I S0

I N TE RN ATI ON AL S TAN D ARD 7884- 3

Fi rst ed i ti on

1 987- 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 XQYH AP Oj J H AR OP r AH M 3 Au M R n0 C TAH AAP Tkl 3 A~ M M

P > <‘ , . ‘ I ” I ; , q. ( ,.-

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,

Gl as s - Vkcosi ty an d vi scomet ri c fi xed poi n ts -

Part 3 :

Determi n ati on of vi scosi ty by fi bre el on g ati on vi scomet er

Re f e ren ce n u mb e r

I S0 78 8 4- 3 : 1 9 8 7 ( E)

‘,
Foreword

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

nati onal s tan dard s bod i es ( I S0 m em be r bodi es) . Th e work of prepari n g I n ternati on al

St an d ards is n ormal l y carri ed ou t th rou g h I S0 tech n i cal commi t t ees . E ach m em be r

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

the ri g ht to be represen ted on that commi t t ee. I ntern ati onal org ani zati on s, g overn -

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

Draft I ntern ati onal St an d ard s adopt ed by the tech n i cal com mi t t ees are ci rcu l ated to

the m e m ber bod i es for approval before thei r accept an ce as I nternati onal Stan d ard s by

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

l east 75 % approval by th e m e m ber bodi es voti ng .

I n ternati on al St an dard I S0 7884- 3 was prepared by Tech n i cal Com mi t t ee I SO/TC 48,

Laborat ory g l ass ware an d rel ated apparatu s.

U s ers sh ou l d n ote that al l I nternati on al St an d ard s u n d erg o revi si on f rom 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 ntern ati onal St an d ard i mpl i es i ts

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

0 I nternati onal Org an i zati on for St an dardi zati on , 1 997 0

Pri n ted in Swi tz erl an d

I N TE RN ATI ON AL S TAN D ARD I S0 7884- 3 : 1 9 87 ( El

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

Part 3 :

Det ermi n at i on of vi scosi ty by fi bre el on g at i on vi scomet er

0 I n trod u cti on f o rmu l ae o ve r th e wh o l e r an g e of g l as s vi scosi ti es an d fo r a

more d et ai l ed s u rve y on t h ermal h i st ory i n f l u en ces t h an can be

I n t ern at i on al St an d ard I S0 78 8 4, G l as s - Vi scosi t y an d

d eri ve d f ro m fi xed - po i n t meth od s al o n e .

vi s co met ri c fi xed po i n t s, co n si s t s of th e fo l l o wi n g s e par at e

part s :

2 Fi el d of appl i cati on

Part 1 : Pri n ci pl es fo r d et e rmi n i n g vi scosi t y an d vi s co met ri c

fi xed poi n t s. Th e meth od i s appl i cabl e mai n l y i n a vi scosi ty r an g e f ro m 1 0 s to

1 0 1 3 d Pas * bu t speci al d e vi ce s mi g h t be abl e to e xt e n d the

Part 2: De t e rmi n at i o n of vi scosi t y by rot at i on vi s co met e rs.

r an g e up to 1 0 1 4 , s d Pas . Th i s co rr e s po n d s to a r an g e of

t e mp e rat u re f ro m S O0 t o 400 OC fo r al l g l as s e s of n o rmal bu l k-

Part 3: De t e rmi n at i o n of vi scosi t y by fi bre e l o n g at i o n
pro d u ct i o n co mpo s i t i o n s .
vi s co met e r.

N OTE S

Part 4: De t e rmi n at i o n of vi scosi t y by b e am ben d i n g .

