[ SO

I N TE RN ATI ON AL S TAN D ARD 7884- 5

Fi rst ed i ti on

1 9 8 7- 1 2 - 1 5

I N TE RN ATI ON AL ORG AN I ZATI ON FOR STAN D ARD I ZATI ON

ORG AN I SATI ON I N TE RN ATI ON ALE DE N ORM ALI SATI ON

M E XAYH AP OAH AR OP TAH M 3 Al &l R n0 CTAH ~ APTM 3 Al . Wl kl

, ‘ 1 , . . ( ?,. c.p-, : I ,. ’ :/

i &$; , ~ , , , ! { ; y: . 1 , 1 , ~ ~ , : ?. : ~ l i ~ . 9. : : - : : , ~ . : ei ~;;~ ‘ - $; ; y; ,

Gl ass - Vi scosi ty an d vi scometri c fi xed poi n ts -

Part 5 :

Determi n ati on of worki n g poi n t by si n ki n g bar vi scometer

Re f ere n ce n u m be r

I S0 7884- 5 : 1 987 ( E)
Foreword

I S0 ( the 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 ) is a wor l d wi d e f ed erat i on of

n at i on al s t an d ar d s bo d i es ( I S0 m e m be r bod i es ) . Th e wor k of prepar i n g I n t ern at i on al

S t an d ar d s is n ormal l y carri ed ou t t h rou g h I S0 t ech n i cal commi t t ees . E ach m em ber

bo d y i n t eres t ed in a s u bj ect for wh i ch a t ech n i cal commi t t ee h as been es t abl i s h ed h as

th e ri g h t to be r epr es en t ed on t h at commi t t ee. I n t ern at i on al org an i z at i on s , g over n -

men t al an d n o n - g o ver n men t al , in l i ai son wi t h I SO, al s o t ake part in the work.

Draf t I n t ern at i on al S t an d ar d s ad o pt e d by the t ech n i cal commi t t ees ar e ci rcu l at ed to

the m em ber bod i es f or approval bef o r e th ei r accept an ce as I n t ern at i on al S t an d ar d s by

the I S0 Cou n ci l . Th ey ar e appr o ved in acco r d an ce wi t h I S0 pr o ced u r es req u i ri n g at

l east 75 % appr oval by th e m e m be r bod i es vot i n g .

I n t ern at i on al St an d ar d I S0 78 8 4- 5 was pr epar ed by Tech n i cal Comm i t t ee I SO/TC 48,

Laboratory g l as sware an d rel ated apparat u s.

U s ers s h ou l d n ote t h at al l I n t ern at i on al St an d ar d s u n d erg o revi si on f rom ti me to t i me

an d t h at an y r ef er en ce m ad e h er ei n to an y ot h er I n t ern at i on al S t an d ar d i mpl i es i ts

l at est edi t i on , u n l es s ot h er wi s e s t at ed .

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 , 1 997 0

Pri n t ed i n Swi t z erl an d

I N TERN ATI ON AL S TAN D ARD I S0 7 8 8 4- 5 : 1 9 8 7 ( El

G l ass - Vi sco si ty an d vi sco me tri c fi xed po i n ts -

Part 5 :

Determi n ati on of wo rki n g poi n t by si n ki n g bar vi sco me ter

0 I n trod u cti on 3 Re fe re n ce

i n tern ati o n al Stan d ard I S0 7 8 8 4, G l ass - Vi sco si ty an d I EC Pu bl i cati o n 58 4- 1 , Th e rmo co u pl e s - Part 7 : Re fe re n ce

vi sco me tri c fi xe d po i n ts, co n si sts of th e fo l l o wi n g se parate tabl es.

parts :

4 Defi n i ti on s
Part 1 : Pri n ci pl es fo r d e termi n i n g vi sco si ty an d vi sco me tri c

fi xe d po i n ts.
Fo r th e pu rp o se s of th i s part of I S0 7 8 8 4, th e fo l l o wi n g d efi n i -

Part 2 : Dete rmi n ati o n of vi sco si ty by ro tati o n vi sco me te rs. ti o n s appl y.

