I S0

I N TE RN ATI ON AL S TAN D AR D X3 84- 2

Fi rst ed i t i 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 XJ J YH AP OAH AR OP TAH M 3 AL/M R I - I O CTAH ~ AP TM 3 Al &l M

&, j ‘ : f y, : . ‘ -. ’ . -
‘” !
: . ” ‘ : . ‘ L.ti c: ; ! i ’ y( . ; , g : +i t ~ - J &j ~~~~~

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

Part 2 :

Determi n ati on of vi scosi ty by rotati on vi scometers

Re f e re n ce n u mbe r

I S0 7884- 2 : 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 ) i s a worl d wi d e f ed er at i on of

n at i on al s t an d ar d s bod i es ( I S0 m em ber bod i es ) . Th e wo r k of pr epar i n g I n t ern at i on al

St an d ar d s is n ormal l y carri ed ou t th rou g h I S0 t ech n i cal commi t t ees . E ac h m e m be r

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 be e n es t abl i s h ed h as

the 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 o ver n -

men t al an d n on - g over n m en t al , in l i ai son wi t h I SO, al s o t ake par t in the wor k.

Draft I n t ern at i on al St 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 be r bod i es for appr oval bef or e t h ei r accept an ce as I n t ern at i on al St an d ar d s by

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

l eas t 75 % approval by the m em ber bod i es vot i n g .

I n t ern at i on al S t an d ar d I S0 788 4- 2 was pr e par e d by Tech n i cal Com mi t t ee I SO/TC 48,

Laboratory g l as sware an d rel ated apparatu s.

U s er s sh ou l d n ot e 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 t i me to ti me

an d t h at an y ref eren ce m ad e h erei n to an y o t h er I n t ern at i on al S t an d ar d i mpl i es i ts

l atest edi t i on , u n l es s ot h erwi 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 , 1 987 0

Pri n t ed in Swi t zerl an d

I N TERN ATI ON AL S TAN D ARD I S0 7884- 2 : 1 987 ( E)

G l ass - Vi scosi t y an d vi scomet ri c fi xed poi n t s -

Part 2 :

Det ermi n at i on of vi scosi t y by rotati on vi scomet ers

0 I n trod u cti on t u re r an g e f rom abo u t 1 600 to 600 “ C, the t o rq u e n eces s ary

ran g i n g f ro m 0, l to 20 N . mm acco rd i n g to th e con s t ru ct i on of

I n t ern at i on al St an d ard I S0 788 4, Gl as s - Vi scosi t y an d th e apparat u s . Th e me t h o d is appl i cabl e if th e rot at i on al fre-

vi scomet ri c fi xed poi n ts, con si st s of the fol l owi n g s eparat e q u e n cy d oes n ot e xce e d 8 s - 1 ; h o we ve r, at rot at i on al f req u en -

part s : ci es abo ve 1 s- t it sh ou l d b e ascert ai n ed t h at i n ert i a f orces are

n eg l i g i bl e.

Part I: Pri n ci pl es for d et ermi n i n g vi scosi t y an d vi scomet ri c

fi xed poi n ts.

2 Referen ce

Part 2: Det ermi n ati on of vi scosi t y by rotati on vi scomet ers.

I EC Pu bl i cat i on 58 4- 1 , Th ermocou pl es - Part 1 : Referen ce

Part 3: Det ermi n at i on of vi scosi t y by fi bre el on g ati on tabl es.

vi scomet er.

Part 4: Det ermi n at i on of vi scosi t y by be am ben di n g .

3 Defi n i ti on s

Fo r the pu r po s e s of th i s part of I S0 788 4, th e f ol l owi n g defi n i -

Part 5: Det ermi n at i on of worki n g poi n t by si n ki n g bar

ti on s appl y.
vi scomet er.

3. 1 Fi el d of fl ow, cru ci bl e an d pl u n g er
Part 6: Determi n at i on of soften i n g poi n t.

Part 7: Determi n at i on of an n eal i n g poi nt an d strai n poi nt by 3. 1 . 1 fi el d of fl ow: Th e wh o l e g ap fi l l ed by th e mol t en g l as s

be am ben d i n g . s ampl e an d the spat i al d i st ri bu t i on of the f l ow vel oci t i es wi t h i n

i t, i n cl u d i n g i ts bou n d ari es .

Part 8: Det ermi n at i on of ( d i l at ometri cl t ran sformat i on

temperatu re. 3. 1 2 cru ci bl e : Th e o u t er bo u n d ary of th e mo l t en g l as s s am-

pl e co rres po n d i n g to th e i n n er s u rf ace of the cru ci bl e up to the

l evel of the mel t.

1 Scope an d fi el d of appl i cati on

3. 1 . 3 pl u n g er : Th e i n n er bo u n d ar y of the mol t en g l as s s am-

Th i s part of I S0 7884 speci fi es a me t h o d of d et ermi n i n g , by pl e co rres po n d i n g to th e o u t er s u rf ace of the pl u n g er up to the

m e an s of rot at i on vi s comet ers, the d yn ami c vi scosi t y of g l as s l evel of the mel t.

an d , in part i cu l ar, the vi scosi t y- t emperat u re rel at i on sh i p at an y

t emperat u re o r vi scosi ty wi t h i n th e r an g e of meas u re me n t . Th i s 3. 2 Fl o w fi el d coeffi ci en t an d i n s t ru men t con s t an t

co vers the r an g e s of vi scosi ty for mel t i n g , refi n i n g an d wo rki n g

of g l ass. 3. 2. 1 Ro t at i o n vi s comet ers are ei t h er of the Searl e t ype or of

the Cou et t e t ype, bo t h of wh i ch al l ow the d et ermi n at i on of th e

Th i s me t h o d al l ows for co n t i n u o u s me as u r e me n t s an d for

vi scosi ty acco rd i n g to basi c eq u at i on (I 1 :

me as u r e me n t s u n d er vari ou s s h eari n g st res ses ( i . e. for the

d et ermi n at i o n of fl ow cu rves ) in o rd er to ch eck wh e t h er or n ot

rl =fT
the g l ass be h ave s as a N e wt o n i an l i q u i d. . . . (I )
n

Depen d en t on the part i cu l ar vi scosi t y- t emperat u re rel at i on sh i p

wh e r e

of the g l ass t est ed , the vi scosi ty r an g e co vere d by th i s me t h o d

ext en d s approxi mat el y f rom 1 0 to I O* d Pas * in the t empe ra- q i s th e vi scosi t y;

dN. s
*
1 d P as = 1 ~ = 1 P

m2

( P i s t h e s ymbol for poi s e)

