I n tern ati on al St an d ard f@ 1 776

14!4
0 !
I N TE RN ATI ON AL ORG AN I ZATI ON FOR S TAN D ARD I Z ATI ON * M E R , Wi AP OAH AR OPrAH l 43 At W4 ~ OCTAH ~ AP TM 3 AU M b l * ORG AN l S ATl ON I N TE RN ATI ON ALE DE N ORM ALl S ATl ON

G l ass - Resi st an ce to at t ack by h yd roch l ori c aci d

at 1 00 OC - Fl ame emi ssi on or f l ame at omi c absorpt i on

spect romet ri c met h od

Verre - R&st an ce B I ’ attaqu e par I ’ aci d e ch l orh yd ri q u e 2 1 00 OC - M &h o d e de d &t ermi n at i on par spect romet ri e d ’ absorpt i on

at omi q u e de f l am me ou d ’ &mi ss i o n de f l am me

Fi rst ed i t i on - 1 985- 1 0- 1 5

U DC 666. 1 : 62 0 . 1 9 3 . 41 : 543 . 42 Ref. N o. I S0 1 776 - 1 9 8 5 ( E)

Descri pt ors : g l ass, tests, boi l i n g t emperat u re tests, aci d resi st an ce tests, h yd roch l ori c aci d , spect roph ot omet ri c an al ysi s.

Pri ce base d on 5 pag es

Foreword

I S0 ( th e I nternati onal Org an i zati on for Stan dardi zati on ) is a worl d wi de federati on of

nati on al st an dards bod i es ( I S0 m e m be r bodi es) . Th e work of prepari n g I nternati onal

St an dard s is n ormal l y carri ed ou t th rou g h I S0 tech ni cal commi t t ees . E ach m e m be r

bod y i n terested in a su bj ect for wh i ch a tech n i cal comm i t t ee h as been establ i sh ed h as

th e ri g ht to be represen ted on that commi t t ee. I nternati onal org an i zati ons, g overn -

men t al an d n on - g overn men tal , in l i ai son wi th I SO, al so take part in th e work.

Draft I nternati on al St an d ard s adopt ed by th e techn i cal comm i t t ees are ci rcu l ated to

th e m e m be r bod i es for approval before thei r accept an ce as I n ternati onal St an dard s by

th e I S0 Cou n ci l . Th ey are approved in accord an ce wi th I S0 procedu res requ i ri ng at

l east 75 % approval by the m e m ber bod i es voti ng .

I ntern ati onal St an d ard I S0 1 776 was prepared. by Tech n i cal Comm i t t ee I SO/TC 46,

Laboratory g l ass ware an d rel ated apparatu s.

It can cel s an d repl aces I S0 Recom m en d at i on R 1 776- 1 970, of wh i ch it con sti tu tes a

tech n i cal revi si on .

U s ers sh ou l d n ote that al l I nternati onal St an d ards u n d erg o revi si on from t i me to t i me

an d that an y referen ce m ad e h erei n to an y other I nternati onal St an d ard i mpl i es i ts

l atest edi ti on, u n l ess oth erwi se stated.

0 I n t ern at i on al Org an i z at i on for St an d ard i z at i on , 1 985 0

Pri n t ed in Swi t z erl an d

I N TERN ATI ON AL S TAN D ARD I S0 1 776- 1 985 ( E)

G l ass - Resi st an ce to at t ack by h yd roch l ori c aci d

at 1 00 OC - Fl ame emi ssi on or f l ame at omi c absorpt i on

spect romet ri c met h od

1 Sco pe I S0 6351 2, Laborat ory g l assware - Grad u at ed pi pettes -

Part 2: Pi pet tes for wh i ch no wai t i n g t i me is speci fi ed.

Th i s I n tern ati onal St an d ard speci fi es f l ame emi s si o n spec-

trometri c ( FE S) an d fl ame at omi c absorpti on spect romet ri c I S0 1 042, Laboratory g l assware - On e - mark vol u met ri c fl asks.