1 In th e vi scosi t y ran g e above 1 01 2 d Pas th e t h ermal eq u i l i bri u m of

b ar th e l i qui d stru ctu re is n ot i ceabl y d el ayed fol l owi n g a t emperat u re

Part 5: De t ermi n at i o n of wo rki n g po i n t by si n ki n g

ch an g e. Fo r tests wi th i n th at ran g e it sh ou l d be ag reed wh et h er it is

vi s co met er.
n e ces sary to wai t for th e fi n al eq u i l i bri u m vi scosi t y at a g i ven

temperatu re, or to t ake th e vi sco si t y val u e correspon d i n g to a con ven -

Part 6: De t e rmi n at i o n of s o f t en i n g poi n t .
ti on al t emperat u re- t i me pro g ramme . In th e l atter cas e a n on -

eq u i l i bri u m vi sco si t yi s d en oted by I ] , , ~. Th e s ym bo l r] wi th ou t i n d ex

Part 7: D et e rmi n at i o n of an n e al i n g po i n t an d st rai n po i n t by
d en otes al ways eq u i l i bri u m vi scosi ty.
b e am be n d i n g .

2 Th e soften i n g poi n t, th e an n eal i n g poi n t, an d th e strai n poi n t are

Part 8: De t ermi n at i o n of ( d i l atomet ri cl t ran s f o rmat i o n

con ven t i on al temperatu re poi n ts ( so- cal l ed fi xed poi n ts) , wh i ch are ob-

t e mpe rat u re . tai n ed by speci al test proced u res in appropri ate, wel l - d efi n ed ap-

paratu s ( see I S0 7664- 6 an d I S0 7664- 7) . Th e s e poi n ts ch aracteri ze

th e fl ow beh avi ou r of g l ass in th e ran g e of soften i n g an d g l ass tran si -

ti on , bu t on l y appro xi mat e vi scosi t y val u e s are assi g n abl e.

1 Sco pe

Th i s part of I S0 7884 s peci fi es a meth od of d et e rmi n i n g th e

3 Ref eren ce
d yn ami c vi scosi ty of g l as s by m e as u ri n g th e el o n g at i o n of a

g l as s fi bre u n d er a d efi n ed u n i axi al s t ress. In ad d i t i o n , th e

I EC Pu bl i cat i o n 5 8 4- 1 , Th e rmo co u pl e s - Part 1 : Re f e r e n ce
vi sco s i t y- t emperat u re rel at i o n sh i p an d the d e p e n d e n ce of th e
t abl es .
vi scosi t y on th e t h e rmal h i st o ry can be d e t e rmi n ed .

N OTE - U s i n g th i s met h od , al l parts of th e tested mat eri al are su bj ect

4 Defi n i ti on s
to th e s am e me ch an i cal st ress wh en th e sh ape of th e fi bre i s correct,

th e g l ass i s h o mog e n e o u s an d i sotropi c, an d th e i n fl u en ce of g ravi t y on

Fo r th e pu rposes of th i s part of I S0 7884, th e f ol l owi n g d efi n i -
th e fi bre i tsel f can be n eg l ected . Th e d eformat i on i s a pu re el on g ati on
ti on s appl y.
i n stead of a s i mpl e sh ear. Wi t h ou t maj o r u n certai n ty, th e d ete rmi -

n ati on of th e sh ear vi scosi t y by an el on g ati on e xpe ri me n t i s possi bl e

on l y wh en th e mat eri al beh aves l i ke a N ewt on i an fl u i d.

4. 1 Sampl e, test speci men , fi bre, bal l

Th e kn o wl e d g e of eq u i l i bri u m vi scosi t i es in th e l o w- t e mpe ra- Th e t est s pe ci me n is p r e p ar e d f ro m a mo l t en t est po rt i o n of

t u re r an g e is u sef u l for fi tti n g s u i t abl e vi sco s i t y- t emperat u re th e s ampl e . Th e fi bre is th e cyl i n d ri cal part of th e t est

*
1 d Pas = 1 z = 1 P

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

1
I S0 78 8 4- 3 : 1 987 ( El

sp e ci me n wi th co n st an t cro ss- se ct i o n S = n d * /4 o ve r i ts I n practi ce it i s o fte n m o re co n ve n i e n t to u se Al , i . e. th e ch an g e

l e n g th 1 . Th e d i amete r d of th e fi bre i s smal l co m par e d wi th th e in l e n g th 1 2 - I t, wh i ch is m e asu r e d u si n g a d i fferen t d e vi ce

l e n g th 1 . fro m th at fo r 1 1 . In th i s cas e e q u ati o n ( 2) can be re- wri tten as

Each en d of th e fi bre is me l ted i n to a bai l , wh i ch e n abl e s th e

test spe ci me n to be su spen d ed verti cal l y, fi xe d at i ts u ppe r en d q = 3 2 70 0 rn AtI ' x ’ + A; 2 : l ” . . . (3)

V
1
an d co n n e ct e d to a l o ad i n g d e vi ce at i ts l o wer en d .