1
I S0 78 8 4- 2 : 1 987 ( El

f i s th e fl o w fi el d co effi ci en t; 3. 2. 3 I n m an y case s th e ro tati o n al fre q u e n cy n an d th e to rq u e

Tare n ot re ad o r re co rd e d d i rectl y. Fo r th e sake of co n ve n i e n ce

T i s th e to rq u e appl i ed to th e pl u n g e r; al l th e facto rs n eed ed fo r th ei r cal cu l ati o n an d th e fl o w fi el d

co effi ci en t can be co m bi n e d i n to a speci al i n stru me n t co n s-

n i s th e ro tati o n al fre q u e n cy ei th er of th e pl u n g er ( Se arl e tan t k* . Th i s co n stan t sh al l b e d e te rmi n e d by cal i brati o n u si n g

type ) or of th e cru ci bl e ( Co u e tt e type ) . vi sco me tri c stan d ard l i qu i ds wi th N e wt o n i an be h avi o u r. 1 )

Th e fl ow fi el d co effi ci en t f is a fu n cti o n on l y of th e
3. 2. 4 Th e fl o w fi el d co effi ci e n tf an d th e i n stru men t co n st an t s
g e o me tri cal sh ap e of th e fi el d of fl o w an d h as th e d i me n si o n of
k an d k” are , fo r N e wt o n i an l i q u i d s, i n d e pe n d e n t of th e ro ta-
reci pro cal cu bi c l en g th .
ti on al fre q u e n cy, of th e t o rq u e an d of th e vi sco si ty. Th e y are

sl i g h tl y d ep e n d e n t on te mperatu re b e cau s e of th e th e rmal e x-

Th e an al yti cal cal cu l ati o n of th e fl o w fi el d co effi ci e n t i s po ssi bl e
pan si o n of th e g l ass mel t, of th e cru ci bl e an d of th e pl u n g e r
i n a restri cte d n u mb e r of g e o me tri e s, e. g . i n th e fo l l o wi n g case s
( se e 7. 3 ) .
( se e al so an n e x A) .

3. 3 To rq u e s
a) Cru ci bl e an d pl u n g er are s h ap e d l i ke i n fi n i te co n ce n tri c

cyl i n d ers; meth od s of el i mi n ati n g expe ri men tal l y th e effe ct

of th e pl an e en d su r face s are kn o wn fro m l i teratu re, bu t 3. 3. 1 d ri vi n g to rq u e : Th e to rq u e appl i ed by th e d ri ve to th e

th ey are d i ffi cu l t to appl y in th e cas e of g l ass mel ts. bo u n d ar y su r face ro tati n g wi th th e ro tati o n al fr e q u e n cy n.

b) Cru ci bl e an d pl u n g e r fo rm t wo co n fo cal ro tati o n su r-

3. 3. 2 fri cti on al to rq u e: To rq u e of th e o ppo si t e si g n to th e

face s of th e se co n d o rd e r, e. g . t wo h al f- el l i pso i d s, cu t
d ri vi n g to rq u e , ari si n g fro m th e vi sco u s fl o w b e t we e n th e t wo

perpe n d i cu l arl y to th e axi s of ro tati o n .

bo u n d ari e s, th e on e ro tati n g an d th e o th e r be i n g at rest.

I f th e sh ap e s of th e cru ci bl e an d of th e pl u n g er are m ad e up by
3. 3. 3 to rq u e qf me ch an i cal l o sse s : Th e fri cti o n al
se ve ral ro tati o n al su rface s, th e bo u n d ari e s of th e perpe n d i cu l ar
resi stan ce cau se d by i n fl u e n ce s o th e r th an th e g l ass mel t ( e. g .
me d i an cu ts bei n g i rreg u l ar cu r ve s ( e. g . cyl i n d e rs wi th pl an e or
fri cti on in beari n g s, ai r fri cti on ; in th e case of ro tati o n al vi bra-
co n e - sh ap e d or h emi - sph eri cal e n d s) , th e fl o w fi el d co effi ci en t
ti o n s, al so th e se l f- d ampi n g of th e to rsi o n spri n g ) .
can be d e termi n e d on l y by m e an s of vi sco me tri c st an d ard

l i qui ds wi th N e wt o n i an beh avi o u r. 1 )

3. 3. 4 In th e case of stati o n ary ro tati o n , wh i ch i s essen ti al for

o btai n i n g co rre ct resu l ts, th e se th re e t o rq u e s ad d up to ze ro

3. 2. 2 I f, fo r th e to rq u e, th e l e n g th an d /o r th e ro tati on al fre- ( acti o n = reacti o n ) . To rq u e s of me ch an i cal l o sse s, cau se d by

q u e n cy, u n i ts are u se d wh i ch do n ot co r re spo n d to th e uni t fo r th e parti cu l ar co n stru cti o n of th e i n stru me n t, sh al l be

th e vi sco si ty, an d if th e resu l ti n g facto r is co m bi n e d wi th th e el i mi n ated t h ro u g h a co rrecti o n .

fl o w fi el d co effi ci en t, a n ew co n st an t, th e i n stru me n t co n -

stan t k, can be d e fi n e d by eq u ati o n ( 2) :

4 Apparatu s ( se e an n e x B)

. . . ( 2)

