FORD FLTM AJ 109-1-2001 DETERMINATION OF RECOVERED UNSAPONIFIABLES AND NONSAPONIFIABLES IN SOLUBLE OILS AND DRAW COMPOUNDS.pdf

1、 FORD LABORATORY TEST METHOD AJ 109-01 Date Action Revisions 2001 01 16 Revised Editorial no technical change A. Cockman 2000 03 21 Editorial no technical change A. Cockman 1992 06 03 Printed copies are uncontrolled Page 1 of 4 Copyright 2001, Ford Global Technologies, Inc. DETERMINATION OF RECOVERE

2、D UNSAPONIFIABLES AND NONSAPONIFIABLES IN SOLUBLE OILS AND DRAW COMPOUNDS Application This test method is used to determine the percent unsaponifiables and nonsaponifiables in soluble oils and draw compounds. Apparatus Required Steam Bath Oven Capable of being maintained at 105 +/- 3 C. Separatory F

3、unnels 500 mL, with Pyrex ground glass stoppers. Hot Plate Electric Extraction Apparatus Analytical Balance Precision +/- 0.1 mg Beaker 250 mL Graduated Cylinder 200 mL Materials Required Isopropyl Alcohol Reagent grade; CAUTION: Low flash point FORD LABORATORY TEST METHOD AJ 109-01 Printed copies a

4、re uncontrolled Page 2 of 4 Copyright 2001, Ford Global Technologies, Inc. Petroleum Ether Reagent grade, BP 30-60 C; CAUTION: Low flash point. Hydrochloric Acid Concentrated, reagent grade; CAUTION: Corrosive. Potassium Hydroxide Reagent grade; CAUTION: Corrosive. Ethyl Ether Reagent grade; CAUTION

5、: Low flash point. Sodium Sulfate Reagent grade, anhydrous, crystalline Cotton Distilled or Deionized Water 10 ppm max total dissolved solids (ASTM D 1888). Solutions Required Isopropyl Alcohol 50/50 v/v/ with distilled water. Sodium Sulfate Solution 20 % aqueous solution. Methyl Orange Indicator Di

6、ssolve 0.1 g of methyl orange reagent in 100 mL of distilled water. Alcoholic Potassium Hydroxide 1.0 N 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

7、 prior to testing and tested under the same conditions unless otherwise specified. FORD LABORATORY TEST METHOD AJ 109-01 Printed copies are uncontrolled Page 3 of 4 Copyright 2001, Ford Global Technologies, Inc. Procedure After the removal of soaps, emulsifiers and wetting agents, continue extractio

8、ns as follows: 1. Drain the combined petroleum ether extracts from step 9 of FLTM AJ 108-01 (“Determination of Soaps, Emulsifiers and Wetting Agents in Soluble Oils and Draw Compounds“) into a tared saponification flask. 2. Evaporate the ether on a steam bath. 3. Dry to constant weight. 4. This port

9、ion contains the unsaponified saponifiables and nonsaponifiables (oil). 5. To this dried extract, add 25 mL of 1.0 normal alcoholic KOH. 6. Saponify for 3 h. 7. Cool and wash into a separatory funnel using 50 % isopropyl alcohol/water followed by petroleum ether. 8. Rinse flask two or three times to

10、 remove all products formed. 9. Shake and separate into layers, repeating procedure steps 2 through 10 used in determining soaps, emulsifiers and wetting agents. 10. Dry the petroleum ether extract to constant weight in a tared beaker, using: (a) Steam bath (b) Followed by constant weight at 105 C i

11、n an oven. % Non-Saponifiable Matter = Difference in Weight x 100 Sample Weight 11. Drain alcoholic layer into a beaker. 12. Evaporate on steam bath until all alcohol is removed. 13. Add 10 mL of concentrated hydrochloric acid to break up the soap. 14. Heat to coagulate fat (do not boil). 15. Cool t

12、o 23 +/- 2 C. 16. Wash into a separatory funnel using water and then with 100 mL of ethyl ether. FORD LABORATORY TEST METHOD AJ 109-01 Printed copies are uncontrolled Page 4 of 4 Copyright 2001, Ford Global Technologies, Inc. 17. Shake well and allow to separate. 18. Extract acid layer three to five

13、 times with 25 mL of ethyl ether for each extraction. 19. Combine all ethyl ether extractions. 20. Wash with 25 mL of a 20 % sodium sulfate aqueous solution. 21. Drain aqueous solution and repeat until washings show neutral to methyl orange (color changes from red to orange). 22. Dry ether layer wit

14、h 10 g of anhydrous, crystalline sodium sulfate. 23. Drain through cotton into a tared beaker. 24. Wash funnel and cotton with ethyl ether until fat free. 25. Evaporate ethyl ether on a steam bath. 26. Dry to constant weight in an oven at 105 C. % Recovered Unsaponified Saponifiables = Difference in

15、 Weight x 100 Sample Weight Notes: 1. Pressure is built up in the separatory funnel during each extraction with ether. 2. The pressure must be relieved after each shaking by inverting the separatory funnel and opening the stop cock cautiously while in the inverted position. 3. The shaking and invert

16、ing are repeated until the pressure is completely dissipated. 4. This procedure must be followed after each shaking. 5. This procedure is done for each addition of petroleum ether used for successive extractions until the manipulation and extractions are complete. 6. These precautions, steps 2 through 5, must also be followed when using ethyl ether for the extractions. 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.