In e q u ati o n (3) m is e xpr e sse d in g rams; I,, I2 an d AI in

4. 2 Lo ad , l o ad i n g pi e ce s, d e ad - we i g h t
mi l l i metres; V in cu bi c mi l l i metres; At in se co n d s; an d q in

d e ci pascal s e co n d s ( d Pas) .
Th e l o ad co n si sts of al l parts of th e apparatu s on wh i ch g ravi ty

acts to pr o d u ce a fo rce on th e l o we r en d of th e fi bre - i . e. th e

l o ad i n g pi e ce s ( vari abl e) , an d th e d e vi ce fo r su sp e n d i n g th e N OTE - I n cal cu l ati n g t h e vi sco si ty, co rrecti o n s so m e t i m e s h ave to b e

appl i ed ( se e 9 . 2 ) .
l o ad i n g pi e ce s bel ow th e sp e ci m e n ( a g i ve n val u e fo r th e appar-

tu s) - pl u s th e we i g h t of th e l o wer bal l ( to be e sti mat ed after

prepari n g th e test spe ci me n ) . Th e l o ad pr o d u ce s th e fo rce Fc

5. 2 Prel i mi n ary e sti mati o n of ti me i n terval
acti n g on th e test spe ci me n in th e axi al d i recti o n .

an d e l o n g ati o n

Th e d e ad - we i g h t st e m s fro m th e part of th e fi bre be l o w th e

cro ss- se cti o n u n d er co n si d erati o n ( se e 9. 2) . Th e fo rce due to Th e tabl e s h o ws th e e xpe ct e d val u e s of th e ti me i n terval At, for

g ravi ty vari es l i n earl y fro m ze ro at th e l o we r en d to g . e. 1 . S at g i ve n l o ad s in rel ati on to th e vi sco si ty. Th e val u e s are

th e u ppe r en d of th e fi bre ( g an d Q be i n g th e acce l e rati o n o f free cal cu l ated fo r a fi bre wi th a d i ame te r d, = 0 , 73 7 mm at th e

fai l , an d th e g l ass d en si ty, respecti vel y) . be g i n n i n g of th e me asu re me n t, an d an el o n g ati o n of 2 % d u r-

i ng th e ti me i n terval At, ( Al /l , = 0, 021 . Be t we e n th e t wo h e avy

st e pp e d l i n es i n th e tabl e th e sen si ti vi ty of th e me asu ri n g d e vi ce

4. 3 Effe ct of su rface ten si o n
for th e el o n g ati o n Al sh o u l d be i n cre ase d by th e facto r 1 0 ( th e

el o n g ati o n sh o u l d b e d e cre ase d b y th e facto r 1 /I O) fo r sh o rten -

Th e effe ct of su rface te n si o n i s to d e cre ase th e su rface are a of

i ng th e ti me i n terval At, b y th e facto r I! 1 0. Be l o w th e l o wer l i ne

th e spe ci me n , i . e. to sh o rte n th e fi bre. Th e re fo re , it i s a fo rce

th e facto r is 1 0 0 i n stead of 1 0 ( l /1 0 0 i n stead of l /I O) .

wh i ch acts u pon th e fi bre in th e o ppo si te s e n se to th at of th e

g ravi tati o n al fo rce of th e l o ad an d of th e d e ad - we i g h t.

