1、 FORD LABORATORY TEST METHOD AJ 108-01 Date Action Revisions 2000 08 07 Editorial no technical change A. Cockman 2000 03 21 Editorial no technical change A. Cockman 1990 05 30 Printed copies are uncontrolled Pa ge 1 of 2 Copyright 2000, Ford Global Technologies, Inc. DETERMINATION OF SOAPS, EMULSIFI
2、ERS AND WETTING AGENTS IN SOLUBLE OILS AND DRAW COMPOUNDS Application This test method is used to determine the percent of soaps, emulsifiers and wetting agents in soluble oils or draw compounds. In the case of difficult separations, deviations from this method may be agreed upon between the compete
3、nt laboratory and the supplier. Apparatus Required Analytical Balance Precision +/ - 0.1 mg. Steam Bath Oven Mechanical convection; capable of being maintained at 105 +/ - 3 C. Separatory Funnels 500 mL; with Pyrex ground glass stoppers. Graduated Cylinder Beaker 250 mL; Pyrex The above apparatus is
4、 available from any reputable laboratory equipment supply house. Materials Required Isopropyl Alcohol Reagent grade; CAUTION : Low flash point Petroleum Ether Reagent grade; BP 30 - 60 C; CAUTION: Low flash point Distilled or Deionized Water 20 micromhos/cm at 25 C maximum conductivity (ASTM D 1125)
5、 Solutions Required Isopropyl Alcohol Solution 50/50 by volume with dist illed water. FORD LABORATORY TEST METHOD AJ 108-01 Page 2 of 2 Copyright 2000, Ford Global Technologies, Inc. Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a controlled a
6、tmosphere 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 otherwise specified. Procedure 1. Weigh 5 - 7 g of sample into a separatory funnel. 2. Add 100 mL of 50 % by volume isopropyl alcohol (50/50 with distilled w
7、ater). 3. Shake well to disperse sample. 4. Add 50 mL of petroleum ether. 5 . Shake well again. 6. Allow to stand and separate into two layers. Notes: 1. Additional concentrated isopropyl alcohol may have to be added to compensate for the presence of water in the sample so that the resultant final m
8、ixture is 50/50 alcohol/water . 2. Mixture may have to be filtered if pigment (insolubles) is present in the sample. 7. Drain the alcoholic layer (bottom) into a second separatory funnel. 8. Extract the alcoholic layer five times with 30 mL of petroleum ether and combine all extrac ts. 9. Shake the
9、combined ether extracts with 25 mL of 50 % isopropyl alcohol to remove any soap that may be in this part of the extract, usually three to five times will be sufficient. 10. Combine all alcoholic extractions. 11. Drain alcoholic extractio ns from step 10 into a tared beaker. Evaporate on a steam bath
10、 to dryness and place in an oven at 105 C and dry to constant weight. This represents the soaps, emulsifiers and wetting agents. % Soaps, Emulsifiers, Wetting Agents = Difference in Weight x 100 Sample Weight See Notes under Recovered Unsaponified Saponifiables (FLTM AJ 109 - 01) for precautions to use in manipulation 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.