Part 3 : Dete rmi n ati o n of vi sco si ty by fi bre e l o n g ati o n

4. 1 wo rki n g po i n t : Te mpe rat u re at wh i ch th e mel t of u su al
vi sco me ter.
si l i cate g l asse s p o ss e ss e s an eq u i l i bri u m vi sco si ty of

1 0 4 d Pa. s* .
Part 4 : De te rmi n ati o n of vi sco si ty by b e am be n d i n g .

Part 5 : Dete rmi n ati o n of wo rki n g po i n t by si n ki n g bar

4. 2 si n ki n g bar te mpe rat u re : Wo rki n g po i n t as d ete r-
vi sco me te r.
mi n ed by m e an s of th e si n ki n g bar me t h o d .

Part 6 : Dete rmi n ati o n of so fte n i n g po i n t.

4. 3 si n ki n g bar meth od : Si mpl e pro ce d u r e fo r d ete rmi n i n g

Part 7 : De termi n ati o n of an n eal i n g po i n t an d strai n po i n t by
rapi d l y th e vi sco si ty wi th i n a ran g e of abo u t 1 0 3 , 7 to I O%5 d Pa. s
b e am be n d i n g .
as expl ai n ed in cl au se 5.

Part 8 : De te rmi n ati o n of l d i l atometri cl tran sfo rmati o n

te mpe ratu re.

5 Pri n ci pl e

A verti cal l y po si ti o n e d n ar ro w me tal ro d ( th e bar) of d i amete r d

1 Sco pe
i s al l o we d to si n k u n d er a fo rce F ( i ts o wn we i g h t) i n to th e mel t.

Fro m th e rate of si n ki n g of th e bar i n to th e mel t, th e d yn ami c

Th i s part of I S0 7884 spe ci fi es a me t h o d of d e termi n i n g th e

vi sco si ty q of th e mel t i s cal cu l ated . Un d er th e g eo metri cal co n -

wo rki n g po i n t of g l ass by m e an s of th e si n ki n g bar vi sco me ter.
d i ti on s speci fi ed in 6. 1 an d 6. 3, th e d e vi ati o n s of th i s me t h o d
Th i s meth od h as been fo u n d u se fu l for ch aracte ri zi n g th e l o w-

fro m e q u ati o n (1 ) are smal l co mpar e d wi th th e e xperi me n tal

vi sco si ty ran g e of g l ass wo rki n g . Th i s vi sco me tri c fi xed po i n t

u n certai n ti es as spe ci fi ed in 9. 2.
can be u se d in d etermi n i n g th e vi sco si ty- temperatu re rel ati o n -

sh i p ( se e I S0 788 4- l 1 .
t
q = C. rn . 1 2 . . . (I )

2 Fi el d of appl i cati on
wh e r e

Th i s meth od is appl i cabl e to al l g l asse s of n o rmal bu l k-

C i s a co n stan t;
pro d u cti o n co mpo si t i o n s u n l e ss d evi tri fi cati o n or e vapo rati o n

of vol ati l e co mp o n e n t s t ake s pl ace d u ri n g th e pre parati o n or

2 is th e d e pt h of si n ki n g i n to th e mel t;

te sti n g of th e spe ci me n .

m i s th e m ass of th e bar;

Th e wo rki n g po i n ts ran g e b e t we e n 800 an d 1 200 OC, d e p e n -

di ng on th e type of g l ass. t i s th e si n ki n g ti me co rre spo n d i n g to 1 .

* 1 d Pa. s = 1 s = 1 P

( P i s th e sym bo l for poi se)

1
I S0 78 8 4- 5 : 1 9 67 ( E)

If f i xed val u es of th e d ept h I an d the mas s m ar e speci fi ed , a Th e wi res sh al l h ave a su ffi ci en t l en g t h wi t h i n the f u r n ace ( wi t h

co n s t an t K for the bar may be d ef i n ed acco rd i n g to r espect to h eat co n d u ct i o n al o n g th e wi res) . Pl at i n u m- met al -

eq u at i o n ( 2) : s h e at h e d t h er mo co u pl e s sh o u l d be pref erred .

