Tiêu chuẩn iso 01065 1991 scan

I NTERNATI ONAL STAN DARD I S0 1 065 Secon d edi ti on 1 991 09 01 Non i oni c surface acti ve agents obtai ned from ethyl ene oxi de and mi xed non i oni c surface acti ve agents Determi nati on of c[.]

STANDARD 1 065

Seco d e itio

19 1-0 -01

point

A ge ts d s rface n n io iques o te u B pa r-ir d Iox d d’&hy/&n

trouble)

Refere ce numb r

Foreword

IS0 (the Internationa l Orga niza tion for Sta nda rdiza tion) is a worldwide

federa tion of nationa l sta nda rd b dies (IS0 memb r b dies) T he work

of pre a rin International Sta nda rd is norma lly c a rried out throu h IS0

re resented on tha t commite Interna tiona l orga niza tion , gov ern-

menta l an non-gov ernmenta l, in laison with ISO, a lso ta ke pa rt in the

work IS0 cola bora tes c losely with the Interna tiona l Elec trotec nic a l

Commis ion (IEC ) on all ma tters of elec trotec hnical sta nda rdiza tion

Dra ft Interna tiona l Sta nda rd a do ted by the tec hnic a l commite s a re

c irc ulated to the memb r b dies for votin Publc a tion as an Inter

na tiona l Sta nda rd req ires a pprov a l by at lea st 7 % of the memb r

b dies c a stin a v ote

Internationa l Sta nda rd IS0 10 5 was pre a red by T ec nica l Commite

ISO /T C 91, Surfa ce ac tiv e a gents

in order to exten the s o e to cov er mixed non-ionic s rfa c e-a c tiv e

a gents

0 IS0 19 1

All rig ts re erv ed I\i p art of this p ub licatio may be repro u e or uti z d in an form

or by an mean , ele to ic or me ha nical in lu in ph to opyin a nd microfim, with ut

permls lo in writin fom th pub lis er

internatio al Orga niza tio for Standardiza tio

Cas Po ta le 5 l C -121 Ge bv e 2 l Switz rlan

Printe in Switz rla nd

Intro u tio

ra ised, b cau e of the forma tion of two lq id pha ses T he temp ra ture

a ov e whic this phenomenon occ \ Jrs is refered to as the clou p oint

c a lled the “temp ra ture of c larific ation” as defined in IS0 8 2:19 4,

Surfa ce a c tiv e a gents - Voca bula ry (definition No.10)

T he temp ra ture of c larific ation is ofen determined as the “clou

p oint”

T he knowled e of the clou p int is of grea t imp rta nce in all app li-

c ation , as the s rfa ce-a ctiv e pro erties v a ry v ery ra p idly arou d this

temp ra ture

T he determina tion of the clou p int of a non-ionic prod ct is a ra pid

an prec ise method of c ontrol In ma nufa cture, it is the q ick st method

of a sses in the q a ntity of eth lene oxide b n ed to a giv en b se

p oint an the extent of ethox la tion ten s towa rd an a symptote; a s a

con eq en e, this method of c eckin is les prec ise for prod cts with

a lon ethox l c ha in

T he clou temp ra ture is a lower cr itic al temp ra ture of se a ra tion;

