ASTM D5630-13 pdf free download.Standard Test Method for Ash Content in Plastics.
1.1 This test method was developed to determine the inorganic content of plastics by destructive ashing procedures. Ash levels of 0.01 % or above are covered by this test method.
1.2 These ashing procedures are used only to quantify the residual solids in the polymer and can not be used to identify the individual chemical components of the ash, qualitatively.
1.3 This test method is limited to those materials (including glass) that are stable to 900°C. Test Method D2584 is recommended for unknown samples, and in instances where fusion of the inorganic portions may be of concern.
1.4 Fluorinated polymers and polymers containing halogenated components have not been included in these procedures.
1.5 Two procedures for determining the inorganic residue in plastics are listed as follows:
1 .5. 1 Procedure A, Muffle-Furnace Technique— For 5 — 50 gram samples. Samples are flamed over a burner prior to being ashed in a mufile furnace.
1 .5.2 Procedure B, Rapid—Ash Muffle-Furnace Technique— For 2—10 gram samples. Samples are ignited and ashed in a muffle furnace.
9. Safety Precautions
9.1 Always wear safety glasses when working in the laboratory.
9.2 Exercise all normal safety precautions when working with opcn flames and high temperatures. Use insulated gloves and long crucible tongs when transferring crucibles.
9.3 Always work with an appropriately vented muffle furnace or under a fume hood when ashing. Irritant fumes are given off by the polymer during ashing.
10. Sampling, Test Specimens, and Test Units
10.1 For hygroscopic materials such as nylons, etc., dry sample specimens to constant weight before testing.
11. Preparation and Apparatus
11 . I Crucible Preparation—Clean the porcelain or platinum crucibles with tap water and an abrasive detergent. Ensure that any baked-in residue is removed from the crucibies completely. Quartz-fiber crucibles are disposable items and do not require ci caning.
11.2 Fire (condition) the clean crucibles in a muffle furnace at the set operating temperature for 5 mm to burn off any residue in the crucibles.
11.3 After tiring (conditioning) the crucibles, place them in a desiccator to cool for 20 to 30 mm (porcelain or platinum crucibles) or 2 mm (quartz-fiber crucibles). Handle the crucibles with tongs only.
12. Calibration and Standardization
12. 1 Calibrate the analytical balances in accordance with the manufacturer’s procedure.
13. Procedure A—Muffle Furnace Technique
13.1 Sample Tvpe—Determ Inc the type of polymer and anticipated amount of inorganics in the polymer to he ashed. Determine the ashing temperature. ashing time, and sample size required to perform the ash analysis in accordance with Table A1.1.
13.2 Preaching Procedure—Weigh a clean, dry porcelain or platinum crucible to the nearest 0.0001 g. Record the resulting value as W1.
13.2.1 Weigh approximately the amount of material in accordance with Table Al.l into the preweighed crucible. Record the resulting value as W2.
13.2.2 Place the crucible on a burner. (The diameter of the flame equals approximately 2.5 cm, and the height of the flame equals just enough to touch the wire gauze holding the crucible.) Ensure that the material does not overOow the crucible. ASTM D5630 pdf download.