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Analysis of initiator content of prepreg by near-infrared spectroscopy
Reviews in Analytical Chemistry ( IF 4.3 ) Pub Date : 2022-01-01 , DOI: 10.1515/revac-2022-0035
Qianfa Liu 1 , Dan Li 1 , Chiji Guan 1
Affiliation  

During the production process of some copper clad laminate (CCL), the content of 3,3,5,7,7-pentamethyl-1,2,4-trioxepane in prepreg can affect the cross-linking and curing degree of resin directly, and thereby affect the properties of CCL. In this article, near-infrared (NIR) spectroscopy combined with partial least square regression using high performance liquid chromatography as a reference method were used for the determination of 3,3,5,7,7-pentamethyl-1,2,4-trioxepane in the CCL production progress. 160 spectra of prepreg samples randomly formed the calibration set, and 50 spectra of prepreg samples formed the validation set. The value of the root mean square error of calibration (w/w) and root mean square error of prediction (w/w) were 0.011% and 0.013% for 3,3,5,7,7-pentamethyl-1,2,4-trioxepane content (%, w/w), and the calculation and validation of the regression equation resulted in high correlation coefficients of 0.99 and 0.98, respectively. The scatter plot value of calibration set which was obtained from the root mean square error of cross-validation (w/w) was 0.015%, and the regression equation resulted in high correlation coefficient of 0.98. The results of the paired t-test revealed that there was no significant difference between NIR and HPLC method. Thus, the results obtained in this study reflect that NIR could be used as a rapid, accurate, and simultaneous technique to determine 3,3,5,7,7-pentamethyl-1,2,4-trioxepane content of prepreg in the production process.

中文翻译:

近红外光谱分析预浸料引发剂含量

一些覆铜板(CCL)生产过程中,预浸料中3,3,5,7,7-五甲基-1,2,4-三氧杂环己烷的含量会直接影响树脂的交联固化程度,从而影响覆铜板的性能。本文采用近红外(NIR)光谱结合偏最小二乘回归,以高效液相色谱法为参考方法测定3,3,5,7,7-pentamethyl-1,2,4-三恶烷在覆铜板生产中的进展。160张预浸样品光谱随机形成校准集,50张预浸样品光谱形成验证集。对于 3,3,5,7,7-pentamethyl-1,2,校准的均方根误差 (w/w) 和预测的均方根误差 (w/w) 的值分别为 0.011% 和 0.013%, 4-三恶烷含量(%,w/w),回归方程的计算和验证分别产生了 0.99 和 0.98 的高相关系数。由交叉验证的均方根误差(w/w)得到的校准集散点图值为0.015%,回归方程的相关系数高达0.98。配对 t 检验的结果表明,NIR 和 HPLC 方法之间没有显着差异。因此,本研究中获得的结果表明,近红外可作为一种快速、准确、同时测定生产中预浸料中 3,3,5,7,7-五甲基-1,2,4-三氧杂环己烷含量的技术。过程。由交叉验证的均方根误差(w/w)得到的校准集散点图值为0.015%,回归方程的相关系数高达0.98。配对 t 检验的结果表明,NIR 和 HPLC 方法之间没有显着差异。因此,本研究中获得的结果表明,近红外可作为一种快速、准确、同时测定生产中预浸料中 3,3,5,7,7-五甲基-1,2,4-三氧杂环己烷含量的技术。过程。由交叉验证的均方根误差(w/w)得到的校准集散点图值为0.015%,回归方程的相关系数高达0.98。配对 t 检验的结果表明,NIR 和 HPLC 方法之间没有显着差异。因此,本研究中获得的结果表明,近红外可作为一种快速、准确、同时测定生产中预浸料中 3,3,5,7,7-五甲基-1,2,4-三氧杂环己烷含量的技术。过程。
更新日期:2022-01-01
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