Tabl e - Ti me i n terval At, fo r an e xte n si o n Al /l 1 = 0, 02

u n d er a l o ad of m as s m ( as co rre cte d fo r d e ad - we i g h t

5 Pri n ci pl e an d su rface te n si o n ) , for a fi bre of i n i ti al

d i ame te r d, = 0, 737 mm

5. 1 Basi c rel ati o n

Ti me i n terval At, in se co n d s for l oad of m as s

Co n si d e r th e fo rce Fe of th e l o ad acti n g on a spe ci m e n

pre pare d fro m a g l ass wi th N e wt o n i an be h avi o u r an d sh o wi n g

1 ~~~ ‘ g , 6i ph i 1 ~ ; ~ i 21 g l

no d e fe cts. Wh e n th e e ffect s of d e ad - we i g h t an d su rface ten -

si o n are n eg l i g i bl e an d al l el asti c d e fo rmati o n s by th e l o ad i n g

b e co m e co n stan t , th e re e xi sts to a g ood appro xi mati o n an e x-

1 0’0 2560 640 1 60 40 -
ten si o n al fl o w at co n st an t vo l u me as d e scri be d b y e q u ati o n (1 ) :

1 0” 25 600 6 40 0 1 600 40 0 1 00

dl 1 Fol *
- = - xx 1 0’2 256000 64000 1 6000 4 000 I 1 000
. . .

dt 3rj V
1 0' 3 - ( I ( 1 6~ 00 / 40 : ‘ E(

wh e re I 1 0' 4
I-
q i s th e d yn ami c vi sco si ty;

Fo r o th er d i ame te rs of th e fi bre th e ti me i n terval At 3 fo r an

V = I x S i s th e vo l u me of th e fi bre ( th e o th er sym bo l s e l o n g ati o n of 2 % can be est i mate d fro m e q u ati o n ( 4) :

h ave th e me an i n g as i n tro d u ce d abo ve ) .

At; = Ats. ft . . . ( 4)
Du ri n g th e ti me i n terval At of th e m e asu r e me n t , th e fi bre

e l o n g at e s fro m th e i n i ti al l e n g th I, to th e fi n al l e n g th 1 2 Th e n

Th e val u e of th e d i me n si o n l e ss co n ve rsi o n facto r ft as a fu n c-

th e vi sco si ty is cal cu l ate d u si n g e q u ati o n ( 2) :

ti o n of th e d i amete r i s fo u n d fro m th e d i ag ram in fi g u re 1 .

g At
1 2 x 1 1
* . . ( 2)
Th e e sti mate d val u e s At, an d At: d e ri ve d fro m th e tabl e,
q = 3 Xm xTX-
1 2 - 4
fi g u re 1 an d e q u ati o n ( 4) g i ve on l y a su rve y of th e e xpe ct e d

wh e r e ti me req u i red fo r th e me asu re m e n t an d an esti mati o n of th e

wh o l e e l o n g ati o n of th e fi bre d u ri n g a se q u e n ce of

g is th e ave r ag e accel erati o n of free fal l ; me asu r e m e n t s on th e sam e fi bre. Fo r th e q u an ti tati ve e val u a-

ti o n of th e el o n g ati o n expe ri me n t, h o we ve r , th e starti n g po i n t

m is th e m as s of th e l o ad th at pr o d u ce s th e fo rce Fo . i s e q u ati o n (31 , u si n g th e actu al val u e s ( se e cl au se 8) .

2
 I S0 78 8 4- 3 : 1 9 8 7 ( E)

6. 2 . 2 Co n tro l th e rmo co u pl e s sh o u l d be l o cate d as cl o se as

po ssi bl e to th e fu rn ace wi n d i n g s fo r fast re sp o n se . Th e h ot

j u n cti o n s of th e m e asu r e me n t t h e rmo co u pl e, h o we ve r, sh al l be

pl ace d in th e i mme d i ate vi ci n i ty of th e spe ci me n ( se e th er-

mo co u pl e A in fi g u re 2) . Th e t empe ratu re d i stri bu ti on al o n g

th e fi bre sh al l be mo n i to red by su i tabl e d e vi ce s su ch as

-
a h i g h - mass bl o ck of n i ckel or si l ver aro u n d th e fi bre,

wi th a n u m be r of h ol es fo r fi xed t h ermo co u pl e s; or

-
a mo bi l e t h e rmo co u pl e ( su ch as th e rmo co u pl e B in

fi g u re 2) .

