1、 FORD LABORATORY TEST METHOD EU-AZ 053-01 Date Action Revisions 2001 01 31 Revised Editorial no technical change A. Cockman 1994 02 28 Printed copies are uncontrolled Page 1 of 4 Copyright 2001, Ford Global Technologies, Inc. PYROLYTIC GAS CHROMATOGRAPHIC ANAYLSIS OF FRICTION MATERIALS Application T
2、his procedure provides a characteristic quantitative chromatogram of the pyrolysis products from a friction material and shall also be used to establish the specification limited for the reference sample of a given formulation. Apparatus Dual Flame Gas Chromatograph Hewlett Packard 5750 Series Strip
3、 Chart Recorder 200 - 250 mm chart width with a sensitivity of 1 - 2 mV full scale. Chromatographic Columns 1.829 m x 3.175 mm stainless steel, packed with 10 % silicone gum rubber on 80 - 100 mesh silsanised diatomaceous earth support. Alternative columns may be required for some analyses. The reso
4、lution of the column shall comply with the Appendix. Electronic Integrator Infotronics CRS.100 Pyrolysis Equipment Model 80 - Pyrolysis unit manufactured by Hewlett Packard Ltd. A 0 3 volt A.C. voltmeter with input impedance of 10 ohms or more must be conducted across the output cable. Compressed Ga
5、ses Hydrogen - Electrolytic grade. Air - Prepurified air. Carrier gas - High purity inert gas. Where equipment is no longer available, alternative units are permissible provided the equipment does not substantially alter the requirements in the Materials Specification and that prior Materials Engine
6、ering approval is obtained. FORD LABORATORY TEST METHOD EU-AZ 053-01 Page 2 of 4 Copyright 2001, Ford Global Technologies, Inc. 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 humidit
7、y for not less than 24 h prior to testing and tested under the same conditions unless otherwise specified. Procedure A thorough description of the chromatograph and pyrolysis unit and their operation is given in the instruction manuals for the instruments. The operator must familiarize himself with
8、the contents of these manuals. From a transverse section of the sample filed to approx 45, an homogeneous powder sample is abraded from the surface. Introduce the tip of the probe into the powdered sample such that the sample is retained in the apex of the tip. Remove residual material on exterior o
9、f the probe. Perform test run with operating conditions as follows: 1. Injection port temperature 250 C 2. Detector temperature 25 C above final column temperature. 3. Post injection interval 0 minutes. 4. Upper limit interval: 20 minutes or until column is clear, whichever is longer. 5. Starting co
10、lumn temperature 50 C 6. Final column temperature 230 C unless stated otherwise in the Material Specification. 7. Temperature programme rate: 4 C/min unless stated otherwise in the Material Specification. 8. Chart speed 10.0 mm/min nominal. 9. Integrator settings shall be optimised for the analysis.
11、 10. Pyrolysis conditions are 1200 C for 12 seconds (alternative equipment may require different conditions). FORD LABORATORY TEST METHOD EU-AZ 053-01 Page 3 of 4 Copyright 2001, Ford Global Technologies, Inc. Allow the oven temperature to cool to 40 C. When the oven temperature reaches 50 C, pyrols
12、e for 12 seconds. When the pyrolsis period is commenced the start buttons on the chromatograph and the integrator are pressed simultaneously to commence the programme. Do not alter attenuation during a test run. At the end of the temperature programmed interval the oven temperature is held at maximu
13、m temperature for 20 minutes or until the column is purged clear to avoid contaminating succeeding runs. Calculation The chromatogram obtained is accompanied by a quantitative print out of the individual peak areas, and a summation of the total peaks. Individual peaks are expressed as a percentage o
14、f the total peak area. 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. FORD LABORATORY TEST METHOD EU-AZ 053-01 Page 4 of 4 Copyright 2001, Ford Global Techn
15、ologies, Inc. PYROLYTIC GAS CHROMATOGRAPHIC ANALYSIS OF FRICTION MATERIALS Appendix 1 Resolution The chromatograph is operated with the usual 6.35 mm stainless steel column for a test run except that no sample is pyrolysed but 0.1 L of a standard liquid is injected onto the column. The standard liqu
16、id is a mixture of equal parts by weight 18 phenols and hydrocarbons commonly found in friction material pyrolysate. The chromatogram below is required and carries a list of the component materials. This diagram is qualitative only. Peaks 5 and 6 must occur as single peaks with no evidence of splitting. Peak 10 should show at least a shoulder and preferably two separate peaks. Peaks 11 and 12 must also be separated as indicated.
