1、 FORD LABORATORY TEST METHOD BO 106-04 Date Action Revisions 2000 11 09 Revised Editorial no technical change A. Cockman 1995 10 30 Printed copies are uncontrolled Page 1 of 6 Copyright 2000, Ford Global Technologies, Inc. DETERMINATION OF INERT FILLERS IN POLYMERS Application This method determines
2、 the concentration of inert fillers in polymer resins. Method A is primarily applicable to PTFE fillers but may also be used for other fillers if the hydrolysis products are s oluble in the solvent. Method B is primarily applicable to graphite fillers but may also include diamond, silicon carbide, g
3、lass, bronze, and molybdenum disulfide (MoS2). Method 1 Apparatus Erlenmeyer flask, 500 mL Reflux condenser to fit flask Balance, analytical Weighing paper Graduated cylinders, 5 mL and 1000 mL Hot plate Filter flask with rubber adapter Buchner funnel, medium fritted glass disk, 50 mL capacity Wash
4、bottle Vacuum source Vacuum oven Reagents 50 % aqueous sodium hydroxide Aqueous pyri dine in volumetric ratio of water to pyridine of 4 to 1 Procedure 1. Weigh on glassine weighing paper approximately 2.0 grams of sample to the nearest 50 mg. 2. Carefully transfer sample to a 500 mL Erlenmeyer flask
5、. 3. Reweigh paper. 4. Add 250 mL a queous pyridine to sample. FORD LABORATORY TEST METHOD BO 106-04 Page 2 of 6 Copyright 2000, Ford Global Technologies, Inc. 5. Add 4 mL of 50 % sodium hydroxide solution measured with a 5 mL graduated cylinder. 6. Assemble the flask and condenser on the hot plate.
6、 7. Heat the mixture to a gentle boil, and maintain boiling for 30 minutes for margin resin. Extend the time for powder ground from part. Time will depend on particular size. 8. Swirl the mixture occasionally and wash the sides of the flask with a little aqueous solvent as needed to keep the sample
7、down in the liquid. 9. Turn the hot p late off and let the solution cool slowly. 10. Weigh a Buchner funnel, previously dried 2 hours at 150 C and cooled in a desiccator or dry box, to the nearest 0.1 mg. 11. When the flask is cool enough to be handled comfortably, filter the suspension, ta king car
8、e to transfer the filler completely and to wash the filter cake well with water - pyridine solution. 12. Be sure no residue is left in the stem of the funnel due to evaporation; wash with pyridine if necessary to remove any deposit. 13. Dry the fun nel and contents for at least 3 hours in a vacuum o
9、ven at 150 C, 2.9 - 3.2 kPa vacuum, 0.03 m3/h N2 gas purge. 14. Cool the funnel in dry box or desiccator and then weigh to the nearest 0.1 mg. 15. Clean the funnel with soap and water. Residual graphit e may be removed with “Chromerge“ cleaning solution. Calculations A. Total Filler Funnel tare weig
10、ht Weight dry funnel + filler Paper tare weight Weight paper + sample Weight % Filler = (f - t) x 100 (s - p) Where: f = weight of funnel from Step 14, mg t = weight of funnel from Step 10, mg s = weight of initial sample from Step 1, mg p = weight of paper from Step 3, mg FORD LABORATORY TEST METHO
11、D BO 106-04 Page 3 of 6 Copyright 2000, Ford Global Technologies, Inc. Method 2 Apparatus Du Pont 900 Differential Thermal Analyzer (DTA). Du Pont 950 Thermogravimetric Analyzer (TGA). 0 - 1000 C chart paper, Du Pont Catalog #950252 Eye dropper with capillary tip Tongs, needle nose Microspatula Wire
12、, 100 mm long Microburner Oven at 100 +/ - 2 C Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a con trolled 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
13、 unless otherwise specified. Procedure Measurement of Volatiles 1. Calibrate instruments according to Manufac turers instructions. 2. Set “T“ scale to 50 E C/25 mm. 3. Set “Delta T“ scale to 4 mg/25 mm (2 C/25 mm). 4. Place approximately 22 mg of sample on the balance pan, checking amount added peri
14、odically by turning power switch to “Record“ and back to “Stand By“. 5. Slide sample pan into quartz envelope in the furnace and fasten. 6. Turn on fan. 7. Turn “Power“ switch to “Record“. 8. Set pen at the line, 125 mm above the chart zero with the “100 % Span“ knob. 9. Suppress sample weight using
