1、 FORD LABORATORY TEST METHOD AP 001-01 Date Action Revisions 2001 01 31 Revised Editorial no technical change A. Cockman 2000 04 17 Editorial no technical change A. Cockman 1992 03 18 Printed copies are uncontrolled Page 1 of 3 Copyright 2001, Ford Global Technologies, Inc. DETERMINATION OF ADEQUATE
2、 SEAL CURE OF ACRYLIC RUBBER Application This procedure describes a method of solvent extraction for amount of adipic acid to check new acrylic rubber seals for proper processing - specifically, in-process and post-mold curing. Apparatus and Reagents Required Analytical balance Soxhlet extractor wit
3、h interchangeable ground joints Flask - 250 mL, flat bottom, glass, 24/40 joint Flask - with Glass topper Steam bath - with controlled temperature Shaker - with Wrist action, Burrel Model 75-775, or equivalent Filter paper Ethyl ether - anhydrous Petroleum ether Alcohol or methanol Phenolphthalein i
4、ndicator Sodium Hydroxide - .01 N Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a controlled atmosphere of 23 +/- 2 C and 50 +/- 5 % relative humidity for not less than 24 h prior to testing and tested under the same conditions unless otherwis
5、e specified. FORD LABORATORY TEST METHOD AP 001-01 Page 2 of 3 Copyright 2001, Ford Global Technologies, Inc. Analysis Procedure Ethyl Ether Extraction Soxhlet Method 1. Reduce seals to particles of 3 mm or less by either cutting or dry ice freezing and shattering with a hammer. 2. Accurately weigh
6、to 0.1 mg approximately 3 g of rubber and transfer into extraction thimble, then place thimble in Soxhlet extractor. 3. Put 75 mL ethyl ether into Soxhlet flask, assemble to Soxhlet extractor and extract for a period of 4 hours. 4. Disconnect flask and evaporate the ethyl ether extract on a steam ba
7、th to dryness. FORD LABORATORY TEST METHOD AP 001-01 Page 3 of 3 Copyright 2001, Ford Global Technologies, Inc. Alternate Method 1. Prepare sample as in Soxhlet method and accurately weigh to 0.1 mg approximately 3 g of rubber in a 250 mL glass (24/40 joint) flat bottom flask. 2. To the contents of
8、the flask add 150 mL of anhydrous ethyl ether. Seal the contents with a glass stopper and transfer the stoppered flask to a shaking machine (Burrel wrist action shaker, Model 75-775) and extract for 4 hours under gentle agitation at 23 +/- 2 C. 3. Filter the contents through a dry filter paper into
9、a second 250 mL glass flat bottom flask. Rinse the first flask and filter paper with several 20 - 25 mL portions of ethyl ether into the second flask. 4. Evaporate the ethyl ether extract in the second flask on a steam bath to dryness. Petroleum Ether Extraction 1. To the residue obtained in Step 4
10、of the ethyl ether extraction, add 50 mL of petroleum ether and warm on a steam bath to boil. 2. Allow the insolubles to settle and decant off the petroleum ether extract. 3. Repeat Steps 1 and 2. Retain the flask. Titration of Adipic Acid 1. To 50 mL of 3A alcohol or anhydrous methanol, add 0.5 mL
11、phenolphthalein indicator and titrate with 0.01 N NaOH to end point stable for 30 seconds. 2. Add the above neutralized 3A alcohol to the residue from the petroleum ether extraction (#3 above). 3. Titrate to the phenolphthalein end point with 0.01 N NaOH under moderate agitation in a nitrogen atmosp
12、here. Note: If titration is made at a fairly rapid rate, nitrogen atmosphere may be omitted. 4. Calculations: mL of 0.01 N NaOH x 0.07307 = % adipic acid grams of original rubber sample 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.