4. 1 Ro tati o n vi sco me te r

Two t yp e s of ro tati o n vi sco me te r co mpl y wi th th i s part of

I S0 73 3 4:

q i s th e vi sco si ty me asu re d , in d e ci pascal se co n d s;

a) Vi sco me te r of th e Co u e t t e t ype wi th ad j u stabl e,

k is th e i n stru me n t co n stan t ( n u meri cal val u e ) , resu l ti n g re vo l vi n g cru ci bl e. Th e cru ci bl e st an d s on a tu rn tabl e wh i ch

fro m e q u ati o n ( 3) ; i s to be po si ti o n ed i n th e fu rn ace th ro u g h i ts l o we r o pe n i n g ;

th e sh aft of th e pl u n g e r re ach e s t h ro u g h th e u ppe r o pe n i n g

T i s th e to rq u e , in n e wt o n mi l l i metres; of th e fu rn ace up to th e to rq u e - me asu ri n g d e vi ce .

n i s th e rotati o n al fre q u e n cy, in reci pro cal se co n d s. b) Vi sco me te r of th e Se arl e t yp e wi th th e cru ci bl e at

rest an d th e pl u n g er revo l vi n g , th e revo l vi n g m o ve m e n t be -

Th e i n stru me n t co n st an t k i s rel ated to th e fl o w fi el d co effi ci en t i ng i n d u ce d th ro u g h a sh aft re ach i n g ou t of th e u pp e r o pe n -

f by e q u ati o n (31 , if th e fl o w fi el d co e ffi ci en t f i s e xpr e sse d in i ng of th e fu rn ace . Th e to rq u e- me asu ri n g d e vi ce i s appl i ed

reci pro cal cu bi c mi l l i metres ( mm - 3) : to th e sh aft of th e pl u n g er.

. . . Bo th t yp e s can be o pe rate d
k = I O' f ( 3)

a) ei th er at fi xed ro tati o n al fre q u e n ci e s ( e. g . by m e an s of a

N OTE - Th e factor 1 07 i n eq u ati on ( 3) resu l ts fro m th e rel ati on

co mbi n ati o n of syn ch r o n o u s mo to r an d g e ar tran smi ssi o n ,

1 N . s/m m * = 1 07 d Pa. s
th e vari ati o n ran g e of th e rotati o n al fre q u e n cy n be i n g at

1 ) Se e for e xam pl e I S0 7884- l : 1 987, an n ex B, “ Exam pl e s of certi fi ed referen ce g l asse s for vi sco m e tri c cal i brati on ”.

‘,
 I S0 78 8 4- 2 : 1 9 8 7 ( E)

4. 4 Cru ci bl e an d pl u n g er
l east 1 : l OO) wi th a torq u e- measu ri n g d evi ce ( torsi on wi re s,

torsi on spri n g or torsi on bal an ce) wh o se po ssi bl e i n accu r-

acy sh al l n ot excee d 2 % at a torqu e of abou t 5 N- mm;

4. 4. 1 Cru ci bl e s

b) or at fi xed torq u es ( e. g . by m e an s of a wei g h t an d

Acco rd i n g to th ei r ch e mi cal re si stan ce to th e g l ass mel t u n d er

pu l l ey s yst e m or by me an s of an el ectri c moto r) wi th a

test, th e cru ci bl e s sh al l be mad e of ce ram i c materi al ( e. g .

measu ri n g d e vi ce for th e rotati on al freq u en cy ( freq u en cy

al u mi n a) or n obl e metal . If ce rami c cru ci bl e s are u sed ( n o rmal l y

meter, el ectron i c speed mete r wi th opti cal or i n d u cti ve sen -

th ey can be u se d on l y on ce) , it is re co mme n d e d th at su ch a

sor, m i cro sco pe for ve ry l ow rates) .

cru ci bl e be pl aced in a l arg er cru ci bl e m ad e of th i n n obl e sh eet-

me tal , in ord er to protect th e fu rn ace in case th e ce ram i c . cru -

To protect th ese parts of th e apparatu s, speci al scre en i n g
ci bl e breaks. Nobl e me tal cru ci bl e s ( preferabl y pl ati n u m or
ag ai n st h eat or, if n e ce ssary, water- cool i n g is re co mme n d e d .
pl ati n u m- rh o d i u m al l oys) req u i re cl ean i n g , e. g . in a h yd ro-

fl u ori c aci d bath . Th e vo l u me of th e cru ci bl e s ( sam pl e vo l u me )

sh al l n o rmal l y be between 20 an d 250 e m s.

4. 2 Fu rn ace

El e ctri cal l y h eated tu be- sh aped fu rn ace, d esi g n ed for a

4. 4. 2 Pl u n g ers

ve rti cal wo rki n g posi ti on , for temperatu res up to 1 400 OC (i n

spe ci al case s up to ‘I 600 OC) , wi th co ve rs for th e u pper an d th e

Th e pl u n g ers sh al l be mad e of n obl e metal , preferabl y of

l o wer en d s of th e tu be wh i ch sh al l be m ad e of h eat- resi stan t

pl ati n u m- rh od i u m al l o ys. Th e y sh al l be wel d ed to a l on g th i n

ce ram i c materi al . Th e temperatu re in th e fl o w fi el d area or in sh aft, reach i n g ou t of th e fu rn ace to th e torq u e- measu ri n g in-

th e ad j acen t space in th e fu rn ace sh al l be con stan t to + 2 OC

stru men t. Th e sh aft m ay be mad e en ti rel y of n obl e me tal , or

wi th respe ct to ti me , an d th e temperatu re g rad i en t sh al l n ot ex- al tern ati vel y on l y th at part of i t wh i ch pl u n g es i n to th e mel t m ay

ce ed 1 OC/cm .
be of n obl e me tal , th e part above th e mel t bei n g mad e of

ce ram i c materi al .

