2.20l. D鏡餅m血虹ion of血eAcid Value (A.V.

) and the Acidity

(rifth雷dition : Method工I.D.1)

1. SCOP電

Thie St狐d種rd describe3調o meぬods forぬe dete重富止mtio種of the free fatty acid coatetlt Of
まn辻はI紬d vegetable oilg,∴紬d fats. mis c紬be e坤re年製d as an aL⊂id valu亀, Qr租acidity.

2. F工珊O雷蝕や重工C鯖工00

Thi8 tand種rd is applicable to animl狐d vegecable oils and f種陶. Ic is not applicable亡o

青さ糠e3●

3. 耽雷鄭重重工〇㍍§

Tbe acid value (A・Ⅴ・) is∴the nt血e章of ng of poね38iu血hydroxide required ⊂o neuCralize the
free f種cty acidさi寄l g of the fat.

でbe acidity ie a co調Ventio調l e可re的ion of the percentage o毒free fatty acids・ According co
the aature of the fa亡it c狐be e禦PreS3ed as :

Naヒu臓Of fat E可re83ed種8   Mblect11ar ueighc

Coconuc. pal面kemel and si血lar oils Lauric acid

Pal種oil Pal珊icic acid
All otheでoils Oleic acid

tmen the reeult i8 r勘orted a8 "acidity"J bu[ not further definedl then conventiona11y the
種cidicy is always e禦PreS3ed as oleic acid.

rf the saIIPle c〇〇tai調心neral acids● by convencion軸ey are calcul種ted as fatty acids.

4. J虹￨D VAI.UE - IⅢ)ICA富OR M細田阻D

4.1. Princi

Soluti調of a kno場面quantity of the fat co be軸ralysed in a血xture of ethnol and diethyl

e亡her, follo耽d by titr亀tion of the free f亀と亡y acid種PreSetlt竜th紬ethanolic solu互on of
PoCa蜘itn hydroxide.

ん.2.健やara亡u章

4.2.1. 250ml cotlical flask.

4・2・2・ 25「n bure耽e' graduated in O・l nl.

4.う.鼠ea慮en亡s

4.3.l. Solvent正xt耽e l11 (VlV) of 95 per cent (VIv) e血anol and diethyl ether. Neutralize
exac叫y, just before t鳩e, by means of the pot種s雷i調hydroxide solu互on (4.3.2) i種
とhe presence of O・3 ut of phenoIphthalein solu亡ion (4.3.3) per 100 nl of亡he壷xture
毎〇号e j).

4.3.2. Potas種i皿trydroxide' 0.1 N, Or if nece33まry O.5 N書SOlution in ethanoll aCCur亀Cely

stand亀rdi2ed.
me exact concentratio寄should be ktlOml and checked i筋腫diacely befo富e uSe. U3e a
3olution p職p種red a[ 1e種3⊂ 5 day種previously and decan亡ed into a bottle of brown

glass' ProVided正th a rubbe富3tOPPer.珊e solution should be colourle3S Or∴さtrav

yello曾くれOきe 2).

4.3.3・ PhenoIphchalein, 10 g/1 solucion in 95 per∴Cetlt (Ⅴ/V) e血種nol.

与2

j
 うう

4.4. Procedure

Prep寄re the s坤le according to 2・001, "preparation of the s坤le". Deter血ine size of脚や1e
according to the follot'ing table:

Expected acid value 陥s容of test portionl in g

Weighing accuracyl in g
1 4 与

▲0 1-′-ヽ-

02 00
0.0与
- - - >

0.02
重ブ う

雫ノ "⊃ lふ
●   ●   ●
1

0.01
7

0.○○1
0.0002
蝿gh tlhe亡es[ portion into aぐOnical fla8k (4・2.1)・ DissoIve it in about 150 ml of the soIvent

誌ee措霊i藍d霊h薄黒,t: #葦喜ぶa誌葦霊4蕊in.
seconds)くれ0鼻夢3.れ0お4).

If亡he qu弧tity of O.1 N potas8i調hydroxide golution required exceed8 20 ml' a O.5 N solu血n
蜜豆ou重d bさused (耽汚e 5).

4.与. E re§8ふon of 鬼esul書6

The acid value (A・Ⅴ・) is given by the fomula :

う6.1 Ⅹ T x∴V

A.Ⅴ.な
聯

where V ig∴the nuめer of ml of the standardized potaきsium hydroxide∴gOlution (4.3.2) used

くれoきe 6)書
出s the exact no冒mality of the standardized potasslum hydroxide soluこ1on (4.3.2).
巾is the ‘0凪雷電} in g● Of the te雷t POrtion.

う. A寄重D馳耽農PO富掛け重飢露骨櫨職場棚的D

う.l. すore勘〇着d

旺$雌thod should be e中loyed in8tead of Method 4 for the detemination of free acidi亡y in
highly coIoured oi1雷劃d fat9.