( FAAS) met h od s for d et ermi n i n g th e amou n t s of al kal i met al

I S0 1 773, Laborat ory g l assware - Boi l i n g fl asks I n arrow-

oxi d es rel eased f rom th e su rfaces of g l assware wh en su bj ect ed

n ecked ) .
to att ack by an aq u eou s sol u ti on of h yd roch l ori c aci d at

1 00 OC. Th e amou n t of al kal i met al oxi d es d et ermi n ed is a

I S0 3565, Gl as s pl ant, pi pel i n e an d fi tti ng s - Properti es of

meas u re of th e aci d resi st an ce of th e g l ass.

borosi l i ca te g l ass 3. 3.

I S0 3696, Wat er for l aborat ory u se - Speci fi cat i on s. I)

2 Fi el d of appl i cati on

I S0 361 9, Laboratory g l assware - Beakers. ‘ )

Th i s I n tern ati on al St an d ard appl i es to pi eces of g l ass, prefer-

abl y fl at bu t, if n ecessary, cu rved , cu t f rom arti cl es of l aboratory

I S0 6955, An al yt i cal spect roscopi c met h od s - Fl ame emi ssi on ,

g l assware, f rom compon en t s of g l ass pl an t, pi pel i n e or fi tti n g s

at omi c absorpti on , an d at omi c fl u orescen ce - Vocabu l ary.

or f rom an y oth er art i cl es u sed for pu rposes wh i ch m ay be

d escri bed as “ ch emi cal ”.

4 Pri n ci pl e

Th e aci d resi st an ce of g l ass “ as del i vered”, i . e. th e aci d resi s-

tan ce of th e ori g i n al fi re- pol i sh ed su rfaces, m ay be d et ermi n ed Th e met h od is a test for g l ass “as d el i vered ” or for g l ass “ as a

wh en the su rface area of th e cu t an d smoot h ed ed g es d oes n ot mat eri al ’ . ‘ .

exceed 1 0 % of th e total su rface area of the sampl e.

At t acki n g of s ampl e pi eces of 30 to 40 cm2 by an aq u eou s

Th e aci d resi st an ce of th e g l ass “ as a mat eri al ” m ay be deter- h yd roch l ori c aci d sol u ti on , c( H CI ) = 6 mol /l , at 1 00 OC for 3 h.

mi n ed wh en th e ori g i n al su rface h as been removed by th e

h yd rofl u ori c aci d treat men t d escri bed in 7. 3. Th i s prel i mi n ary Det ermi n at i on of the amou n t of al kal i met al oxi d es extracted

aci d t reatmen t sh al l be appl i ed to al l s ampl es of borosi l i cat e per uni t area by f l ame emi s si on or f l ame at omi c absorpt i on

g l ass 3. 3 taken f rom compon en t s of g l ass pl ant, pi pel i n e or spect romet ri c met h od s.

fi tti ng s.

Th e di sti n cti on bet ween th e aci d resi stan ce of g l ass “as 5 Reag en t s

d el i vered ” an d “as a mat eri al ” m ay be of i mport an ce in case s

Du ri n g th e an al ysi s, u n l ess ot h erwi se stated, u se on l y reag en ts

wh ere arti cl es h ave been g i ven a su rface treatmen t du ri n g or

of recog n i zed an al yti cal g rad e.

after produ cti on .

5. 1 Grad e 2 water, compl yi n g wi th th e req u i remen t s of

I S0 3696.
3 Referen ces

I S0 71 9, Gl as s - Hyd rol yt i c resi st an ce of g l ass g rai n s at 5. 2 H yd roch l ori c aci d , sol u ti on , c( H CI ) = 6 ? 0, 2 mol /l ,

96 T - Met h od of test an d cl assi fi cati on . prepared by add i n g 1 vo l u me of con cen trat ed h yd roch l ori c aci d

sol u ti on (e = 1 ,1 8 g /ml ) to 1 vol u me of g rad e 2 wat er ( 5. 1 ) .