15、 “Suppression“ kn obs until pen is approximately 2 1/2 lines above the zero. 10. Set the “Delta T“ scale at 0.2 mg/25 mm (0.1 C/25 mm). FORD LABORATORY TEST METHOD BO 106-04 Page 4 of 6 Copyright 2000, Ford Global Technologies, Inc. 11. Complete suppression adjustment to return the pen to the 125 mm
16、 line. 12. On the 900 DTA, press the “Program Reset“ button and set the “Temperature Rate Control“ to 20 C/min. 13. Set “Starting Temperature“ control by turning the “Control“ knob until the meter indicates a small voltage. 14. Turn “Program Mode“ switch to “Heat“. 15. Drop recorder pen. 16. Quickly
17、 make any adjustmen t at the 125 mm line with the “Fine Suppression“ knob before temperature rise begins. 17. Lift pen when sample temperature reaches 200 C. 18. Turn “Program Mode“ to “Off“. 19. Turn “Power“ switch to “Stand By“. 20. Remove sample pan from furnace. Measurement of Percent Graphite 1
18、. Press “Reset“ button and turn “Starting Temperature“ to reading C - 12. 2. Set “Temperature Rate Control“ to 5 C/min. 3. Switch from “Temperature“ to “Time Base“. 4. Set “Program Mode“ to “Isothermal“. 5. Turn “Power“ s witch to “Record“. 6. While furnace is equilibrating, set “Delta T“ scale to 4
19、 mg/25 mm (2 C/25 mm). 7. Remove all suppression with “Suppression“ knobs. 8. Reset pen at the 125 mm line with the “% Span“ knob. 9. After furnace has equilibrated 5 minute s, reset pen to zero time by pressing “Reset“ button. Note 1: Pen assembly will travel 25 mm along the “T“ scale in a 5 minute
20、 period. 10. Slide sample pan carefully into furnace. FORD LABORATORY TEST METHOD BO 106-04 Page 5 of 6 Copyright 2000, Ford Global Technologies, Inc. 11. Drop recorder pen. 12. Quickly make any adjustment to the 125 mm line with “% Span“ knob before weight loss begins. 13. Record weight loss until
21、weight percent remaining is less than 25 % for SP - 21 or 50 % for SP - 22. 14. Without raising recorder pen, change the “Delta T“ scale to 1 mg/25 mm (0.5 C/25 mm) or 2 mg/25 mm (1 C /25 mm) for SP - 21 and SP - 22, respectively. 15. Record weight loss for at least 30 minutes after sample has lost
22、10 % of its original weight. 16. Raise recorder pen. 17. Set “T“ scale to 100 C/25 mm. 18. Change from “Time Base“ to “Temperature“. 19. M ake dot on chart paper with recorder pen for a temperature record. 20. Turn “Power“ switch to “Stand By“. 21. Change “Program Mode“ to “Off“. 22. Return “Span“ k
23、nob to “100 %“. 23. Remove sample pan from furnace to cool. 24. Turn off fan. 25. Detach furnace and cool with stream of air. 26. Reposition furnace on 950 TGA. 27. Slide sample pan into furnace and disconnect quartz envelope. 28. Remove sample pan from furnace. 29. Clean samples pan by carefully bl
24、owing residue from it with an eye droppe r having a capillary tip. 30. Heat sample pan in place to red heat with a microburner to remove any remaining contaminants. 31. Run next sample starting with Step 1 of Measurement of Volatiles or slide sample pan into furnace for protection until next ru n is
25、 made. FORD LABORATORY TEST METHOD BO 106-04 Page 6 of 6 Copyright 2000, Ford Global Technologies, Inc. Calculations The percent volatiles and percent graphite (on a volatiles - free basis) are read directly from the chart record. Record as the volatiles level the percent weight loss up to 150 C. Re
26、cord as percent graphite, the percent of samp le weight remaining 25 minutes after 10 % of the weight is lost. (Read to nearest 0.5 %). (Correction factor for MoS2 is 1.11 x % weight remaining.) Alternate Method B Apparatus DuPont Thermal Analyser 9900 Thermogravimetric Analysis Program Procedure 1.
27、 Set up equipment to Manufacturers instructions. 2. Place 20 mg of sample into analyzer pan. 3. Select Gas 1 (Argon) 4. Set ramp temperature for 20 C/minute up to 700 C. 5. Set ISO - track for 20 minutes. 6. Equilibrate at 450 C. 7. Select G as 2 (Air). 8. Set ramp temperature for 5 C/minute up to 7
28、00 C. 9. Set ISO - track for 20 minutes. Calculations The % graphite by weight is determined as the weight change that occurs after the introduction of the air. The residual ash content (if fo und present) would have to be subtracted from this figure. 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.
