1、FoRDLABORAToRYTESTMEJrBOD Eu-AJ 5-1 DETERMINATION OF MOLYBDENUM DISULPHIDE IN GREASES Amlication This procedure is used to determine the molybdenum disulphide content of greases. The method is also applicable to molybdenum disulphide - polyethylene filled greases since this plastic dissolves in chlo
2、rinated solvents. ApDaYatUS and ReaPents Required Analvtical Balance Accuracy +/- 0.1 mg Mechanical Convection Oven Capable of maintaining temperatures up to 105 +/- 2 C. Muffle Furnace Capable of maintaining temperatures up to 520 +/- 5 C. Hood and Hot Plate Water Bath Desiccator With wing agent (e
3、.g. calcium chloride) Seitz Filter Size F. Type K 5 or other suitable filter. Gooch Crucible With fine asbestos mat. Filter Paper Whatman No. 41 H or similar. Cruicibles with Lid Nickel and porcelain. Erlernever Flasks 150 mL capacity. HvdrocJen Sulphide Kipps apparatus or equivalent incorporating a
4、 gas take off line and valve. Trichlorobenzene Technical grade. Automotive Safety and hgineering Standards Ofce Page 1 of 3 1993 10 18 - - 9009160 0041092 326 = - - - FORD LABORATORY TESTMEIIiOD Eu-AJ 5-1 Al coho 1 Denatured I Benzol Sodium Hydroxide 5 normal. Dilute SulDhuric Acid 50 % (V - V) 1 %
5、(v - v) 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 8 relative humidity for not less than 24 h prior to testing and tested under the same conditions unless ocherwise specified. Procedure Pro
6、cedure A - Molvbdenum Disuhhide Present Only as Filler 1. Weigh out approx 5 g of grease into a tared 250 mL beaker. 2. Add 100 mL of trichlorobenzene and bring to a slow boil on a hot plate under a hood. Maintain slow boiling until grease (exclusive of Mo$ or other fillers) has completely dissolved
7、. 3. Filter sample through a tared Seitz filter, maintaining the filter apparatus at approx 80 C or higher by means of a water jacket heater, or equivalent, around the filter. 4. Wash flask and filter several times with hot trichlorobenzene, followed by several washes with benzol. Remove filter pad
8、with MOS, and, if no other filler is present, &y in an oven at 105 +/- 2 C for 30 minutes. 5. Cool in a desiccator and weigh. Evaluation Mos2 (%) - Gain in Weirrht x 100 Weight of Sample - . FORD LABORATORY TEsTMEiOD Eu-AJ 5-1 Procedure B - Fillers Other than Molvbdenum Diculphide Precenc 1. 2. 3. 4
9、. 5. 6. 7. 8. 9. Remove filter pad from crucible, place in a porcelain crucible and heat in a muffle furnace at 510 - 520 C for 2 h. This converts the black Mos2 to brownish yellow Moo3. Treat the contents of the crucible with hot 5 N NaOH solution to dissolve the Mo4 and filter through filter paper
10、 into a 150 mL Erlenmeyer flask. Wash filter with hot NaOH and hot water. Dilute to 100 mL with distilled water, heat to boiling and treat with H2S for 10 minutes. Add dilute H2S04 (1-1) until acid and then 4 mL in excess per 100 mL of solution. Gas with H2S for 5 minutes and digest on a water bath
11、until the precipitate settles. Filter through a tared Gooch crucible that has been prepared with fine asbestos and heated to 520 C for 1 h and cooled in a desiccator. Wash the precipitate on the filter several times with dilute H2SO4 (1-99) and finally with alcohol until free from acid. Place the Go
12、och crucible in a larger nickel crucible with a porcelain lid. Dry at 100 C and heat gently in a muffle furnace at 425 C until the odour of SO, can no longer be detected. Remove the cover, heat to 510 - 520 C until constant weight is obtained. 10. Cool in a desiccator and weigh. Gain in weight of cr
13、ucible represents weight of MOO,. Evaluation MOO, (%) - Weight of MOO? x 111.1 Weight of Sample 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. Materials & Fastener Quality Research & Engineering Centre Dunton Engineering Materials & Standards Environmental & Safety Engineering Dearborn Automotive Safety and Engineering Standards Office 1993 10 18 9009160 0041094 IT9 Page 3 of 3
