MPOB Test Method p2 Peroxide og lug FOR PALM OIL AND PALM OIL PRODUCTs, MET HO OS TERMINATION OF PEROXIDE VALUE 1 Scope This test species a method forthe determination of the peroxide value of palm oil and pain a products, : 2 Referenced documents folowing method contains provisions which, through reference in this text, poveone tis MEOB Test Mobos. Fer dated reference, subsequent amendments to of revision of, any ofthese publications do not apply. However, parties to agreements based en tie MPOB Test Method are encouraged to investigate the possibilty of applying the most mers ition of the referenced documents. For undated references, the latest edition of the docimert referred to apples. MPOB Test Methods p1.1: 2004 — Sampling of palm oil and palm oil products. MPOB Test Methods p1.2: 2004 Preparation of test samples. This method is technicaly equivalent to ISO 3960 Animal and vegetable fats. and ols - Determination of peroxide value. 3 Definition For the purpose ofthis MPOB Test Method, the folowing shall apply, a4 Peroxide value Cuantty of those substances in the sample, expressed in terms of active oxyger , ctive oxygen, which oxidise Paiassium iodide under the conditions specified in this Test ‘Method, divided by the mass of te NOTE: Perosde vate may also be expressed (in un expressed M it) ii Iiols per Wogan ha al eressed in Dorks io done ah 4 Principle Use only reagents of nise ed sera an Sc A, Sn dt Ange 4 # 172MPOB Test Method p2.3: 2004 Peroxide value pistilled water.. “” ee setttogeny, 2 170 by Bung wah a cunt of pure andy ne wen = auth tnd ecue ' moderately toxle by Ingestion and inhalation. It le Wa eine from oxygen by purging with a current of pure and dry inet vas = Iso-octane Is flammable and a fire risk. Explosive we 6 *.0% (by volume). It Is toxic by Ingestion and inhalation a ieee sod should Be used when working with this solvent. + property operating Acatic acid/iso-octane solution (60:40 54 ot ecate aid(6.2) wih 2 volumes elses i Prepared by mixing 3 volumes js Potassium lodide solution, saturated, recently prepared and free from free iodine pdotates wake sure the solution remains saturated as indicated by the presence of undissolved crystals. Wet ne dark. Test daily by adding 2 drops of starch olution (58) to 0.5 mL. of the potassium ‘ade solution in 30 mL of the acetic acid/iso-octane solution (5.4). If a blue colour is formed Sren requires more than 1 drop of sodium thiosulphate solution (6.7) to aischarge the colour, Yoazsd the potassium iodide solution and prepare a fresh solution. ry ‘Sodium thiosulphate solution, c(NazS.03) = 0.1 mol/L, standardised just before ize, Dissolve 24.9 9 of sodium thiosulphate pentahydrate (Na,S:0s, SH,0) in dstiled water and ute to a Sodium thiosulphate solution, c(Na,S;02) = 0.01 moll, standardised just before se Prepare by diluting solution (5.6). a Starch solution, 5 g/l. . 200 Mz 1g of starch and a small amount of cold distiled water. Ad this mitre, while stiring, to 1L of boling water, Add 250 mg of salicylic acid 2s preservative and boil for 3 min. immediately ‘encve from the heat and cool. "long storage is required, the solution shall ach soliton shall be prepared when the endpo a 2880 If stored under refrigeration the starch solution shou! The tena tested as follows. sodium ie mt ee nosiinn ese feaioe (6.5) solution ond 3 a ed Of 0.0 mL. {rotor solton. It is essential that the deep PY? covour prod ‘hiosuiphate solution (5.6). 136 Apparatus Al equipment used shall be free from reducing or oxidizing substances. Do not reaue glass surtaces. Wong Usual laboratory apparatus snd, in particular, the folowing, 64 Conical flasks, of 250 mL capacity with ground glass stoppers, NOTE: Do not grease ground glass aurtaces. 62 Burette, 63 ‘Analytical balance, capable of weighing tothe nearest 0.001 g, Pipette, 1 mL. capacity. 7 Sampling dame at ta the laoreor recaives a sample that Wy representative and hs ot en ‘damaged or changed during transport or storage, Skmping is not pat of the method specified in ths MPOB Test Method. A recommend) ‘sampling method is given in MPOB Test Methods | 1.1; 2004. Ensure that the sample is taken and stored away ftom strong light, kept cold and contained a completely filed glass containers, hermetically sealed with ground glass or waxed carksoppes, Engure thatthe packaging ofthe fat or oil is not damaged, and is wel closed. When parametes other than the Peroxide value have to be investigated, the test portion for the peroxide vale ‘Should be taken frst from the laboratory sample. Prepare the test sample in accordance with MPOB Test Method P'1.2: 2004, Conwy 0K samples shall be homogenisd by mixing and if necessary gente warming, aking cae {2 exclude air from the sample. The test portion should be taken from the midele ofthe sania. For ols, pipette the test portion from the middle of the sample, 9 Procedure 4 General Carry out the test in atfcial ight or dtuse dayight, NOTE: If its requied to check that