1、 FORD LABORATORY TEST METHOD AJ 005-01 Date Action Revisions 2000 08 07 Editorial no technical change A. Cockman 2000 03 10 Editorial no technical change A. Cockman 1992 04 28 Printed copies are uncontrolled Page 1 of 2 Copyright 2000, Ford Global Technologies, Inc. DETERMINATION OF MOLYBDENUM DISUL
2、FIDE IN GREASES Application This procedure is used to determine the molybdenum disulfide content of greases. The method is also applicable to MoS 2 - polyethylene filled greases since this plastic dissolves in chlorinated solvents. Apparatus Required Laboratory Balance Oven Muffle Furnace Hood and H
3、ot Plate Water Bath Desiccator Seitz Filter Gooch Crucible with Fine Asbestos Mat Reagents Required Hydrogen Sulfide Trichlorobenzene - Technical Grade Alcohol - Denatured Benzol Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a controlled atmos
4、phere of 23 +/ - 2 C and 50 +/ - 5 % relative humidity for not less than 24 h prior to testing and tested under the same c onditions unless otherwise specified. Procedure 1. Weigh out approximately 5 g of grease into a tared 250 mL beaker. 2. Add 100 mL of trichlorobenzene and bring to a slow boil o
5、n a hot plate under a hood. Maintain slow boiling until grease (exclusive o f MoS 2 or other fillers) has completely dissolved. 3. Filter sample through a tared Seitz filter, Size F, Type K5 (or other suitable filter medium), maintaining the filter apparatus at approximately 180 F or higher by means
6、 of a water jacketed heater, or equivalent, around the filter. FORD LABORATORY TEST METHOD AJ 005-01 Page 2 of 2 Copyright 2000, Ford Global Technologies, Inc. 4. Wash flask and filter several times with hot trichlorobenzene, followed by several washes with benzol. Remove filter pad with MoS 2 and,
7、if no other filler is present, dry in an oven at 220 F for 30 minutes. Cool in a desiccator and weigh. Gain in Weigh x 100 = % MoS 2 Wt. of Sample If fillers other an MoS 2 are present: 5. (a) Remove filter pad from crucible, place in a porcelain crucible and heat in a muffle furnace at 950 - 975 F
8、for 2 h. This converts the blac k MoS 2 to brownish - yellow MoO 3 . 6. (a) Treat the contents of the crucible with 5 N NaOH solution to dissolve the MoO 3 and filter through Whatman No. 41H paper into a 150 mL Erlenmeyer flask. Wash filter paper with hot NaOH and hot water. 7. (a) Dilute to 100 mL
9、with distilled water, heat to boiling and treat with H 2 S for 10 minutes. 8. (a) Add dilute H 2 SO 4 (1 - 1) until acid and then 4 mL in excess per 100 mL of solution. 9. (a) Gas with H 2 S for 5 minutes and digest on a water bath until the precipitat e settles. 10. (a) Filter through a tared Gooch
10、 crucible (prepared with fine asbestos and heated to 975 F for 1 h). 11. (a) Wash the precipitate on the filter several times with dilute H 2 SO 4 (1 - 99) and finally with alcohol until free from acid. 12. (a) Place the Gooch crucible in a larger nickel crucible with a porcelain lid. Dry at 210 F a
11、nd heat gently in a muffle furnace at 800 F until the odor of SO 2 can no longer be detected. 13. (a) Remove the cover, heat to 950 - 975 F until constant wei ght is obtained. 14. (a) Cool in a desiccator and weigh. Weight of MoO 3 x 111.1 = % MoS 2 Weight of Sample Chemicals, materials, parts, and equipment referenced in this document must be used and handled properly. Each party is responsible for determin ing proper use and handling in its facilities.
