Tiêu chuẩn iso 01067 1974 scan

NAL STANDARD INTERNATIONAL ORGANIZATION FOR STANDARDlZATlON+ WX~YHAPO~HAI I OPrAHHJA~I l l l I I0 CTAH!JAPTH3ALWi~ORGANISATION INTERNATIONALE DE NORMALISATION Analysis of soaps Determination of unsapo[.]

INTR ATIO AL O G NIZATIO FO STADR lZATlO +.WX~Y HAO~HI O rA HHJA ~I I0 CTA H!JA PTH3ALWi~O GNISTIO INTR ATIO AL DE N RMALISTIO

Analy e d s sav n - D& termina tio d la te e r e mat&e in a p onifia b le , e mat&e in a po ifig s

et e mat&e sa po ifia ble in a po ifik s

F ir st editio - 197 -06-15

i

6

!2

Desc riptors : soa ps, s rfac ta nts, c emica l ana ly sis, determina tion of content sa ponifica tion

;

IS0 (h Interna tio a l O rga nizatio for Sta d rdiza tio ) is a worldwid fe era tio

of na tio a l sta d rds institutes (IS 0 Memb r B odies) The work of d v lo in

Interna tio a l Sta d rds is ca rrie out throug IS0 Tech ical Com m ite s Ev ry

Memb r Bo y intereste in a s bject for which a Tech ical Com mite h s b e set

up h s th rig t to b re rese te o tha t Com m ite Interna tio a l orga niza tio s,

g v rnm ental a d n n-g v ernm ental in la iso with ISO , a lso take pa rt in th work

D ra ft Interna tio a l Sta d rds a o te by th Tech ical Com mite s are circ la te

to th Memb r Bo ies for a pro al b fore th ir ac e ta ce as Interna tio a l

S ta d rds by th IS0 C ounci

P rior to 19 2, th res lts of th work of th Tech ical Com mite s were publsh d

tra sform ed into Interna tio a l Sta d rds A s pa rt of this proces , Tech ical

s ita ble for tra nsform a tio Interna tio a l Sta d rd IS0 10 7 th refore re laces

IS0 Recom e d tio R 10 7- 19 9

folowin countries :

Au tria

Belgium

Ca a a

C hie

Czech slo ak ia

Egypt, Ara Re of

F ra ce

Germa y

Hun ary

In ia

Ira n

Irela nd

Isra el

Ja a

Kore , Re of

Neth rla ds

New Z eala d

Pola d

P ortug l

Roma ia

South Afric a , Re of

Sp in

Sw ed n

S witzerla d

Turkey

Yug slav ia

No Memb r Bo y expres e disa prov al of th Recomm en atio

ISO /R 10 7 into a Interna tio a l Sta d rd :

Unite Kin d m

0 Interna tiona l Orga niza tion for S ta nda rdiza tion, 194 l

Analysis of soaps - Determination of unsaponifiable,

This Internatio al Stan ard spec ifie a meth d f or th

c om ercial s a s, ex c lu in c ompo n pro uc ts

2 FIE D OF A PPLICA TION

c onte ts of pro uc ts, oth r tha n fe faty ac id , whic a re

s luble in h x an or lg t petole m (u sa po ifia le

(u sa po ifie sa po ifiale mater

The meth d is n t aplc able to s a s e ric he with sterols

or lo g c hain alc oh ls, n r to s a s c onta inin perume

Ex tractio of mater sluble in h x an , an titatio of th

s lutio

Sa o ific atio of pro uc ts s luble in h x an n utalzd in

this way a nd ex trac tio of th u sa po ifia ble mater by

h x a ne

e uivale t purity T he reag nts s al have th folowin

c harac teristic s :

with th etha nolc potas ium hydrox id s lutio (4.4) u in

th ph n lphtha lein s lutio (4.6) as in ic a tor

4.2 So ium hydro e c arbo a te, 10 g slutio

4.3 n-Hex an , tec hnic al gra de or, fa iln this, lg t

bromin n mber le s tha n 1, a nd fe fom re id e

s lutio in etha nol

s lutio in etha nol

4.6 Ph n lphtha lein, 10 g/l s lutio in 9 % (V / V )

etha nol

O rdinary la boratory a pp ratu a nd, in pric ula r :

5.2 Sepratin fu n ls, 5 ml a nd 2 0 ml

c mplyin with ISO/R 17 3

5.4 Mic roburete, 2 ml

5.5 Pipete, 10 ml c omplyin with ISO/R 648

5.6 Ov en, c ap ble of bein c ontole at 10 + 2 “C

T he la ora tory sample of s a s al be prep a re a nd store

in ac c ordanc e with th in tuc tio s given in ISO

Soa s - Sampln 1)