I S0 720, Gl as s - Hyd rol yt i c resi st an ce of g l ass g rai n s at Th e al kal i ( N a20 an d K20) con ten ts of th i s sol u ti on sh al l be l ess

1 21 OC - Met h od of test an d cl assi fi cati on . th an 0, 2 pg /ml per oxi de.

1 ) At presen t at the st ag e of draft.

1
I S0 1 77 6 - 1 9 8 5 ( El

Hyd ro ch l o ri c aci d of an al yti cal g rad e q u al i ty m o st l y m e e ts th i s N OTE - Th e lid m ay be fi tted wi th an open i n g of up to 5 mm in

req u i remen t. Th i s sh al l be en su red for e very n ew bottl e of d i amete r so th at a th ermocou pl e can be i n serted so th at th e

temperatu re can be measu red an d con trol l ed at 1 00 f 1 OC i n si d e th e

h yd ro ch l o ri c aci d d el i vered .

d i sh , e. g . an i ron - copper/n i ckel ( Fe - Cu Ni ) th ermocou pl e.

If th e al kal i me tal con ten ts are h i g h er, th e h yd roch l ori c aci d

sol u ti on sh al l be pu ri fi ed , for exampl e , by u si n g th e proced u re

6. 6 Ton g s, ti pped wi th a su i tabl e ch e m i cal l y resi stan t

d escri be d in th e an n ex.

materi al , e. g . pl ati n u m or resi stan t pl asti cs. Th e ti ps sh ou l d be

pretreated wi th th e h yd ro ch l o ri c aci d sol u ti on ( 5. 3) an d sh ou l d

5. 3 H yd ro ch l o ri c aci d , sol u ti on , c( H CI ) = 2 mo l /l , prepared be wash ed in g rad e 2 water ( 5. 1 ) i mm e d i ate l y before u se.

by ad d i n g 1 vo l u me of con cen trated h yd roch l ori c aci d sol u ti on

IQ = I,1 8 g /ml ) to 5 vo l u m e s of g rad e 2 water ( 5. 1 ) .

6. 7 Beaker, m ad e of pl asti cs, h avi n g a capaci ty’ of 250 ml ,

fi tted wi th a rack ( see fi g u re I), mad e of pl ati n u m wi re, to h ol d

5. 4 Hyd ro ch l o ri c aci d , sol u ti on , c( HCI ) = 1 mo l /l .

th e sampl e s d u ri n g th e prel i mi n ary aci d treatmen t.

5. 5 Hyd ro fl u o ri c aci d , sol u ti on , HF = 40 % ( m /m ) .

6. 8 Be ake rs, h avi n g a capaci ty of 50 ml , co mpl yi n g wi th th e

req u i remen ts of I S0 381 9 an d mad e of borosi l i cate g l ass 3. 3

5. 6 I on i zati on bu ffer, for preci se al kal i me tal d etermi n ati on , co mpl yi n g wi th th e req u i remen ts of I S0 3585.

espe ci al l y wh en g l asse s wi th h i g h er l i me con ten ts are extracted .

Th e al kal i ( Nap0 an d K, O) con ten ts of th e i on i zati on bu ffer

E ach new beaker or co n tami n ated beaker sh al l be pretreated in

wh en me asu red in a sol u ti on of 1 0 % ( V/V) i on i zati on bu ffer in

th e fol l owi n g man n er: Th e beaker sh al l be i m m e rse d in

g rad e 2 water ( 5. 1 ) sh al l be l e ss th an 0, 5 pg /ml per oxi d e.

h yd roch l ori c aci d ( 5. 3) an d boi l ed for 2 h. Th e beaker sh al l th en

be ri n sed wi th water, i m m e rse d in water an d h eated , as above,

N OTE - Th e i on i zati on bu ffer can be prepared by d i ssol vi n g 250 g of

for two peri od s of 1 h, u si n g fresh water each ti me.

