1、 FORD LABORATORY TEST METHOD AJ 150-02 Date Action Revisions 2001 01 16 Revised Editorial no technical change A. Cockman 2000 03 22 Editorial no technical change A. Cockman 1991 09 24 Printed copies are uncontrolled Page 1 of 3 Copyright 2001, Ford Global Technologies, Inc. MOLYBDENUM DISULFIDE AND
2、POLYETHYLENE IN GREASES Application This method is used to determine the polyethylene and the molybdenum disulfide content in greases when solid lubricant components are exclusively polyethylene and/or molybdenum disulfide. Refer to FLTM AJ 106-02 when solid lubricants and/or fillers in addition to
3、polyethylene and/or molybdenum disulfide are present. Apparatus Required Analytical Balance Precision +/- 0.1 mg Mechanical Convection Oven Capable of maintaining a temperature of 105 +/- 2 C Muffle Furnace Capable of maintaining a temperature of 550 +/- 10 C Desiccator Hydrosol Stainless Filter Hol
4、der (Millipore) Filter Paper #42, cut out a circle the same size as a millipore filter. Porcelain Crucible Beaker 400 mL, low form Beaker 100 mL, tall form Funnel Approximately 50 mm diameter, glass Mixer Vacuum Pump FORD LABORATORY TEST METHOD AJ 150-02 Page 2 of 3 Copyright 2001, Ford Global Techn
5、ologies, Inc. Suction Bottle Woulff (Vacuum) Bottle The above apparatus may be obtained from any reputable laboratory equipment supply house. Materials Required Toluene Reagent grade; CAUTION: Low flash point* Petroleum Naphtha (U-MC 004-8004-2) (M14J148) Reagent grade; CAUTION: Low flash point* Eth
6、yl Alcohol (Absolute) Reagent grade; CAUTION: Low flash point* Xylene Reagent grade; CAUTION: Low flash point* Acetic Acid Concentrated Reagent grade; CAUTION: Corrosive substance* Filter Paper No-42 (Cut out a circle the same size as a millipore filter). * Users of this test method should ensure th
7、at they comply with all governmental and (if a Ford Motor Company activity) Company regulations regarding the handling and use of the above materials. Company users shall contact their industrial hygiene and environmental activities for appropriate precautions. Conditioning and Test Conditions All t
8、est 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. Procedure 1. Weigh out 10 g grease to the nearest 0.01 g in
9、 a 400 mL beaker. 2. Mix 80 mL toluene, 80 mL petroleum naphtha, 80 mL ethyl alcohol, and 20 mL acetic acid. Add 160 mL of this mixture to the 400 mL beaker. FORD LABORATORY TEST METHOD AJ 150-02 Page 3 of 3 Copyright 2001, Ford Global Technologies, Inc. 3. Stir with the mixer until grease (i.e., th
10、e oil and soap portion) has completely dissolved (approximately 30 min). 4. Dry and weigh the filter paper to the nearest mg and place the filter on the diaphragm-filter equipment. 5. Filter the grease solution with the aid of a vacuum. Wash the residue with the remaining 100 mL solvent-acid mixture
11、, followed by washing with 50 mL acetone, ensuring that nothing is visually perceived to adhere to the sides of the beaker. 6. Remove filter together with residue and dry in the oven for 2 h at 105 +/-2 C. 7. Cool in the desiccator and weigh. Subtract from this weight the weight of the filter and re
12、cord the result as “weight 1“. 8. Place the filter with residue in the tared porcelain crucible and heat in the muffle furnace for 2 h at 550 +/- 10 C. 9. Cool in a desiccator and reweigh. The gain in weight of crucible represents weight of MoO3. This weight must be multiplied by 1.112 and recorded
13、as “weight 2“ (MoS2). Calculations MoS2 (%) = weight 2 x 100 weight of sample Polyethylene (%) = weight 1 - weight 2 x 100 weight of sample Note: If it is necessary to extract polyethylene for IR identification, repeat procedure, paragraphs 1 to 6 for the second sample. (The accuracy of the weight i
14、s not important). The residue will be dissolved in approximately 50 mL xylene at a temperature of 135 C for 30 minutes. Then filter the hot solution into a 100 mL beaker. Evaporate xylene and press a film from the recovered polyethylene for an IR scan according to FLTM AO 150-01. 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.