N OTE - Th i s re q u i re me n t is ach i e ve d by one or mo re of th e fo l l o wi n g

d evi ces: extra h eaters at th e t wo en d s of th e ce rami c tu be; baffl e s

Th e l ower en d of a cyl i n d ri cal pl u n g er sh al l be con e- sh aped ,
m ad e fro m n o bl e me tal s ( e. g . pl ati n u m) ; a su i tabl e cover on th e cru -

n ot pl an e, in ord er to avoi d bu bbl es ad h eri n g to i t; th i s wou l d

ci bl e ; a th i ck- wal l ed cru ci bl e m ad e of n o bl e m e tal . Good th e rmal i n su -

prod u ce scatte r in th e resu l ts. Moreove r, th e pl u n g er sh al l h ave

l ati o n of th e fu rn ace is req u i red in an y case .

no sh arp ed g es, as sh arp ed g es wo u l d be mo re e asi l y attacked

by th e me l t. Th erefore, th e pl u n g ers sh ou l d be sph eres,

cyl i n d e rs wi th h e mi - sph e ri cal en d s, or e l l i psoi d s.

4. 3 Temperatu re measu ri n g an d i n d i cati n g i n stru me n ts

N OTE - Th e co n tri bu ti o n to th e torq u e of fl o w ari si n g from th e sh aft

4. 3. 1 Th e al u mi n a- i n su l ated pl ati n u m- 1 0 % rh od i u m/pl ati n u m
can be restri cted to l e ss th an 1 5 %.

( type S accord i n g to I EC 584- I ) , or ( for e xten si ve u se above

1 200 OC) pl ati n u m- 3 0 % rh od i u m/pl ati n u m- 6 % rh od i u m ( type B

If th e fl o w fi el d coeffi ci en t is to be d etermi n ed by cal cu l ati on ,
accord i n g to I EC 584- l ) th ermo cou pl es sh al l exh i bi t l ow
th e sh ape of th e pl u n g er sh al l be ch o se n accord i n g l y.
th ermal i n erti a ( th e d i ameter of th e wi re s sh ou l d n ot be g reater

th an 0, 5 mm) . Th e wi re s sh al l h ave a su ffi ci en t l en g th wi th i n

By m e an s of a se t of pl u n g ers of d i fferen t si ze s, th e rati o of th e
th e fu rn ace ( wi th respect to h eat con d u cti on al on g th e wi res) .
si ze s bei n g for e xampl e 1 : 2, th e po ssi bl e ran g e of me asu re me n t

can be exten d ed by abou t on e ord er of mag n i tu d e.

4. 3. 2 Con trol th ermo cou pl es sh ou l d be l ocated as n ear as

po ssi bl e to th e fu rn ace wi n d i n g for fast respon se. Th e h ot j u n c-

4. 5 Apparatu s for q u an ti fyi n g th e test sampl e
ti on of th e me asu re me n t th ermocou pl e, h owever, sh al l be

pl aced in th e i mme d i ate vi ci n i ty of th e fl ow fi el d ( th e cru ci bl e) .

On e of th e fol l owi n g meth o d s sh al l be u sed :
In acco rd an ce wi th I S0 7884- 1 , th e me asu re me n t th ermo-

cou pl e sh al l be cal i brated an d th e cal i brati on ch e cke d reg u l arl y.

a) a bal an ce an d d evi ce for d etermi n i n g th e d en si ty of th e

g l ass at ro o m temperatu re ( between 1 8 an d 28 “Cl ; or

N OTE - Fu rth er i mpro ve m e n t in th e accu racy of th e te mperatu re

d e te rmi n ati o n is ach i e ve d by d i ppi n g th e ( el ectri cal l y i sol ated )

m e asu re m e n t th e rmo co u pl e i n to th e mel t an d /or by o bse rvati on of th e b) a d e vi ce for d etermi n i n g th e d i stan ce between th e su r-

temperatu re d i stri bu ti on by m e an s of t wo fu rth er th e rm oco u pl e s face of th e mel t an d th e u pper ed g e of th e cru ci bl e at a

pl ace d abo ve an d be l o w th e cru ci bl e. If th e co n stru cti on of th e vi scom-

temperatu re above th e me l ti n g ran g e of th e sampl e , e. g . at

eter pe rmi ts th e po si ti o n i n g of th e m e asu re me n t th e rm o co u pl e at th e

1 000 OC; or

cen tre of th e pl u n g e r, th e be st assi g n me n t of tempe ratu re to th e sh ear

area, wh i ch is m ai n l y re spo n si bl e for th e m e asu re d vi scosi ty, is ach i ev-

c) a d e vi ce for th e vi su al d etermi n ati on of th e l e ve l of th e
ed ; in th at case oth er spe ci al d e vi ce s ( see n o te to 4. 2) m ay be o mi tte d .

mel t in th e cru ci bl e .

4. 3. 3 Th e el ectri cal ou tpu t of th e th e rmo cou p! e s sh al l be

4. 6 De vi ce s for th e ad j u stmen t of th e fl ow fi el d
d etermi n ed at zero cu rren t by m e an s of poten ti ometers or hi gh-

resi stan ce el ectron i c ampl i fi e rs h avi n g a sen si ti vi ty of 1 pV.

Pre cau ti on s sh al l be taken th at th e i ce- bath for th e co l d j u n c- 4. 6. 1 De vi ce for th e ad j u stmen t of th e posi ti on of th e fu rn ace

ti on is mai n tai n ed at 0 OC th rou g h ou t th e test. If th e an d /or of th e torq u e- meter, if n e ce ssary wi th a faci l i ty for

temperatu re me asu ri n g e q u i pmen t i s fi tted wi th au to mati c co l d swi n g i n g th e fu rn ace or th e vi sco me te r asi d e an d pre ci sel y back

j u n cti on co mpe n sati on , th e i ce- bath can be omi tted . in th e sam e pl an e ag ai n .

3
I S0 7664- 2 : 1 967 ( E)

4. 6. 2 Devi ce for cen t ri n g cru ci bl e an d pl u n g er. Gl as s es wi t h an u n u s u al l y hi gh t e n d en cy to f o am, evapo rat e or

at t ack ch emi cal l y the cru ci bl e an d pl u n g er mat eri al s g i ve ri se t o

speci al req u i remen t s for th e preparat i o n of the s ampl e an d for

4. 6. 3 Devi ce f or ch ecki n g the con cen t ri c ru n n i n g of the
th e mat eri al s wh i ch co me i nto con t act wi t h th e mel t .
pl u n g er or of the cru ci bl e; d evi at i on s sh al l n ot e xce e d l /1 00 of

the pl u n g er d i amet er; s u ch fau l t s n ormal l y ori g i n at e f rom be n d s

in the pl u n g er sh aft .