a ov e this c r itical temp ra ture, the solution se a ra tes into two pha ses,

an the a p ara nce of these two phases when the temp ra ture is ra ised

lea ds to the clou in of the solution This pro erty is not sp ec ific to

ethox la ted deriv a tiv es an it is p s ible to determine clou temp ra -

tures for other typ s of deriv ativ e

Method A, B an C sp c ified in this Interna tiona l Sta nda rd dea l p r i-

mariy with the determina tion of the clou p int of non-ionic s rfa c e-

lp op hi c b se molec les s c a s fatty a lcohols, fatty amines, fatty a c-

id , a lkylphenols an esters of fatty a c id

Other non-ionic s rfa c e-a c tiv e a gents, e.g eth lene oxide/pro ylene

oxide block co olymers, a re k nown to hav e pro erties whic mak e it

dific ult to determine their clou p ints Su h pro erties inc lu e the a p-

p a ra nce of a progres iv e clou in ov er a temp ra ture ran e of sev era l

degre s, an the existenc e of two or thre v ery distinc t clou p oints

T w o further method (D an E) a re therefore sp c ified for the determi-

C a re n s ita b le

Non-ionic surfa ce-a ctiv e agents obtained from ethylene oxide

This Interna tio a l Sta d rd sp cifies fiv e meth ds

for th me s reme t of th cloud p int of n n-io ic

s rfa ce-a ctiv e a e ts

s rfa ce-a ctiv e a e ts d riv d from ethyle e oxid

Meth ds D a d E are inte d d for u e, a fter a re -

for whic method A, B an C prov e u sa tisfa c tory

Su h prod cts inc lu e mixed non-ionic s rfa ce-

a c tiv e a gents s c as those deriv ed from eth lene

oxide/ pro ylene oxide block co olymers

T he selec tion of the method (D or E) de en s on the

temp ra ture at whic the a c id aq e u solution of

is not a pplc a ble, howev er, to prod cts deriv ed from

fatty a c id or fatty -ac id esters

NOT 1 Th cloud p int of pro u ts d riv d from fa tty

a c id or fatty -a c id esters can only b determined if the

re ea ta bi ty of th d termina tio is v erifie

throu h referen e in this tex t, c on titute prov ision

of this Interna tiona l Sta nda rd At the time of p ubl-

c a tion, the edition in ic a ted were valid Al sta n-

a re en ouraged to inv estiga te the p os ib ilty of a p-

plyin the most recent edition of the sta nda rd in-

dica te b low Memb rs of IEC a d IS0 ma inta in

re isters of c re tly v a lid Interna tio a l Sta nd rds

IS0 6 7:19 0, Surface a ctiv e a e ts a d d terg nts

- Meth ds of sa mple div isio

IS0 17 3: 19 6, L b ratory glas ware - Boi n flasks

(n row-n ck ed)

IS0 217 :19 0, Surfa ce activ e a e ts - Pre aratio

of water with k ow n ca lcium h rd es

temp rature of certa in v ry pure d riv a tiv es of ethyle e

oxid if dis olv ed in disti e water of v ry low co du -

tivity In s ch ca ses, th solutio d es n t b come h t

ero e e u a t a d finite temp ra ture; instea d, o ly a

slg t los of c la rity is o serv d

th cloud temp rature to b me s re

If the aq e u solution of the non-ionic s rfa c e-

a c tiv e agent b comes clou y at a temp ra ture b -

twe n 10 “C an 9 “C, c a rry out the me s rement

in disti ed wa ter (se 8.1)

If the aq e u solution of the non-ionic s rfa c e-

a c tiv e a gent b comes clou y a t a temp ra ture lower

tha n 10 O C, or if the prod ct is not s fic iently soluble

in wa ter, c a rry out the me s rement in an aq e u

2 % (m/m) solution of n-b uty ldigly c ol (se 8.2)

Howev er, this method is not a pplc a ble to c erta in

prod cts with low eth lene oxide contents an whic

n-buty ldigly c ol

3.3 Meth d C

a c tiv e agent b comes clou y a t a temp ra ture

hig er tha n 9 ‘C , c a rry out the me s rement in a

by o era tin u der pres ure, to rea ch temp ra tures

hig er tha n the b oi n p int of the solution at at-

-

water content les tha n 0,l % (m/m)

NOT 4 Ev n with th giv n sp cifica tio , va ria ble

amounts of impurities in th n-butyldigly ol wi influe ce

th cloud p oint to a certa in exte t

5.2 Hydrochloric a cid,

sta nda rd v olumetric sol-

utio , c(HCI) = I0 mol/ l, for meth d D

NOT 3 It is a lso p s ible, if a re d b tw ee th pa r-

ties co cern d, to d termin th cloud p int in sa lt sol-

utio but this tech ioue is n t so se sitiv e a d th re is

n simple corela tio ‘b twee th res lts o tain d in sa lt

meth d

5.3 Buta -l-01, 5 % (17 /m) solution in wa ter of

p re in ac ord nce with IS0 217 , for meth d E

O rdin ry la bora tory a p ratu a d:

s rfa c e-a c tiv e a gent tested b comes clou y a t a

temp ra ture b twe n 10 “C an 9 “C, c a rry out the

me s rement in sta nda rd v olumetric hy droc loric

a cid solution, c(HCI = I0 mol/ l (se 8.4)

