ASTM D6953-03

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 BHT, BHEB, Isonox 129, erucamide slip, Irgafos 168, Irganox 1010, Irganox 1076 and TNPP levels in polyethylene samples. This test method should be applicable for the determination of other antioxidants such as Ultranox 626, Ethanox 330, Santanox R, and Topanol CA, but the stability of these during extraction has not been investigated.

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.

Methods other than refluxing that have been used to remove additives from the polymer matrix include 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.

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

1.1 This test method covers a liquid-chromatographic procedure for the separation of some additives currently used in polyethylene. 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 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 and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9.

Note 1—There is no equivalent ISO standard.