al u m i n i u m n i trate n on ah yd rate fAI ( N Os) s. 9 H2 0 1 an d 50 g of cae si u m

ch l ori d e ( C&I ) in g rad e 2 water ( 5. 1 ) , an d d i l u ti n g to 1 l i tre. Co m m e r-

ci al l y avai l abl e sol u ti on s, su ch as “ Sch u h kn e ch t- 9 ch i n ke LBu ffe r”,

6. 9 Boi l i n g fl asks ( e. g . con i cal or vo l u me tri c fl asks) , h avi n g
m ay al so be u sed .
a capaci ty of 50 ml , co mpl yi n g wi th th e req u i reme n ts of

I S0 1 773 an d mad e of pol ypropyl en e or vi treou s si l i ca. Th e

5. 7 Eth an ol ( C, H , OH ) or aceton e ( CH s COCH s) . n e ck of th e pol ypropyl en e fl asks sh al l be sh orten ed to a l en g th

su ffi ci en t to h ol d th e fl asks in th e h eati n g bath ( 6. 1 0) . A th i n

l ayer of al u mi n i u m sh al l be wrapped rou n d th e n e ck of vi treo u s

si l i ca fl asks for i n su l ati n g pu rposes.

6 Apparatu s

N O TE - Pol ypro pyl en e wi th stan d s temperatu res z 1 30 OC.

Ord i n ary l aboratory apparatu s, an d

6. 1 0 Heati n g bath , for e xampl e oi l , capabl e of mai n tai n i n g a

6. 1 Dryi n g oven , capabl e of mai n tai n i n g a temperatu re of
temperatu re of 1 25 f 5 OC.
l oo f 1 T.

N OTE - For fl asks of vi treou s si l i ca, a san d bath m ay al so be u sed .

6. 2 Dryi n g oven , su i tabl e for operati on at a temperatu re up

to 1 30 T.

6. 1 1 Mag n eti c sti rrer, wi th a pl asti cs- co ated rotor.

6. 3 Fl ame e m i ssi o n or fl ame ato mi c absorpti on spe c-

trometer.

6. 4 Li n ear measu ri n g i n stru me n ts, su i tabl e for me asu ri n g

l en g th s an d d i amete rs to an accu racy of 0, 2 mm.

6. 5 Di sh e s, mad e of high d en si ty presse d pol ytetrafl u or-

eth yl en e ( PTFE) of e xtre me l y l ow porosi ty, h avi n g a capaci ty of

abou t 70 ml ( overfl ow capaci ty) , a wal l th i ckn e ss of abou t

5 mm, an i n n er d i ameter of abou t 60 mm an d an i n n er h ei g h t of

abou t 25 mm. Th e d i sh sh ou l d be cl o sed wi th a screw- th read ed

l i d.

Th e d i sh sh ou l d be eq u i pped wi th a su i tabl e rack, m ad e of

pol ytetrafl u oreth yl en e ( PTFE) , or wi th fou r pe aks, mad e of

PTFE , abou t 3 mm hi gh an d fi xed on th e bottom to keep th e Fi g u re 1 - Be ake r wi th rack to h ol d sam pl e s d u ri n g

sam pl e s at th i s d i stan ce fro m th e bottom. th e pre l i mi n ary aci d treatmen t

2
 I S0 1 776- 1 985 ( El

6. 1 2 On e - mar k vol u met ri c fl asks, h avi n g a capaci t y of 8 Proced u re

5 ml , compl yi n g wi th th e req u i remen t s speci fi ed for cl ass A

on e- mark vol u met ri c fl asks in I S. 0 1 042, mad e of g l ass of

8. 1 N u mb e r of d et ermi n at i on s
h yd rol yt i c resi stan ce g rai n cl ass HGA 1 as speci fi ed in

I S0 720”.
Test th ree s ampl e pi eces an d th ree bl an k sol u t i on s as speci fi ed

in 8. 2.