6.1 Co ica l fla sk, ca pa c ity 2 0 ml, complyin with

IS0 17 3

6.2 T hermometer, gra dua ted in 0,l “C, with a ra nge

6.3 Gra uate c ln er, ca pa c ity 10 ml

s rfa ce-a ctiv e a gent tested b comes clou y at a

buta n-1-01 (se 8.5)

6.4 Be k er, ca pa c ity 10 0 ml, c onta inin a tra ns-

pa rent hea t-transfer fhld (eth lene gly c ol, for ex-

a mple)

6.5 Test tub , ca pa city 2 ml

4 Prin iple

6.6 A mp ule, made of sa fety gla ss cov ered with

wire ga uze, outside dia meter 14 mm, in ide dia m-

eter 12 mm, heig t 12 mm

T he prod ct u der test is hea ted in solution a t the

req ired c on entra tion u ti the lq id is completely

o a que I is then c ooled, with con ta nt stir rin T he

temp ra ture at whic the o a c ity disa pp a rs is o -

serv ed

6.7 Ana lytica l b la ce

6.9 Ma n tic stirer with h ater

only Re gents of recog ized a na ly tic a l gra de an

only disti ed wa ter or water of e uiva le t purity

5.1 n-Butyldigly ol [2-2-butox eth x )etha nol

T he la bora tory sample of s rfa c e-a c tiv e a gent s all

struc tion giv en in IS0 8 7

T he n-buty ldigly c ol [C 4H,0(C H, 0(C H, 0H] s a ll

hav e the folowin c ha rac teristic s:

- den ity, ~ 0 = 0,9 4 g/ ml + 0,0 2 g/ ml;

n mb r of eth lene oxide u its b n ed to the b se

molec le, but it a lso de en s on the con entra tion

of the solution I is therefore es entia l to o era te

-

refra c tiv e in ex, np = 1.4 2 + 0,O O 1;

the test a t a c learly defined c on entra tion

8.1 Meth d A (Use when clou ines a p a rs

8.1.1 Test p rtio

Weig out, to th n arest 0,O l g, 0,5 g of th la bora -

tory sam ple (se clau e 7)

Proce d as in meth d A (se 8.1.2, b gin in a t th

seco d p ra ra ph)

at a tempera ture hig er tha n 9 “C )

8.3.1 Test p rtio

8.1.2 Determ in tio

Place th test p rtio in th co ica l fla sk (6.1) A dd

dis olv ed or disp rse

Place 15 m l of this solutio in th test tub (6.5) Put

th th rm om eter (6.2) in th tub , place th tub in

th b ak er (6.4) a d h at with th h atin a pla ce

it is com pletely o a ue (The o a city a p ars in th

forn of b n s which thick n a d th n co les e At

n tim e sha ll th tem perature of th solutio ex e d

by more th n 10 “C th tem perature a t which th

o acity a pp ars.) Alow to co l slowly whie stirin

disa p a r

NOT 5 The lquid may sta y clea r or o a les e t, d -

purity of th raw m a teria ls u e for th ir pre ara tio (se

clau e 3 n te 2 o purity of ma teria ls)

difere t test p rtio s unti a t lea st two res lts dif

ferin by n t more th n 0.5 ‘C are o tain d

at a tempera ture b low 10 “C , or when the

prod c t is in olub le in water)

8.2.1 Test p rtio

Weig out, to th n arest 0.01 g, 5 g of th la bora -

tory sample (se clau e 7)

8.2.2 Determ ina tio

Place th test p rtio in th co ica l fla sk (6.1) Add

4 g of th n-butyldigly ol solutio (5.1) Stir unti th

test p rtio is dis olv ed

Weig out, to th n arest 0,Ol g, 0,5 g of th la bora -

tory sample (se clau e 7)

8.3.2 Determ in tio

Place th test p rtio in th co ica l fla sk (6.1) Add

com pletely dis olv ed

Tra nsfer a qua ntity of this solutio to th gla ss

am-p ule (6.6), to a d pth of a proxim ately 4 m Se l

th amp ule by me ns of a flam e a d co er it with

co rse wire g u e Put it in th b ak er (6.4) co

-ta inin th h a t-ra nsfer fluid The up er e d of th

amp ule sha ll project slg tly from th b aker

tectiv e s re n of sa fety glas or tra spa re t pla stic

burst if it h s n t b e wel se le (se figure 1)

