Comparative study of calibration-free laser-induced breakdown spectroscopy methods for quantitative elemental analysis of quartz-bearing limestone

Fahad, Muhammad; Farooq, Zahid; Abrar, M.

doi:10.1364/ao.58.003501

Cited by 22 publications

(9 citation statements)

References 35 publications

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“…In this scenario, the CF-LIBS method appears to be a suitable and effective alternative to the calibration method. In some previous studies, the CF-LIBS method was utilized for measurement of elemental composition of geological samples such as limestone, granite, malachite, and nephrite, and results were compared with standard techniques such as energy dispersive X-ray spectroscopy (EDX), X-ray fluorescence (XRF), and laser ablation-time of flight-mass spectrometer (LA-TOF-MS) [24][25][26]44,45]. In all of these studies, quantitative results obtained with CF-LIBS showed reasonable agreement with the standard analytical techniques.…”

Section: Discussionmentioning

confidence: 99%

“…However, sulfur (S) was not identified in the spectrum, which was not surprising because of the spectral limitation of the detection system. Most of the intense lines of S lie in vacuum ultraviolet (VUV) region, 10-200 nm and these lines fall outside the spectral range of spectrometer used in this study [24]. Iron is known for its busy spectrum, having…”

Section: Qualitative Analysismentioning

confidence: 96%

“…Previously, the CF-LIBS technique had been adopted for compositional analysis of meteorites and other extraterrestrial objects [22,23]. The quantitative analysis of quartz-bearing limestone using the CF-LIBS technique has been previously reported [24].…”

Section: Introductionmentioning

confidence: 99%

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Compositional Analysis of Chalcopyrite Using Calibration-Free Laser-Induced Breakdown Spectroscopy

et al. 2020

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This article presents elemental analysis of an economically important mineral (chalcopyrite) of local origin. Calibration-free laser-induced breakdown spectroscopy (CF-LIBS) methodology based on the assumption of optically thin plasma and local thermodynamic equilibrium was employed for quantitative analysis. Plasma on the surface of the chalcopyrite target was generated by an Nd:YAG laser beam of wavelength 532 nm, pulse width 5 ns, and operated at repetition rate of 10 Hz. A LIBS2000+ detection system, comprised of five spectrometers, covering the spectral range from 200–720 nm, was used to record the signal of the optical emission from the chalcopyrite plasma. Recorded optical spectrum revealed the presence of Cu and Fe as the major elements while Ca and Na were recognized as the minor elements in the target sample. Quantitative analysis has shown that the relative concentrations of Cu, Fe, and Ca in the sample under study were 58.9%, 40.2%, and 0.9% by weight respectively. However, Na was not quantified due to the unavailability of suitable spectral lines, required for CF-LIBS analysis. Results obtained by CF-LIBS were validated by X-ray fluorescence (XRF) analysis, which showed the presence of five compositional elements viz. Cu, Fe, Si, Se and Ag with weight percentages of 58.1%, 35.4%, 5.7%, 0.7%, and 0.1% respectively. These results endorse the effectiveness of the CF-LIBS technique for quantitative analysis of major elements, however, its usefulness in case of minor and trace elements needs further improvement.

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Section: Discussionmentioning

confidence: 99%

Section: Qualitative Analysismentioning

confidence: 96%

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Compositional Analysis of Chalcopyrite Using Calibration-Free Laser-Induced Breakdown Spectroscopy

et al. 2020

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“…Quantitative LIBS analysis can be performed using calibration curves derived from analysis of certified reference materials. However, the disadvantage of this technique is that reference samples should be matrix-matched, and references materials with a composition similar to unknown samples are not always available e.g., complex rocks having several mineralogical phases in a variety of concentrations [33]. Multivariate algorithms that make use of the information contained in the entire spectrum can also be applied to derive accurate geochemical compositions from geological materials [34,35].…”

