ASTM D6953-18 - 1.11.2018
 
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

E131-10(2023)

Standard Terminology Relating to Molecular Spectroscopy

E169-16(2022)

Standard Practices for General Techniques of Ultraviolet-Visible Quantitative Analysis

E275-08(2022)

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

E691-23

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

D1600-18

Standard Terminology for Abbreviated Terms Relating to Plastics (Withdrawn 2024)

IEEE/ASTM SI 10

Standard for Use of the International System of Units (SI): The Modern Metric System

D883-26

Standard Terminology Relating to Plastics

D4697-95(2001)

Standard Guide for Maintaining Test Methods in the User's Laboratory (Withdrawn 2009)

E1657-98(2026)

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