5.2. Principle

me free fatty acidg are titrated potentiooo露trically in a non-aqueOug耽di調Yith a golution

of po亡as雷i調hydroxide inあ。PrOPanOl.

5.3. Apさaすa亡us

5.3.1. 150-田l tall fom beakers.

5.3.2. 1000-露l volu血etric flasks.

5.3.3. 25叫l burette, graduated in O.1血.

5・3.4・ P櫨能ter equipped vith glasg∴and cal調el electrodes (北房e 7).

Contact bet鵬en亡he $aturated pota構ium chloride solution and the te6t∴solution is
血ade acro雷s a sintered gla雷8 Or POrCelain disc. at leas亡0.3 (聞直thick.

5.3.5. Stirrer, Preferably調gnetic stirrer.

う.4. __鼠eagen亡s

5.4.1. 2-Prop種nol (砧opropanol)・ analytical reagent quality.

5・4.2. Hlethyli雷Obutylketone. analytical reagent quality● neu亡ralized imediately before uge

by theあopropanolic potagsi調hydroxide∴Solution (5.4J) to a faint pink coIour with
PhenoIphthalein indicator.

5・4・3. Benacic acid, aCidi調triぐgtandard quality.

5膏・4・ Pota雷Si調hydroxide・ O.1 N solution in 2-PrOPanol (う・4.1)● aCCur命tely star]dardized.

j
 与4

DissoIve 7 g of potassiun hydroxide pellecs in lOOO nl of 2-PrOPanOl (5.4.1)・

5.4.5. Potas3iu血hydroxide, O.5 N solution in 2-PrOPanOl, aCCuraCely standardized・

Di響gO ve 35 g of poc亀皐Si血hydroxide pellet寄in lOOO nl of 2-PrOPanOl (5・4.1).

Stand亀rdi露e∴the solutions as follow5 : Weigh accurately co vi亡hin O.OOO2 g abouc O.15 g

〈for che O.1 N solution) or O.75 g (for the O.5 N solution) of the sc組dard benzoic
acid (5.4.3).富ransfer inco a be亀ker (5.3.1) and dissolve in 5O ml of勘eChylisobu亡ylke-
亡one (う.4.2).                                            .
工nsert∴亡he electrodes of the p寄りeter (5.3.4.), S博rt Che sCirrer (5.3.5) and citrate
with the pocassiu孤hyd富OXide solution (5.4.4 or 5.4・5) co the equivalence poinc (枇7te 8).

軸掛嘉ity - 1翳謁

where *: E# #:r需l#蕊書誌豊島OXide solution (5.4A or 5.4・5) used・

与.与. P富ocedu富e

Prepare亡he s劇中1e a⊂eOrding亡O 2.OOl, "p￨噛P年輪t主o櫨Of the sa迫やIe".

Weigh亡o Vichin O.01 g 5 to 10 g of prep種red fat inco a be種ker (5.3.1). DissoIve in 5O ml of

面ethylisobu亡ylketone (5.4.2).

Insert∴the electrodes of che pH孤ete重(5.3.4)袖d scart∴Che stirrer (5.3.5). Titrace Yith

Che pota8Si調hydroxide solution (5.4.4 or 5.4.5) 0.l or O.5 N (according to∴the acidi亡y of
the s劃Ple) to tl鴨equivalence point (れ0‡e 8).

与.6. E 冒eSSion of Results

The aぐid value (A.Ⅴ.) is given byぬe fo調ulal :

う6.1 ⅩgI xⅣ
A.Ⅴ.暮
珊

t'here y ig che nu血er of 。l of the st紬d種rdizedあoprop紬olic pota雷Si調hydroxide solu互on

(5.4.4 o重与.4.与) used,
r i§亡he exacc∴nOrmli亡y of the s[andardized j80prOPanOlic po調§Siun hydroxide solution
(5.4.4 or与.4.与) used,
億is che珊asS. in g, Of the ces[ portion.

6. AC工D工でr

6.1. Principle

The acidity is calculated fron Che results obcained in. the decemi調tion of che acid value
by the indicator 。ethod or che potencio面etric∴面ethod.

6.2. 雷 重esさ王on of 京e3ul亡s

The acidity, in pe富∴Cent, is g￨Ven by Che formul種:

審議 V x付
10 競

tinere y is∴Che n軸心er of the standardized e耽anolic (4.3.2) or秦opropanolic (5.4.4 or 5.4.5)
PO亡assi細o hydroxide solu正on u容ed.
T is∴亡he exacc nor噌Iity of the scand靴dized echanolic (4.3.2) orあopropanolic
(5.4.4 or 5.4.5) potassi調hydroxide solution used.
M i3 Che面Olecular競ighc∴8dopted (20O, 256 or 282 according co the Table in 3),
押上竜王h豊.細幽占う.玉露さきof血豊エ亀S主審o重珪o租・

7. 押O重量S

Z.血the 8OIvent面ixture die[trylethe富eVenCually狐y be substitu⊂ed by toluene.

