IR-UV联合法测定固相微萃取涂层中单体含量

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摘要：合成了作为固相微萃取涂层的苯乙烯-丙烯酸丁酯-乙烯基三乙氧基硅氧烷三元共聚物。采用红外光谱(IR)和紫外光谱(UV)相结合的方法测定了聚合物中苯乙烯和丙烯酸丁酯的含量。由IR法测得样品中二者的摩尔比。采用双波长紫外光谱法测得苯乙烯的含量。由苯乙烯与丙烯酸丁酯的摩尔比及苯乙烯的含量得出样品中丙烯酸丁酯含量，进而得出乙烯基三乙氧基硅氧烷的含量。苯乙烯与丙烯酸丁酯的摩尔比测定的外标曲线方程为A_r=0.114m_r+0.032，相关系数r²=0.999 3；苯乙烯含量测定的标准曲线方程为ΔA=0.078 6c+0.081 2，相关系数r²=0.998 9。苯乙烯含量测定的相对标准偏差(RSD)为0.41%，加标回收率为97.8%～104.0%；丙烯酸丁酯含量测定的相对标准偏差(RSD)为0.39%，加标回收率为97.1%～99.6%。

关键词：固相微萃取涂层;苯-丙-硅聚合物;IR-UV联合法;单体含量

Abstract：In the present paper, phenylethylene-butyl acrylate-vinyl triethoxy siloxane terpolymer, as SPME coating, was synthesized. Combining infrared spectrum and ultraviolet spectrum, the contents of the monomers were determined. The two monomers’ mole ratio of phenylethylene to butyl acrylate was obtained by IR. The content of phenylethylene was obtained by UV. Then the contents of butyl acrylate and vinyl triethoxy siloxane were calculated from the phenylethylene quantity and the mole ratio. For the determination of the mole ratio of phenylethylene to butyl acrylate, the standard curve was A_r=0.114m_r+0.032 (A: absorptance ratio, m_r: mole ratio), and the corre lation efficient(r²) was 0.999 3; for the determination of the content of phenylethylene, the standard curve was ΔA=0.078 6c+0.081 2(ΔA: absorptance difference, c: concentration of phenylethylene), and the correlation efficient(r²) was 0.998 9. The relative standard deviation (RSD) for phenylethylene was 0.41%, and recoveries were 97.8%-104%. The relative standard deviation (RSD) for butyl acrylate was 0.39%, and the recoveries were 97.1%-99.6%.

Key words：Solid phase microextraction coating;Phenylethylene-butyl acrylate-vinyl triethoxy siloxane terpolymer;Combining RI and UV;Monomer content

收稿日期: 2006-08-10 修订日期: 2006-10-28

中图分类号:

O657.8

通讯作者: 申书昌 E-mail: sscfxzx @163.com

引用本文:

申书昌¹,柳彩云¹,付双¹,张维冰²,王文波¹. IR-UV联合法测定固相微萃取涂层中单体含量[J]. 光谱学与光谱分析, 2007, 27(11): 2235-2238.
SHEN Shu-chang¹,LIU Cai-yun¹,FU Shuang¹,ZHANG Wei-bing²,WANG Wen-bo¹. Determination of the Monomers in Phenylethylene-Butyl Acrylate-Vinyl Triethoxy Siloxane Terpolymer for Solid Phase Microextraction Coating by Combining IR and UV. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2007, 27(11): 2235-2238.

链接本文:

https://www.gpxygpfx.com/CN/Y2007/V27/I11/2235

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