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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 Analysis of Minerals
Geostandards and Geoanalytical Research ( IF 3.8 ) Pub Date : 2020-06-02 , DOI: 10.1111/ggr.12346
Gioacchino Tempesta 1 , Ferdinando Bosi 2 , Giovanna Agrosì 1
Affiliation  

Laser‐induced breakdown spectroscopy (LIBS) is a valuable technique for performing qualitative and quantitative chemical determinations 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 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.

中文翻译:

“无标”激光诱导击穿光谱和X射线衍射单晶精制法对红绿柱石的晶体化学表征:矿物化学分析创新方法的验证实例

激光诱导击穿光谱法(LIBS)是一项有价值的技术,可以对一次注射中的所有元素进行定性和定量化学测定,包括低原子序数元素(例如Li和Be)。即使存在痕量(<0.01%m / m),该技术也不需要任何样品制备即可揭示原子种类。)。在这项研究中,我们首次结合了使用传统的单晶X射线衍射技术获得的晶体学数据和通过创新的“无标准”方法获得的定量化学数据,为富含Cs的红色绿柱石提供了准确的矿物配方。 :免校准LIBS(CF-LIBS)。特别是,新的LIBS原型与岩相显微镜(CF-μLIBS)结合使用,可分析斑点大小约为10μm的化学均质区域,对矿物的损害最小。结果表明,无需校准的定量分析适用于对绿柱石中主要和次要的低和高原子序数元素进行定量。CF‐LILIBS定量低原子序数元素的准确性得出了经验公式:[12](Cs 0.006Na 0.019 K 0.017 Ca 0.019Σ0.061 [4](Be 2.989 Li 0.011Σ3.000 [6](Ti 0.053 Mn 0.051 Mg 0.007 Al 1.890Σ2.000 [4](Be 0.116 Fe 0.024 Si 5.860Σ6 .000 O 18.该公式与晶体结构的精炼数据一致,证明了CF-μLIBS在化学分析含低原子序数元素的矿物中的有效性。
更新日期:2020-06-02
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