6. 1 3 G r ad u at e d pi pet t e for part i al d el i very, h avi n g a

capaci t y of 2 ml an d compl yi n g wi th th e req u i remen t s for

8. 2 Aci d l each i n g an d bl an k t est s
type 1 pi pettes of cl ass A in I S0 835/2.

Heat the d ryi n g oven ( 6. 2) to 1 1 5 OC an d th e oth er d ryi n g oven

( 6. 1 ) to 1 00 f 1 OC. Pu t each s ampl e pi ece ( prepared in

accord an ce wi th cl au se 7) by me an s of th e t on g s ( 6. 6) i nto a

7 Preparati on of s ampl e pi eces

separat e d i sh ( 6. 51 , cl ose th e th ree d i sh es l oosel y wi t h th e l i ds

an d pu t t h em i n to th e hot d ryi n g oven ( 6. 2) overn i g h t. In th e

s am e way, h eat th ree mo re d i sh es for bl an k tests omi tt i n g th e

7. 1 Con d i t i o n of s ampl e pi eces for preparat i o n

sampl e pi eces, an d an oth er on e for t emperat u re con trol .

Th e s ampl e pi eces sh al l h ave a total su rface of 30 to 40 cm* ,

an d sh al l be taken f rom th e g l assware wh i ch h as been d el i vered N ext d ay h eat seven porti on s of exact l y 25 ml of th e h yd ro-

wel l an n eal ed. Re m o ve f rom th e ed g es an y sh arp an g l es, ch l ori c aci d sol u ti on ( 5. 2) in th e beakers ( 6. 8) u n ti l boi l i n g . Th en

“ h ackl es” or spl i n t ers by a mi n i mu m of g ri n di n g . Do n ot fi re- tran sfer th e h ot d i sh for th e t emperat u re con trol ( wi th ou t a

pol i sh the ed g es. sampl e pi ece) to a f u me cu pboard an d pou r in th e boi l i n g

h yd roch l ori c aci d sol u ti on . Cover an d cl ose th e di sh , i n sert th e

th ermocou pl e, an d repl ace the d i sh in th e oth er d ryi n g oven

7. 2 M eas u r e me n t of l i n ear d i men s i o n s ( 6. 1 ) at 1 00 ‘ Y. Repeat th e fi l l i ng proced u re wi th the th ree

oth er d i sh es wi th ou t s ampl e pi eces ( for the bl an k tests) , an d

Measu re al l d i men s i on s to the n earest 0, 2 mm an d cal cu l at e the fi n al l y wi th th e th ree d i sh es con tai n i n g th e s ampl e pi eces ( i . e.

actu al total su rface area. the extracti on sol u ti on s) . Cou n t th e peri od of 3 h f rom the t i me

wh en the fi rst d i sh con tai n i n g a sampl e pi ece was pl aced back

in th e d ryi n g oven .

7. 3 For t est i n g g l as s “as a mat eri al ” an d g l ass

for g l ass pl an t , pi pel i n e an d fi tti n g s ( prel i mi n ary

N OTE - Th e peri od before a d i sh is pl aced back in the d ryi n g oven

aci d t reat men t ) sh al l n ot exce ed 2 mi n . Prot ect , as wel l as possi bl e, the d i sh es in the

d ryi n g oven f ro m col d ai r en t eri n g t h rou g h the d ryi n g oven d oor.