rj =K. t . . . ( 2)
6. 4. 2 Con t rol t h er mo co u pl es sh ou l d be l o cat ed as cl ose as

possi bl e to the f u r n ace wi n d i n g s for fast r espo n s e. Th e

In th i s part of I S0 788 4, the d e pt h of si n ki n g an d the mas s of

me as u r e me n t t h er mo co u pl e i s pl aced n e ar t h e wal l of th e cru ci -

th e bar ar e speci f i ed as I = 20 mm an d m = 0, 902 g. res pec-

bl e, d i ppi n g abo u t 1 mm i nto the mel t ( see f i g u re I). In accor -

ti vel y.
d an ce wi t h I S0 7884- l the me as u r e me n t t h e r mo co u pl e sh al l be

cal i brat ed an d the cal i brat i on ch e cke d reg u l arl y.

N OTE - Th e bu oyan cy act i n g u pon th e i mme r s e d part of th e bar is

taken i n to accou n t for the d en si t y of the referen ce g l ass u sed for

cal i brat i on ( see 6. 1 ) . Th e bu oyan cy correct i on for oth er val u es of g l ass 6. 4. 3 Th e el ect ri cal ou t pu t of the t h e r mo co u pl e s sh al l be

den si t y is n eg l ect ed . d et er mi n ed at zer o cu rren t by me an s of pot en t i o met ers or hi gh-

resi st an ce el ect ron i c ampl i fi ers h avi n g a sen si t i vi t y of 1 0 pV or

bet t er. Pr ecau t i o n s sh al l b e t aken t h at the i ce- bat h for the co l d

6 Apparat u s j u n ct i on is mai n t ai n ed at 0 OC th rou g h ou t the t est . If the

t emper at u r e me as u r i n g eq u i pme n t i s fi t ted wi t h au t o mat i c co l d

j u n ct i on co mpe n s at i o n , the i ce- bat h may be omi t t ed .

6. 1 Si n ki n g bar

Bar mad e f rom pl at i n u m- r h o d i u m al l oy wi t h a mas s fract i on of 6. 5 Ti mer

rh odi u m be t we e n 0, 2 an d 0, 3, wi t h d i amet er 0, 5 mm an d mas s

0, 902 g ( co r res po n d i n g to a l en g t h b e t we e n 240 an d 245 mm Th e si n ki n g t i me sh al l be me as u r e d by me an s of a s t o pwat ch

d e pe n d i n g u pon the d en si t y of the pl at i n u m- rh o d i u m al l oy h avi n g scal e i n t erval s of 0, l s, or by an eq u i val en t t i mer.

u sed ) . Th e en d s of the bar sh al l be h emi sph eri cal .

6. 6 Ot h er e q u i pmen t
N OTE - Wi t h su ch a bar, for a vi scosi t y of 1 04 d Pa. s th e t i me for

si n ki n g to a depth of 20 mm i s 60 s. Th i s correspon d s to a bar con stan t

Th e f ol l owi n g e q u i pme n t is n ecessary.
K of abou t 1 40 to 1 70 d Pa. s/s.

a) Cl amp for h an d l i n g an d h ol d i n g the bar.

Fo r rou t i n e me as u r e me n t s it is co n ven i en t to h ave avai l abl e

sever al bar s ma d e f rom the s ame bat ch of the al l oy. Used bar s
b) Amme t e r for i n d i cat i n g the posi t i on wh e n the bar ti p
sh al l be g en t l y cl ean e d of ad h e r en t g l ass resi d u es by su dd en
t o u ch e s the su rf ace of th e mel t .
h eat i n g an d ch i l l i n g , or by d i ssol vi n g the g l ass in h yd rof l u ori c

aci d . Af t erward s t h ey sh al l be st rai g h t en ed bef o r e re- u se.

c) Mi rror scal e for paral l ax- f ree r ead i n g for me as u r i n g the

d e pt h of si n ki n g of the bar; a g r o o ve sh o u l d be g rou n d in

6. 2 Fu r n ace
th e mi rror scal e for g en t l y gu i di ng th e u ppe r en d of the bar

wi t h mi n i mu m fri cti on .

