1、 FORD LABORATORY TEST METHOD AJ 001-02 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 Technologies, Inc. TOTAL SAPONIFIABLE MATTER AND ADDED SULFUR IN GEAR LUBRICANTS Application This proced
2、ure is used to determine the total saponifiable matter and added sulfur in petroleum oil base lubricants which are used for lubrication of gears. Description of Methods This procedure describes two methods - one for total saponifiable matter and the other for added sulfur. The two methods are combin
3、ed in this procedure since it is necessary to separate the saponifiable material when determining added sulfur. The proced ure involves a dilution of the heavy oil, acidification to free the added sulfur compounds, saponification of the neutral fats and fatty acids, and extraction of the soap thus f
4、ormed from the mineral oil with alcohol and ether. Sulfur is determined by the bomb method on the original sample and the extracted mineral oil and the difference calculated as added sulfur. Apparatus Required Saponification Flask The 300 mL saponification flask and the condenser tube are both Corni
5、ng No. 7280. They are made of b oron - free, alkali resistant glass with Ts 24/60 joints. Additional Apparatus Separatory funnel, 500 mL, Pyrex with ground glass stopper; water or steam bath; laboratory balance; electric hot plate. Reagents Required Benzol, ACS - Sulfur free; isopropyl al cohol, ACS
6、; hydrochloric acid (1:1); petroleum ether, reagent grade (BP 30 - 60 C); ethyl ether, ACS. Alcoholic Potassium Hydroxide Weigh 60 g of KOH (ACS) and heat in 500 mL of 3A alcohol with stirring. When dissolved, allow to stand overnight to precip itate carbonates. Decant or siphon through asbestos and
7、 dilute to one liter with 3A alcohol. 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 under the same conditions unless ot
8、herwise specified. FORD LABORATORY TEST METHOD AJ 001-02 Page 2 of 3 Copyright 2000, Ford Global Technolo gies, Inc. Procedure 1. Weigh 5 to 6 grams (+/ - 0.001 g) of sample into a 250 mL beaker. 2. Add 25 mL of benzol to dilute the sample and then 25 mL of isopropyl alcohol and 20 mL of dilute HCl
9、(1:1). 3. Heat to boiling and boil gently for 20 minutes on the hot plate. 4. Transfer the hot sample to a 200 mL separatory funnel, washing with a little benzol and hot water. 5. Allow the layers to separate as much as possible and draw off bottom layer. Note: It is difficult to obtain a clean sepa
10、ration between the benzene and water layers because of the formation of an emulsion at the interface. Therefore it is suggested that, in the washing p rocedure, the emulsion layer be left with the benzene layer and the final separation be made as complete as possible on the last washing. 6. Wash the
11、 oil layer five times with 50 mL portions of hot water, allowing each wash to separate as much as possible before drawing off. The washings should be done carefully, as follows: Add hot water to the benzol in the separatory funnel and swirl with the stopper off. Stopper the flask, invert the separat
12、ory funnel and open the stopcock cautiously while in the i nverted position to relieve pressure. Close stopcock, swirl gently and again open to relieve pressure. Do this for each of the water additions. 7. Collect the total water washes and add 40 - 50 mL of the benzol. Shake well, let settle and dr
13、ain off th e water. Wash with one or two washings (25 mL each) of warm water and draw off water layer. 8. Combine the benzol extracts from Steps 6 and 7 and transfer to a saponification flask and evaporate the solvent. (Avoid open flame!) 9. Add 50 mL of alcoholic potassium hydroxide, attach condens
14、er to flask, place on electric hot plate and saponify under reflux for one hour. 10. Cool, transfer to a separatory funnel, rinsing flask with small portions of distilled water (45 mL total). Rinse flask with small por tions of petroleum ether (50 mL total) and finally rinse with 50 % alcohol. Shake
15、, allow to settle and drain off the alcoholic solution into a separatory funnel. 11. Shake the alcoholic soap solution with portions of petroleum ether to separate mineral o il, and add to the mineral oil extract in Step 10. The first extraction should be made with 50 mL of petroleum ether and then
16、four additional extractions made with 30 mL portions of petroleum ether to completely separate the mineral oil from the soap. Sa ve both the alcohol soap extract and the ether - oil extract. 12. Shake the combined petroleum ether extracts three times with 15 mL portions of 50 % alcohol to which has
17、been added a trace of alkali. Add these extracts of alcohol to the soap solution obta ined in Step 11. FORD LABORATORY TEST METHOD AJ 001-02 Page 3 of 3 Copyright 2000, Ford Global Technolo gies, Inc. 13. Evaporate the alcoholic soap solution until free from alcohol. 14. Dissolve the soap in 50 - 10
18、0 mL of distilled water, treat with an excess of dilute H 2 SO 4 (1:4), swirl and allow to cool. Transfer to a separatory funnel and rinse f lask with 100 mL of ethyl ether. 15. Drain off the acid layer into another separatory funnel and wash this acid layer with 50 mL of ethyl ether and combine the
19、 extracts of ethyl ether. Wash the combined extracts with sodium sulfate solution (20 %) until the washings will not turn methyl orange red. 16. Dry the ether by adding 10 g of granular, anhydrous sodium sulfate and filter through a Whatman No. 41H paper and evaporate the ether (avoid open flame!).
20、17. Dry the residue of fatty acids for 15 - 30 mi nutes at 190 +/ - 2 F, cool and weigh. weight of fatty acids x 100 = % recovered fatty acids weight of sample recovered fatty acids x 1.05 = % neutral fat 18. Transfer the petroleum ether extracts of mineral oil from Step 11 to an extraction flask an
21、d evaporate the ether on a water or steam bath. The oil should be completely free from ether, water and alcohol after evaporation. 19. Determine the sulfur content of the oil according to ASTM Procedure D 129. An alternate routine method for Steps 19 and 20 is to determine sulfur on the original and
22、 extracted mineral oil sample by means of a Leco combustion furnace and sulfur determinator. 20. Determine the total sulfur content of the original sample by the same method and calculate the added sulfur from the difference in sulfur content found by the two determinations, assuming that the origin
23、al material contains 75 % petroleum oil. natural sulfur = (BaSO 4 ) (0.1373) (100) wt of mineral oil x 1.33* * 1.33 = wt of mineral oil .75 Note: The accuracy and reproducibility of this method for added sulfur is dependent on the stability of the natural sulfur compounds in the petroleum oils since most petroleum oils do not yield their natural sulfur on saponification. Chemicals, materials, parts, and equipment r eferenced in this document must be used and handled properly. Each party is responsible for determining proper use and handling in its facilities.