6 Proced u re

It is r e co mm e n d e d to u se a sel f- cen t ri n g s u s pen s i o n d evi ce,

e. g . a u n i versal j oi nt; i ts ef f ect i ven es s sh al l be ch ecked .

6. 1 Cal i brat i on

Wh e n the posi t i on of the apparat u s i s ch an g e d or the f u rn ace

Th e rot at i on vi s co met er sh al l be cal i brat ed by m e an s of
an d /o r th e meas u ri n g d evi ce are s wu n g asi d e, the ad j u s t men t
vi scomet ri c s t an d ard l i qui ds wi t h N ewt o n i an beh avi ou r, e. g .
of the fl ow fi el d sh al l be mai n t ai n ed .
certi fi ed ref eren ce g l as s es ( s ee I S0 7884- l : 1 9 8 7, an n e x B) ,

u n l es s th e fl ow fi el d coeffi ci en t an d th e i n s t ru men t co n s t an t

4. 6. 4 Devi ce to ch e ck the rel at i ve posi t i on s of cru ci bl e an d can be d et ermi n ed by cal cu l at i on . Wh e n cal i brat i n g wi t h s t an -

pl u n g er in the f u rn ace, e. g . scal e or marks or wi n d o ws in the d ar d l i q u i ds ot h er t h an ref eren ce g l as ses, meas u rabl e h eat i n g

wal l of th e f u rn ace. by fri cti on sh al l be avo i d ed an d the t o rq u e of mech an i cal l oss

sh al l be t aken i nto accou n t .

N OTE - If it i s i . mpossi bl e to avoi d th e u se of wi n d ows, th ey sh ou l d be

of mi n i mu m si ze. Take care to mi n i mi z e d i st u rban ce of th e temperatu re

Th ermo co u pl e s sh al l be cal i brat ed by co mpari s o n wi t h a

h omog en ei t y, e. g . by su i t abl e wi ri n g of th e h eaters.

cal i brat ed s t an d ard an d /o r wi t h t h ermomet ri c f i xed poi n t s.

4. 7 Ot h er eq u i pmen t Every cal i brat i on sh al l be re pe at ed reg u l arl y.

Th e fol l owi n g m ay be n eces s ary :

6. 2 Preparat i o n

-
cru ci bl e pi n cers wi t h pl at i n u m poi n t s;
Th e cru ci bl e con t ai n i n g th e mo l t en g l as s t est s peci me n sh al l be

posi t i o n ed i n the h eat ed f u rn ace of th e vi scomet er. Th e pl u n g er

-
ro d s of cerami c mat eri al , d i amet er be t we e n 3 an d
sh al l be d i ppe d sl owl y i nto the mel t , d o wn to i ts d es i red posi -
1 0 mm, l en g t h abo u t 400 mm;
t i on rel at i ve to the posi t i on of the cru ci bl e, th e vi scosi t y of the

mel t bei n g l ess t h an 1 000 d Pas .

-
t ool s f or cru s h i n g th e g l ass;

N OTE - It i s ad van t ag eou s to rotate sl owl y th e pl u n g er - or the cu p

-
t h ermal i n su l at i n g g l oves ;
i n the case of a Cou ett e- type d evi ce - wh i l e di ppi n g th e pl u n g er sl ow-

ly i n to th e mel t .
-
i n f ra- red prot ect i ve g o g g l es ;

Th en , the co vers sh al l b e fi tted on th e u ppe r an d l o wer ori fi ces

-
mel t i n g f u rn ace.
of th e t u be of the f u rn ace; if n eces s ary, the ext ra h eat ers sh al l

be s wi t ch ed on .

5 Test speci men

6. 3 M e as u r eme n t

5. 1 Th e s ampl e of the g l ass to be t es t ed sh al l con si st of

6. 3. 1 Con t rol th e el ectri cal i n pu t of th e f u rn ace so as t o h eat
pi eces l arg er t h an 3 mm. If th e pi eces do n ot fi t i nto th e cru -
th e s pe ci men to a cert ai n t emperat u re. Swi t ch on the rot at i n g
ci bl e, t h ey sh al l be cru s h e d carefu l l y, avoi d i n g an y con t ami -
s ys t em of the vi scomet er. Ch o o s e the me as u re me n t r an g e for
n at i on ( s ee I S0 7884- l : 1 9 87, s u b- cl au s e 7. 1 ) .
rot at i on al f req u en cy an d t o rq u e so as t o o bt ai n a su i t abl y hi gh

re s po n s e f rom th e i n st ru men t s. Wh e n the t emperat u re of th e

5. 2 Th e q u an t i t y n eeded sh al l b e d et ermi n ed acco rd i n g to the fl ow fi el d an d th e read i n g of the t o rq u e- met er h ave b e co m e

si ze of th e f l ow fi el d, kn o wn f ro m th e cal i brat i on experi men t . con st an t , r e ad an d reco rd the o u t pu t of the t h ermo co u pl e,

rot at i on al f req u en cy an d t o rq u e. If n eces s ary, repeat th e

me as u re me n t wi t h o t h er val u es of rot at i on al f req u e n cy an d

5. 3 Th e g l ass s peci men sh al l be mel t ed ei t h er in the f u rn ace
d ri vi n g t orq u e.
of th e vi scomet er or in a s e parat e mel t i n g f u rn ace; the mel t

sh al l be f ree f rom bu bbl es . N ormal l y the bu bbl e s ri se q u i ckl y

N OTE - I t wi l l be di ffi cu l t to carry ou t th e me as u re me n t s exact l y at th e
en ou g h if th e vi scosi t y is abo u t 1 000 d Pas . Th e mel t i n g
n omi n at ed temperat u res or vi scosi ti es. I t i s su ffi ci en t to me as u re cl ose
t emperat u re sh al l be ch o s e n accord i n g l y. It sh al ! be t aken i nto
to t h ose poi n t s an d to fi nd th e n omi n at ed t emperatu res or vi scosi t i es
acco u n t t h at , wi t h i n creas i n g t emperat u re ( d ecreas i n g vi s-
by appl yi n g equ ati on ( 2) g i ven in I S0 7884- l : 1 987 for i n terpol ati on .

