Haider Markus M, Hartinger Ingrid, Göschl Karin, Demmelmair Andreas
Zentrale Analytik, Wacker Chemie, Johannes Hess Str. 24, Burghausen D84480, Germany.
Appl Spectrosc. 2004 Jun;58(6):679-82. doi: 10.1366/000370204872935.
The silanol concentration of quartz was determined by mixing 50 mg ground silica sample with 500 mg KBr followed by diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy and chemometric data analysis. Reference samples were prepared by blending ground quartz of different silanol content. Good correlation was achieved between 10 and 240 ppm Si-OH by mass. The chemometric model's quality is characterized by a correlation coefficient of 0.965 (cross-validation) using five latent variables (factors) and a root mean square error of calibration (RMSEC) of 7 ppm. Chemometric data is compared to results from univariate data analysis. The biggest impact on the reproducibility is due to sample preparation (grinding and blending), which is dependant on the operator involved.
通过将50毫克磨碎的石英样品与500毫克溴化钾混合，然后进行漫反射红外傅里叶变换（DRIFT）光谱分析和化学计量数据分析，测定了石英的硅醇浓度。通过混合不同硅醇含量的磨碎石英制备参考样品。质量分数在10至240 ppm Si-OH之间实现了良好的相关性。化学计量模型的质量由使用五个潜变量（因子）的0.965相关系数（交叉验证）和7 ppm的校准均方根误差（RMSEC）表征。将化学计量数据与单变量数据分析的结果进行比较。对重现性影响最大的是样品制备（研磨和混合），这取决于相关操作人员。