7.1 T est porio

Weig , to th n are t 0,0 1 g, a bo t 5 g of th laoratory

sample, th s a bein fin ly gra te , into th 2 0 ml beak r

(5.1)

7.2 Determinatio

Add 5 ml of th n uta lizd etha nol (4.1) a nd 5 ml of

porio (7.1) Dis olv e th s a by h a tin to n t ao e

70 Oc

Afer th s a is c mpletely dis olved, alow th slutio to

s pa ra tin f un el (5.2), rin in th beak r s veral time

with a mixture of e ua l v olume of th n uta liz d etha nol

(4.1) a nd th s dium hydro e c a rbo a te s lutio (4.2)

a nd ex trac t thre time , stirin c arefuly , eac h time with

5 ml of th h x an or th lg t petole m (4.3) C ombin

th ex trac ts, f ilter th m if n c s ary , a nd was th m u ti

1) In prepa ratio

n utral to p e olp th lein, u in for e ch wash 5 ml of a

mixture of e ual v olumes of th n utralze eth n l (4.1)

a d water Normaly thre washin s are s fic ie t T ra sfer

prev iou ly drie in th ov en (5.6) c ontrole at 10 rt 2 ‘C,

alowe to co l in a d sic ator a d weig e to th n arest

0,2 mg

Ev ap rate most of th solv ent o a b i n water b th a d

remov e th last traces with th aid of a g ntle c re t of

dry a ir directe into th flask whie it is h ld o lquely ,

almost e tirely im erse in th b th, a d rotate

Dry th flask a d residue for 5 min in th ov en (5.6)

c ontrole at 10 f 2 “C, alow it to co l in a d sic ator

a d weig to th n arest 0,2 mg Re e t th o eratio s of

two s c es iv e weig in s d es n t ex e d 2 mg L t this

Dis olv e th residue in a few mi ltres of th n utralze

eth n l (4.1) Usin th micro urete (5.4), titra te th fre

a c idity with th p tas ium hydroxid solutio (4.4) u in

th p e olp th lein solutio (4.6) as in ic ator, unti th

solutio turns pin Note th v olume V of this solutio

u e for th titra tio

a d b i it un er reflux for 3 min T he a d a v olume of

water e ual to th v olume of th solutio a d tra sfer th

solutio qua titatively to th 5 ml se aratin fun el (5.2)

u in a few mi ltres of a mix ture of e ual v olumes of th

n utralze eth n l (4.1) a d water to rinse th flask

Extract thre times, e ch time with 10 ml of th h xa e or

th m unti n utral to p e olp th lein, u in for e ch wash

10 ml of a mix ture of e ual v olumes of th n utralze

s fic ie t T ra sfer th solutio qua titatively into th

10 ml flask (5.3) previou ly drie in th ov en (5.6)

c ontrole at 10 f 2 O , alowe to co l in a d sic ator

a d weig e to th n arest 0,2 mg

Ev ap rate most of th solv ent o a b i n water b th a d

remov e th la st traces with th aid of a g ntle c re t of

dry a ir directe into th flask whie it is h ld o lquely ,

almost e tirely im erse in th b th, a d rotate

Dry th flask a d residue for 5 min in th ov en (5.6)

c ontrole at 10 + 2 ‘C, alow it to co l in a d sic ator

a d weig to th n arest 0.2 mg Re e t th o eratio s of

two s c es iv e weig in s d es n t ex e d 2 mg L t this

Th

mater i- unsa o ifia le mater in th so p is e ual to

Th p rce ta e, by mas , of unsa o ifia le mater in th

so p is e ual to

10

m2 x -

%

mater in th so p is e ual to

10

X-

m

where

m, is th mas , in grams, of th test p rtio ;

m, is th mas , in grams, of th first extract;

m2 is th mas , in grams, of th seco d extrac t;

of th so p (se n te);

V is th v olume, in mi ltres, of th 0, N sta d rd

volumetric eth n lc p tas ium hydroxid solutio (4.4)

NOT - T he me n rela tiv e molar mas M of the fa tty ac id of the

sop c an b determined by titra tion of the fa tty ac id isolated a fter

the sa ponific a tion of a sample of the origina l sop, the elmination

of u sa onifiale mater an the a c idific a tion of the sop solution

res lts o tain d It sh l also me tio a ll test co ditio s

a d proce ural d tais n t sp c ifie in this Intern tio al

Sta d rd, or which are o tio al a d a y factors which may

Th test re ort sh l giv e a ll informatio n ces ary for th

complete id ntific atio of th sample