聚羧酸系减水剂大单体的检测分析

发布时间：2018-01-08 05:18

本文关键词：聚羧酸系减水剂大单体的检测分析　出处：《中国日用化学工业研究院》2015年硕士论文　论文类型：学位论文

【摘要】：聚羧酸系减水剂是目前混凝土减水剂研究课题中的重点,也是今后发展前景最好的一类减水剂。聚羧酸系减水剂大单体是合成聚羧酸系减水剂的主要原料,大单体性能直接决定了合成减水剂的效果,因此本文主要是对大单体的性能进行研究,采用化学法对聚羧酸系减水剂大单体双键值进行测定研究,同时采用仪器法对大单体的组成及其聚乙二醇含量进行了分析研究。研究了聚羧酸系减水剂大单体双键值的碘值法测定,论述了溶剂加入量、溴酸钾-溴化钾溶液加入量、静置时间等对测定结果的影响,不同的实验条件会产生不同的结果。通过实验确定了碘值法测定大单体双键值的最适宜操作条件,且其相对标准偏差不大于1.5%,回收率在95.5%~99.5%之间。该方法简便快速,重现性好。提出了高效液相色谱测定聚羧酸系减水剂大单体聚乙二醇含量。在设定的实验条件下,标准样品聚乙二醇峰面积与浓度之间具有良好的线性关系,且样品中的聚乙二醇能够被很好的分离。通过外标法定量对其聚乙二醇含量进行分析,其相对标准偏差(RSD)不超过6.5%,加标回收率在93%~104%之间。该方法简便、快速、重现性好,适用于聚羧酸系减水剂大单体聚乙二醇含量的测定。建立了一种高效液相色谱-电雾式检测器(HLPC-CAD)分析聚羧酸系减水剂大单体的组分的方法,该方法主要依据大单体(属于脂肪醇聚氧乙烯基醚类)中EO加合数的不同进行分离。分离柱为Agilent ZORBAX SB-C8柱,流动相为甲醇(A)和水(B),采用梯度洗脱:65%A线性升至70%A运行60min,检测器为电雾式检测器(CAD)。在选定的色谱条件下,样品各组分间有良好的分离效果。
[Abstract]:Polycarboxylate superplasticizer is currently the focus of research in concrete reducing agent, but also the future development prospects of the best water reducer. Polycarboxylate superplasticizer is the main raw material for the synthesis of macromonomer of polycarboxylate superplasticizer, properties of macromonomer directly determines the synthesis of water reducing agent effect, so this paper mainly carries on research the performance of the macromonomer, the polycarboxylate superplasticizer macromer double value were measured by chemical method, and the composition and content of PEG macromonomer was analyzed by instrument method. Study the Polycarboxylic Water Iodine Method macromer double value determination, discusses the amount of solvent, amount bromate bromide solution, incubation time on the determination results, different experimental conditions will produce different results. Through the experiment to determine the determination of monomer double value of the optimal iodine value method Appropriate operation conditions, and the relative standard deviation is less than 1.5%, the recovery rate was 95.5%~99.5%. The method is simple and rapid with good reproducibility. The HPLC determination of polycarboxylate superplasticizer macromonomer polyethylene glycol content. In these experimental conditions, the standard sample of poly ethylene glycol concentration between the peak area and has a linear a good relationship, and polyethylene glycol samples can be separated very well. The external standard method for quantitative analysis of the content of PEG, the relative standard deviation (RSD) less than 6.5%. The recoveries were 93%~104%. The method is simple, rapid, reproducible and suitable for determination of polycarboxylic acid agent macromonomer polyethylene glycol content. A high performance liquid chromatography electrospray aerosol detector was established (HLPC-CAD) analysis method of polycarboxylate superplasticizer monomer component, this method mainly based on large monomer (belong to fat Fatty alcohol polyoxyethylene ether) were separated in different number of EO units. The column with Agilent ZORBAX SB-C8 column, the mobile phase of methanol (A) and water (B), using linear gradient elution: 65%A to 70%A 60min operation, a charged aerosol detector (CAD) under the selected chromatographic conditions. Next, sample components have good separation effect.

【学位授予单位】：中国日用化学工业研究院
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TU528.042.2

【相似文献】