SAMPLING AND ANALYSIS OF COMMERCIAL FATS AND OLS AOCS& AOCS Official Method Cd 34-63 a Reaporoved 2009 Acid Value a DEFINITION ‘The acid value is the number of miligrams of potassium hydroxide necessary to neutrelize the free acids in 1 gram of test sample. With test samples chat contain virtually no free acids other than fatty acids, the acid value may be directly converted by means ofa suitable factor to percent fre fay acids. SCOPE Applicable to crude and refined animal, vegetable, and matine fas and oils, and various products derived from them. Formerly Cd 32-63. APPARATUS, 1, Erlenmeyer flasks—250 or 300 mL. 2. Magnetic stirring 3. Burerte—10 mL, graduated in 0.05 mL divisions with a tip drawn to fine opening and extending atleast 10 cm below the sopcock. 4, Analytical blance—accurate 190.0001 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 traccable standardization to +1 part in 1000 in wares, methanol, or ethanol. 2, Solvent mixture consisting of equal parts by volume of isopropyl alcohol (AOCS Specification H 18-58) and toluene (ACS Specification H 19-58). See Notes, Caution. The mixcure must give a distinct and sharp end point with phenol pphthalein in che titration as noted in Procedure, 5. - 43. Phenolphthalein indicator solution—1.0% in isopropyl alcohol. PROCEDURE 1. Add indicator solution ro the required amount of solvent in ratio of 2 mL. to 125 mL. and neutralize with alkali to a faine but permanent pink color. 2. Determine the test portion sie from the following cable: Aad vue Mass g of exe portion (210%). g ing accuracy, = on 20 0.05 4 10 0.02 415 25 oot 1575 D5 0.001 75 and over oa 0.0002 3. Weigh the specified amount of a well-mixed liquid test portion into an Erlenmeyer flask 4. Add 125 ml of che neuttalized solvent mixture. Be sure that the test portion is completely dissolved before titrating ‘Warming may be necessary in some cass. 5. Shake the cst portions vigorously while titrating with standard alkali ro the first permanent pink color of the same intensity as that ofthe neutralized solvent before che latter was added to the est portion. The color must persist for 30s 6, Perform 2 blanke titration using 125 ml of the neutralized solvent mixture CALCULATIONS 1 Ad vale, mg KOHYg of ex poron = AB) M > 561 where— volume, mL of standaed alkali used in the titration ng the blank - M = molarity of standard alkali W = mass, grams of test portion “To express in terms of free fatry acids as percent laurie, oleic, oF palmitic, divide the acid value by 2.81, 1.99, of 2.19, respectively. Page tof 3[SAVPLING AND ANADISS OF COMMERCIAL FATS AND ONS Cd 3d-63 © Acid Value PRECISION 1, Single deterrainations performed in two different laboratories should not differ by mote than 0.22 for values less than 4 nor by more than 0.36 for values in the range 4-20. ALTERNATE PROCEDURE FOR HIGHLY COLORED TEST SAMPLES, APPARATUS 1. Glas electrode—ealomel electode pH merer for clectromerr Numbered Notes, 2). 2. Variable-speed mechanical sirer—with glass siting paddle, 3, Buretce—10 mL, graduated in 0.05 ml. divisions with 3 ip deawn to fine opening and extending at lease 10 em below the sopcock. 4, Beskers—250 mL 5, Stand and mountings for electrodes, stirer, and burett. 6. Magnetic sirting device. titration, A sleevesype calomel electrode should be used (see REAGENTS. 1, Sameas for the phenolphthalein rtrimeurie procedure, except thatthe standard alkali should be standardized by cleetromet- tic tration of pure potassium acid phthalate and no indiextor solution is necessary PROCEDURE 1, Decermine the test portion size from Procedure, 2 and weigh the test portion into a 250 mL beaker. 2 Add 125 mL of solvent mixture, 53, Mount the beaker in the titration assembly so thatthe electrodes are half immersed. Star che sttrer and operate a speeds that will give vigorous agitation without splattering, Immerse the tip of the burette to | em below the surface of the test portion. 4, Tittate with suitable increments of alkali, After each addition of alkali, wait until the meter ceading is essentially constant (usually within 2 min), chen record burette and meter ceadings graphically. Limie inerements 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 water. 6. Perform a blank titration, using 125 mL of solvent mixture. CALCULATIONS 1. Acid value, mg KOHg of tet portion = A= 8) x M x 56.1 w where— ‘Ac volume, mL of standard alkali used in ceraing co middle of inflection in titration curve of est portion B= volume, mL of seandard alkali used in vitrating co sime pH meter reading forthe blank ‘M. molarity of standard alkali W-= mass, grams of tex portion ‘To express in terms of fice fatty acids as percent oleic, lautic, oleic or palmitic, divide the acid value by 2.81, 1.99, ot 2.19, respectively: PRECISION “Table 1 shows the precision data from interlaboratory studies evaluated according to 150 $725:1994, Noes Caution Isopropyl alcohol is flammable and a dangerous fire risk. The explosive limits in sir are 2-129, leis toxic by ingestion and inhsla- tion, The TLV in air is 400 ppm. Toluene is flammable and a dangerous fire risk. Explosive limits in air ae 1.27~79. Iti toxic by ingestion, inhalasion, and skin absorption. The TLY is 100 ppm air. A fume hood should be used a¢ all times when using toluene, rage 2 of 3TAMPIING AND ANAINGS OF COMMERCIAL FATS AND OWS Cd 34-63 * Acid Value NUMBERED NOTES 1. A standard methanolic potassium hydroxide (0.1 M) solution (see AOCS Specification H 15-52) may be used 2s an alternate titrant in place of the standard aqueous solution. The methanolic potassium hydroxide is reported to provide a complete solvent system, having 2 distinct, clea end point. See References, 1 regarding the ruggedness of the acid value method. 2. The pH meter should be standardized ro pH 4.0 with standard buffer solution. Immediately before using, wipe the elec- trodes thoroughly with clean cloth oF tissue and soak for several minutes in disilled water. At weekly intervals, or more often af necessary, clean the glass electrode in a suitable cleaning solution. Also, drain calomel electcode and refill with fresh potas- sium chloride (KCI) electrolyte at weekly incervals. Both clecrodes should be stored in distilled water when not in us. REFERENCES 1. J. Aasoe. Off: Anal. Chem. 59:658 (1976). Table Precision data from interlaboratory studies. Pe _ "Palm Palm Palm Palm Lampanie Lampante out kemel Sunflower Coconut _oil_cil__kernch__kemmel__olieoil olive, Number of laboratories B B 25 noo al a 28 2s Number of acceprable sults 22 2 25 ton 273940 26 4 Mean acidity values, 95 726 083. 1431409 GGT 3.8 1955 Repeatability, « 007 0025 0.025008 0060.07 006.07 026 Reproduciilry. R 024 wo7s 0750s ONS 020.0033, 167 Page 3 f3