Pl ace the s ampl e pi eces of an y t h i ckn ess in the rack ( 6. 7) fi tted

i n si d e the beaker ( 6. 71 , as sh own in fi g u re 1 . I n sert the rotor of Measu re the temperatu re in on e d i sh an d correct th e t empera-

th e sti rrer ( 6. 1 I) an d th en ad d, carefu l l y, d own the wal l of th e tu re of the d ryi n g oven ( 6. 1 1 , if n ecessary, to mai n t ai n th e t em-

beaker, a mi xt u re con tai n i n g 1 part of the h yd rofl u ori c aci d peratu re at 1 00 * 1 OC.

sol u ti on ( 5. 5) an d 9 parts of th e h yd roch l ori c aci d sol u ti on ( 5. 3)

u nti l th e sampl e pi eces are compl et el y i mme rs ed . Th e t empera-

After 3 h re move th e d i sh es from th e dryi n g oven an d d ecan t

tu re of th e mi xt u re sh ou l d be abou t ambi en t temperat u re. St i r

th e extract i on sol u t i on s an d th e bl an k test sol u ti on s i n to

th e mi xt u re mag n et i cal l y for 1 0 mi n . H ol d i n g the s ampl e pi eces

separate boi l i n g fl asks ( 6. 91 , except th e d i sh for th e t empera-

in posi ti on wi th a pl ast i cs rod, pou r ou t th e mi xt u re. Fi l l th e

tu re con trol . Di p, as d eep as possi bl e, the fl asks i nto the

beaker wi th g rad e 2 water ( 5. 1 ) an d ag ai n d ecan t th e l i qu i d.

h eati n g bath ( 6. 1 0) at 1 20 to 1 30 OC. Re m o ve th e s ampl e pi ece

Re m o ve each s ampl e pi ece, u si n g th e t on g s ( 6. 61 , an d was h

from a d i sh u si n g th e ton g s. Was h t h orou g h l y wi t h a few j ets of

th orou g h l y in g rad e 2 water. Fi n al l y ri n se th e s ampl e pi eces

g rade 2 water ( 5. 1 ) . Accord i n g to th e evaporat i on of the

wi th the eth an ol ( 5. 7) or the aceton e ( 5. 7) an d d ry th em for

sol u ti on s in th e fl asks, ad d th e wash i n g s an d compl et e th e

30 mi n in th e d ryi n g oven ( 6. 2) at abou t 1 1 5 OC.

cl ean i n g of th e d i sh es wi th mo re j ets of the water.

Du ri n g st ori n g of th e wash i n g s, th e d i sh es sh al l be covered .

7. 4 Fo r t est i n g g l ass “ as d el i vered ”
Wh e n the l i qu i d s h ave al most compl et el y evaporated, ad d fou r

d rops of th e h yd rofl u ori c aci d sol u ti on ( 5. 5) an d con ti n u e th e

Th e t h i ckn ess of th e s ampl e pi eces sh al l n ot exceed =2 mm for
evaporat i on u nti l d ryn ess ( total t i me abou t 3 h) .
a total su rface of 30 to 40 cm* . Th at me an s that th e n ew cu t

su rface area is n ot mo re th an abou t IO % of th e total su rface

N OTE S
area.

1 If a vi t reou s si l i ca fl ask h as be e n u sed , th e ad d i t i on of h yd rofl u ori c

Was h th e sampl e pi eces th orou g h l y wi th g rade 2 wat er ( 5. I),

aci d sol u t i on sh al l be omi t t ed .

th en ri n se wi t h th e eth an ol ( 5. 7) or th e acet on e ( 5. 7) . Dry th e

s ampl e pi eces in the d ryi n g oven ( 6. 2) for 30 mi n at abou t

2 If d ryn ess is n ot reach ed after 3 h ( d rops of sol u t i on remai n i n g ) , pu t

1 1 5 T. th e fl ask i nto a d ryi n g o ve n at 1 25 OC for 30 mi n .

