红外光谱法结合偏最小二乘回归法测定干混砂浆中的聚合物含量  

Determination of Polymer in Dry-Mixed Mortar by IR Combined with PLS Regression Method

作　　者：毛志毅[1,2,3] 刘家臣[1] 刘彤 王冬梅 

机构地区：[1]天津大学材料科学与工程学院,天津300072 [2]天津市建筑材料集团(控股)有限公司,天津300381 [3]天津市建筑材料科学研究院,天津300381

出　　处：《理化检验（化学分册）》2017年第3期249-253,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金项目(51372164)

摘　　要：采取来自不同厂家和不同型号的干混砂浆产品组分,通过改变灰砂比和掺入添加剂,制备一系列聚合物有效含量不同的干混砂浆标准样品。取干混砂浆实际样品20份和所配制的标准样品80份,用衰减全反射-傅里叶变换红外光谱法测得其所含聚合物的光谱数据,用偏最小二乘回归法对数据进行校正。分别采用连续小波变换、Savitzky-Golay平滑和求导方法对光谱信号进行预处理,提高所建模型的精密度,其中以信号平滑的效果最好。结合蒙特卡洛无信息变量消除方法优化所建模型,建模集和验证集测定值的均方误差分别由0.213和0.217下降至0.170和0.180,验证集数据的相关系数为0.991。该方法与国家标准方法之间具有很好的相关性。A series of standard samples of dry-mixed mortar with different and known available contents of polymer were prepared by sampling of the mortar components from various producers with various models and by variation of ratio of cement and sand and mixing of additives. Twenty samples of the mortar with unknown polymer contents and eighty samples of the standard samples of mortar prepared above were taken and analyzed by ATR- FTIR spectrometry to obtain the IR-spectra of the polymer and corrected by applying the chemometric method of PLS regression. The methods of continuous wavelent transform, Savltzky-Golay smoothing and differentiation were applied to pretreat the IR-spectra signals, to raise the precision of the established model. The method of signal smoothing gave the most effective result. After optimization with the method of MC-UVE, values of mean square deviations of the measurements of the samples of the calibration set and the testing set were reduced from 0. 213 and 0. 217 to 0. 170 and 0. 180 respectively. The correlation coefficient of data of the testing set found was 0. 991. Good correlationship was obtained between data obtained by the proposed method and the national standard method.

关 键 词：衰减全反射-傅里叶变换红外光谱法 偏最小二乘回归法 聚合物含量 干混砂浆 

分 类 号：O657.33[理学—分析化学]