SAMPLING AND ANALYSIS OF COMMERCIAL FATS AND OS OE AGCS& AOCS Recommended Practice Co 17-95 Soap in Oil Titrimetric Method DEFINITION The titrimetric method determines the alkalinity of che test sample as sodium oleate. SCOPE Applicable only o refined vegetable oils (sce References, 1). Formesly Ce 17-79, APPARATUS 1. Test tubes approximately 150 % 40 som of borosilicate glas fitted with ground glass stoppers and flarened at the base 2. Microbuzet—5 mt. 3. Steam bath—hot water bath may also be used. REAGENTS, 1. Acecone—containing 29% wate, prepared by adding 20 ml. distilled water to 980 ml. of reagent-grade aoetone (sce Notes, Caution) 2. Hydrochloric ace (HCD approximately 0.01 M, accurately standardized, See AOCS Specification H 14-52. 3. Bromophenol blue indicator solurion—1.0 % in water, 4, Sodium hydroxide (NaOH) —approximacely 0.01 M. PROCEDURE 1. Just prior co the analysis, prepate the tes solution by adding 0.5 ml. ofthe bromophenol blue indicator solution (Reagents, 3) tocich 100 ml. of the aqueous aectone solution (Reagenes 1) and testing with 0.01 M Hl (Reagents, 2) or 0.01 M NaQH_ (Reagents, 4) unl the ees solution is just yellow in olor. 2, Weigh 40 g (Notes, 1) of che oil or fie co be ested into a rst tube (Apparatus, 1) which has been well rinsed with the exe solution (Procedure, 1) 3. Add 1 ml. of water co the est sample, warm on a steam bath (or in water bath) and shake vigorously. Add 50 ml. ofthe est solution (Procedure, 1), and after warming, shake the tube well and allow the contents to separate until ro distinct layers are formed. Note—IEsoap is present inthe oil o fat, the upper layer will be colored green to ble. 4, Slowly add 0.01 M HCI (Reagents, 2} from the mieroburet uns che color just changes from grcen/bluc to yellow. Repeat the warming, shaking and addition of 0.01 M HCl uns che yellow color of the upper layer cemains permanent. Record the total volume of acid required as ml, 5. Ablanke correction should be determined on soap-frce oil, using Procedure, steps 1-4, Record the volume of acid required for the blank as ml, CALCULATIONS (al, —t,) x M_x 304,400 1. ppm soap as sodium oleage =e Ma) * MX SOAOE prion Ra & NOTES Caution Acetone is highly flammable, Forms explosive peroxides with oxidizing agencs, Use effective fame-removal device, Do not mix with chloroform, Hydrochloric acid isa strong.acid and will cause severe burns, Protective clothing should be worn when wotking with this acid. Ie is toxic by ingestion and inhalation and a strong irritant co eyes and skin. The se of a properly operating fume hood is recommended. When diluting the acid, always add the acid co the water, never the reverse NUMBERED NOTES 1. The method as written is suitable forthe determination of soap at concentrations of up to 0.05% in oils and fas. Ar higher concentrations ite bersr to analyze 4 g of tes portion and use 0.01 M HC Page 1 of2€€17-95 * Soap in Oil Titimetric Method REFERENCES, 1. A study among seven industrial organizations indicated thac chis method is suitable only for refined oils. Yukagatu (lepan) 3951056 (1990) 2. This method is idencical with Codex Alimensarius method CACIRM 13-1969 and similar to Beitish Standard 648:1958, 3. Wolf, J.P. Oléaginews, p. 197 (April, 1948) Page 2 of2