cosi t y) , the s ampl e can ch an g e i ts propert i es t h ro u g h i n co n g ru -

en t evapo rat i o n an d /o r ch an g e s i n wat er con t en t . For t h e t reat -

me n t of mel t s, see al so I S0 7884- l : 1 9 87, s u b- cl au s e 7. 3. 6. 3. 2 Th e me as u r eme n t may al so be carri ed ou t at varyi n g

t emperat u re, as l on g as t h e vi scosi t y can be m e as u re d wi t h i n a

N OTE - For the u su al fl at g l asses a mel t i n g t emperat u re bet ween su ffi ci en t l y sh o rt t i me i n t erval . Th e maxi mu m rat e of ch an g e of

1 209 an d 1 250 OC i s su ffi ci ent. t emperat u re wh i ch m ay be t ol erat ed d e pe n d s on the co n s t ru c-

4
 I S0 7884- 2 : 1 987 ( E)

ti on an d mat eri al s of th e fu rn ace, cru ci bl e an d pl u n g er, on the d epen di n g on the type of apparatu s) equ ati on ( 2) sh al l be

d i men si on s of th e fl ow fi el d, the posi ti on of th e t h ermocou pl e repl aced by equ ati on ( 4) :

an d the absol u t e val u e of the t emperatu re. Th e tol erabl e rate of

ch an g e of t emperat u re sh al l be d et ermi n ed empi ri cal l y by co m - TD - =L

r/=k . . . ( 4)
pari n g t h ese resu l ts wi t h th e resu l ts of th e exact me as u re men t
n

carri ed ou t accord i n g to 6. 3. 1

TL can be d evel oped i n to a seri es wi th i n creasi n g powers of th e

rotati on al freq u en cy n :
6. 4 Ti me s ch ed u l e for me as u r e me n t s

TL = TLo + T, , n + . . . . . .
U n l ess th ere is a speci al ag reemen t, the g l ass sh al l be tested in

i ts d el i very state.
I f th i s seri es can be tru n cated after th e con st an t t erm, TL eq u al s

approxi mat el y T, , wh i ch can be d et ermi n ed s i mpl y by vari a-

Th e t i me n eed ed for th e me as u remen t sh al l be kept sh ort in

ti on of TD. If it is n ecessary to d et ermi n e TL1 , th i s can on l y be

ord er to avoi d, as far as possi bl e, an y al terati on of the ch emi cal

ach i eved by me an s of several - at l east two - vi scomet ri c

an d/or ph ysi cal propert i es of th e g l ass u n d er test.

st an d ard l i q u i ds or by me an s of on e st an d ard l i qu i d an d th e

an al yti cal cal cu l ati on of the fl ow fi el d coeffi ci en t f.

In addi ti on to a possi bl e ch emi cal reacti on between th e g l ass

mel t an d th e mat eri al s of cru ci bl e an d pl u n g er, pri mari l y t wo

7. 3 D e pe n d e n ce of th e i n st ru men t co n s t an t
effects h ave to be t aken i n to accou n t.

on t emperat u re

al Sel ect i ve evaporat i on . If h eated above 1 300 OC for a

If th e g eomet ri cal sh ape of th e fl ow fi el d remai n s con stan t an d

few h ou rs, m an y g l asses of bu l k- prod u cti on composi t i on s

if a l i n ear approach to the i n fl u en ce of th e t h ermal expan si on is

sh ow a con si d erabl e i n crease in vi scosi t y, especi al l y above

su ffi ci en tl y accu rate, th e d epen d en ce of the i n st ru men t con -

1 05 d Pas. In th i s case th e g l ass sh al l be mel t ed at a

stan t k on th e t emperat u re L9 can be cal cu l at ed accord i n g to

temperat u re correspon d i n g to a vi scosi t y of abou t

equ ati on ( 6) :
1 000 d Pas; th e vi scomet ri c measu remen t s sh al l th en be

carri ed ou t, fi rst at l ower t emperatu res; aft erward s th e g l ass

k( t 9) = ko[ l - 34~ 5 - &) I . . . ( 6)
sh al l be h eated ag ai n , the repeatabi l i ty of the me as u re me n t s

sh al l be ch ecked an d fi n al l y the ran g e of h i g h er

wh ere
t emperat u res ( l ower vi scosi t i es) sh al l be tested.

k. is the i n st ru men t con st an t at th e referen ce t emperat u re

b) Devi tri fi cati on . If th e g l ass ten d s to devi tri fy, th e

&;
read i n g s for th e d ri vi n g torq u e an d for th e rotati on al fre-

q u en cy ch an g e wi th t i me at a con st an t t emperat u re. sl i g h t

rx is th e coeffi ci en t of l i n ear t h ermal expan si on of th e
devi tri fi cati on can be ch ecked by repeti ti on of measu re-
mat eri al s of cru ci bl e an d pl u n g er.
me n t s after di fferent t h ermal pretreat men ts; e. g . t empera-

tu res in th e ran g e bet ween 750 an d 950 “C can be appl i ed

If the g eomet ri cal sh ape of th e fl ow fi el d ch an g es wi t h th e
ei ther by q u i ckl y cool i n g d own f rom 1 200 “C or after a
t emperat u re, a sh al l be repl aced in equ ati on ( 6) by an ot h er con -
l on g er t emperi n g peri od in th e cri ti cal t emperatu re ran g e.
stant wh os e val u e is to be est i mat ed from experi men t s.

