V-A346_ Appendix X E ‘The hyelronyl value is then given by the equation: Jon = (hydroxyl value as determined) — 31.1y E. lodine Value (Ph. Bur. method 25.4) ‘The iodine value fis the number tha expreses in grams the quantity of halogen, calculated a8 iodine, that can be fixed in the prescribed conditions by 100 g ofthe substance. When the monograph doesnot specify the method tbe used, mahod A is applied. Any change from method A to method B is validane, METHOD A Unless otherwise prescribed, use the fellowing quantities (Table 2.5.41) for the determination, Table 2.5.41 Presumed vale h Quant of sampie Tee tan 2 10 20-40 05-035, «0-100 025-015 swore hn 100, 015-010 Introduce the prescribed quantity ofthe substance to be ‘examined (mg) into a 250 mi. flask fitted with a ground- slass stopper and previously dried or rinsed with glacial acetic acid R, and dissolve it in 15 mL. of chlorform R unless ‘otherwise prescribed. Add very slowly 25.0 ml. of iadine bromide solution R. Close the fask and keep i in the dark for 30 min unless otherwise prescribed, shaking frequently. Add 10 mL of « 100 g/L solution of porassim iodide R and 100 mL. of water R, Titrate with 0.1 M sodium thieulfate, shaking vigorously until the yellow colour is almost discharged. Add 5 mL of sch solution R and continue the tration adding the 0.1 M sodiuom thionlate dropwise ‘until the colour is discharged (1, mL of 0.1 M sodium thiosulfate). Camry our a blank test under the same conditions (ny mL of 0.1 M sodium thiosulfate). 1269 (mm) METHOD B Unless otherwise prescribed, use the following quantities (Table 2.5.4.2) for the determination, Table 25.4.2 Provumed value Mase (=) ‘Mass (5) odine chloride 4 Georresponding (corespning ‘salon (sh) Noanerceas of anencen of 150 percent IG) _100 per eeat 1) 3 eaeia asie0 2s 5 5070 6260 es 10 2308 so 20 0 ons coms 20 o osm 0058 20 0 oars > 03006 20 100 02536 oats 20 129 ons 02648 2» 10 oue 02066 2 16 ose? 1983 20 190 ono ote » 20 om ous 20 Te mf hemp i ut wg of aie cre soon of 50 percent n 69 the amount sed e100 percent 130 po amount absorbed. of Irae he rected say of beans examined (mg) into a 250 mi. flask fited wih 2 8 ts soe tnd evita we oil an dein of a Wn of beg a a etc ped ens ek Ser nag pant ges ae soniye nese a ne a Tie 25.02 can de ht eo es 30 in lon ote paced ese ee AAI mies 0 ph otaeestpensee To) of ome evita fen ‘shaking vigorously until the yellow colour is almost Athol Ad ch cha a a itt ng te 0.7 lan hae ee theirs chapel at oro ai Cy us Dk wr cae coe O1 nn tds Todine Monochloride Method (No Ph. Bur. method) ‘When the use of iodine flasks is prescribed, use flasks with @ ‘nominal capacity of 250 mL and complying with British Standard 2735:1956 (Specification for iodine flasks), unless otherwise specified. Dissolve the specified quantity of the substance being ‘examined in 10 mL of dichloromethane in a dry iodine Sask Add 20 mL. of iodine monachiorde solution, inser the stopp, Previously moistened with diuze potassium iodide soluion, and allow to stand in the dark at 15° to 25° for 30 minutes, Place 15 ml. of dilute potassium iodide solution in the top cup, carefully remove the stopper, rinse the stopper and the sides ‘of the flask with 100 ml. of water, shake and titrate with 0.1M seam thisuffate VS using starch muclage, added ‘towards the end of the titration, as indicator. At the same time carry out the operation in exactly the same manner, but ‘without the substance being examined, Caleulate the iodine value from the expression 1.269 ole Where v is the difference, in mL, between the titrations and 12s the weight, in g, of the substance taken, ‘The approximate weight, in g, ofthe substance to be taken ‘may be calculated by dividing 20 by the highest expected iodine value. If more than half ofthe available halogen is | absorbed, the test must be repeated, using a smaller quantity of che substance. F. Peroxide Value (Ph, Bur, method 25.5) ‘The peroxide value Ip isthe number that expresses in amiliequivalens of active oxygen the quantity of peroxide contained in 1000 g ofthe substance, as determined by the methods descibed below When the monograph doesnot specify the method wo be wed, method A is applied. Any change from method A to method B is alia2019 Appendix X A. Acetyl Value (No Ph. Eur. method) “Te ae value ofa substance isthe numberof mg of ‘ovum hytong roped to news he acted Ferned bythe hyd of 1g of he aceuted bance | Determine the saponification value, Appendix X G. | aeyateby the