and mathematical hypothesis, compared with other methods, the method proposed in this paper has better accuracy in quantitative analysis, and fully reflects its adaptive ability.

Minimally invasive non-thermal laser technology using laser-induced optical breakdown for skin rejuvenation

NARCIS (Netherlands)

Habbema, L.; Verhagen, R.; Van Hal, R.; Liu, Y.; Varghese, B.

2011-01-01

We describe a novel, minimally invasive laser technology for skin rejuvenation by creating isolated microscopic lesions within tissue below the epidermis using laser induced optical breakdown. Using an in-house built prototype device, tightly focused near-infrared laser pulses are used to create

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.

Determination of uranium concentration in an ore sample using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Kim, Y.-S.; Han, B.-Y.; Shin, H.S.; Kim, H.D.; Jung, E.C.; Jung, J.H.; Na, S.H.

2012-01-01

Laser-induced breakdown spectroscopy (LIBS) has been recognized as a promising technique for analyzing sensitive nuclear materials such as uranium, plutonium, and curium in a high-radiation environment, especially since the implementation of IAEA (International Atomic Energy Agency) safeguards. The uranium spectra of ore samples were quantitatively analyzed prior to analyzing sensitive materials in the nuclear industry. The purpose of this experiment is to extract quantitative information about the uranium in a uranium ore using a standard addition approach. The uranium ore samples containing different concentrations of U were prepared by mixing raw ore powder with natural uranium oxide powders. Calibration sets of 0.2, 0.4, 0.6, 0.8 and 1.0 wt.% uranium concentrations within the uranium ore sample were achieved. A pulsed and Q-switched Nd:YAG laser at a wavelength of 532 nm was used as a light source. An echelle spectrometer that covers a 190–420 nm wavelength range is used to generate a calibration curve and determine the detection limit of uranium in the ore matrix. The neutral atomic-emission peak at a wavelength of 356.659 nm indicated a detection limit of ∼ 158 ppm for uranium, and the uranium concentration was determined in a raw ore sample that has an unknown quantity of uranium. - Highlights: ► The feasibility of LIBS application to monitor uranium element was carried out. ► The detection limit of U in ore was determined by a standard additional approach. ► Quantitative analyses of U concentration in a natural uranium ore were performed.

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)

Effects of polarization and absorption on laser induced optical breakdown threshold for skin rejuvenation

Science.gov (United States)

Varghese, Babu; Bonito, Valentina; Turco, Simona; Verhagen, Rieko

2016-03-01

Laser induced optical breakdown (LIOB) is a non-linear absorption process leading to plasma formation at locations where the threshold irradiance for breakdown is surpassed. In this paper we experimentally demonstrate the influence of polarization and absorption on laser induced breakdown threshold in transparent, absorbing and scattering phantoms made from water suspensions of polystyrene microspheres. We demonstrate that radially polarized light yields a lower irradiance threshold for creating optical breakdown compared to linearly polarized light. We also demonstrate that the thermal initiation pathway used for generating seed electrons results in a lower irradiance threshold compared to multiphoton initiation pathway used for optical breakdown.

Sampling considerations when analyzing micrometric-sized particles in a liquid jet using laser induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Faye, C.B.; Amodeo, T.; Fréjafon, E. [Institut National de l' Environnement Industriel et des Risques (INERIS/DRC/CARA/NOVA), Parc Technologique Alata, BP 2, 60550 Verneuil-En-Halatte (France); Delepine-Gilon, N. [Institut des Sciences Analytiques, 5 rue de la Doua, 69100 Villeurbanne (France); Dutouquet, C., E-mail: christophe.dutouquet@ineris.fr [Institut National de l' Environnement Industriel et des Risques (INERIS/DRC/CARA/NOVA), Parc Technologique Alata, BP 2, 60550 Verneuil-En-Halatte (France)