El ect ri cal l y h e at e d t u be f u rn ace capabl e of ach i evi n g

t empe r at u r e s up to 1 200 ‘ X. Th e l en g t h of the h e at e d t u be

In pl ace of the d evi ces l i st ed u n d er b) an d c) o t h er su i t abl e

sh al l be abo u t 200 mm, an d i ts i n n er d i amet er at l east 30 mm.

d evi ces may be u s ed .

Wi t h i n a zon e of 40 mm in l en g t h in wh i ch the cru ci bl e is

pl aced , the t emper at u r e sh al l be co n st an t wi t h i n 3 ‘ X.

Fu rt h er d evi ces may be u sef u l for th e ad j u st men t of the z er o

posi t i on , e. g . cat h et omet er, ad j u st abl e cl ampi n g d evi ce to

ach i eve cen t ral an d vert i cal posi t i on i n g of the bar ( ad mi t t abl e
6. 3 Cru ci bl e

max i mu m ti l t, 5O) , et c.

Th e i n n er d i amet er of th e cru ci bl e at the su rf ace of th e mel t

sh al l be at l east 23 mm. I ts d ept h sh al l be 30 to 40 mm.

6. 7 As s e mbl y of appar at u s
Cru ci bl es mad e f rom pl at i n u m or pl at i n u m al l oys ar e pref erred .

Fo r si n g l e u se, cru ci bl es ma d e from n o n - po r o u s refract ory may

Fi g u r e 1 s h o ws an e xampl e of the t est ass e mbl y. It is co n ve -
al so be u se d .
n i en t if the cru ci bl e i s set on a f i xed s t an d wh e r e as the f u r n ace

can be mo ve d d o wn war d s ; thi s faci l i tat es the fi l l i ng of the

6. 4 Te mpe r at u r e meas u r i n g an d i n d i cat i n g cru ci bl e an d r e mo val of the t est s peci me n . Th e me as u r e me n t

i n st ru men t s t h er mo co u pl e ( posi t i on ed acco r d i n g to 6. 4. 2) or the pl at i n u m

al l oy cru ci bl e s er ve at t h e s ame t i me as an el ect rod e for the am-

6. 4. 1 Th e al u mi n a- i n su l at ed pl at i n u m- 1 0 % r h od i u m/pl at i n u m met er ; th e o t h er el ect ro d e i s the bar wh i l st it i s f ast en ed in the

t h e r mo co u pl es ( t ype S acco rd i n g to I EC 584- l ) sh al l exh i bi t l ow cl amp. Dr au g h t wi t h i n the f u r n ace t u be sh o u l d be d i mi n i sh ed

t h ermal i n ert i a ( the d i amet er of th e wi res sh o u l d n ot b e g r eat er by cl osi n g th e ori fi ce in the bo t t o m of the f u r n ace ( e. g . by

t h an 05 mm) . me an s of ce r ami c wo ol ) .

2
 I S0 78 84- 5 : 1 987 ( El

7 Preparat i on of test speci men s

Th e sampl e of th e g l ass to be t est ed sh al l con si st of pi eces

l arg er t h an 3 mm. I f the pi eces do n ot fi t i nto the cru ci bl e, t h ey

sh al l be cr u sh ed carefu l l y, avoi d i n g an y co n t ami n at i o n ( s ee

I S0 79 94- l : 1 9 87, s u b- cl au se 7. 1 ) .

If a pl at i n u m cru ci bl e is u s ed , th e t est s p e ci me n ( abo u t 20 to

30 cm? of the h o mo g e n e o u s g l ass s ampl e is mel t e d in t h at

cru ci bl e. If a ref ract ory cru ci bl e is u s ed , it is mo r e co n ven i en t ,

b e cau s e of possi bl e corrosi on , to mel t the t est s pe ci me n in

an o t h er f u rn ace an d to cast it i nto a mo u l d h avi n g a form

si mi l ar to t h at of the me as u r e me n t cru ci bl e.

En s u r e t h at no ai r bu bbl es ar e i n cl u d ed in the mo l t en sampl e.

