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INTERNATIONAL STANDARD INTERNATIONAL ORGANlZATlON FOR STANDARDlZATlON MEX~YHAPO~HAR OPrAHM3AUMR no CTAHDAPTA3AUAA ORGANISATION INTERNATIONALE DE NORMALlSATlON Cryol i te, natural and arti ficial Deter[.]

INTR ATIO AL O GNlZATlO FO STA DRlZATlO MEX~YAO~H R O rAM3A MR n CTADPTA3AA O G NISTIO INTR ATIO AL DE N RMALlSTlO

F ir st editio - 197 -0 -15

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Desc rip tors : aluminium ores, c ry olte, cemica l a na ly sis, determina tion of content si c on dioxide, spc trohotometric a na lyis

:

IS 0 (h Internatio al Orga niza tio for Sta ndardiza tio ) is a worldwid fe eratio

g v ernm ental a nd n n-g v ernmenta l, in la is n with ISO, als ta ke p art in th work

te h ic a lly s itable for ta nsformatio Internatio al Stan a rd IS0 16 0 th refore

replac es IS 0 R ec mm en atio R 16 0-1970 to whic it is tec hnica lly id ntic al

Au ta lia

Au tia

Belgium

B razi

C hie

C ze h slov akia

Fran e

German

Hu ga ry

In ia

Iran

Israel

Italy

Neth rla nd

Norway

Peru

P olan

R om ania

S outh Afic a , Rep of

S pain

S witz rlan

Tha ila nd

Turkey

U.S.S.R

Yu o lav ia

Internatio al Sta nda rd

8 Interna tiona l Orga niza tion fo r S ta nda rdiza tion, 196 0

Printed in S witzerla nd

C ry ol te, natural and a rtific ia l - Determination of si ic a

minatio of th si c a c onte t of na tura l a nd a rtific ial

c ry olte a nd of na tura l a nd sy nth tic materials havin a

molar ra tio (Na / AI F a) betwe n 3 a nd 1.7 a prox imately

0,0 % (m/ m)

1.1 Spec ial cas (u d r stu y )

IS0 1619, C ryolte, na tura l a nd arific i - Prep ratio a nd

stora ge of tet sample

3 PR IN IPL

s dium c a rbo a te a nd boric ac id Disolutio of th fu e

s lutio is betwe n 0,7 a nd 0,9 a f ter diutio to 5 0 ml or

betwe n 0.3 a nd 0,5 a f ter diutio to 2 0 ml

Formatio , in a s ita le a liq ot, of th (y elow) ox idiz d

moly bd si cate u d r c learly d fin d c on itio s of ac idity ,

c onc enta tio of reag nts, temperature a nd time

s lph ric me ium a nd in th pre e c e of ta rta ric ac id

c mple a t a wavele gth of a bo t 815 nm

analytic al gra de a nd o ly re istie water

4.1 So ium c a rbo ate, an ydro s

4.2 Boric ac id (H,BO ,)

4.3 Nitic ac id, a prox imately 8 N s lutio

Diute 540 ml of nitic ac id, p a prox imately I40 g/ ml

a bo t 6 % (m/ m) slutio , with water to 1 0 0 ml

mately)

In a polyteta flu ro thyle e (PT FE) beak r, disolv e 19,5 g

water a nd, a f ter c ooln , diute to 10 ml

Tra nsfer th s lutio to a botle mad of si c a- e material

a nd, if n c es ary, fiter bef ore u e

4.5 Tararic ac id.10 g s lutio

4.6 Sulph ric ac id, a prox imately 16 N s lutio

C arefuly a dd 45 ml of s lph ric ac id, p a pro imately

I84 g/ ml a bo t 9 % (m/m) s lutio , to a bo t 5 0 ml of

water C ool diute to 1 0 0 ml an mix

4.7 R ed c in slutio

1,5 g s lutio

hy drox y-I-na htha le e s lph nic ac id (C,oH,NO,S)

b ) Disolv e 9 g of an y dro s s dium metais lphite

(Na,S2 5) in 9 0 ml of water

a nd mix F ilter if n c sary

Store in a c ool plac e in a n amberc olo re botle mad of

4.7.2 A sc rbic ac id, 2 g slutio

Prepre this s lutio ju t bef ore ue

4.8 S ilc a , standard s lutio c re po din to 0,5 0 g of

SiO , per lte

Into a pla tin m cru ible of s ita b le capacity, weig , to th

n are t 0,0 1 g, eith r

-

(H,SiO,), ig ite at 1 0 0 “C to c n ta nt mas, ie u ti

0,0 1 g, or

-

ig ite at 1 0 0 ‘C for 1 h a nd c ole in a d sica tor

Add to th cru ible 5 g of th s dium carbo a te (4 1) Mix

th ro g ly , prefera b ly with a pla tin m sp atula, a nd fu e

carefuly A dd h t w er to th c ru ible, h at g ntly to

C ool diute to a b out 5 0 ml tansfer q antitativ ely to a

1 0 0 ml o e-mark v olumetic flask, diute to th mark a nd

mix Tra nsfer im e iately to a b otle mad of si c a -fe

m eria l

1 ml of this sta nda rd s lutio c nta in 0,5 0 mg of SiO,

SiOz p er ltr e

Tra nsfer 40.0 ml of th sta nda rd si ca slutio (4.8) to a

1 0 0 ml o e-mark v olumetic flask, diute to th mark a nd

mix

1 ml of this sta nda rd s lutio c ntain 0,0 0 mg of SiO z

Prepa re this s lutio ju t b efore u e

4.10 S ilc a , standard s lutio c re po din to 0,0 5 g of

SiO , p er lte

Tra nsfer 5 ,O ml of th standard si ca s lutio (4.9) to a

2 0 ml o e-ma rk v olumetic flask, diute to th mark a nd

mix

1 ml of this sta nda rd s lutio c ntain 0,0 5 mg of Si0

Prep re this s lutio ju t b efore u e

Ordinary lab oratory a p pa ra tu a nd

with a pla tin m ld

at 5 0 i 2 “C

at 7 0 f 2 “C

5.5 Sp ctro h tometer

NOT - Gla sswa re sa ll b c arefuly was ed with hot cromic-

slph ric a c id, ta kin a ll nec esa ry prec a ution, thorou hly rined

with wa ter an finally with redistied wa ter I sould not b dried

Av oid the u e of gla ss v esels for a lka line solution

sample, drie at 1 0 “C (s e 3.3 of IS0 1619)

