1、 FORD LABORATORY TEST METHOD AP 150-04 Date Action Revisions 2001 01 31 Revised Editorial no technical change A. Cockman 2000 04 19 Editorial no technical change A. Cockman 1991 12 10 Printed copies are uncontrolled Page 1 of 3 Copyright 2001, Ford Global Technologies, Inc. POLYMERIC MATERIALS - EXT
2、RACTABLES CONTENT Application This test is used to determine the percent of plasticizer, oils, and/or soluble additives present in elastomeric compounds. Scope This method provides a procedure for extracting plasticizers, mineral oils, extenders, low molecular weight waxes, prelubricants as in “pres
3、wollen“ compounds, and other soluble additives typically found in polymers. It is also useful in obtaining an “oil-free“, additive-free base elastomer for cognate analysis by Thermogravimetric Analysis (TGA) and Infrared Analysis (IR). Selection of the appropriate solvent is based upon the type of p
4、olymer, requirements of the Engineering Material Specification, and/or knowledge of the solvent and anticipated solubilities of the materials to be extracted (i.e., alcohols may extract more selectively than acetone). Apparatus Required Extraction Apparatus With block tin condenser (ASTM D 297, Figu
5、re 1) Flask Erlenmeyer, 400 Ml Glass Extraction Cups Soxhlet-type or equivalent Analytical Balance Precision +/- 0.0001 g Oven ASTM E 146, Type IIB or equivalent; capable of maintaining 70 +/- 2 C Hot Plate Laboratory-extraction format, outfitted with water-cooled “block tin-type“ condensers FORD LA
6、BORATORY TEST METHOD AP 150-04 Page 2 of 3 Copyright 2001, Ford Global Technologies, Inc. Steam Bath (Located under a laboratory hood or other suitable ventilation) Materials Required Filter Paper Coarse porosity, Reeves Angel, Grade 802, 15 cm, “fluted“, or equivalent Solvent Reagent grade acetone,
7、 toluene, ethanol, diethyl or petroleum ether, chloroform, n-hexane, or any other solvent as specified by the engineering document. WARNING: Flammable, Hazardous Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a controlled atmosphere of 23 +/- 2
8、 C and 50 +/- 5 % relative humidity for not less than 24 h prior to testing and tested under the same conditions unless otherwise specified. Procedure 1. Using a mechanical “chopper“ or scissors, cut 1 - 2 g of material into pieces approximately 2 - 3 mm x 2 - 3 mm x 2 - 3 mm. (Suggestion for the sc
9、issor method: First cut the material into several long, thin strips, then cross-section the bundle of strips into pieces.) 2. Accurately weigh the cut material on an analytical balance to the nearest 0.0001 g and record as “weight of sample“. 3. Place the sample pieces in fluted filter paper and ins
10、ert into a glass extraction cup. 4. Weigh a clean, dry 400 Ml Erlenmeyer flask and record as “weight of flask“. 5. Add to the flask approximately 100 mL of reagent grade solvent. 6. Suspend the glass extraction cup in the flask over the solvent. 7. Place the assembled apparatus on the extraction hot
11、 plate. 8. Cover the top of the flask with the block tin condenser. (Note: Ensure that there is an adequate flow of water through the condenser.) FORD LABORATORY TEST METHOD AP 150-04 Page 3 of 3 Copyright 2001, Ford Global Technologies, Inc. 9. Adjust the heat to reflux at a rate that the extractio
12、n cup will empty by siphon action between approximately 2 - 3 min. The required period of time of test will be as described in the applicable Engineering Material Specification. (Note: Use standard times of 2, 4, 8, 16, and 24 h. If not otherwise specified, use 16 - 18 h.) 10. After the refluxing is
13、 complete, empty any remaining solvent from the glass extraction cup into the flask and remove the sample. Place the flask on a steam bath under a hood or other suitable ventilation. (Save the extracted polymeric sample for subsequent analysis if required.) 11. Evaporate the solvent in the flask (no
14、w containing extracted materials) on the steam bath. To hasten evaporation, direct a gentle current of filtered air across the surface of the liquid. 12. Remove the final traces of the solvent by placing the flask into an oven at 70 +/- 2 C for 1 - 2 h. 13. Remove the flask from the oven, cool to 23
15、 +/- 2 C, and weigh. Record as “weight of flask and solubles“. Determine the extractables content by the calculation as given below: % extractables = (weight of flask + solubles) - (weight of flask) x 100 (weight of sample) 14. Report the % extractables, including the solvent used and the duration o
16、f the extraction. Note: Unless the extractable material is known to be the sole additive to the base polymer (as in the case of siloxane or mineral oil “inherently prelubricated“ silicone elastomers) mixtures of the materials will likely be extracted. Materials selectively extracted by solvents othe
17、r than those recommended in ASTM D 297 should be identified by Infrared Analysis or other suitable technique. Depending upon the solvent used, values may be reported as total percent extractables (identify the solvent used) by itself or in conjunction with TGA for elastomeric compositional analysis. Chemicals, materials, parts, and equipment referenced in this document must be used and handled properly. Each party is responsible for determining proper use and handling in its facilities.