6. 5 Fi n al ch e ck N OTE - Th e d epen d en ce of the i n st ru men t con stan t k on temperatu re

i s i l l u strated by th e fol l owi n g exampl e, wh i ch h ol d s tru e, as to th e ord er

of mag n i t u d e, for m an y typi cal rotati on vi scomet ers.

After the s amol e h as cool ed to ro o m t emoerat u re, it sh al l be

ch ecked for vi si bl e i n h omog en ei t i es, e. g . devi tri fi cati on, traces

If th e t emperat u re ri ses by 1 00 OC, th e i n st ru men t con stan t d ecreases

of di ssol u t i on of th e cru ci bl e an d pl u n g er mat eri al s, bu bbl es,
by abou t 0. 4 %. Th i s i n fl u en ce i s of pract i cal i mport an ce an d n eed s to
d i scol ou rati on . An y u n u su al al terati on s of al l mat eri al s wh i ch
be t aken i nto accou n t if the vi scomet er is cal i brated at ro o m
h ave been in con tact wi th th e mel t sh al l be taken i nto con -
temperatu re; it can be n eg l ected, h owever, if th e cal i brati on i s carri ed

si derati on .
ou t at el evat ed t emperat u res, not too far f rom th e t emperatu re ran g e

of th e measu remen t s.

7 Expres s i on of resu l ts
7. 4 Eval u at i on of meas u re me n t s

Th e ou tpu t of th e t h ermocou pl es sh al l be read or record ed ; th e

7. 1 M e as u r e d vi scosi ty

correspon d i n g t emperat u res are to be t aken f rom the cal i bra-

ti on ( see 6. 1 ) . Th e i n st ru men t con st an t k sh al l be d et ermi n ed

For th e eval u ati on start f rom eq u at i on ( 21 , u si n g th rou g h ou t th e

for th ese temperat u res accord i n g to 7. 3. Th e i n st ru men t con -

u n i ts speci fi ed in 3. 2. 2 an d equ ati on ( 3) for k.

stan t k an d th e measu re d val u es of th e torqu e TD an d th e rota-

ti onal freq u en cy n sh al l be i n serted in equ ati on ( 4) an d the

7. 2 Co rrect i o n f or fri cti on al l oss es d yn ami c vi scosi t y q sh al l be cal cu l ated accord i n g l y.

If th e d ri vi n g torqu e TD is meas u red or ad j u sted an d if th e

In man y cases, the torqu e of mech an i cal l osses is n eg l i g i bl e. If

cau ses for th e torqu e TL of mech an i cal l osses lie between th e

not, it sh al l be d et ermi n ed accord i n g to 7. 2 an d i n serted in

torqu e- met er in the d ri ve an d th e rotati n g pl u n g er ( or cru ci bl e,

eq u ati on ( 4) .

5
I S0 78 8 4- 2 : 1 9 8 7 ( El

7. 5 Prese n tati o n of resu l ts; pre ci si o n c) meth od of sampl i n g ;

Th e m e asu r e me n ts sh al l be u se d for th e n u meri cal or g raph i cal d) n u m be r of te st spe ci me n s;

re pre se n tati o n of th e vi sco si ty- tempe ratu re rel ati o n sh i p.

el ti me an d te mpe rat u re of mel ti n g d o wn th e test

Th e preci si o n is i n fl u en ce d mai n l y by th e scatter of seve ral spe ci m e n ;

re ad i n g s at co n stan t te mperatu re , th e d evi ati o n of th e

me asu r e d po i n ts fro m th e cu r ve of be st fi t, th e u n ce rtai n ty in

f) type of ro tati o n vi sco me t e r u se d ;

th e d etermi n ati o n of th e te mpe ratu re an d of th e me ch an i cal

val u e s ( to rq u e an d ro tati o n al fre q u e n cy) an d th e u n ce rtai n ty in

g) sh ape , d i me n si o n s an d materi al s of cru ci bl e an d

th e d etermi n ati o n of th e fl o w fi el d co effi ci en t o r th e i n stru men t

pl u n g er;

co n st an t.

h) t ype an d po si ti o n of th e th e rmo co u pl e s;
Erro rs sh o u l d be pr e se n te d acco rd i n g to I S0 7884- l .

i) co mpl e te ti me- tempe ratu re sch e d u l e of th e me asu r e -

me n t;
8 Te st repo rt

j) vi sco si ty- tempe ratu re rel ati o n sh i p of th e sam pl e as

Th e test re po rt sh al l i n cl u d e :
d e scri be d in I S0 788 4- I ;

a) re fe ren ce to th i s part of I S0 78 8 4;

k) an y ch an g e in th e g l ass, o bse rve d d u ri n g an d /o r after

b) d e scri pti o n of th e sampl e ; th e te st.

6
 I S0 78 8 4- 2 : 1 9 8 7 ( E)

An n e x A

Typi cal e xampl e s of fl ow fi el d s in rotati on vi sco me te rs

( 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 . )

Searl e- type Cou ette- type

Vi sco me te r Searl e- type

Pl u n g er Cyl i n d er wi th con e- sh aped Sph ere at en d of l on g

en d s, cyl i n d ri cal sh aft cyl i n d ri cal sh aft Co n focal h al f- el l i psoi d s

( rotati on el l i psoi d s)
Cru ci bl e Cyl i n d er wi th pl an e bottom Cyl i n d er wi th h e mi sph eri cal bottom

( Tamman n - cru ci bl e )

fl ed i an secti o n

of fl ow fi el d

c3 r

2 fi 2

-- ---
- ---

- ---

- -

_2ri l _

Determi n ati on Rel ati ve ; appro xi matel y absol u te if

Absol u te or rel ati ve

of th e fl o w ri l l ri . 2 > 5

fi el d an d

coeffi ci en tf
ral ri l > 4, 5

Fo rmu l ae for Sph e re :

f= -. !L
cal cu l ati n g or
l 6 x2 c3
e sti mati n g f
' i mf1 = +
r, - m
1 1
wh ere c2 = u2
a - 2 = u: - !I: an d

4=, : ( ~ - ~ ) - 2, 3 026l g [~ ~ ; ~ ~ ~ ~ ;

Sh aft: Sh aft: Li mi t val u e for l arg e cru ci bl e s :

1 c. ai

l i mf2 = ~ l i mf2 = 1 I i mA = -

r, - m rg rn b;
87~ 2 1ri, ~ 8791 ri
. bpm

b&- l

f = f, . fJ l f, + f2)

Di sreg ard ed in Con e- sh aped en d s. Tran si ti on I n fl u en ce of cru ci bl e. Tran si ti on area Th ermoco u pl e, if pl u n g ed i n to mel t.

cal cu l ati on area co n es/cyl i n d er an d u pper sph ere/sh aft. Th ermo co u pl e, if

con e/sh aft. Th ermocou pl e, if pl u n g ed i n to me l t.

pl u n g ed i n to mel t.

