1、 FORD LABORATORY TEST METHOD AJ 106-01 Date Action Revisions 2000 08 07 Editorial no tech nical change A. Cockman 2000 03 21 Editorial no technical change A. Cockman 1990 09 24 Printed copies are uncontrolled Page 1 of 2 Copyright 2 000, Ford Global Technologies, Inc. SAPONIFIABLES IN OILS Applicati
2、on This procedure is used to determine percent unsaponified saponifiables, soaps, emulsifiers and wetting agents in base soluble oil materials. Reagents Isopropyl Alcohol and Distilled Water - (50:50) Petroleum Ether: R eagent grade Hydrochloric Acid: Concentrated Potassium Hydroxide: 1.0 normal alc
3、oholic solution. Weigh 60 g KOH (ACS grade) and heat in 500 mL of methyl alcohol while stirring. Allow to stand overnight to precipitate carbonate. Decant or filter throu gh a fritted glass filter # 0 and dilute to one liter with methyl alcohol. Ethyl Ether: Reagent grade Sodium Sulfate: Reagent gra
4、de 20 % in water with methyl orange indicator. Sodium Sulfate : Reagent grade, Anhydrous, granular. 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 p
5、rior to testing and tested under the same conditions unless otherwise s pecified. Procedure 1. Weigh 5 - 10 g of sample into a separatory funnel. 2. Add 100 mL 50 % isopropyl alcohol (Reagent #1) and shake well to disperse material. 3. Add 50 mL of petroleum ether and shake well again. 4. Allow to s
6、tand and separate into t wo layers. 5. Drain alcohol layer (bottom) into a second separatory funnel. 6. Extract the alcoholic layer five more times with 30 mL petroleum ether and combine all extracts. FORD LABORATORY TEST METHOD AJ 106-01 Page 2 of 2 Copyright 2000, Ford Global Technologies, Inc. 7.
7、 Shake combined ether extracts from above with 25 mL 50 % isopropyl alcoho l to remove any soap that may be in this part of the extract, usually three to five extractions. 8. Combine all alcoholic extractions. 9. Drain petroleum ether extract into a tared flask. Evaporate the ether on a steam bath a
8、nd dry to a constant weight. This portion contains unsaponified saponifiables and non - saponifiables (oil). 10. Drain alcoholic portions from Step 8 into a tared beaker. Evaporate on a steam bath to dryness and place in oven at 100 C, dry to constant weight. This portion contains soaps, emulsifiers
9、 and wetting agents. % Soaps, emulsifiers = difference in weight x 100 & wetting agents weight of sample 11. To extract from Step 9 in flask, add 25 mL 1.0 N alcoholic KOH and saponify for 2 1/2 hours. 12. Cool and wash into a separ atory funnel, using 50 % isopropyl alcohol water followed by petrol
10、eum ether. Rinse flask two or three times to remove all products formed. 13. Shake and separate into layers, repeating Steps 2 - 8. 14. Dry evaporate the petroleum ether extract on a ste am bath and dry in oven at 100 +/ - 2 C to constant weight in tared beaker. This is the non - saponifiable matter
11、 (oil). Unsaponified total extracted % = difference in weight x 100 weight of sample 15. Drain alcoholic layer into a beaker and evaporate unt il alcohol is removed. 16. Add 5 - 10 mL concentrated HCl to break up the soap and heat to coagulate fat. 17. Cool after heating and wash into separatory fun
12、nel, using water and 100 mL ethyl ether. Shake well and allow to separate. 18. Extract acid la yer three to five times with 25 mL of ethyl ether for each extraction. 19. Combine all ethyl ether extractions and wash with 25 mL, 20 % sodium sulfate. Drain aqueous solution and repeat until washings sho
13、w neutral to methyl orange (color change from red to orange). Dry ether layer with 10 grams anhydrous, granular sodium sulfate. 20. Drain through cotton into a tared 250 mL beaker. Wash funnel and cotton with ethyl ether until fat free. Evaporate ethyl ether on steam bath and dry at 100 +/ - 2 C to c onstant weight. % Recovered unsaponified = difference in weight x 100 saponifiables weight of sample Chemicals, materials, parts, and equipment referenced in this document must be used and handled properly. Each party is responsible for determining pro per use and handling in its facilities.