H o we ve r , avoi d mel t i n g d u ri n g too l on g peri od s, especi al l y in

the cas e of a g l ass wh i ch d evi t ri fi es easi l y.

N OTE - I f th e worki n g poi n t l i es above 1 1 50 ‘ C, a si mpl e preparat i on

fu rn ace for t emperat u res h i g h er th an 1 200 OC i s con ven i en t. In th i s

fu rn ace th e g l ass can be mel t ed su ffi ci en tl y fast to prod u ce a bu bbl e-

free sampl e, before it i s i n t rodu ced i n to th e t esti n g fu rn ace.

8 Proced u re

8. 1 Cal i brat i on
1 Mi rror scal e wi t h g roove ( see al so fi g u re 2)

2 Amme t e r wi t h ci rcu i t
Cal i brat e th e t est as s e mbl y by me an s of a ref eren ce g l assl ) , car-
3 Me asu r e me n t t h ermocou pl e

ryi n g ou t th e t est pr o ced u r e d escr i bed in 8. 2 at t h at

4 Cover

Fu rn ace pl aten mad e of ce r ami cs

t e mper at u r e wh i ch co r r e s po n d s to the vi scosi t y 1 0 4 d Pa. s of
5

6 Fu rn ace tu be mad e of ce rami cs the r ef er en ce g l ass. Th e co mpo si t i o n s of the r ef er en ce g l ass

7 Bar an d of the g l ass u n d er t est sh ou l d be si mi l ar.

8 Cru ci bl e con t ai n i n g g l ass me l t u n der test

9 Fu rn ace pl aten mad e of ce r ami cs

Cal cu l at e the bar co n s t an t K from th e me as u r e d si n ki n g t i me t,

1 0 Ce r ami c wool ( drau g h t protecti on )

by me an s of eq u at i o n ( 3) :
1 1 Cru ci bl e stan d ( e. g . mad e of ce rami cs )

1 2 Heat er

1 3 I n su l ati on K = l o”
. . . ( 3)
1 4 Con t rol t h ermocou pl e
t c

wh e r e

Fi g u re 1 - Sch e mat i c e xampl e of th e si n ki n g

bar vi scomet er
K i s e xpr e s s e d in d eci pas cal s e co n d s pe r s eco n d ;

t, i s e xpr e s s e d in se co n d s .

Re pe at th e cal i brat i on reg u l arl y an d af t er an y ch an g e i n the ap-

parat u s.

Th e co n s t an t K d e t e r mi n e d as abo ve i s u sed i n eq u at i o n ( 2) for

the d et ermi n at i on of th e vi scosi t y of o t h er g l asses.

8. 2 Me as u r e me n t

H e at the s pe ci me n in the f u r n ace to t h at t emper at u r e wh i ch is

e xpect e d to co r r e s po n d to a vi scosi t y of 1 0 4 d Pa. s.

N OTE - In th e case of sod a- l i me g l ass, thi s t emperat u re is abou t

Fi g u re 2 - Mi rror scal e wi t h g roove 1 000 oc.

“ Examp l e s of certi fi ed referen ce g l asses for vi sco me t ri c cal i brat i on ”.

1 ) Se e for e xampl e I S0 7884- l : 1 987, an n ex B,

’
I S0 7884- 5 : 1 997 ( E)

Be f o re be g i n n i n g th e t est, the t e mpe rat u re of the f u rn ace sh al l 9. 2 Preci si on

be co n s t an t f or ab o u t 1 0 mi n . Th e n h ol d th e b ar fo r ab o u t

1 mi n in th e cl amp j u st ab o ve the mel t s u rf ace. Th e repeat abi l i t y ( on e o bs e r ve r u si n g th e s am e appar at u s ) is

3 OC . Th e reprod u ci bi l i t y ( d i fferen t o bs e rve rs an d d i fferen t ap -

Ke e p i n g th e b ar as verti cal as po s si bl e an d in the axi s of th e parat u s ) is 8 “ C.