In th i s cas e care sh o u l d be take n th at th e th e rmo co u pl e

d oes n ot affect th e te mpe ratu re of th e fi bre ( se e I S0 78 84- l :

1 9 8 7, su b- cl au se 5. 3 ) .

In acco rd an ce wi th I S0 7884- l th e m e asu re me n t th ermo -

co u pl e s sh al l be cal i brated an d th e cal i brati o n ch e cke d

reg u l arl y.

6. 2. 3 Th e el ectri cal o u tpu t of th e t h e rmo co u pl e s sh al l be

d et ermi n ed at ze ro cu rren t by m e an s of po te n ti o mete rs, or

h i g h - resi stan ce el ectro n i c ampl i fi ers h avi n g a sen si ti vi ty of 1 pV

fo r t ype S ( acco rd i n g to I E C 584- l 1 , or 4 u V for t ype K ( acco rd -

i ng to I E C 58 4- I ) t h e rmo co u pl e s. Precau ti o n s sh al l be t ake n

0. 6 I.0 I4 1 .8 th at th e i ce- bath fo r th e co l d j u n cti o n is mai n tai n e d at 0 OC

th ro u g h o u t th e test. I f th e te mperatu re me asu ri n g e q u i pme n t is

Co n ve r si o n factor ft

fi tted wi th au t o mati c co l d j u n cti o n co mpe n sat i o n , th e i ce- bath

can be o mi tte d .
Fi g u re 1 - Co n ve r si o n facto r ft as a fu n cti o n of th e fi bre

d i amete r dl

6. 3 H an g i n g d e vi ce fo r te st sp e ci me n an d l o ad

6 Apparatu s
6. 3. 1 Th e co n stru cti o n of th e su ppo rt for th e te st spe ci m e n

d epen d s on th e type of fu rn ace u se d . Wh e n th e top of th e

6. 1 Vi sco me te r fu rn ace wo rki n g sp ace of a ch am b e r fu r n ace is cl o se d ( as s h o wn in

fi g u re 2) . th en a t u be of fu se d si l i ca i s u se d as a su ppo rt stan d .
El ectri cal l y h e at e d fu rn ace fo r te mpe rat u re s at l e ast up to
Th e t u be pro j e cts i n to th e wo rki n g sp ace of th e fu rn ace fro m
900 OC. Th e fu rn ace sh al l be capabl e of acce pt i n g th er-
be l o w. Th e ce n t re d su ppo rt pl ate on to p of th e stan d is m ad e
m o co u p l e s fo r me asu ri n g th e t empe ratu re an d i ts d i stri bu ti o n
fro m cerami c or fro m stai n l e ss steel . Th e test spe ci m e n is
al o n g th e spe ci m e n . Th e te mpe ratu re g rad i e n t at th e l o cu s of
su sp e n d e d by i ts u ppe r bal l wh i ch l o cate s in a cen tral re ce ss in
th e spe ci m e n sh al l n ot e xce e d 0, 2 ‘ C/cm .
th e su ppo rt pl ate. Be cau se of po ssi bl e ad h e si o n of th e g l ass, a

cen tral l y bo re d ce rami c b e ad of appro pri ate d i me n si o n s ( on l y

