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Analysis of Cuban nickeliferous minerals by laser-induced breakdown spectroscopy (LIBS): non-conventional sample preparation of powder samples
Analytical Methods ( IF 3.1 ) Pub Date : 2018-01-04 00:00:00 , DOI: 10.1039/c7ay02521a
Marco Aurelio Sperança 1, 2, 3, 4 , Mario Siméon Pomares-Alfonso 5, 6, 7, 8 , Edenir Rodrigues Pereira-Filho 1, 2, 3, 4
Affiliation  

In the present study, a new method to quantify Al, Cr, Fe, Mg, Mn, and Ni in nickeliferous minerals by laser-induced breakdown spectroscopy (LIBS) is proposed. Thirty-three mineral powder solid samples, previously analyzed by inductively coupled plasma optical emission spectroscopy (ICP OES), and two certified reference materials were used as reference samples for the calibration, and an innovative sample preparation was implemented and described. The use of Bi, Sc and Y as internal standards and the usefulness of other normalization modes were assessed in the normalization of the LIBS emission signals from the analytes. A slurry was made by mixing the solid mineral samples, grinding them into a fine powder, and using water in different proportions. Then, the mixture was homogenized and instantly weighed with a constant mass of a standard liquid solution of Y, which was preliminarily chosen as the internal standard among the three elements assessed, and a 10% (w v−1)-polyvinyl-alcohol solution. After 2 h in an oven at 50 °C, the samples, which were immobilized in the polymer film, were subjected to LIBS analysis. The best sample dilution, emission line and normalization of the emission signal were selected for each analyte. The concentrations of the assessed analytes varied from 0.49 to 26.82% for Al, 0.40 to 2.21% for Cr, 6.8 to 52.93% for Fe, 0.41 to 20.53% for Mg, 0.11 to 1.50% for Mn and 0.23 to 3.02% for Ni. The standard error of validation (SEV) for the newly developed method was 1.34, 0.16, 6.08, 0.88, 0.09, and 0.35% for Al, Cr, Fe, Mg, Mn, and Ni, respectively.

中文翻译:

激光诱导击穿光谱法(LIBS)分析古巴含镍矿物:粉末样品的非常规样品制备

在本研究中,提出了一种通过激光诱导击穿光谱法(LIBS)量化含镍矿物中Al,Cr,Fe,Mg,Mn和Ni的新方法。先前通过电感耦合等离子体发射光谱法(ICP OES)分析的33种矿物粉末固体样品和两种认证的参考材料用作校准参考样品,并实施和描述了一种创新的样品制备方法。在分析物的LIBS发射信号的归一化中,评估了Bi,Sc和Y作为内标物的使用以及其他归一化模式的有用性。通过混合固体矿物样品,将它们研磨成细粉并使用不同比例的水来制得浆料。然后,-1)-聚乙烯醇溶液。在50°C的烤箱中2小时后,将固定在聚合物膜中的样品进行LIBS分析。为每种分析物选择最佳的样品稀释度,发射谱线和发射信号的归一化。被测分析物的浓度范围为:Al为0.49至26.82%,Cr为0.40至2.21%,Fe为6.8至52.93%,Mg为0.41至20.53%,Mn为0.11至1.50%,Ni为0.23至3.02%。对于新开发的方法,Al,Cr,Fe,Mg,Mn和Ni的标准验证标准误差(SEV)分别为1.34、0.16、6.08、0.88、0.09和0.35%。
更新日期:2018-01-04
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