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    ASTM D6953 - 18

    Standard Test Method for Determination of Antioxidants and Erucamide Slip Additives in Polyethylene Using Liquid Chromatography (LC)

    Active Standard ASTM D6953 | Developed by Subcommittee: D20.70

    Book of Standards Volume: 08.03

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    Significance and Use

    5.1 Separation and identification of stabilizers used in the manufacture of polyethylene resins are necessary in order to correlate performance properties with polymer composition. This test method provides a means to determine the polymer additives listed in Table 1 in polyethylene samples. This test method is capable of the determination of other antioxidants, but the stability of these during extraction has not been investigated.

    5.2 The additive extraction procedure is made effective by the relatively low solubility of the polymer sample in solvents generally used for liquid chromatographic analysis. In this method, isopropanol and cyclohexane were chosen because of their excellent extraction efficiencies as well as for safety reasons. Other solvents including ethylacetate, isobutanol, chloroform and methylene chloride can also be used.

    5.3 Methods other than refluxing that have been used to remove additives from the polymer matrix including pressurized liquid, microwave, ultrasonic, and supercritical fluid extractions. For the separation of the extracted additives, SFC and GC have been used successfully for several of the additives.

    5.4 Under optimum conditions, the lowest level of detection for an antioxidant is approximately 2 ppm.

    1. Scope

    1.1 This test method covers a liquid-chromatographic procedure for the separation of primary and secondary antioxidant and slip additives currently used in polyethylene plastics. These additives are extracted with either isopropanol (resin densities < 0.94 g/cm3) or cyclohexane (resin densities > 0.94 g/cm3) prior to liquid-chromatographic separation. The ultraviolet absorbance of the eluting compound(s) is measured and quantitation is performed using external calibration.

    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 standard.

    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.

    2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

    ASTM Standards

    D883 Terminology Relating to Plastics

    D1600 Terminology for Abbreviated Terms Relating to Plastics

    D4697 Guide for Maintaining Test Methods in the Users Laboratory

    E131 Terminology Relating to Molecular Spectroscopy

    E169 Practices for General Techniques of Ultraviolet-Visible Quantitative Analysis

    E275 Practice for Describing and Measuring Performance of Ultraviolet and Visible Spectrophotometers

    E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method

    E1657 Practice for Testing Variable-Wavelength Photometric Detectors Used in Liquid Chromatography

    ICS Code

    ICS Number Code 83.040.20 (Rubber compounding ingredients)

    UNSPSC Code

    UNSPSC Code 12162200(Anti oxidants); 13111016(Polyethylene)

    Referencing This Standard
    Link Here
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    DOI: 10.1520/D6953-18

    Citation Format

    ASTM D6953-18, Standard Test Method for Determination of Antioxidants and Erucamide Slip Additives in Polyethylene Using Liquid Chromatography (LC), ASTM International, West Conshohocken, PA, 2018, www.astm.org

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