Th e fu rn ace h e ate rs sh al l be co n tro l l ed by a d e vi ce wh i ch en -

to be u sed o n ce ) sh o u l d be pl ace d b e t we e n th e su ppo rt pl ate

su r e s th at th e t empe ratu re re mai n s co n st an t wi th re spe ct to

an d th e u pp e r bal l of th e test sp e ci me n .
ti me, wi th i n th e wo rki n g s p ace of th e fu rn ace, to f 1 OC or bet-

ter. Li n earl y i n cre asi n g ti me- tempe ratu re p ro g ramm e s wi th a

m axi mu m rate of 6 ‘ Y/mi n sh al l be ach i evabl e by th e sam e 6. 3. 2 Wh e n u si n g a verti cal l y mou n ted mu ffl e fu rn ace ( bo th

d e vi ce . en d s o pe n ) , th e fi bre is co n n e ct e d to an u p pe r ro d of fu se d

si l i ca. Examp l e s of d e vi ce s fo r co n n e ct i n g th e te st sp e ci m e n to
Th e fu rn ace an d i ts co n tro l d e vi ce sh al l h ave ch aracte ri sti cs
th e ro d ( by m e an s of bal l s) are s h o wn in fi g u res 3 an d 4. It is

su ch th at th e d e si re d ti me - te mperatu re p ro g ramme i s attai n ed

e ssen ti al th at th e ro d an d th e fi bre h an g verti cal l y, co axi al l y an d
at th e l atest 5 mi n after starti n g fro m a co n st an t i n i ti al
ce n tral l y i n th e tu be o f th e fu rn ace. Asi d e fro m th e su ppo rt, th e

te mperatu re . Th e val u e of th e rate sh al l be h el d wi th i n + 1 0 %

to p of th e fu rn ace tu be sh o u l d be co ve re d .

th ro u g h o u t th e d e te rmi n ati o n .

6. 3. 3 Th e l o ad i n g l i n kag e co n si st s of a ro d ( m ad e of fu se d
6. 2 Te mperatu re me asu ri n g an d i n d i cati n g i n stru me n ts
si l i ca, abo u t 1 mm in d i ame te r) bel ow th e te st spe ci me n , wi th

fu se d bal l s on b o th en d s an d co n n e ct o rs as s h o wn i n fi g u re 3 or

6. 2 . 1 Th e al u mi n a- i n su l ate d pl ati n u m- 1 0 % rh o d i u m/pl ati - 4. Be l o w th e l o wer co n n e cti o n ( o u tsi d e th e fu rn ace ) th e attach -

num ( type S acco rd i n g to I E C 584- l 1 t h e rmo co u pl e s, or n i ckel - men t of th e l o ad carri es a su i tabl e i n d i cato r fo r th e el o n g ati o n

ch ro mi u m/n i ckel ( type K acco rd i n g to I EC 5 84- I ) th e rmo - m e asu re me n t ( marker or tran sd u ce r co re) . Fo r th e me d i u m

co u p l es sh al l exh i bi t l ow th e rmal i n erti a ( th e d i ameter of th e r an g e of vi sco si ty th e to tal m as s of al l parts of th e l o ad i n g

wi re s sh o u l d n ot b e g reater th an 0, 5 mm) . Th e wi res sh al l h ave l i n kag e d e vi ce sh o u l d am o u n t to appro xi matel y 4 g. In th e

a su ffi ci en t l e n g th wi th i n th e fu rn ace ( wi th re spe ct to h e at r an g e of h i g h er vi sco si ti es an d h e avi er l o ad s th e d i ame te r o f th e

co n d u cti o n al o n g th e wi res) . si l i ca ro d sh o u l d be g reater.

3
I SO 78 8 4- 3 : 1 987 ( El

I
F- - . - * - . . . . . . . . . . . <

31 H o t j u n cti o n of

‘ th e rmo co u pl e B

H o t j u n cti o n o

th e rmo co u pl e
2’

-
1 ’

8,

Y
z?i !

