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Measurement of glass transition temperature, residual heat of reaction and mixing ratio of epoxy resins using near infrared spectroscopy: a preliminary study

机译:用近红外光谱法测量玻璃化转变温度,反应余热和环氧树脂的混合比:初步研究

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摘要

As a measure of the degree of curing of epoxy resins, the glass transition temperature, T{sub}g, and the residual heat of reaction, ΔH{sub}r, are often used. In this study, near infrared spectroscopy and multivariate calibration [partial least squares regression (PLSR)] have been used to monitor the two variables, using differential scanning calorimetry (DSC) as the reference method. The epoxy under study was a commercial system consisting of the resin, trimethylolpropanetriglycidylether, and the hardener, 3-aminomethyl-3,5,5,-trimethylcyclohexylamine. Using samples cured under different conditions, calibrations resulted in root mean square errors of cross-validation (RMSECV) of 18 Jg{sup}(-1) for ΔH{sub}r (range for ΔH{sub}r: 6.1-231.3 Jg{sup}(-1)) and 7.2℃ for T{sub}g (range for T{sub}g: 41.5-98.8℃). Also, a PLSR model for mixing ratio of hardener and resin was obtained, resulting in a RMSECV of 0.0040 (range for mixing ratio: 0.180-0.380).
机译:作为环氧树脂的固化程度的量度,通常使用玻璃化转变温度T {sub} g和反应残余热ΔH{sub} r。在这项研究中,使用差示扫描量热法(DSC)作为参考方法,近红外光谱法和多元校正[偏最小二乘回归(PLSR)]已用于监视这两个变量。所研究的环氧树脂是一种商业体系,由树脂,三羟甲基丙烷三缩水甘油醚和硬化剂3-氨基甲基-3,5,5,-三甲基环己胺组成。使用在不同条件下固化的样品,校准会导致ΔH{sub} r的交叉验证均方根误差(RMSECV)为18 Jg {sup}(-1)(ΔH{sub} r的范围为6.1-231.3 Jg {sup}(-1))和T {sub} g为7.2℃(T {sub} g的范围为41.5-98.8℃)。另外,获得用于硬化剂和树脂的混合比的PLSR模型,得到0.0040的RMSECV(混合比的范围:0.180-0.380)。

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