Place th th rm om eter (6.2) in th h atin fluid n xt

-n tic stirer (6.9) in o era tio ; sto th h atin whe

th lquid co tain d in th amp ule b comes cloudy

Alow to co l whie stirin th h a t-ra nsfer fluid

a d n te th tem perature a t which th cloudin s

disa p ars, as in ica te for meth d A (se 8.1.2)

difere t test p rtio s unti a t lea st two res lts dif

ferin by n t more th n 0,5 “C are o ta in d

cloud p int ca b d term in d in sa lt solutio ra th r th n

in a se le am poule

T he tech ique is a alo ou to tha t of meth d A (se 8.1),

th s rface-a ctiv e a e t b in dis olv ed in 10 m l of a

a ue u 5 g/ l solutio of so ium chlorid instea d of in

10 m l of disti e wa ter

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8.4.1 Test p rtio

Weig out to the nea rest 0,Ol g, 1 g of the la b ora -

tory sam ple (se cla use 7 )

8.4.2 Determ in tio

Place the test p rtion in the c onic a l flask (6.1) Ad

5 ml of the hy droc hloric a c id solution (5.2) m eas-

ured with the gra dua ted c y lin er (6.3) Stir u ti the

test p rtion has dis olv ed or disp rsed, then ad

hy droc hloric a c id solution (5.2) to giv e a final v olum e

of 10 m l

Place 15 ml of this solution in the test tub (6.5) Put

the therm om eter (6.2) in the tub , pla c e the tub in

the b a ker (6.4 ) an hea t with the hea tin a ppla nc e

(6.8) stirin the solution with the therm om eter u ti

it is completely o a que (The o a c ity a pp a rs in the

form of b n s whic thic ken an then coa lesc e At

- S afety sc ren

- Thermom eter

- Seled amp ule

- Tst solution

- Hea t-tra nsfer fluid

Stirer

n tim e sha ll th tem perature of th solutio ex e d

by more th n 10 “C th tem perature a t which th

o a city a p ars.) Alow to co l slowly whie stirin

disa p ar

NOT 7 The lquid may stay clea r or o a les e t, d -

purity of th raw m a teria ls u e for th ir pre a ra tio (se

clau e 3, n te 2)

difere t test p rtio s unti a t lea st two res lts dif

ferin by n t more th n 0,5 “C are o tain d

in m ethod D at a tempera ture hig er tha n

9 “C )

Weig out, to th n arest 0,Ol g, 1 g of th la bora -

tory sample (se clau e 7)

8.5.2 Determination

Place th test p rtio in th co ica l fla sk (6.1) Ad

me s re with th gra uate c ln er (6.3) Stir unti

p rse

Proce d as in meth d D (se 6.4.2, b gin in at th

seco d p ra ra h)

T ak e as th res lt th a rithmetic me n of at le st

tw o res lts which d n t difer by more th n 0,5 ‘C

In ica te, to th first d cimal place, th me n tem-

Cloud p int at 5 g/ l in disti e water:

n-butyldigly ol

Cloud p int at 5 g/ l in se le amp ule:

Cloud p int at 10 g/ l in I0 mol/ l hydrochloric

acid solutio : _

Cloud p int a t 10 g/ l, in water of calcium h rd-

n s 4 mg of Ca*+ io s p r ltre in th prese ce

of buta -l-01: _

10.1 Re ea ta i ty

n tio s carie out simulta e u ly, or in ra id s

o erator, sha ll n t ex e d 0,5 ‘C

10.2 Re rod c ibi ty

ex e d 1 “C

la rs:

a) a ll d ta ils re uire for complete id ntifica tio of

th sample;

b) a refere ce to this Intern tio al Sta d rd a d th

meth d u e , e.g “IS0 10 5, meth d A ”;

rie out:

d) th res lts a d th units in w hich th y h v b e

expres e :

n tio :

f a y o eratio n t includ d in this Intern tio al

Sta d rd, or re ard d as o tio al

5

IS0 10 5:19 1(E)

_ _ _-

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.-

=

._ -_ _

De criptors: s ra cta nts, n n-lo lc s racta nts, ethy le e ox id , te ts, clo d p oint d termina tio

Pric ba se o 5 p g s