1 Co n n e ct o r fo r th e l o wer bal l of th e te st sp e ci m e n an d th e 5 Lo ad i n g d e vi ce ( on l y th e ro d i s sh o wn )

l o ad i n g d e vi ce ( for co n n e ct o r s o fferi n g d i fferen t m ag n i t u d e s of

l o ad , se e fi g u res 3 an d 4) 6 Su ppo rt st an d : tu be of fu se d si l i ca

2 Te st sp e ci m e n 7 Scre e n i n g b e t we e n wo rki n g sp ace an d h e ate rs

3 Su pp o rt pl ate 8 Ch am b e r fu rn ace wi th h e ate rs

4 Upper bal l of th e test spe ci me n 9 Co ve r ri n g bel ow th e fu rn ace ( fi xed at th e si l i ca tu be )

Fi g u re 2 - Fi bre el o n g ati o n me t h o d e xamp l e of a testi n g d e vi ce ( sch e mati c)

Fi g u re 3 - Co n n e ct o r bl o ck ( metal ) b o re d to act as h an g i n g d e vi ce

Fi g u re 4 - Co n n e cto r h o o ks ( wi re) to act as h an g i n g d e vi ce s

4
 I S0 7884- 3 : 1 9 97 (I 3

6. 3. 4 Wh e n meas u ri n g wi t h i n the r an g e f rom I Os t o 1 0 s d Pas , 6. 6 Eq u i pmen t for preparat i on of t est s peci men s

th e l o ad i n g l i n kag e d evi ce con si st s of a co n n ect o r an d l ower

rod , wi t h a d i amet er of abo u t 0, 5 mm, wi t h ou t f u rt h er d evi ces

6. 6. 1 Bl ast f l ame bu r n e r or el ectri cal l y h e at e d f u rn ace
be l o w the en d of the ro d ( th i s en d i s bel o w the f u rn ace an d act s
for mel t i n g th e s ampl e an d d rawi n g fi bres.
as i n d i cat or) . Th e t ot al mas s of thi s d evi ce sh ou l d amo u n t to

approxi mat el y 1 g.

6. 6. 2 Two ro d s m ad e f ro m pl at i n u m met al al l oys, cerami cs

N OTE - Th e meas u re me n t of th e el on g ati on by m e an s of a travel l i n g

or h ard g l ass for f l ame- worki n g a s ampl e port i on .

mi croscope i s faci l i tated wh en th e l ower en d of th e rod i s g en tl y g u i d ed

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

6. 6. 3 Pl at i n u m cru ci bl e an d ro d s m ad e f rom pl at i n u m met al

al l oys or f u s ed si l i ca, wh e n an el ectri cal l y h e at ed f u rn ace for the

preparat i o n is u s ed .
6. 4 Lo ad i n g pi eces

A set of l oad i n g pi eces m ad e f ro m bras s, wi t h mas s e s d et er-

6. 6. 4 Sl i d e- g au g e wi t h vern i er g rad u at i o n 1 /l O for the d et er-
mi n ed to the n eares t 0, Ol g. Th e pi eces sh al l be fi tt ed by
mi n at i on of the fi bre l en g t h .
su i t abl e at t ach men t d evi ces ( e. g . h o o ks ) . It is co n ven i en t to

ch o o s e pi eces of mas s e s s u ch t h at the t ot al l oad co rres po n d s

n earl y to the val u es g i ven in the t abl e. Wh e n th e mas s of the 6. 6. 5 Mi cro met er cal i per, wi t h a l east me as u r eme n t of

l oad i n g l i n kag e d evi ce (i n acco rd an ce wi t h 6. 3. 3) is 4 g, th en 0, 005 mm, for meas u ri n g th e fi bre d i amet ers. Th e s u rf ace of

the appropri at e mas s e s of th e pi eces are 1 2 g, 60 g an d 252 g, the fi bre sh al l n ot b e d am ag e d by t h e ad van ce me n t of the spi n -

respect i vel y. dl e h ead .

I n s t ead of the cal i per, a mi cro s co pe wi t h mi cro met er s cal e m ay

be empl o yed by expe ri en ced u s ers.

6. 5 Ext en s o met er arran g emen t s

6 . 51 Mo vi n g marker bel o w th e f u rn ace as an i n d i cat or of

7 Sampl e an d test speci men

the el o n g at i o n of the fi bre.

Th e s ampl e sh al l be u n i form, bu bbl e- f ree an d h o mo g e n e o u s .

6. 5. 2 Devi ce for d et ermi n i n g the fi bre el o n g at i o n Al

d u ri n g th e t i me i n t erval At.