the repeatabi cut ose ‘determinations in accordance with 8.2 and 9.3, My rqurament (800 11 See 174MPOB Test Method p2.3: 2004 Peroxide value “ Test portion the conical flask (6.1) with a current of pure di Bestar weigh a mass ofthe Sample to the accu ry inert gas (carbon dioxide or nitrogen) Into. (pected peroxide value, racy given in table 1 and in accordance with the Table 1. Mass of test portion and accuracy of weighing ‘Expected peroxide Wi value ‘arte Weighing accuracy meqikg in to Oto 12 201050 v 42 to 20 421020 a 2010 30, 081042 O01 30 to 50, 05 t00.8 0.007 ‘50 to 90 0.31005 0.001 a3 Determination ‘Add 0 mL of acetic acid/iso-octane solution (5.4) to the conical flask (6.1) and replace ‘Swirl the flask until the sample has dissolved. Using a suitable ‘oumert pate co, $0105 mL of saturated potassium iodide solution (6.5) and replace the stopper. Allow the fouion to stand for 1 min 2 1 '., thoroughly shaking the solution atleast three times during the t ‘min, and immediately add 30 mL. of distiled water. ‘Twate the solution with sodium thiosulphate solution (6.7), adding it gradually and with constant, vigorous agtation, until the yellow iodine colour has almost disappeared. Add about 0.6 mL of arch solution (§.8) and continue the titration, with constant agitation especially near the ‘endpoint, to liberate all of the iodine from the solvent layer, adding the sodium thiosuiphate ‘solution (6.7) drop by drop until the blue colour just disappears. There is a 18 8 to 30 6 delay in neutralising the starch indicator for peroxide values of 70 mean tnd greater, due tothe tendency of io-octane to float on the surface of he aqueovs Deir ee) the time necessary to mix adequately the solvent and the aqueots us " traces of iodine. A small amount [0.5% to 1.0% (m/m)] of a high HLB emulsifier (e.g. Tween 60)" Fane action misture to retard the phase separation and decree he lvl 9 the liberation of iodine. Inte case of fts of ow sotbilty, suchas hard stern, te follwing procedure shal be ust ‘da 20 mL. is-octane to the fask, replace the stopper, and dissolve the sample by swirling. Immediately add 30 ml of acetic acid. “ Blank determination : ation. If the result of the Dian} Cary out a blank determination in parallel withthe sample PT es icg ne pure reagent ‘osulphate solution (5:7) (etermination exceeds 0.1 mL of sodium th ‘8nd repeat the sample determination. 175MPOB Test Method po 3. Peroxide 2004 Valug Expression of results we peroxide value expressed In miliequivalents of active oxyG0n per Kilogram Caiculate the peroxide value, P, by the following equation: 1000(V-Vol.e Ps where, V_tethe volume, in mL, of sodium thiosulphate used forthe determination; Vo is the volume, in mL, of sodium thiosulphate used for the blank determination; cis the concentration, in moles per litre, of the sodium thiosulphate; and m is the mass, in grams, of the test portion. 10.2 Peroxide value expressed in millimoles per kilogram Calculate the peroxide value, P;, by the following equation: 1000(V-Vo) ¢ Pe 2m "1 Precision 114 Intertaboratory tests Detaiis of interlaboratory tests on the precision of the method are summarized in Appendix A. The values derived from these interlaboratory tests may not tances ater than those gen ny 'ay not be applicable to concentration ranges and 112 Repeatability ‘equipment within a short interval of time, will in ‘Not me : 1ore thar 10% dle near oe ores, pote vane ee a czas reste a 13 Reproducibility 176MPOB Test Method p2.3: 2004 Peroxide value Tost report rail wrong acorsance wth which sampling was cared out known the method used, ‘ : the test result(s) obtained; and the units in which the result is expressed; and * ithe repestabilty has been checked, the final quoted resuit obtained, aso mention all operating detas not specie in thie MPOB Test Meth ronal ther wih any incidents which may have influenced the resus) ean ve wat ropet shal la all ination necessary forthe compete Wentfestion ofthe woe 177‘Appendix A (informative) MPOB Test Method pa Results of interlaboratory tests. Peroxide 23: 2094 Valug International Collaborative tests have been carried out on the method given in this MPOB Teg Method in accordance with ISO 5725: 1986" AAtest on coconut ol lard, soln oi, ove oil and palm stearin was organised by Research Laboratory, UK, under the EU Standards, Measurement and Testing Programme, n 1999. The results are given in Table A.1 ‘Table A.1 Test on coconut oll, lard, solin oll, olive oll and palm stearin Food Tard Solin off ‘Coconut Olive olf] Pain oll stearin ‘Number of laboratories 14 8 5 6 16 Mean value, meqikg 134 288 Bat 24.10 | Sar Repeatabilty standard deviation, 5, core | 0783 | 0160 | 0983 OTe meqikg 0202 | 0513 | 0445 | 2752 | 204 Repeatability limit, , mea/kg Reproducibilty standard deviation, Se, | 0349 | 0308 | 0088 | 3910 | 2a megkg Reproducibility mit, R, mearkg os7s_| osez | 2768 | 10975 | 67% —— "180 8726: 1008 (now wahcravn) was used 1 btn the precton taba 178