2014-01-01

Pollution of water is a matter of concern all over the earth. Particles are known to play an important role in the transportation of pollutants in this medium. In addition, the emergence of new materials such as NOAA (Nano-Objects, their Aggregates and their Agglomerates) emphasizes the need to develop adapted instruments for their detection. Surveillance of pollutants in particulate form in waste waters in industries involved in nanoparticle manufacturing and processing is a telling example of possible applications of such instrumental development. The LIBS (laser-induced breakdown spectroscopy) technique coupled with the liquid jet as sampling mode for suspensions was deemed as a potential candidate for on-line and real time monitoring. With the final aim in view to obtain the best detection limits, the interaction of nanosecond laser pulses with the liquid jet was examined. The evolution of the volume sampled by laser pulses was estimated as a function of the laser energy applying conditional analysis when analyzing a suspension of micrometric-sized particles of borosilicate glass. An estimation of the sampled depth was made. Along with the estimation of the sampled volume, the evolution of the SNR (signal to noise ratio) as a function of the laser energy was investigated as well. Eventually, the laser energy and the corresponding fluence optimizing both the sampling volume and the SNR were determined. The obtained results highlight intrinsic limitations of the liquid jet sampling mode when using 532 nm nanosecond laser pulses with suspensions. - Highlights: • Micrometric-sized particles in suspensions are analyzed using LIBS and a liquid jet. • The evolution of the sampling volume is estimated as a function of laser energy. • The sampling volume happens to saturate beyond a certain laser fluence. • Its value was found much lower than the beam diameter times the jet thickness. • Particles proved not to be entirely vaporized.

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.

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

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.

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

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)

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

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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.

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

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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.

Analysis of explosive and other organic residues by laser induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Lazic, V., E-mail: lazic@frascati.enea.i [ENEA, FIS-LAS, Via. E. Fermi 45, 00044 Frascati (RM) (Italy); Palucci, A. [ENEA, FIS-LAS, Via. E. Fermi 45, 00044 Frascati (RM) (Italy); Jovicevic, S. [Institute of Physics, 11080 Belgrade, Pregrevica 118 (Serbia); Poggi, C.; Buono, E. [ENEA, FIS-LAS, Via. E. Fermi 45, 00044 Frascati (RM) (Italy)

2009-10-15

With the aim of realizing a compact instrument for detection of energetic materials at trace levels, laser induced breakdown spectroscopy was applied on residues from nine explosives in air surroundings. Different potentially interfering organic materials were also analyzed. The residues were not uniformly distributed on an aluminum support and single-shot discrimination was attempted. For a single residue type, large shot-to-shot fluctuations of the line intensity ratios characteristic for organic samples were observed, which made material classification difficult. It was found that both atomic and molecular emission intensities, as well as their ratios, are strongly affected by an amount of the ablated support material, which mainly determines the plasma temperature. With respect to the spectra from the clean support, emission intensities of atomic oxygen and nitrogen are always reduced in the presence of an organic material, even if its molecules contain these elements. This was attributed to chemical reactions in a plasma containing carbon or its fragments. Hydrogen atomic emission depends strongly on the local humidity above the sampled point and its line intensity shows shot to shot variations up to 50%, also on a homogeneous sample. It is argued that shock waves generated by previous spatially and/or temporally close laser pulses blow away a relatively heavy water aerosol, which later diffuses slowly back towards the sampled point. C{sub 2} and CN exhibit a peak emission behavior with atomic Al emission, and their variable ratio indicates an existence of different formation or removal mechanisms from the plasma, depending on the plasma parameters and on the composition of the organic residue. On the basis of these observations, an attempt is made to establish a suitable procedure for data analysis and to determine the optimal experimental conditions, which would allow for discrimination of explosives from other, potentially interfering, residues.

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

Quantitative measurement of Au and Fe in ferromagnetic nanoparticles with Laser Induced Breakdown Spectroscopy using a polymer-based gel matrix

International Nuclear Information System (INIS)

Borowik, T.; Przybyło, M.; Pala, K.; Otlewski, J.; Langner, M.