cru ci bl e, l o we r it sl owl y in ord er to fi n d the po i n t of co n t act

wi t h th e s u rf ace by m e an s of th e am me t e r i n d i cati on . I n doi n g

so , th e u pper en d of the bar i s g u i d ed in th e g r o o ve of th e mi r-

ro r s cal e. Take th e po i n t of co n t act as t h e z e ro po i n t of th e u p- IO Test report

pe r e n d of th e b ar o n th e mi rro r s cal e to d e t e rmi n e th e d epth of

si n ki n g 1 . Th e t est repo rt sh al l i n cl u d e :

At the s am e t i me, re l eas e t h e bar f ro m th e cl amp an d st art th e a) re f e re n ce to th i s part of I S0 7884;

ti mer. St o p th e t i mer wh e n th e u pper en d of th e bar h as su n k

20 mm bel ow th e zero po i n t on th e mi rror scal e. b) d escri pt i o n of th e s ampl e;

c) meth od of s ampl i n g ;

9 Expressi on of resu l ts

d) n u mber of t est s pe ci me n s ;

9. 1 Det ermi n at i on of th e si n ki n g bar t emperat u re

e) meth od of preparat i o n ;

Th e vi scosi t y is cal cu l at ed f ro m th e m e as u r e d si n ki n g t i me by
f) t ype of si n ki n g b ar app ar at u s u sed ;
m e an s of e q u at i o n ( 2) . On l y o ccas i o n al l y wi l l th e vi scosi t y be

1 0 4 d Pa. s . Th e ref o re , aft er th e b ar h as b e e n r e m o ve d , a s e co n d

g) cal i brat i o n t e mpe rat u re;
ru n in acco r d an ce wi t h 8. 2 an d u si n g a new b ar sh al l b e carri e d

ou t at a t e mpe r at u re wh i ch is es t i mat e d to be more ap -

h) si n ki n g bar t e mpe rat u re , in d eg rees Cel si u s;
pro pri at e. Th i s pr o ce s s sh al l be r e p e at e d u n ti l th e t e mpe rat u r e

co rre s po n d i n g to 1 0 4 d P a. s can be fou n d by l i n ear i n t erpo l at i on

i) an y ch an g e in th e g l ass, o b s e r ve d d u ri n g an d /o r aft er
wi t h re s pe ct to t e mpe rat u re an d th e l o g ari t h m of vi scosi ty; th e
the test.
i n t erval of i n t erpol at i o n sh al l n ot e x ce e d 30 OC wi t h i n th e r an g e

of si n ki n g t i mes b e t we e n 40 an d 90 s.

4
 I S0 78 8 45 : 1 9 8 7 ( E)

An n e x

Bi bl i og raph y

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

DI ETZE L, A. an d BRU CKN E R, R. Ei n Fi xpu n kt d er Zah i g kei t im Ve rarbe i tu n g sbe rei ch d er G i ber; Sch n e l l be sti mmu n g d es Vi sko si tats-

Tempe ratu r- Verl au fs [A vi sco me tri c fi xed po i n t in th e wo rki n g r an g e of g l ass; rapi d d etermi n ati o n of vi sco si ty/temperatu re rel ati on -

sh i p] . Gl astech n . Beri ch te. 1 957 ( Vol . 301 , pp. 73 - 79 .

M E RKE R, L. Vi sko si tat und Obe t - fl ach e n span n u n g der Emai l s im Ei n bre n n bere i ch , i h re e i n fach e M e s su n g und i h re Be d e u t u n g fu r d as

G l attfl i eBen [Vi sco si ty an d su rface te n si o n of vi tre o u s e n ame l s in th e fi ri n g ran g e , th ei r si mpl e m e asu re me n t an d th ei r i mpo rtan ce fo r

th e su r face smo o t h i n g pro ce ss] . Mi tt. Vere i n De u tsch er Emai l fach l e u te . 1 962 ( Vo l . I O) , pp. 5 7- 6 2 .

5
I S0 78 8 4 - 5 : 1 9 8 7 ( E)

U DC 66 6. 1 1 . 0 1 : 532. 1 3

De scri pto rs : g l ass, tests, d etermi n ati on , th e rmo d yn ami c properti es.

Pri ce based on 5 pag es