1、 This document is restricted and may not be sent outside International Truck and Engine Corporation or reproduced without permission from Corporate Technical Standards. Suppliers are required to assume all patent liability. Ga42001 by International Truck and Engine Corporation. OCTOBER 2001 Page 1 o
2、f 3 INTERNATIONAL TRUCK AND ENGINE CORPORATION CEMS (CORPORATE ENGINEERING MATERIAL SPECIFICATION)NUMBER: CEMS DT-3 TITLE: Methods of Determining Glass And PTFE Fillers In Thermoplastic UrethaneCURRENT ISSUE DATE: October 2001 WRITTEN/REVIEWED BY: Materials Engineering APPROVED BY: Materials Enginee
3、ring SUPERSEDES ISSUE OF: July 1999 PRINTED COPIES OF THIS DOCUMENT MUST BE VERIFIED FOR CURRENT REVISION This specification may involve hazardous materials, equipment, and procedures. This specification does not purport to address all of the safety issues associated with its use. The user is respon
4、sible to consult appropriate safety and health practices and to determine the applicability of regulatory limits prior to use. Change Notice: Reformatted and Editorial Changes 1.0 SCOPE These are wet and thermogravimetric methods (Method A and B respectively) for determining the respective amounts o
5、f fiber glass and PTFE fillers in thermoplastic urethane. METHOD A: Wet Method 2.0 APPARATUS 2.1 Flasks, Pyrex, 125 ml 2.2 Crucibles, 30 ml, Nickel or Platinum 2.3 Centrifuge Tubes, 100 ml 2.4 Balance 0.1 mg Sensitivity 2.5 Hot Plate 2.6 Oven, Gravity or Recirculating; Capable of Maintaining Tempera
6、ture of 650 5C 2.7 Centrifuge, Capable of 700 rcf 2.8 Fume Hood 2.9 Desiccator 3.0 MATERIAL 3.1 1 - Methyl, 2 - Pyrrolidinone, Commercial Grade 3.2 Acetone, ACS 3.3 Filter Paper, Ashless, Whatman 541 or Equivalent 4.0 PROCEDURE WET METHOD 4.1 Dry an empty 125 ml flask 10 minutes at 105 + 5C. Cool in
7、 a desiccator. 4.2 Weigh the dried flask to 0.1 mg, record this tare weight as (W1). Weigh into the tared flask approximately 2 grams of the material to be tested. Record weight of flask and sample as (W2). 4.3 Add 50 ml of 1-methyl, 2-pyrrolidinone and heat on hot plate to 200C; agitate the flask f
8、requently until the urethane is completely dissolved. NUMBER: CEMS DT-3 TITLE: Glass And PTFE Fillers In Thermoplastic Urethane Wet MethodCURRENT ISSUE DATE: October 2001 This document is restricted and may not be sent outside International Truck and Engine Corporation or reproduced without permissi
9、on from Corporate Technical Standards. Suppliers are required to assume all patent liability. Ga42001 by International Truck and Engine Corporation. OCTOBER 2001 Page 2 of 3 4.4 Weigh an empty dried 100 ml centrifuge tube, record this tare weight as (W3). Quantitatively transfer the contents of the
10、flask to the tared tube. Rinse the flask into the tube with two 10 ml portions of 1-methyl, 2 pyrrolidinone. Centrifuge for 10 minutes at 700 rcf. (CAUTION: For balance, centrifuge tubes must be run in pairs and each tube must contain approximately the same amount of liquid.) 4.5 Carefully decant of
11、f the liquid and wash the solids twice with 1-methyl, 2-pyrrolidinone; then twice with acetone using 25 ml of fresh solvent each time; centrifuge and decant, as above, after each washing. 4.6 After the final wash, dry the tube and residue in a hot air oven for 45 minutes at 105 + 5C; cool in a desic
12、cator, and weigh; record the weight of the dried tube and contents as (W4). 4.7 Using either acetone or 1:1 acetone-distilled water mixture, quantitatively transfer and filter the residue. Discard the filtrate. 4.8 Weigh a dried empty 30 ml Pt or Ni crucible; record this tare weight as (W5). Transfe
13、r the filter paper and residue to the tared crucible. Ignite the filter paper and place in an oven at 650 + 5C for 2 hours. (CAUTION: Decomposition products of PTFE should not be inhaled; therefore, the ignition should be done in a fume hood and the oven should be located in a fume hood.) 4.9 Cool i
14、n a desiccator and weigh the crucible and contents; record as (W6). 5.0 CALCULATIONS Calculate percent fillers as shown below: 100%1256xWWWWGlass= 100)()(%125634xWWWWWWPTFE= W1= Tare Weight of Flask W2 = Weight of Flask and Sample W3= Tare Weight of Centrifuge Tube W4= Weight of Centrifuge Tube and
15、Residue W5 = Tare Weight of Crucible W6= Weight of Crucible and Residue after ignition 6.0 REPORT Report filler content as % glass and % PTFE. METHOD B: Thermogravimetric Method 7.0 THERMOGRAVIMETRIC ANALYSIS METHOD This is an instrumental method for determining the respective amounts of fiberglass
16、and PTFE fillers in thermoplastic urethane. 8.0 APPARATUS Thermogravimetric Analysis (TGA) system capable of continuously recording temperature and sample weight as sample is heated in a controlled atmosphere. The system will be capable of uniformly increasing the temperature at a rate of 15C per mi
17、nute between 20 and 900C. The integral balance will have a minimum capacity of 25 mg and 0.5 mg sensitivity. NUMBER: CEMS DT-3 TITLE: Glass And PTFE Fillers In Thermoplastic Urethane Wet MethodCURRENT ISSUE DATE: October 2001 This document is restricted and may not be sent outside International Truc
18、k and Engine Corporation or reproduced without permission from Corporate Technical Standards. Suppliers are required to assume all patent liability. Ga42001 by International Truck and Engine Corporation. OCTOBER 2001 Page 3 of 3 9.0 PROCEDURE 9.1 Place approximately 20 mg of material to be tested on
19、 the pan. Maintaining a Nitrogen atmosphere, heat sample at a rate of 15C per minute from room temperature to 800C. 9.2 When temperature reaches 800C change the atmosphere to air and continue heating until sample reaches 900C. 9.3 From the resulting thermogram (sample weight versus temperature) determine and record the sample weight at 25C, 510C, 595C, and 900C. 10.0 CALCUATIONS 10025595510% xCWeightatCWeightatCWeightatPTFE= % Fiber Glass = Weight at 900CWeight at 25Cx 100 11.0 REPORT Report filler content as % glass and % PTFE.