2011-01-01

The medical applications of nanomaterials require substantial changes in the research and development stage, such as the introduction of new processes and methods, and adequate modifications of the national and international laws on the medical product registration. To accomplish this, proper parameterizations of nano-scaled products need to be developed and implemented, accompanied by suitable measuring methods. The introduction of metallic particles to medical practices requires the precise, quantitative evaluation of the production process and later quantification and characterization of the nanoparticles in biological matrices for the bioavailability and biodistribution evaluation. In order to address these issues we propose a method for the quantitative analysis of the metallic nanoparticles composition by Laser Induced Breakdown Spectroscopy (LIBS). Au/Fe ferro-magnetic nanoparticles were used to evaluate the method applicability. Since the powder form of nanoparticles spatters upon laser ablation, first we had to develop fast, convenient and quantitative method for the nano-powdered sample preparation. The proposed method is based on the polymer gelation of nanopowders or their water suspensions. It has been shown that nanopowders compositional changes throughout the production process, along with their final characterization, can be reliable performed with LIBS technique. The quantitative values obtained were successfully correlated with those derived with ICP technique. - Highlights: ► The atomic composition of nanoparticles was analyzed with LIBS. ► The amount of gold on ferromagnetic particles was quantified by the method. ► Gel fixation was used as new way of handling powdered samples. ► LIBS results are comparable with other equivalent methods (ICP). ► There was a difference between measured and assumed nanoparticle composition.

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.

Quantitative analysis of lead in aqueous solutions by ultrasonic nebulizer assisted laser induced breakdown spectroscopy

Science.gov (United States)

Zhong, Shi-Lei; Lu, Yuan; Kong, Wei-Jin; Cheng, Kai; Zheng, Ronger

2016-08-01

In this study, an ultrasonic nebulizer unit was established to improve the quantitative analysis ability of laser-induced breakdown spectroscopy (LIBS) for liquid samples detection, using solutions of the heavy metal element Pb as an example. An analytical procedure was designed to guarantee the stability and repeatability of the LIBS signal. A series of experiments were carried out strictly according to the procedure. The experimental parameters were optimized based on studies of the pulse energy influence and temporal evolution of the emission features. The plasma temperature and electron density were calculated to confirm the LTE state of the plasma. Normalizing the intensities by background was demonstrated to be an appropriate method in this work. The linear range of this system for Pb analysis was confirmed over a concentration range of 0-4,150ppm by measuring 12 samples with different concentrations. The correlation coefficient of the fitted calibration curve was as high as 99.94% in the linear range, and the LOD of Pb was confirmed as 2.93ppm. Concentration prediction experiments were performed on a further six samples. The excellent quantitative ability of the system was demonstrated by comparison of the real and predicted concentrations of the samples. The lowest relative error was 0.043% and the highest was no more than 7.1%.

Advanced signal processing analysis of laser-induced breakdown spectroscopy data for the discrimination of obsidian sources.

Science.gov (United States)

Remus, Jeremiah J; Harmon, Russell S; Hark, Richard R; Haverstock, Gregory; Baron, Dirk; Potter, Ian K; Bristol, Samantha K; East, Lucille J

2012-03-01

Obsidian is a natural glass of volcanic origin and a primary resource used by indigenous peoples across North America for making tools. Geochemical studies of obsidian enhance understanding of artifact production and procurement and remain a priority activity within the archaeological community. Laser-induced breakdown spectroscopy (LIBS) is an analytical technique being examined as a means for identifying obsidian from different sources on the basis of its 'geochemical fingerprint'. This study tested whether two major California obsidian centers could be distinguished from other obsidian localities and the extent to which subsources could be recognized within each of these centers. LIBS data sets were collected in two different spectral bands (350±130 nm and 690±115 nm) using a Nd:YAG 1064 nm laser operated at ~23 mJ, a Czerny-Turner spectrograph with 0.2-0.3 nm spectral resolution and a high performance imaging charge couple device (ICCD) detector. Classification of the samples was performed using partial least-squares discriminant analysis (PLSDA), a common chemometric technique for performing statistical regression on high-dimensional data. Discrimination of samples from the Coso Volcanic Field, Bodie Hills, and other major obsidian areas in north-central California was possible with an accuracy of greater than 90% using either spectral band. © 2012 Optical Society of America