folowing method, To 10g ina 20-m ‘Rell sk nd 20 ml of ect andr. Suppor the sk on sheet ofest resistant material in whi hole {Bout fm in dtmeer ha bon ct and eat witha sal ‘hat flame, not more than 25 mum in height and wich does Spine onthe boom ofthe sk Bo gen under ‘thar toons for 2 hous allow to cool, pou into 00 mf eatr contined in age beak ad 0.2 of sce peor eof 30 mates. Col, waster & Jererrng fae tnd dacard te lower layer Wash he feud pct wih thee or more 50m quanits of a Tam, sated solution of dim cle unl he washings Se no longer aie ofa paper Fall shake with 20 mi. Sf rar we an rezone the aque lage compete os possible. Pour the aceylated substance into small dish, add Pot powdered ens suns, sr torogh and fe trough «dy, pleted iter paper: Determine the tepnfcnin wc of te aceyated sabe Calculate the acetyl value from the expression 1335(b— £)0335-0) whereas the sgponicaton valve of the Subance tod b's the saponfeatin val ofthe acetjlted mance _B. Acid Value (Ph. Bur. method 2.5.1) he acid valu isthe number that expresses, in milligrams se quant of potassium hydroxide required to neutralise he fee acids present in 1 g ofthe substance. Dirore 10.00 g of the substance to be examined, or the prescribed, (m g), in 50 mL of a minture of equal Shumes of ethanol (96 per cont) R and lige pelea 3, ously netalied with 0.1 M potasionIoxborde or 01M sodium narod, unless oberwisespecied, using 05 ml. ofphenlphhalin soluion RY as indicator. Hccrscary, eat to about 90 °C to dissolve the substance to be cxmined. When the substance tobe examined has paced, ate with 0.1 Mf pasion Idee or [a eon hydride wnt the pink colour persists for st 15 s(n. of tran). When heating has been applied 4 soli, maintain the temperate at about 90 °C he tron, 5.6ln k= ster Value Be. mead 2.5.2) sa tle Fs isthe mamber that expresses in migrams ae of potassium hydroxide required to saponify the Min 1 of dhe mbstance, I is eaculated from ton Yale Jy and the aid value Ie Isla Appendix XD V-A345 D. Hydroxyl Value (Ph, Bu. method 2.5.3) ‘The hytromyl value Joy is the number that expresses in zlligrams the quantity of potassium hydroxide required to neutralise the acid combined by acylation in 1 g of the substance, # METHOD A <4 Introduce the quantity of the substance to be examined shown in Teble 25.3.1 (w'g) into a 150 mL acetylation flask fited with an air condenser, unless another quantity is prescribed in the monograph. Add the quantity of acetic anhydride solution RI stated i Table 2.5.31 and ettach the sir condenses. ‘Table 2.5.31 Presumed vale Ton Quantiy ofsample Volume of © scegating reagent (aL) 10-08 20 30 100-150 1s 50 150-200 10 50 20.250 07s 50 250-300 060 6120, s00r100 300-350 10 100 950-700 075 150 709-950 as Bo ‘Heat the flask in a water-bath for 1 Keeping the level of the water about 2.5 cm above the level ofthe liquid in the flak Withdraw the flask and allow to cool. Add 5 ml. of water R through the upper end of the condenser. If cloudiness appears add sulicient pyridine R to clear it, noting the volume added. Shake the flask and replace in the water-bath for 10 min, Withdraw the flask and allow to cool. Rinse the ‘condenser and the walls of the flask with 5 mL. of aliohol R, previously neutralised to pholphuhalen soluion RI. Tirate With 0.5 M alcoholic potassiom hydroxide using 0.2 ml. of ‘phenolphihalsin solution RI as indicator (my mL of 0.5 M alcoholic potassium hydroxide). Carry out a blank test under the same conditions (n, mL. of 0.5 M alcoholic porasiom Inydroide). +h METHOD B Introduce the prescribed quantity of the substance to be examined (m g) into a perfectly dry 5 mL. conical flak fied ‘with a ground-glass or suitable plastic stopper and add 2.0 mL. of propionic ankycride reagent R. Close the flask and shake gently to dissolve the substance. Allow to stand for 2 h unless otherwise prescribed. Remove the stopper and transfer the flask and its contents into a wide-mouthed 500 mL. conical flask containing 25.0 mL. of a9 g/L. solution of aniline Rin. eelohexane R and 30 mil of glacial acetic acd R. ‘Switl the contents ofthe flask, allow to stand for 5 min, add 0.05 mi. of ental vile solution R und titrate with 0.1 Mi perchloric acid until an emerald-green colour is obtained (im mL. of 0.1 M perchloric acid). Cazry out a blank test under the same conditions (r mL. of 0.1 M perchloric acid) 5.610(m ~ ma) Jon To take account of any water present, determine this (per cent) by the semi-micro determination of water 25.12.