微观设备在分析聚羧酸高性能减水剂方面应用.docVIP

微观设备在分析聚羧酸高性能减水剂方面应用【摘要】高性能减水剂尤其是聚羧酸高效减水剂由于其优异的减水性能，坍落度保持等性能而备受各国重视，而减水剂的微观检测和分析是探索创新新型聚羧酸高性能减水剂的重要基础。本文详细介绍了红外光谱分析技术在聚羧酸减水剂官能团种类检测中的应用原理和方法，系统阐述了用凝胶渗透色谱技术计算聚羧酸减水剂分子量和分子量分布的方法和原理。? 【关键词】红外光谱；凝胶色谱；聚羧酸减水剂?? The application of micro equipments in analysing polycarboxylate high preformace water reducer? Wang Lei,Chi Pei-yun,Yang Pei-dong,Niu chang-hui? (School of Architecture and Civil Engineering, Qingdao Technological UnivercityQingdaoShandong266033) ? 【Abstract】High performance water reducing agent especially polycarboxylate water reducer has increasingly been come under recognition because of its remarkable water-reducing ability and slump retention ect. And micro test methords lay an important foundation and server a supporting power for exploring new kinds of polycarboxylate water reducer. In this paper, detailed discription has been made about the priciple of infrared spectorscopy technology and its application in detecting functional groups of polycarboxylic acid, and priciple of Gel permeation Chormtography techonlogy and its using in calculating molecular weight and molecular weight distribution of polycarboxylate water reducer is also been systematically introduced.? 【Key words】 Infrared spectorscopy;Gel permeation Chromtography technology;Polycarboxylate water reducer?? 1. 红外光谱分析（infrared spectrum analysis）? 1.1红外光谱分析原理 当PC样品受到频率连续变化的红外光照射时，分子会吸收与其振动频率一样的红外光波使其从振动――转动能级的基态跃迁到激发态，相应与这些区域的投射光波强度就会降低，记录百分透过率他T%对波数或波长的曲线即可得到PC样品的红外光谱。由于聚合物中的官能团的红外光谱特征吸收峰总是在一定范围之内变动，因此通过分析PC样品的红外光谱即可得出该聚合物所含有的官能团。下表1为PC减水剂中常见官能团的特征吸收峰。? 1.2实验及分析。? 1.2.1实验仪器和样品制备。? （1）实验仪器 傅里叶交换红外光谱仪，德国bruker公司，分辨率优于0.09cm??-1?，光谱范围12500～50cm??-1?。? （2）试样制备 采用薄膜法制样，样品先经过异丙醇和丙酮的分离，然后将PC溶液倒入到低沸点（5～8倍）溶剂中反复沉淀，在60℃浓缩一定时间后再真空抽滤，除去水分然后涂抹在NaCl盐片上成膜。? 1.2.2图谱分析 下图1为两种聚羧酸减水剂MPC-1和MPC-2的红外图谱，通过分析红外光谱结合减水剂中各基团特征峰的位置，可以看到MPC-1和MPC-2有相似的结构 3300，2850，1725，1575，1460，1350，1280，1107，951，845，622及523cm??-1?等波数附近都有 吸收峰，可见这两种减水剂分子结构上具有磺酸基，羧基，聚氧化乙烯基，酯基和羟基等基团。由于MPC-1比MP