1、 FORD LABORATORY TEST METHOD AJ 006-03 Date Action Revisions 2000 08 07 Editorial no technical change A. Cockman 1992 04 28 Printed copies are uncontrolled Page 1 of 3 Copyright 2000, Ford Global T echnologies, Inc. DETERMINATION OF BARIUM SOAP CONTENT IN GREASES Application This procedure is used t
2、o determine the barium soap content in a grease by separating the petroleum ether insoluble components. Apparatus Required Balance Sensitivity of 0.1 g. VWR Catalog No . 11350 - 263 or equivalent. Beaker 1000 mL VWR Catalog No. 13922 - 142 or equivalent. Beaker 300 mL (tall form) VWR Catalog No. 139
3、22 - 062 or equivalent. Round Bottom Flask 1000 mL 24/40 VWR Catalog No. 29122 - 123 or equivalent. Soxhlet Extraction Apparatus Large; top 55/50; bottom 24/40 VWR Catalog No. (TBD) or equivalent. Extraction Condenser Large 55/50 VWR Catalog No. (TBD) or equivalent. Glass-Col Heater To fit 1000 mL r
4、ou nd bottom flask VWR Catalog No. (TBD) or equivalent. Graduated Cylinder 500 mL VWR Catalog No. 24710 - 180 or equivalent. Magnetic Stirrer VWR Catalog No. 58941 - 004 or equivalent. Oven Capable of maintaining 70 +/ - 3 C VWR Catalog No. 52347 - 463 or equiva lent. FORD LABORATORY TEST METHOD AJ
5、006-03 Page 2 of 3 Copyright 2000, Ford Global Technologies, Inc. Steam Bath VWR Catalog No. 13546 - 007 or equivalent. Weighing Bottle VWR Catalog No. 16713 - 182 or equivalent. Whatman Extraction Thimble 25 x 80 mm VWR Catalog No. 27730 - 081 or equivalent. Boiling Chips “Boileezers“ B - 365 or eq
6、uivalent. Source: Fisher Scientific Co. Infrared Spectrophotometer Emission Spectrograph Materials Required Petroleum Ether Reagent grade. Caution: Extremely flammable - refer to Fire Control Bulletin No. 18. Refer to Industrial Hygiene for health and safety precaut ions. Filter Paper Fluted Whatman
7、 No. 42 ashless filter paper. VWR Catalog No. 28480 - 060 or equivalent. 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 % relative humidity for not less than 24 h prior to testing and tested
8、under the same conditions unless otherwise specified. Procedure 1. Dry an extraction thimble containing a fluted Whatman No. 42 ashless filter paper in an oven at 70 +/ - 3 C for 30 minutes. 2. After cooling to ambient in a desiccator, determine the weight of the thimble and filter paper by differen
9、ce using a tared weighing bottle. Weight of thimble and filter paper = A. FORD LABORATORY TEST METHOD AJ 006-03 Page 3 of 3 Copyright 2000, Ford Global Technologies, Inc. 3. Thoroughly mix the grease, place 10 - 15 g o nto the filter paper and replace in thimble. Determine the weight of the thimble,
10、 filter paper and grease by difference using a tared weighing bottle. Weight of thimble, filter paper and grease = B. 4. Make a cap from the bottom of another thimble. Pla ce the cap inside the thimble to cover the filter paper and grease. 5. Place the thimble containing the filter paper, grease and
11、 cap in a soxhlet extraction tube. 6. Fill the flask that is to be used with the soxhlet tube approximately 2/3 full with petr oleum ether. Include a half dozen boiling chips. 7. Reflux until petroleum ether in soxhlet tube is clear and “water white.“ Usually 48 h refluxing is sufficient. Additional
12、 petroleum ether may be added to maintain solvent level throughout refluxing per iod. 8. Remove the thimble containing the filter paper and the grease insolubles and place into a 300 mL tall form beaker and dry on a steam bath with hood for about 2 h. 9. Place the 300 mL beaker containing the thimbl
13、e, filter paper, grease insolubles and cap into a 70 +/ - 3 C oven and dry to a constant weight. Do not include the cap in the weighing. Determine the weight by difference in a tared weighing bottle. Weight of thimble, filter paper, and grease insoluble = C. 10. % grease insolubles = ( C - A ) x 100
14、 = % soap ( B - A ) 11. The portion of the grease insolubles that is a barium soap can be determined using an infrared spectrophotometer and an emission spectrophotometer. Chemicals, materials, parts, and equipment referenced in this docum ent must be used and handled properly. Each party is responsible for determining proper use and handling in its facilities.
