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Standard Test Method for Determination of Phenolic Antioxidants and Erucamide Slip Additives in Polypropylene Homopolymer Formulations Using Liquid Chromatography (LC) 用液相色谱法(LC)测定聚丙烯均聚物配方中酚类抗氧化剂和芥子酰胺滑动添加剂的标准试验方法
发布日期: 2023-11-01
1.1 本试验方法涵盖了目前聚丙烯中使用的一些添加剂的液相色谱分离程序。在液相色谱分离之前,使用回流或超声波浴用环己烷∶二氯甲烷混合物提取这些添加剂。测量化合物的紫外线吸收率(200nm),并使用内标法进行定量。 1.2 以国际单位制表示的数值应视为标准。本标准不包括其他计量单位。 1.3 本标准并不旨在解决与其使用相关的所有安全问题(如有)。本标准的使用者有责任在使用前制定适当的安全、健康和环境实践,并确定监管限制的适用性。 具体的预防说明见第节 9 。 注1: 目前还没有与此测试方法等效的ISO。 1.4 本国际标准是根据世界贸易组织技术性贸易壁垒委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认的标准化原则制定的。 ====意义和用途====== 5.1 聚丙烯生产中使用的稳定剂的分离和鉴定是必要的,以便将性能特性与聚合物组成相关联。该测试方法提供了一种方法来测定聚丙烯样品中芥子酰胺、维生素E、Irgafos 168、Irganox 3114、Irganox1010和Irganox1076的水平。 本试验方法也适用于其他抗氧化剂的测定,如Ultranox 626、Ethanox 330、Santanox R和BHT,但尚未研究本试验方法对这些抗氧化剂的适用性。 5.2 添加剂提取程序由于聚合物样品在通常用于液相色谱分析的溶剂中的不溶性而变得有效。 5.3 在最佳条件下,酚类抗氧化剂的最低检测水平约为2ppm。 注2: 已成功用于从塑料基质中去除添加剂的其他方法包括薄膜、微波、超声波和超临界流体萃取。其他方法已成功用于分离添加剂,包括SFC和毛细管GC。 5.4 Irgafos 168是一种亚磷酸盐抗氧化剂。已知亚磷酸盐同时经历氧化和水解反应。当在处理过程中发生氧化时,将在聚合物中确定较少的Irgafos 168。HPLC分离能够分离亚磷酸盐、磷酸盐(氧化产物)和水解产物,并在获得标准品的情况下对其进行定量。由于本标准中的提取技术或分离,未发现亚磷酸盐抗氧化剂的显著分解。
1.1 This test method covers a liquid-chromatographic procedure for the separation of some additives currently used in polypropylene. These additives are extracted with a cyclohexane:methylene chloride mixture using either reflux or ultrasonic bath prior to liquid-chromatographic separation. The ultraviolet absorbance (200 nm) of the compound(s) is measured, and quantitation is performed using the internal standard method. 1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9 . Note 1: There is no known ISO equivalent to this test method. 1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 5.1 Separation and identification of stabilizers used in the manufacture of polypropylene is necessary in order to correlate performance properties with polymer composition. This test method provides a means to determine erucamide slip, Vitamin E, Irgafos 168, Irganox 3114, Irganox 1010, and Irganox 1076 levels in polypropylene samples. This test method is also applicable for the determination of other antioxidants, such as Ultranox 626, Ethanox 330, Santanox R, and BHT, but the applicability of this test method has not been investigated for these antioxidants. 5.2 The additive-extraction procedure is made effective by the insolubility of the polymer sample in solvents generally used for liquid chromatographic analysis. 5.3 Under optimum conditions, the lowest level of detection for a phenolic antioxidant is approximately 2 ppm. Note 2: Other methods that have been used successfully to remove additives from the plastics matrix include thin film, microwave, ultrasonic, and supercritical fluid extractions. Other methods have been used successfully to separate additives including SFC and capillary GC. 5.4 Irgafos 168 is a phosphite antioxidant. Phosphites are known to undergo both oxidation and hydrolysis reactions. Less Irgafos 168 will be determined in the polymer when oxidation occurs during processing. The HPLC separation is capable of separating the phosphite, phosphate (oxidation product), and hydrolysis product and quantify them if standards are obtained. No significant breakdown of the phosphite antioxidant has been seen due to either extraction technique or the separation presented in this standard.
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归口单位: D20.70
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