1 ) Gl ass of h ydrol yt i c resi stan ce g rai n cl ass I S0 71 9. H GB 1 ad e q u at el y mee t s the req u i remen t s of cl ass HGA 1 speci fi ed in I S0 720 .
I S0 1 776- 1 985 ( E)

On ce d ryn ess is ach i eved , al l ow to cool an d ad d to each fl ask, 9 Expressi on of resu l ts

by me an s of th e g rad u ated pi pette ( 6. 1 3) , 0, 2 ml of th e h yd ro-

Cal cu l at e the me an of the val u es obtai n ed. If th e h i g h est an d

ch l ori c aci d sol u t i on ( 5. 3) an d 2 ml of g rade 2 water ( 5. 1 ) .

th e l owest observed val u es di ffer by mo re th an th e permi ssi bl e

Di ssol ve th e resi d u e by swi rl i n g th e sol u ti on .

ran g e g i ven in th e tabl e, repeat th e test.

Tran sfer each sol u t i on i n to a separat e on e- mark vol u met ri c

fl ask ( 6. 1 21 , add, by me an s of th e g rad u ated pi pette, 0, 5 ml of Tabl e - Permi s si bl e ran g e of the val u es obtai n ed

th e i on i zat i on bu ffer ( 5. 61 , ri n se each boi l i n g fl ask ( 6. 9) wi t h

abou t I,5 ml of water, ad d it to th e on e- mark vol u met ri c fl ask, Permi s si bl e ran g e

Me an of th e val u es obtai n ed

of th e
di l u te to th e m ar k wi th water an d mi x th orou g h l y.
I pg of N a20 per 1 00 cm*
I val u es obt ai n ed I

Up to an d i n cl u d i n g 30 30 % of th e m e an

Fro m 30 up to an d i n cl u d i n g 70 20 % of th e m e an
8. 3 Det ermi n at i on of th e al kal i met al oxi d e
Fro m 70 u pward s 1 5 % of th e m e an
con t en t s

Prepare st an d ard sol u ti on s by d i ssol vi n g d ri ed ch l ori d es of

Su bt ract th e me an val u e of th e al kal i met al oxi des, obtai n ed

sod i u m an d pot assi u m, an d cal i brati on sol u t i on s of appropri ate

f rom th e bl an k test sol u ti on s, f rom th e me an val u e, obtai n ed

con cen t rati on s by ad d i n g 0, 2 ml of the h yd roch l ori c aci d

f rom th e extract i on sol u ti on s. Cal cu l at e th e amou n t of th e al kal i

sol u ti on ( 5. 3) an d 0, 5 ml of th e i on i zat i on bu ffer ( 5. 6) for each

met al oxi d es extracted per 1 00 cm2 of at tacked su rface. If the

5 ml of th e fi nal vol u me.

pot assi u m oxi d e rel ease is l ower th an 5 u g /l OO cm2 , it sh al l be

di sreg arded .

Est abl i sh an d carefu l l y stan d ard i ze i n st ru men t t ech n i q u es so as

to u ti l i ze m ax i m u m sen si ti vi ty, as sodi u m oxi d e con cen t rati on s

Expre ss th e resu l t ei th er as the m as s of sodi u m oxi d e ( N a20) or,

of abou t 0, l mg /l m ay h ave to be measu red .

if req u i red, as th e m as s of th e separat e al kal i met al oxi d e

extracted, per 1 00 cm2 of at tacked su rface.

Th e spect romet ers sh al l be operated in accord an ce wi t h th e

man u fact u rers’ i n stru cti on s, so that measu reme n t can be m ad e

in th e opt i mal worki n g ran g e speci fi ed.

1 0 Test report

Det ermi n e th e al kal i met al oxi d e con ten t s of th e extracti on Th e test report sh al l i n cl u d e th e fol l owi n g i n formati on :

sol u t i on s an d of th e bl an k sol u t i on s ( 8. 2) u si n g th e fl ame

emi s si on or fl ame at omi c absorpti on spect romet er ( 6. 3) . a) a referen ce to th i s I ntern ati on al Stan dard ;