2. A s[able colourless solu亡ion of potassi調hydroxide can be叩ep種red in the follo曹ing man-

ner :∴reflux 10OO ml of ethanol tJith 8 g of potassium hydroxide and 5 g of al細面止tliu種

Pellets for l hour, then di容til ioo腫diately. DissoIve the required a調ount of potassium
hydroxide主n亡he distilla亡e・ Allowi the whole Co gtand for several days and dec袖t the clear
supema亡ant liquid fro鴫the deposited poc種ssiu細c亀めonace.
 うう

The §Olutioれ軸n also be prepさred竜thout distillation in the followi唯調鵬er : add 4 mi

o支alu血ni調butyl●te to 1000 nl eth狐01狐d allo91 the心㌍u冒e to 8龍nd f〇着seVeral days.
De軸nt the supernat種nt liquid and dissolve therein the necessa重y関ount Of pot種s8l調
hydroxide. mi$ SOlution i8 re亀dy for use.

3・ Inl the∴C種露e Of very lo曹aCid v種lue (くl) it is∴useful to blot' a low′ gtre狐Of nitrogen
into the solution to be titr種ted.

4・珊e ethされ01ic 8亡md種rdized potassi調hydroxide solution (4.3.2) c亀n be substituted by an

aqueous $olution tJhen the∴きCid vすlue is lo場.

5. If the∴S0lution becoo唯8∴CIoudy during the titr寄tionl add a further quantity of the solvent
面ix亡ure (4.う.1).

6・珊e nor鴫lity of [he ethmolic∴st寄nd耽di粧d poca§slu面tryd関孤de golutlm v亀でie8 uth the

te重Pe軸tu冒e∴さnd it皿y be ugeful to co冒rect a§嘗o11ot'§:

V雪㌔【l-0・0011(e-冨l

where yt is the volu鵬at the t餌Per種ture t’

きis the t餌Pe耽turel i種Oc' at which the dete蘭in種tion i8 nede,

きo is∴the t餌Perature. in Ocl at which the ethmolic po亡きs8i調hydroxide solution

h種g been∴gtand種でdized.

7・ ￨t i8∴種dvisable to store the gl種g8 electrode in Yater Or● better∴still● in鵬亡hyligo-

butylketone for 12 hourg p書ecedi喝the tit耽tion・ D重y it very Bently rith a p￨eCe Of
filte重申すper befo職耽e・面喰diately aftJer the tit馳tiJan● ri寄韓it玩軸me血ylico-
butylketone, then 'ith 2-PrOP亀nol,軸d fi鵬lly竜th distilled Yater.

1f the electrode doeg not function sati8fact○○ily● it調y be pogきible to regener種te it by

ioo鵬でsion f○○ 24 hou冒s in a l N 8olution of hydrochloric耽id in 2￨roP種nOl. After thi§
treatnent∴亡he electtode should be Yashed t'ith di8ti11ed脚ter, then Yith 2-ProP種nOl紬d
Wi亡h nethylisobutylketone.

A thick sintered gl種sg or porcel種in di種C betYeen亡he 8寄[ur亀[ed po[亀s種iu面chloride∴Solution

種nd the test∴Solutim preven誌diffusion currents and p靴asitic potential§.

8. Equiv種leれCe POin亡/inflexion peint

珊e equivalence point us脚lly corresponds approxi種種tely to the re寄ding lO on the叩8Cale,

and c紬be deterI止れed gr亀phic種lly by obgerving the inflexio種point on tbe neut耽li審ation
curve. Altemati÷ely. it∴can be calculated as the figu重e f〇番tJhich血e first differentiすl
Of the variation of ]Ⅲ as a function of the軸oou調書of d8OP重OPmOlic potな容giun hydroride
golution added reaches a皿xio鵬。, Or∴the value for whlch the second dlfferent撮l becomes

髄.B. ￨t ig not possible to dete冒血ne the inflexion point in theぐ種ee Of crude cottonseed
oils rich in gogsypol.

h血is∴CaSe the inflexion poi種t m坤be・鼠ken arbimrily :g the叩corre坤onding to the

eq噛iv血erLee陣itlt朗艇n Oleic喋魂is n蝕虹塊li之ed by pe龍朗聞襲hydroxide in the∴S卸Oe SOIvent
種s that used for the titration.

Diss0lve about O.282 g of oleic acid in 50 nl of nethylisobutyl露etone (5.4.2). Congtruct

the curve for neutr種lization of the oleic acid by the pot寄s§iu孤hydroxideさOlution (5.4.4
Or 5.4.5) to be u種ed. Re種d off on the curve the pH of the inflexion point (repre8enting
theoretically the addition of 10血of a O.1 N solution of pot種Bsiuoo hyd重oXide).

Apply this fiさure∴to the neut耽Ii露寄tion cu重Ve Of the cotton雷eed oil to deduce the a。ount
of po調ssiu調hydroxide solution required to 'heutralize" the∴COt亡On種eed oil.