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机构地区:[1]宁波出入境检验检疫局,宁波315012 [2]浙江工业大学化材学院,杭州310005
出 处:《理化检验(化学分册)》2009年第3期267-269,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
摘 要:取0.013g共聚物样品,用压片机在压力30MPa和温度(150±10)℃的条件下压制成厚度为0.05mm的样品膜供傅里叶变换红外光谱法分析用。根据苯乙烯-异丁烯酸甲酯共聚物的红外光谱特征性,分别选择波数700cm叫和1730cm叫作为苯乙烯和异丁烯酸甲酯的定量峰位。选用已知苯乙烯单元的共聚物样品,按方法分析并测得相关数据。以苯乙烯单元的质量分数(%)作为纵坐标,以特征峰面积比值(A700/A1730)为横坐标制作标准曲线。根据所测得未知样品的A700/A1730比值,在标准曲线上查得其苯乙烯单元的含量。该法测定聚合物中苯乙烯单元的范围为40%~85%。测得不同苯乙烯单元含量样品的相对标准偏差(n=6)为0.9%~1.9%。将红外光谱法分析结果与核磁共振法分析结果进行比较,相对误差在2%以内。Sample film of thickness of 0. 05 mm was made with 0. 013 g of the sample by the film-forming press under a working pressure of 30 MPa at (150±10)℃. In the IR-speetrometric determination of styrene monomer in the copolymer of styrene (SR) and methyl methacrylate (MMA), based on the m-spectroscopic property of the copolymer, wavenumbers of 700 cm-1 and 1 730 cm-1 were selected as the peak positions for analysis. Copolymer samples with known contents of styrene monomer was used for preparation of standard curve, taking the contents (in %) of styrene monomer as the ordinate and values of ratio of characteristic peak area, AToo/ A~ 730, as the abscissa. Content of styrene monomer in unknown sample was found from the standard curve with the value of the ratio A700/A1730 measured. Range of determination of this method was found over the range 40%-85% of styrene monomer. Values of RSD's (n=6) found by this method were in the range of 0. 9%--1.9%. Relative deviation within 2 % were obtained between results of the present method and the 13C NMR method.
关 键 词:傅里叶红外光谱法 苯乙烯-异丁烯酸甲酯共聚物 苯乙烯单元含量
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