Cal cu l ate th e m e an val u e for th e th ree ext racti on sol u ti on s, an d

b) an i den ti fi cati on of the s ampl e pi eces;
al so for th e th ree bl an k test sol u ti on s (i n mi cro g rams per

mi l l i l i tre) . a stat emen t as to wh eth er th e test was appl i ed to g l ass

cl

“as d el i vered ” or to g l ass “as a materi al ” after etch i n g th e

If th e si n g l e val u es of th e bl an k test sol u ti on s di ffer by mo re su rface ;

th an 0, 2 pg /ml f rom th ei r m e an val u e, or if the absol u t e con -

d) the t h i ckn ess of th e g l ass tested, in mi l l i met res, to th e

tent of N ap is h i g h er th an 5 ug, con t ami n at i on h as occu rred ;

n earest 0, l mm;
wh i l e the su bseq u en t meas u reme n t s an d cal cu l at i on s m ay be

carri ed ou t, th e val u es th u s obtai n ed are for i n formati on on l y.

e) th e su rface tested, in sq u are cen t i metres, to th e n earest

Th e test ( 8. 2) sh al l be repeated . For th i s pu rpose

0, l cm2 ;

f) the ori g i n al con cen trati on of sodi u m oxi d e measu red in

a) wh en testi n g g l ass “ as a mat eri al ”, th e prel i mi n ary aci d

t reat men t ( 7. 3) sh al l be appl i ed beforeh an d; th e extracti on sol u ti on s, expressed as mi cro g rams of N a20

per mi l l i l i tre, to th e n earest 0, Ol u g /ml ;

b) wh en testi n g g l ass “as d el i vered ”, s ampl e pi eces wi th

g) the cal cu l at ed rel ease, expressed as mi cro g rams of
th e ori g i n al su rfaces ( 7. 4) sh al l be tested.
N a20 per sq u are d eci met re, to th e n earest 0, l u g /d m2,

me an val u e;

If the bl an k val u es are su ffi ci en t, th e fi n al resu l ts sh al l be

cal cu l ated . h) an y u n u su al featu res n oted du ri n g the d et ermi n at i on .

 I S0 1 776 - 1 9 8 5 ( El

An n e x

Exampl e of a proced u re for pu ri fyi n g h yd roch l o ri c aci d sol u ti on

( Th i s an n ex d o es n ot fo rm an i n teg ral part of th e stan d ard . )

U se th e asse m bl y sh o wn in fi g u re 2, fi tti n g an an ti - spl ash d e vi ce to th e boi l i n g fl ask an d en su ri n g th at th e pl asti cs tu bi n g d oes n ot

en ter th e water in th e co l l ecti n g fl ask. Th e fl asks sh al l be of hi ghl y resi stan t borosi l i cate g l ass an d sh al l be “ ag ed ”, for i n stan ce by

boi l i n g fi rst for 3 h wi th h yd roch l ori c aci d sol u ti on , c( H CI ) = 1 m ol /l ( 5. 41 , u n der refl u x, th en for 2 h wi th d i sti l l ed water.

Ad d con cen trated h yd roch l ori c aci d (Q = I,1 8 g /ml ) to th e boi l i n g fl ask, ad d water to th e col l ecti n g fl ask, con n ect up th e asse m bl y

an d h eat to boi l i n g . Al l o w on l y th e h yd roch l ori c aci d vapou r to pass over i n to th e water. As so on as l i qui d beg i n s to d i sti l , repl ace th e

aci d wi th a fresh su ppl y an d con ti n u e th e d i sti l l ati on u n ti l th e aci d con cen trati on in th e col l ecti n g fl ask e xce e d s 6 mo l /l . Ad j u st to a

con cen trati on of 6 I ! Z 0, 2 mo l /l .

, - Pl asti cs tu bi n g

An ti - spl ash d evi ce

3- - - -

H yd ro ch l o ri c aci d

(9 = I,1 8 g /ml )

Fi g u re 2 - Preparati on of h yd roch l ori c aci d sol u ti on , c( H CI ) = 6 mol /l , wi th ve ry l ow

so d i u m oxi d e con ten t