SAMPLING AND ANALYSIS OF COMMERCIAL FATS AND O1LS AOCS Official Method Cd 3d-63 Reapprone 2009 Acid Value DEFINITION The acid value is the number of milligrams of potassium hydroxide necessary to neutralize the free acids in 1 gram of tes sample, With test samples that contain virtually no Free acids other than fatty acids, the acid value may be directly converted by means of a sultable factor to percent fre fatcy acids, SCOPE “Applicable to ceude and refined animal, vegetable, and marine fats and oils, and various products derived from them. Formerly Ca 32-63, APPARATUS 1. Erlenmeyer fasks—250 or 300 mL. 2, Magnetic sieving device. 3, Buretee—10 mL, graduated in 0.05 ml. divisions with a ip drawn to fine opening and extending at least 10 em below the sxopeock, 4, Analytical balanco—accurate 0 0.0001 g REAGENTS. 1, Potassium hydroxide (KOH), 0.1 M—Reagent grade KOH having a carbonate specification of 0.5% max, or 0.1 M KOH ‘with NIST traceable standardization to #1 pact in 1000 in water, methanol, or ethanol 2, Solvent mixture consisting of equal pasts by volume of isopropyl alcohol (AQCS Specification H 18-58) and toluene (AOCS Specification H 19-58). See Notes, Caurion. The mixture must give a distinct and sharp end point with phenol- phthalein in che titration as noted in Procedure, 5. 3, Phenolphthalein indicator solution—I.0% in isopropyl alcohol. PROCEDURE 1, Add indicator solution to the required amount of solvent in ratio of 2 mL to 125 mL and neutralize with alkali toa faint but permanent pink color 2. Determine the est portion size from the following table: Reidvalue Mas gel tet portion C10) g———“Weihing ee ot 20 005 14 10 0.02 45 25 0.01 15-75 os. 0.001 75 and ow 0. 3. Weigh the specified amount of a well-mixed liquid test portion inco an Erlenmeyer flask 4, Add 125 mL of the neutralized solvent mixture, Be sure chat the cest portion is completely dissolved before tieracing. Warming may be necessary in some cases. 5. Shake the test portions vigorously while cceating wich standard alkali co the first permanent pink color of the same intensity as chat of the neutralized solvent before the latter was added co the test portion. The color must persist for 30 s 6, Perform a blank titration using 125 mL. of the neutralized solvent mixture. CALCULATIONS 1. Acid value, mg KOH/g of est portion = A= B) Mx 56-1 Ww swhere— ‘A= volume, mL. of standard alkali used in the tcration volume, ml. of standard alkali used in cicrating the blank molarity of standard alkali ass, grams of test portion “To express in terms of free fatey acids as percent laurie, oleic, or palmiic, divide the acid value by 2.81, 1.99, or 2.19, respectively. Page 1 of 3SAMPLING AND ANALSIS OF COMMERCIAL TATS AND OS Cd 3d-63 © Acid Value PRECISION 1. Single determinations performed in ewo dil by more than 0.36 for values in the range 4-20. laboratories should not differ by more than 0.22 for values less chan 4 nor ALTERNATE PROCEDURE FOR HIGHLY COLORED TEST SAMPLES APPARATUS 1. Glas electrode—calomel electrode pH meter for electrometric titration. A sleeve-type calomel electrode should be used (see Numbered Notes, 2). 2. Variable-speed mechanical stirrer —with plas stirring paddle. 3, Burette—10 mL, graduated in 0.05 ml. divisions with a tip drawn to a fine opening and extending at least 10 em below the stopcock. 4, Beakers—250 mL. 5. Stand and mountings for electrodes, tires, and burete, 6, Magnetic tiring device. REAGENTS 1. Same as for che phenolphhalein titrimetric proceduce, except that the standard alkali should be standardized by cloctromet- Fic tration of pure pocassium acid phthalate and no indicator solution is necessary PROCEDURE 1, Determine the tese portion size from Procedure, 2 and weigh the test portion inco a 250 ml. beaker. 2. Add 125 mL of solvent mixture. 3. Moune the beaker in the titration assembly so that the electrodes are half immersed. State the stirrer and operate at speeds ‘hat will give vigorous agitation without splactering. Immerse the tip of the burette co 1 cm below the surface of che test portion. 4, Ticeace with suitable increments of alkali. After each addition of alkali, waie uncil the meter reading is essentially constant (usually within 2 min), chen cecord burette and meter readings graphically. Limit increments of alkali so that changes in meter readings are 0.5 pH units (0.03 volts) or less; when inflections in titration curve occur, add alkali in 0.05 mL portions. 5, Remove titrated solution, rinse electrodes with isopropyl alcohol, and immerse in distilled wacer 6, Pecform a blank titration, using 125 mL. of solvent mixture, CALCULATIONS (A-B) x M x 56.1 1. Acid value, mg KOH/g of test portion = “= =) ~*OO8 1g KOHg of cest pu Ww folume, mL of standard alkali used in crating to middle of inflection in titration curve of test portion, volume, ml. of standard alkali used in titrating to same pH meter reading for the blank ‘molarity of standard alkali |W = mass, grams of test portion “To express in terms of free fatty acids as percent oleic, lautic, oleic or palmitic, divide the acid value by 2.81, 1,99, or 2.19, respectively PRECISION Table I shows the precision data from interlaboratory studies evaluaced according to 150 5725:1994, NOTES Cation Ikoptopy! alcohol i flammable and a dangerous fire risk. The explosive limits in air are 2-126. Icis toxieby ingestion and inhala- tion, The TLY in ar is 400 ppm. “Toluene is flammable and a dangerous fie esk. Explosive limits in ai are 1.2778 Itis toni by ingestion, inhalation, and skin absorption. The TLY is 100 ppm air. fume hood should be wed at all rimes when using toluene. Page 2 0f 3TANPLING AND ANALYSIS OF COMMERCIAL FATS AND OS Cd 34-63 * Acid Value NUMBERED NOTES. 1. Astandard methanolic potassium hydroxide (0.1 M) solution (see AQCS Specification Hi 15-52) may be used as an alternate titant in place of the standard aqueous solution. The methanolic potassium hydroxide is reported co provide a complete solvent system, having a distine, clear end point, See References 1 regarding the ruggedness of the acid value method. 2. The pH meter should be standardized to pH 4.0 with standart bafler solution. Immediately before using, wipe the elec- trodes thoroughly with clean cloth of tissue and soak for several minutes in di 1ecessary, clean the glass electrode in a suitable cleaning solution. Also, drain calomel electrode and refill with Fresh potas- led water. At weekly intervals, or more often sium chloride (KC) electrolyte at weekly intervals. Both electrodes should be stored in distilled water when not in use. REFERENCES 1. J. As0e. Off Anal. Chem. 59658 (1976) Tablet Precision data from interlaboratory studies. Palm Palm Palm Palm Palm Lampante Lampance ol eemnel Sunflower Coconue oll’ -—oil~—sikernel_—kernel_—oliveoil__aliveoil ‘Number of laboratories 2B 23 2 now 4 28 28 Number of accepeable results 22 2 25 wont 27390 26 4 Mean acidity values, % 726 083 1493409 GGT 3.8. 1955 Repeaabilicy, | 007 0025025003 0.06.07 0.06.07 026 Reproducbilsy. R 024 00750073045 OS 9230.20 0.33 167, Page 3 of 3