1、 FORD LABORATORY TEST METHOD EU-AP 050-02 Date Action Revisions 2001 01 31 Revised Editorial no technical change A. Cockman 2000 04 19 Editorial no technical change A. Cockman 1993 10 19 Printed copies are uncontrolled Page 1 of 4 Copyright 2001, Ford Global Technologies, Inc. CHEMICAL-PHYSICAL ANAL
2、YSIS OF VULCANISED RUBBER COMPOUNDS Application This test method is applicable for the testing of vulcanized compounds for all rubber parts (test slabs and finished parts), and is used for the determination of: A. Acetone extract-quantitatively (gravimetric). B. Infrared spectrogram of the acetone e
3、xtract for reference and comparison with subsequent deliveries. C. Ash content-quantitatively (gravimetric). D. Elastomer content quantitatively. E. Infrared spectrogram of the elastomer compound pyrolysate. Apparatus and Chemicals Required Infrared Spectrophotometer Double beam type - capable of re
4、cording over a wavelength range of approx 2 - 15 microns and accessories. Sodium Chloride Plates or equivalent Suitable for the infrared spectrophotometer. Laboratory Distillation (simple type) Electric Heating Mangle For 250 mL flasks - 3 stage adjustable. Soxhlet Extraction Apparatus With 70 mL ex
5、tractor and 250 mL narrow neck flask. Evaporation Dish 100 mL Analytical Balance Accuracy +/- 1 mg FORD LABORATORY TEST METHOD EU-AP 050-02 Page 2 of 4 Copyright 2001, Ford Global Technologies, Inc. Muffle Furnace Capable of maintaining a temperature of 800 +/- 25 C. Retort Stand With 2 round clamps
6、, 3 flask clamps together with a mounting ring to support the soxhlet apparatus and the heating mantle. Acetone (A.R.) Porcelain Crucible with Cover Desiccator with Silica Gel Combustion Apparatus Grote-Krekeler type with electrical heating. Adjustable resistance, temperature recorder and porcelain
7、boat. Inert Gas e.g., nitrogen, helium or argon, pure and free from oxygen and moisture. Test Tubes 130 x 14 mm Fiolax No. 28 or equivalent. Bunsen Burner Cotton Wool Test Tube Clamps n-Propylalcohol (A.R.) Laboratory Convection Oven Capable of maintaining a temperature of 80 +/- 2 C. Glass Beaker 5
8、0 mL 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 otherwise specified. FORD LABORATORY
9、TEST METHOD EU-AP 050-02 Page 3 of 4 Copyright 2001, Ford Global Technologies, Inc. Procedure 1. Cut from the material under test (test slab or finished part) small pieces of max 5 mm side. Weigh approx. 6-8 g of the material to the nearest mg (E1). Before cutting, all parts must first be rinsed wit
10、h ethanol and then briefly with petroleum ether (38-70 C) in order to remove surface materials such as glycerin, grease etc. Allow 5 minutes minimum drying time before weighing. 2. Then extract with acetone for 24 h or as otherwise specified. 3. After extraction, dry in the oven at 80 +/- 2 C for 8
11、h or to constant weight, cool to 23 +/- 2 C, then reweigh to the nearest mg (E2). 4. Approx 1 g of the cleaned rubber is used to determine the ash content according to EU-BO 6-2 with the exception of 800 C instead of 950 C muffle furnace temperature (double determination). 5. The acetone extract mus
12、t be distilled to a volume of approx 10 mL, and finally dried in an oven at 80 +/- 2 C for 5 h. 6. The extract, which has been freed of acetone, is applied to the NaCl window of a demountable cell, using a glass rod, and with the aid of a distance ring and a second NaCl window, pressed to a thicknes
13、s of 0.025 mm, after which the infrared curve is recorded over the range of approx 2 15 microns. 7. Weigh approx 0.5-l.0 g of the extracted rubber to the nearest mg in the porcelain boat of the Grote-Krekeler apparatus (E3) in order to determine elastomer content. Pass the inert gas through for seve
14、ral minutes before commencing the combustion. Thermal decombustion is carried out at 650 700 C under an inert gas flow of approx 50 mL per minute. The combustion should be slow. The moveable oven will be pushed slowly in relation to the sample. The decombustion time should be approx 15 minutes. Afte
15、r cooling to 23 +/- 2 C in the desiccator, reweigh to the nearest mg (E4). In cases of doubt parallel to the above operation a qualitative and quantitative filler determination must be performed. The respective methods must be agreed upon both by supplier and customer. 8. 300 - 500 mg of the extract
16、ed rubber should be transferred into a test tube. Close the opening of the test tube with a cottonwool plug which has been soaked in n-propylalcohol. Pyrolyse for 2 minutes in the hot flame of the Bunsen burner (flame height approx 3 - 4 cm), or by an approved instrumental technique. Filter the pyro
17、lysed products out of the test tube and cottonwool plug using 5 mL n-propylalcohol into a 50 mL glass beaker. The filtrate is applied to the NaCl window of a demountable cell, using a glass rod, dry in the oven at 80 +/- 2 C for 1 h, and with the aid of a distance ring and a second NaCl window, pres
18、sed to a thickness of 0.025 mm, after which the infrared curve is taken at a range of approx 2 - 15 microns. FORD LABORATORY TEST METHOD EU-AP 050-02 Page 4 of 4 Copyright 2001, Ford Global Technologies, Inc. Evaluation A. Quantitative evaluation of the acetone extract. Acetone soluble = E 1 - E 2 x
19、 100 E1 B. Qualitative evaluation of the acetone extract: The infrared spectrum of the acetone extract should be filed for reference and comparison with subsequent deliveries. C. Quantitative determination of ash content. Evaluation - see EU-BO 6-2 D. Quantitative evaluation of the elastomer content
20、. Elastomer content of the acetone extracted rubber in % Percent = E 3 - E 4 x 100 E3 E. Qualitative evaluation of the pyrolysed product of the elastomer content of the acetone extracted rubber: The spectrum of the pyrolysed product should be filed for reference and comparison with subsequent deliveries. 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.