Section: Broader Implicationsmentioning

confidence: 99%

Integrated Laser-Induced Breakdown Spectroscopy (LIBS) and Multivariate Wavelet Tessellation: A New, Rapid Approach for Lithogeochemical Analysis and Interpretation

et al. 2021

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This paper demonstrates a novel approach that uses wavelet tessellation in rapid analysis of raw geochemical data produced by laser-induced breakdown spectroscopy (LIBS) to produce pseudologs that are representative of stratigraphy. Single-line LIBS spectral data for seven major rock-forming elements (Al, Ca, Fe, Mg, Si, Na and K) were collected from a synthetic 22-sample rock-block comprising two distinct lithological groups based on mineralogy, chemistry and texture: plutonic rocks and marble. Seven sublithologies are identified within the rock-block from traditional laboratory whole-rock geochemical analysis: marble, Mg-marble, granite, quartz monzonite, foidolite, granodiorite and gabbroic diorite. Two-domain clustering (k = 2) on raw spectral LIBS data combined with wavelet tessellation was applied to generate a simplified lithological stratigraphy of marble and plutonic rocks and generate a pseudolog identical to the rock-block stratigraphy. A pseudolog generated from seven-domain clustering (k = 7) and wavelet tessellation successfully discriminated most sublithologies within the rock-block slabs, especially marble slabs. Small-scale units were identified within the more mineralogically and geochemically complex plutonic slabs. The spatial resolution of the LIBS analysis, with a measurement spacing of ~0.35 mm, allowed for assessment of individual mineral compositions and rock textures, and small-scale units within the plutonic rocks can be correlated to specific coarse-grained minerals or mineralogical associations. The application of the wavelet tessellation method to raw LIBS geochemical data offers the possibility of rapid and objective lithogeochemical analysis and interpretations which can predate further analysis (quantitative) and supplement geological logging.

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“…The calibration method requires calibration curves for all the compositional elements of a sample and comparison with the optical emission spectrum of the corresponding element [ 20 , 21 ]. The use of this method in quantitative analysis of multi-elemental geological samples is limited by the lengthy and tedious procedure and the error caused by the matrix effect [ 22 , 23 ], whereas the calibration-free method involves the measurement of elemental concentration of elements in a sample by theoretical calculations using values of the plasma parameters [ 24 , 25 ]. This methodology is preferred over the calibration method because it eliminates the matrix effect and requires no reference sample.…”

Section: Introductionmentioning

confidence: 99%

Detection and Quantification of Precious Elements in Astrophyllite Mineral by Optical Spectroscopy

et al. 2021

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With many advantages over well-established methods, laser induced breakdown spectroscopy (LIBS) has emerged as a useful analytical technique for the compositional analysis of multi-elemental geological materials. In this study, LIBS was employed for qualitative and quantitative analysis of a rare mineral, astrophyllite, bearing precious elements of industrial and technological interest. The experiment was carried out using second harmonic generation of Nd:YAG laser of pulse width 5 ns and repetition rate of 10 Hz. Microplasma was produced by focusing laser beam on an astrophyllite target, and optical emissions from the generated plasma were recorded in the spectral range of 200–720 nm with the help of a LIBS2000+ detection system. On analyzing the optical spectra, existence of 15 elements in astrophyllite target were revealed. These elements include: Ti, W, Ag, Al, Ba, Ca, Cr, Cu, Fe, Li, Mg, Na, Ni, Si and H. For quantification, calibration-free method was used. Only ten elements, namely Ti, W, Fe, Cr, Cu, Ca, Mg, Ni, Si and Al, were quantified with relative weight concentrations of 55.39%, 18.79%, 18.30%, 4.05%, 2.66, 0.43%, 0.18%, 0.12%, 0.06% and 0.02%, respectively. To benchmark these results, XRF analysis was performed, which confirmed the presence of all the elements detected in the optical spectrum of the sample, except for Na, Li, and H. The concentrations of these ten elements as measured by XRF were in reasonable agreement, especially for the major elements. The presence of a significant amount of Ti and W in an astrophyllite sample, found in Pakistan, highlights the economic value of this mineral. This study may be of further interest in commissioning LIBS technology for exploration of minerals in the region.

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Comparative study of calibration-free laser-induced breakdown spectroscopy methods for quantitative elemental analysis of quartz-bearing limestone

Cited by 22 publications

References 35 publications

Compositional Analysis of Chalcopyrite Using Calibration-Free Laser-Induced Breakdown Spectroscopy

Compositional Analysis of Chalcopyrite Using Calibration-Free Laser-Induced Breakdown Spectroscopy

Integrated Laser-Induced Breakdown Spectroscopy (LIBS) and Multivariate Wavelet Tessellation: A New, Rapid Approach for Lithogeochemical Analysis and Interpretation

Detection and Quantification of Precious Elements in Astrophyllite Mineral by Optical Spectroscopy

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