Discrimination of paper and print types based on their laser induced breakdown spectra

International Nuclear Information System (INIS)

Metzinger, Anikó; Rajkó, Róbert; Galbács, Gábor

2014-01-01

In the present work, the analytical potential of laser induced breakdown spectroscopy (LIBS) for the discrimination of paper types and prints made by digital printers on these papers was assessed. Six different paper types (including standard office papers, color paper and non-bleached paper), and eight printers (including laser and inkjet, as well as color and black printers) were included in the study. Only one or two laser shots were delivered to each sample in order to cause minimal sample destruction and provide maximum spatial resolution. The statistical evaluation of LIBS spectra was performed by multiple methods including three comparative functions (linear correlation, sum of squared deviations and overlapping integral) as well as two advanced statistical methods (multivariate curve resolution alternating least squares (MCR-ALS) combined with classification tree and discriminant analysis (DA)). The best classification results were obtained with the newly introduced MCR-ALS/DA approach, which proved to be 96.3% accurate in the identification of the paper type and 83.3% accurate in the identification of the printer type, based on the LIBS spectrum collected from just a single laser shot to the sample. It was found that the UV part of the LIBS spectrum can be used most efficiently for the discrimination. - Highlights: • The potential of LIBS for the discrimination of paper and print types was assessed. • Six paper types and eight printers (a total of 54 samples) were included in the study. • Data evaluation was done using 3 comparative and 2 multivariate statistical methods. • The MCR-ALS/DA approach, when applied to UV LIBS data, gave best results. • Only one or two LIBS shots are needed for sample discrimination/identification

Discrimination of paper and print types based on their laser induced breakdown spectra

Energy Technology Data Exchange (ETDEWEB)

Metzinger, Anikó [Department of Inorganic and Analytical Chemistry, University of Szeged, Dóm tér 7, 6720 Szeged (Hungary); Rajkó, Róbert [Department of Process Engineering, University of Szeged, P.O. Box 433, 6701 Szeged (Hungary); Galbács, Gábor, E-mail: galbx@chem.u-szeged.hu [Department of Inorganic and Analytical Chemistry, University of Szeged, Dóm tér 7, 6720 Szeged (Hungary)

2014-04-01

In the present work, the analytical potential of laser induced breakdown spectroscopy (LIBS) for the discrimination of paper types and prints made by digital printers on these papers was assessed. Six different paper types (including standard office papers, color paper and non-bleached paper), and eight printers (including laser and inkjet, as well as color and black printers) were included in the study. Only one or two laser shots were delivered to each sample in order to cause minimal sample destruction and provide maximum spatial resolution. The statistical evaluation of LIBS spectra was performed by multiple methods including three comparative functions (linear correlation, sum of squared deviations and overlapping integral) as well as two advanced statistical methods (multivariate curve resolution alternating least squares (MCR-ALS) combined with classification tree and discriminant analysis (DA)). The best classification results were obtained with the newly introduced MCR-ALS/DA approach, which proved to be 96.3% accurate in the identification of the paper type and 83.3% accurate in the identification of the printer type, based on the LIBS spectrum collected from just a single laser shot to the sample. It was found that the UV part of the LIBS spectrum can be used most efficiently for the discrimination. - Highlights: • The potential of LIBS for the discrimination of paper and print types was assessed. • Six paper types and eight printers (a total of 54 samples) were included in the study. • Data evaluation was done using 3 comparative and 2 multivariate statistical methods. • The MCR-ALS/DA approach, when applied to UV LIBS data, gave best results. • Only one or two LIBS shots are needed for sample discrimination/identification.

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

Science.gov (United States)

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.

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

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.

Spectroscopic analysis of high protein nigella seeds (Kalonji) using laser-induced breakdown spectroscopy and inductively coupled plasma/optical emission spectroscopy