ca rbo a te (4.1) a nd 4 g of th boric a cid (4.2), a nd mix

carefuly , p referably with a platin m sp atula

NOT - Avoid c onta ct of the platin m v esel with r efrac tor y

m eria ls T isola te it from the flor of the furna c e, u e, for

example, platin m spp orts

75 f 2 “C , ta kin ca re to is late it, as b efore, fom th

flo r of th furnace It mu t n t stay at this tempera ture

a nd a llow to c ol in air

dis olutio

Afer c oln slg tly , tansfer th c nte ts of th dis to a

PT E bea ker of sitab le ca p a city, c ontainin 2 ml of th

with 18 ml of th nitic a cid slutio a nd th n with h t

b oi n p oint

q antitatively to a 10 ml o e-mark v olumetic flask Afer

c oln , diute to th mark a nd mix

P

Tra nsfer 2 ml of th ba se s lutio (6.2.1) to a bea ker of

s ita b le ca p a city A dd to th bea ker 15 ml of w er, 15 ml

v a lu with th pH meter (5.4)

This v a lu s o ld le betwe n 0,8 an 0,9 If it d e n t,

a dditio , th re uire q antity of th nitic ac id s lutio

(4.3) D ilute, if n c s ary , s tha t th fina l v olume of th

s lutio , a f ter th a dditio of th nitic ac id slutio , is

0,9 1

Note th v olume of th nitic ac id s lutio a dd d to c orec t

a n optic al pa th le gth of 1 cm

Into eac h of a s rie of six 10 ml o e-mark volumetic

flass, plac e 2 ml of th b s s lutio (6.2.1) a nd th n a dd

th v olume of th nitic ac id s lutio (4.3) u e to adju t

th pH in th prelminary te t (6.2.2)

Stan ard si c a

solution (4.10)

SiO,

ml

mq

5,O

0,05

* C ompnation solution

6.2.4 C olo r d velopme t

T o eac h flas, a dd 5 ml of th s dium moly bdate s lutio

2 “C The a dd 5 ml of th tara ric ac id s lutio (4.5),

to th mark a nd mix a ga in

Afer 10 min b ut n t lo g r tha n 40 min, c ary o t th

spec troph tometer (5.5) a t a wavele gth of a b out 815 nm,

a ga in t th c ompe satio s lutio

NOT - C albrate a c c ura tely the c els u ed for the mesrements

6.2.6 Plotin th c a libra tio gra ph

Plot a gra ph havin , f or ex ample, as a s is ae, th valu s,

in mi grams, of SiOp p er 10 ml of stan a rd c alorimetic

s lutio , a nd, as ordina te , th c ore po din valu s of th

a srb nc es

6.3 Determinatio

6.3.1 Prepa ra tio of th te t slutio

carbo ate (4.1) a nd 4 g of th boric ac id (4.2), an mix

q antity c arefuly , prefera ly with a platin m sptula

C over th dis with its ld a nd plac e it in th elec tric

f urna c e by mean of a s p or fom whic h th re is n ris

of into uc in impuritie

is maintain d for a t least 2 min

R emov e th dis fom th furna c e a nd alow to c ool in a ir

disolutio o c urs

Afer c ooln slg tly , ta nsfer th c onte ts of th dis to

conta inin 2 ml of th nitic ac id s lutio (4.3)

t o th wals of th dis , with 18 ml of th nitic ac id

s olutio a nd c arefuly was th dis a nd ld in h t water,

f re material

6.3.2 C olo re rea c tio

(6.3.1.2) a nd plac e o e in a beakr of s itale c apc ity a nd

th oth r in a 10 ml o e-mark volumetic flas

spec ifie in 6.2.2 a nd disc ard this s lutio

6.3.2.3 C LO R DEVEO MENT

colo re reac tio as spec ifie in 6.2.4

t o th proc ed re spec ifie in 6.2.5, a f ter havin a dju te

th in tume t to z ro a srba nc e again t water

6.3.3 Bla k test

spec ifie in 6.2.1, but diute to a f inal v olume of 2 0 ml

Develop th c olo r as spec ifie in 6.3.2.3

in 6.3.2.4

By refere c e to th c a libra tio gra ph (s e 6.2.5), d termin

of th te t s lutio a nd of th blan te t s lutio

mas , is giv n by th formula

(mo

wh re

minatio ;

s lutio

a ) th refere c e of th meth d u e ;

minatio ;

d) an opera tio s n t inc lu e in this Interna tio a l

refere c e is mad , or re a rd d as optio al

A NEX

IS0 1619 - Prepa ra tio a nd storag of te t sample

IS0 16 0 - D eterminatio of si ca c onte t - R ed c ed moly bd si cate spec troph tometic meth d

IS0 427 - Evaluatio of f re flu rid s c onte t - C onventio a l titimetic meth d

IS0 - Sampln