ASTM F1349:19 pdf download

ASTM F1349:19 pdf download .Standard Test Method for Nonvolatile Ultraviolet (uv) Absorbing Extractables from Microwave susceptors.
4.2.6 Microwave the cell or alternate extraction boat using the time specifications as determined in Test Method F874. Record the probe temperatures, preferably at 5-s intervals, but at intervals not to exceed 15 s,
4.3 Quatitative Analysis:
4.3. 1 Standard Curve:
4.3. 1 . 1 Prepare a standard mixture of 10 ppm (w/v) each of BHET. DMT. DET. and any other identified UV components (see appendix) of the susceptor in DMAC. Proceed to generate chromatograms using high pressure liquid chromatography in accordance with 3.2.5, 3.2.6, and 4.3.2.8. Retention times for BIIET, DMT, and DET will be approximately 7.6, 16.6, and 21.5 mm respectively.
4.3.1.2 Repeat with a standard of 5 ppm of DMT.
4.3.1.3 Repeat with a standard of 1 ppm of DMT.
4.3.1.4 Construct a plot of area response of DMT versus concentration.
4.3.1.5 For quantitation of PETE oligomers use the following response factor to construct an area response plot:
(1nassIarea)1),,7/( mass/area )iri,,u., = 0.9 1 2.
4.3.2 Quantification of Extractables from Susceptor:
4.3.2.1 Prepare and place the sample in the microwave oven in accordance with 4.2.1 — 4.2.6.
4.3.2.2 Microwave at full power using the time determined in 4.1.1.
4.3.2.3 Stir oil in boat or cell. Warning—Be extremely careful when handling the Waldorf P1’FE cell or extraction boat. Use protective gloves. Severe burns can result from extremely hot oil.
4.3.2.4 Weigh 3 ± 0.03 g of stirred oil into a 50-mL beaker. Add 25 mL of hexane, stir, and transfer to a I 25-mL separatory funnel.
4.3.2.5 Rinse the beaker with an additional 25-mL portion of hexane and add to the separator)’ funnel. Rinse the beaker with 25 mL of acetonitrile and add to the separatory funnel. Shake the separatory funnel and draw off the acetonitrile phase into a 50-rnL conical test tube or into a Kuderna-Danish evaporative concentrator with a 10-mL receiver or other solvent concentration apparatus. Rinse the beaker with a second 25-mL portion of acetonitrile, add to the separatory funnel, shake, draw off acetonitrile, and add to the previous acetonitrile extract.
4.3.2.6 Concentrate the combined acetonitrile extracts to 0.4 to 0.5 mL in a 65°C water bath under a gentle stream of nitrogen or using a Turbo Vap or on a steam bath in a Kuderna-Danish evaporative concentrator with a l0-mL receiver and three-ball Snyder column.
4.3.2.7 Cool, take residue in test tube to 2 mL with DMAC.
4.3.2.8 Inject onto HPLC system, with or without filtering as desired, and separate using gradient conditions defined in apparatus in 3.2.6. Dilute sample if necessary if any extractant peaks arc excessively large.
4.3.2.9 To determine a Miglyol 812 or corn oil or blank, place the proper amount of oil in a borosilicate peiri dish. Place a fresh susceptor in the oven, place the petri dish on the susceptor and proceed through 4.3.2.1 — 4.3.2.8.