7
I S0 78 8 4- 2 : 1 9 8 7 ( E)

Fi g u re 1 sh o ws th e i n fl u en ce on th e fl ow fi el d coeffi ci en t, f, if th e i n n er rad i u s ra of th e cru ci bl e is vari ed an d th e rad i u s rr of th e

pl u n g er is h el d con stan t.

0. 2 0. 5 1 2 5 % 1 0

P-

Cu r ve a : co n cen tri c cyl i n d ers, i n fl u en ce of th e en d su rface s d i sreg ard ed .

Cu r ve s b an d c: con focal , l on g rotati on el l i psoi d s.

Here, r- , /c is th e rati o of th e sh ort se m i - axe s of th e cru ci bl e an d pl u n g er.

Th e rati o of th e l on g se m i - axi s to th e sh ort se m i - axi s of th e pl u n g er eq u al s

6 for cu rve b an d 3 for cu rve c.

Cu r ve d : con ce n tri c sph ere s or h al f- sph eres.

N OTE S

1 Th e referen ce poi n t p = 0, if ral ri + ~ 0.

2 Th e smal l e st val u e s of p h ol d for sph e ri cal pl u n g ers.

Fi g u re 1 - Rel ati ve d e cre ase p in th e fl o w fi el d co effi ci en tfas a fu n cti o n of th e rati o of th e rad i u s

of cru ci bl e r, to th e rad i u s of pl u n g e r ri

8
 I S0 78 8 4- 2 : 1 9 9 7 ( E)

An n e x B

Typi cal exampl e of a rotati on vi sco me te r

( 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 . )

Fi g u re 2 s h o ws a sch e mat i c e xamp l e of a Se arl e - type ro tati o n vi sco me te r. Th e su ppo rt fo r th e fu rn ace an d th e d e vi ce fo r th e ad j u st-

me n t of th e rel ati ve po si ti o n s of cru ci bl e an d pl u n g er h ave been o mi tted .

m
1 5
1 Cas e of fu rn ace

2 Th ermal i n su l ati o n

3 Tabl e fo r th e cru ci bl e.

4 Ro tati n g pl u n g e r

5 Cru ci bl e

6 Su r face of th e g l ass mel t

7 Th e rmo co u pl e in pro tecti ve sh eath

8 Scre e n s to pre ve n t ai r co n ve ct i o n

9 Ce rami c t u be an d h e ati n g coi l

1 0 H e ate r fo r th e u ppe r co ve r

1 1 Ce rami c materi al wi th l ow th e rmal co n d u cti vi ty

an d su ffi ci en t me ch an i cal stabi l i ty

1 2 Co ve r, m ad e of ce rami c materi al 1 8

1 3 Swi tch bo ard of th e th e rmo co u pl e

1 3- 1 4 Co mp e n sat i o n cabl e fo r th e th e rmo co u pl e

1 4 Re fe r e n ce po i n t of th e th e rmo co u pl e

1 5 Re co rd e r fo r th e rmo co u pl e an d vi sco me te r re ad i n g

1 6 Re co rd e r swi tch

1 7 Re ad i n g of to rq u e an d /o r ro tati o n al fre q u e n cy

1 8 Dri ve an d to rq u e - me te r

1 9 U n i versal j oi n t fo r sel f- cen tri n g of th e pl u n g er

20 Co n tro l fo r th e el ectri cal i n pu t

21 El ectri c cu rre n t me te r fo r th e byp as s ci rcu i t

22 El ectri c cu rre n t me te r fo r th e total h e ati n g i n pu t

23 Se n so r ( e. g . co n tro l th e rmo co u pl e ) for th e el ectri cal

i n pu t

24 Byp ass ad j u stme n t fo r th e co n tro l of th e

te mperatu re g rad i en t in th e fu rn ace

25 Fi n e ad j u st men t of th e total h eati n g i n pu t

26 H e ate r fo r th e bo tt o m of th e fu rn ace

Ii i6

Fi g u re 2 - Sch e m ati c e xampl e of a Searl e- type rotati on vi sco me te r for g l ass m e l ts

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I S0 76 6 4- 2 : 1 9 6 7 ( E)

An n e x C

Bi bl i og raph y

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

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M E E RL E N DE R, G . A rotati on al meth o d for me asu ri n g th e vi sco si ty of g l ass in th e ran g e between strai n poi n t an d me l ti n g temperatu re.

Pro c. 4th I n tern at. Con g r. Rh e ol og y ( Pro vi d e n ce 1 9631 , Part3. New Yo rk, 1 965, pp. 539- 554.

M E E RL E N DE R, G . Ei n i g e Erg e bn i sse und me ate ch n i sch e Frag en zu r Vi sko si m e tri e an G l assch m e l ze n [ So m e re su l ts an d q u esti on s con -

cern i n g th e me asu ri n g tech n i q u e in vi sco m e try of g l ass me l ts] . Rh eol . Acta, 1 962 ( Vol . 21 , pp. 283- 292.

U DC 66 6. 1 1 . 0 1 : 632. 1 3

Descri pto rs : g l ass, te sts, vi sco si ty me asu re me n t, vi sco si ty.

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