Laser induced breakdown spectroscopy (LIBS) is a valuable technique for performing qualitative and quantitative chemical analyses of all elements in one shot, including low atomic number elements such as Li and Be. This technique does not require any sample preparation to reveal the atomic species, even when present in trace amounts (< 0.01% m/m ). In this study, for the first time, we provide an accurate mineral formula for a Cs‐rich red beryl by combining crystallographic data obtained using the traditional single‐crystal X‐ray diffraction technique and quantitative chemical analysis data obtained with an innovative "standardless" method: Calibration Free‐LIBS (CF‐LIBS). In particular, a new LIBS prototype coupled with a petrographic microscope (CF‐μLIBS) was used to analyse chemically homogeneous areas of about 10 μm spot size, causing minimal damage to the mineral. The results showed that calibration‐free quantitative analysis is suitable for the quantification of major and minor low and high atomic number elements in beryl. The accuracy of quantification of low atomic number elements by CF‐μLIBS led to the empirical formula: [12](Cs0.006Na0.019K0.017Ca0.019)Σ0.061 [4](Be2.989Li0.011)Σ3.000 [6](Ti0.053Mn0.051Mg0.007Al1.890)Σ2.000 [4](Be0.116Fe0.024Si5.860)Σ6.000 O18. This formula is consistent with the crystal‐structure refinement data and demonstrates the validity of CF‐μLIBS for chemical analyses of minerals containing low atomic number elements.

Crystal Chemical Characterisation of Red Beryl by "Standardless" Laser Induced Breakdown Spectroscopy and Single Crystal Refinement by X‐Ray Diffraction: An Example of Validation of an Innovative Method for the Chemical Analyses of Minerals

Tempesta, Gioacchino
;
Agrosì, Giovanna
2020-01-01

Abstract

Laser induced breakdown spectroscopy (LIBS) is a valuable technique for performing qualitative and quantitative chemical analyses of all elements in one shot, including low atomic number elements such as Li and Be. This technique does not require any sample preparation to reveal the atomic species, even when present in trace amounts (< 0.01% m/m ). In this study, for the first time, we provide an accurate mineral formula for a Cs‐rich red beryl by combining crystallographic data obtained using the traditional single‐crystal X‐ray diffraction technique and quantitative chemical analysis data obtained with an innovative "standardless" method: Calibration Free‐LIBS (CF‐LIBS). In particular, a new LIBS prototype coupled with a petrographic microscope (CF‐μLIBS) was used to analyse chemically homogeneous areas of about 10 μm spot size, causing minimal damage to the mineral. The results showed that calibration‐free quantitative analysis is suitable for the quantification of major and minor low and high atomic number elements in beryl. The accuracy of quantification of low atomic number elements by CF‐μLIBS led to the empirical formula: [12](Cs0.006Na0.019K0.017Ca0.019)Σ0.061 [4](Be2.989Li0.011)Σ3.000 [6](Ti0.053Mn0.051Mg0.007Al1.890)Σ2.000 [4](Be0.116Fe0.024Si5.860)Σ6.000 O18. This formula is consistent with the crystal‐structure refinement data and demonstrates the validity of CF‐μLIBS for chemical analyses of minerals containing low atomic number elements.
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11586/303517
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