University of Arkansas, Department of Chemistry and Biochemistry, 119 Chemistry Building, Fayetteville, AR 72701, United States.
University of Arkansas, Department of Chemistry and Biochemistry, 119 Chemistry Building, Fayetteville, AR 72701, United States.
Anal Chim Acta. 2014 Jan 15;808:151-62. doi: 10.1016/j.aca.2013.09.040. Epub 2013 Oct 5.
The influence of the sample preparation parameters (the choice of the matrix, matrix:analyte ratio, salt:analyte ratio) was investigated and optimal conditions were established for the MALDI time-of-flight mass spectrometry analysis of the poly(styrene-co-pentafluorostyrene) copolymers. These were synthesized by atom transfer radical polymerization. Use of 2,5-dihydroxybenzoic acid as matrix resulted in spectra with consistently high ion yields for all matrix:analyte:salt ratios tested. The optimized MALDI procedure was successfully applied to the characterization of three copolymers obtained by varying the conditions of polymerization reaction. It was possible to establish the nature of the end groups, calculate molecular weight distributions, and determine the individual length distributions for styrene and pentafluorostyrene monomers, contained in the resulting copolymers. Based on the data obtained, it was concluded that individual styrene chain length distributions are more sensitive to the change in the composition of the catalyst (the addition of small amount of CuBr2) than is the pentafluorostyrene component distribution.
研究了样品制备参数（基质的选择、基质：分析物比、盐：分析物比）的影响，并为聚（苯乙烯-co-五氟苯乙烯）共聚物的 MALDI 飞行时间质谱分析建立了最佳条件。这些共聚物是通过原子转移自由基聚合合成的。使用 2,5-二羟基苯甲酸作为基质，对于所有测试的基质：分析物：盐比，都得到了 consistently high ion yields 的谱图。优化的 MALDI 程序成功应用于通过改变聚合反应条件获得的三种共聚物的表征。可以确定端基的性质，计算分子量分布，并确定包含在所得共聚物中的苯乙烯和五氟苯乙烯单体的 individual length distributions。根据获得的数据得出结论，单体苯乙烯链长度分布对催化剂组成（添加少量 CuBr2）的变化比五氟苯乙烯组分分布更敏感。
