/pdf/good-practices-in-libs-analysis-review-and-advices-3v4xent5r7.pdf

Good practices in LIBS analysis: Review and advices

Laser-induced breakdown spectroscopy (LIBS) is an elemental analysis technique that is based on the measurement of atomic emissions generated on a sample surface by a laser-induced microplasma. Although often recognized in the literature as a well-established analytical technique, LIBS remains untested relative to the quantitative analysis of elements in chemically complex matrices, such as soils. The objective of this study was to evaluate the capabilities of LIBS relative to the elemental characterization of surface soils. Approximately 65 surface soil samples from the Pond Creek watershed in east Tennessee were collected and subjected to total dissolution and elemental analysis by inductively coupled argon plasma-optical emission spectroscopy (ICP-OES). The samples were analyzed by LIBS using a Nd:YAG laser at 532 nm, with a beam energy of 25 mJ per pulse, a pulse width of 5 ns, and a repetition rate of 10 Hz. The wavelength range for the LIBS spectra collection was 200 to 600 nm, with a resolution of 0.03 nm. Elemental spectral lines were identified through the analysis of analytical reagent-grade chemicals and the NIST and Kurucz spectral databases. The elements that dominated the LIBS spectra were Al, Ca, Fe, and Mg. In addition, emission lines for Ti, Ba, Na, Cu, and Mn were isolated. The emission lines of Cr, Ni, and Zn, which were > 100 mg kg -1 in numerous soil samples, were not detected. Further, spectral emission lines for P and K are >600 nm, eliminating them from LIBS analysis. The integrated peak areas of interference-free elemental emission lines were determined, then normalized to the area of the 288.16 nm Si(I) emission (internal standard) to reduce the variability between replicate analyses. The normalized spectral areas, coupled with linear regression (standard curves for single wavelength response) and multivariate techniques (chemometrics and multiple wavelengths), were used to predict ICP-OES elemental data. In general, the quantitative capabilities of LIBS proved disappointing. Detection and quantitation were generally restricted to those elements with concentrations > 0.5 g kg -1 The correlation between LIBS response and elemental content was poor (r < 0.98). Further, the relative errors of prediction for the LIBS-detected elements were less than acceptable for an analytical technique (<20%), ranging from ∼20 to ∼40% using linear regression analysis, and from 18 to 48% using partial least squares analysis. Based on these findings, the analytical capability of the LIBS method for soil metals analysis should be considered questionable.

Soil Metals Analysis Using Laser-Induced Breakdown Spectroscopy (LIBS)

/pdf/application-of-a-series-of-artificial-neural-networks-to-on-3rehxszat7.pdf

Application of a series of artificial neural networks to on-site quantitative analysis of lead into real soil samples by laser induced breakdown spectroscopy

Laser-induced breakdown spectroscopy (LIBS) has been used as a remote sensing system to analyze seawater samples and to identify their salinities without ordinary calibration curves. The plasma is generated by focusing a pulsed Nd:Y AG laser on the seawater surface in air at atmospheric pressure. Such plasma emission spectrum was collected using wide band fused-silica optical fiber of one-meter length connected to a portable Echelle spectrometer (Mechelle 7500 – Multichannel Instruments, Stockholm, Sweden) with intensified CCD camera. Spectroscopic analysis of plasma evolution of laser produced plasmas has been characterized in terms of their spectra, electron density and electron temperature assuming the local thermodynamic equilibrium (LTE) and optically thin plasma conditions. Three elements Na, Ca and Mg were determined in the obtained spectra to identify the salinity of seawater samples. The electron temperature Te and density Ne were determined using the emission intensity and Stark broadening. The obtained values of Te and Ne for natural seawater sample (salinity 3.753%) are 11580 K ± 0.35% and 3.33×10 18 cm –3 ± 14.3%. These values exhibit a significant change only if the matrix changes (i.e., the salinity changes). On the other hand, no significant difference was obtained if Te and Ne were determined using any of the three elements (Na, Ca and Mg) in the same matrix. It is concluded that Te and Ne represent a fingerprint plasma characterization for a given seawater sample and its salinity could be identified using only one element without need to analyze the rest of elements in the seawater matrix. The obtained results indicate that it is possible to improve the exploitation of LIBS in the remote on-line environmental monitoring, by following up only a single element as a marker to identify the seawater matrix composition and salinity without need to analyze that matrix which saves a lot of time and efforts.

Calibration free laser-induced breakdown spectroscopy (LIBS) identification of seawater salinity

Accuracies of lithium, boron, carbon, and sulfur quantification in geological samples with laser-induced breakdown spectroscopy in Mars, Earth, and vacuum conditions

Laser-induced breakdown spectroscopy (LIBS) has been applied to perform a study of the matrix effect on the plasma characterization of soil sediment targets. The plasma is generated by focusing a pulsed Nd: YAG laser on the target in air at atmospheric pressure. The plasma emission spectrum was detected using a portable Echelle spectrometer (Mechelle 7500 — Multichannel Instruments, Stockholm, Sweden) with intensified CCD camera. Spectroscopic analysis of plasma evolution of laser produced plasmas has been characterized in terms of their spectra, and electron temperature. Four heavy elements V, Pb, Mn and Co were determined in the obtained spectra. The LTE and optically thin plasma conditions were verified for the produced plasma. The electron temperature and density were determined using the emission intensity and stark broadening, respectively, of the spectral lines of the heavy elements in the soil sediments. The electron temperature does not change with concentration. For environmental applications, the obtained results showed the capability of the proposed LIBS setup with the portable Mechelle 7500 spectrometer to be applied in-situ for real-time measurements of the variation of the matrix elemental composition of soil sediments by following up only a single element as a marker for the composition of the soil sediment without need of analysis of the other elements.

Study of the Matrix Effect on the Plasma Characterization of Heavy Elements in Soil Sediments

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Study of the Matrix Effect on the Plasma Characterization of Heavy Elements in Soil Sediments