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采用夹心进样法,无需样品制备,通过液相色谱分析聚酰胺-6中的线性和环状低聚物。II. 检测和定量方法及整体长期性能

Analysis of linear and cyclic oligomers in polyamide-6 without sample preparation by liquid chromatography using the sandwich injection method. II. Methods of detection and quantification and overall long-term performance.

作者信息

Mengerink Y, Peters R, Kerkhoff M, Hellenbrand J, Omloo H, Andrien J, Vestjens M, van der Wal S

机构信息

MI&Q, DSM Research, Geleen, The Netherlands.

出版信息

J Chromatogr A. 2000 May 5;878(1):45-55. doi: 10.1016/s0021-9673(00)00277-6.

DOI:10.1016/s0021-9673(00)00277-6
PMID:10843544
Abstract

By separating the first six linear and cyclic oligomers of polyamide-6 on a reversed-phase high-performance liquid chromatographic system after sandwich injection, quantitative determination of these oligomers becomes feasible. Low-wavelength UV detection of the different oligomers and selective post-column reaction detection of the linear oligomers with o-phthalic dicarboxaldehyde (OPA) and 3-mercaptopropionic acid (3-MPA) are discussed. A general methodology for quantification of oligomers in polymers was developed. It is demonstrated that the empirically determined group-equivalent absorption coefficients and quench factors are a convenient way of quantifying linear and cyclic oligomers of nylon-6. The overall long-term performance of the method was studied by monitoring a reference sample and the calibration factors of the linear and cyclic oligomers.

摘要

通过在夹心进样后,在反相高效液相色谱系统上分离聚酰胺-6的前六种线性和环状低聚物,这些低聚物的定量测定变得可行。讨论了不同低聚物的低波长紫外检测以及用邻苯二甲酸二醛(OPA)和3-巯基丙酸(3-MPA)对线性低聚物进行选择性柱后反应检测。开发了一种用于聚合物中低聚物定量的通用方法。结果表明,通过经验确定的基团等效吸收系数和猝灭因子是定量尼龙-6线性和环状低聚物的便捷方法。通过监测参考样品以及线性和环状低聚物的校准因子,研究了该方法的整体长期性能。

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