SAMPLING AND ANALYSIS OF COMMERCIAL FATS AND OMS vised 2011 Saponification Value DEFINITION rie sapenificaton value isthe amoune of alkali necessary co saponiy a definite quanti of the test sample tha Pressed 5 the number of miligrms of pocasium hydroside (KOM reguted to oper gram of the test sample, SCOPE Applicable to all normal fats and oils (see Notes, 1) APPARATUS 1. Erlenmeyer fasko—alal reicent, 250 or 300 mL, T2440 jround:las joint 2. Condensers—with T24/40 ground-glas joint ro fic Erlenmeser flake 3. Water bath, ora hotplate with variable heat control. REAGENTS J; Hydrochloric acid 0.5 M—aocuratey standardized. ce AOCS Specification H 14-52. ne cium hydroxide (KOH may be puchasl or prepared by placing 5-10 g of ragen-gade KOH (ce bach de Fete .¢ 21 Ma adding 1-15 L of 959% ety aloha (se Nows, CSitn) ed hing oo ee Pyar 30-60 min, Dis and cals alcohol na clean glas-soppered coies Drseke ens potassium {eons ow in carbonate in| L ofthe led alcohol (ee Notes. ain) it socio he oe femperacure at ot blow 15°C. This solution should remain cleat. (Se Notes, 2) 3. Phenolphthalen indicator solution 1.09) in 95% ethyhalecho PROCEDURE sree sample os Notes, 3) fii no aleady liquid and ler hrough dey ter paper to remove any impurities and moisture. The test sample must be completely dry. 2. (Weigh 2 ext portion of such sie thatthe back tization is 45-55% of the blank, This usually requires a test portion of OS ZE 2 RE OFROM GEE used (Table 1) or4-5-piFs0micoPKOH an ond. Mid ene with a pipet and allow the pipet to drain for approximately 10. (Sce Nore.) i. Cebate and conduc blank determinations concurrenuy with the test portion omitting the fat o of 4 Gannect the condense rd bil gealy, but stad, unl che tex portion i compleey ca ived This usually requires ac least 30 min for normal rst portions (See Notes, 5). Make certain thar top of the condense, or loss may occur. > After the flask and condenser have cooled somewhat, bu ot sflcienl o forma gel, wash the inside ofthe condenser with OS ere lstledwacet Disconnect the condense, add about | ml of phenalphihcin rain ce 0.5 Ml until the pink color just disappears. Record the volume of 0.5 MNCL requled tr en, CALCULATIONS. spor ring in the condenser does not tse to the 1. Saponification value = Where— B-9x M56, Ss olume of 0.5 M HCI requized to titrate blank, ml volume of 0.5 M HCI required o titrate test portion, mL, nolarty of HC! solution We mass of tet portion in grams PRECISION Repeatabiliy and reproducibility values fiom an international colabortive study are given in Table 1. NOTES Guation eassiam hydroxide, like alallais, can burn skin eyes, and respiratory tact severely, Wear heavy suber gloves and face shield Mes dea ns concentrated alla liquids Use effective fame-removal device or gus maak ws frovee respiratory tract against atkall dust or vapor, When working with extremely caustic materials such us ports hydroxide, always add pellets to waterTANPIING AND ANANSIS OF COMMERCIAL FATS AND O15 Cd 3-25 * Saponification Value and not the reverse, Alkalies are extremely exothermic when mixed with waccr. Take precautions to contain the caustic solution jn the event that the mixing container breaks from the extreme heat generated. Ethyl alcohol (ethanol) is flammable. Use fume hood when heating or evaporating this solvent. Hydrochloric acd is strong acid and will ease severe burns. Protective clothing should be worn when working with this acid. It is toxic by ingestion and inhalation and a strong irritant to eyes and skin. The use of a properly operating Fume hood is recommended. When diluting the acid, always add the acid ro the water, never the reverse NUMBERED NOTES 1. When the saponification value is required on the fatty acids, the preparation and separation are performed as directed in ‘AOCS Official Method TI 13-64. 2, Ethanol may be stabilized by either of the following methods: a) the addition of 5 g aluminum pelets ro the reflux lak prior to reflaxing and distilaion orb) he addition of 4 g aluminum cer-buryate and allowing it to stand for several days Tn both cases deeant the clear supernatant fiom the preeipicated potassium carbonace formed after dissolving the porassium hydroxide 3, Tear samples must be well mixed and entirely liquid before weighing; however do nor heat the sample more than 10°C over the melting point. 4, For consis results, 425 of 50 mL. class A volumettic pipet calibrated “to deliver” should be used. The pipet should be allowed to drain for about 10 s. And the same pipet should be used forall analyses. 5. Some test portions, particularly those dificult co saponify, may require 1-6 hr tefluxing, This can only be determined by tral Clarity and homogeneity ofthe cst solution are partial indicators of complete saponification, bus they are not neces- sarily absoluce criteria. Table1 Mass of test portion. cation value Mass of text portion Expected sapor 150 co 200 200 ro 250 25010 300 > 300 Table2 Results of a 2000 collaborative study on the determination of saponification value. {609% Coconut oil Test Sample Rapeseed ol Palm oil Coconut oil + 40% MCT oil MCT ei Total number of laboratories accepted » 7 20 18 16 Mean of the laboratory values (mg/e) 190.20 199,50 256.80. 287.50 334.10 Repeatability Standatd deviation, s, o71 056 072 o71 14 Relative standard deviation, RSD,%% 04 03 03 02 04 Repeatability vale, 2.8 x 5, 201 136 202 199) 3.95 Reproductbilicy Scandard deviation, 55 77 2.04 417 2.86 Relative standard deviation, RSD,% 09 Lo 16 09 Reproducibility value, 28 % 55 497 5.72 1.67 8.00