7. 1 Preparat i on of a t est s pe ci men by fl ame-

A mi n i mu m sen si ti vi ty of 0, 02 mm is n eed ed. wo rki n g

Th e i n st ru men t for o bs ervi n g the d o wn war d s mo vi n g marker Mel t a t est port i on of abo u t 2 to 3 cm3 of th e s ampl e in the

sh al l be l ocked in posi t i on d u ri n g an y on e si n g l e d et ermi n at i on fl ame. By t u rn i n g the t est port i on b e t we e n the ro d s, f o rm a

of Al . It sh al l be possi bl e to posi t i on it in ad van ce so t h at th e bal l . Re m o ve the t est port i on f rom the f l ame an d d r aw ou t the

wh o l e el o n g at i o n l en g t h AI in a d et ermi n at i o n is wi t h i n th e bal l to a l on g fi bre. P ro ce e d q u i ckl y be cau s e of poss i bl e evapo r-

r an g e of obs ervat i on . Errors ari si n g f ro m i n correct g rad u at i on at i on of th e mo r e vol ati l e co mpo n e n t s of the g l ass,

of the scal e, o r d evi at i on s f rom l i n eari ty of th e d i spl ay, sh al l n ot

e xce e d 0, Ol mm. N OTE - To prod u ce su ffi ci en t reg u l ari ty of th e d i amet er al on g th e

fi bre, a cert ai n experi en ce of the preparati on tech n i qu e is requ i red,

N OTE - Su i tabl e d evi ces are for exampl e travel l i n g mi cro scope s wi t h especi al l y wi t h respect to the

mi cromet er scal es, or l i n ear di fferen ti al t ran sformers ( core an d coi l

-
t emperatu re at th e beg i n n i n g of drawi n g ;
separated f rom each oth er) . Th e u se of di fferen t ran g es of sen si t i vi ty is

an ad van t ag e. - t emperat u re- vi scosi t y rel ati on sh i p of th e g l ass;

- force an d speed of d rawi n g ;

6. 5. 3 Devi ce f or d et ermi n i n g the l en g t h 1 , o ver the wh o l e

-
u n i formi ty of d rawi n g ; an d

amo u n t of el o n g at i on (I , - /c) f rom th e ori g i n al l en g t h l c af t er

-
con cl u si on of d rawi n g at the correct t i me.
prepari n g th e s pe ci men at room t emperat u re (1 8 to 20 “Cl to

the i ni ti al l en g t h 1 , bef o re st art i n g th e t i me i n t erval At, see

eq u at i o n ( 2) . Th e l en g t h l c sh al l be d et ermi n ed to the n eares t

7. 2 Preparat i on of a test speci men in a fu rn ace
0, 2 mm. Th e l ast val u e of I, - l o at the en d of a s e q u e n ce of

me as u r e me n t s sh ou l d n ot e x ce e d 0, l x lo
Th e me t h o d appl i es to g l as s es wi t h a t e n d e n cy to cryst al l i ze.

N OTE - Th e d evi ce mi g h t con si st of, for exampl e, a cat h etomet er fi t-

A t est port i on of abo u t 1 00 g of th e s ampl e is mel t ed in a
ted wi t h scal e an d vern i er, carryi n g the mi croscope or th e coi l of th e
pl at i n u m cru ci bl e in the el ect ri cal l y h e at e d f u rn ace. Th e g l as s
di fferen ti al tran sformer.

m ay be d el i vered in an y form, bu t th e d i amet er for g rai n s

sh ou l d n ot be l ess t h an 3 mm. A cyl i n dri cal rod of pl at i n u m,

6. 5. 4 Ti mer for d et ermi n i n g th e i n t erval At [ s ee eq u at i o n s ( 2)

cerami cs or f u s ed si l i ca is d i pped i nto th e al mos t bu bbl e- f ree

an d ( 31 1 ,ran g i n g f rom 20 to 2 000 s, wi t h a l east co u n t of 0, l s.

mol t en t est port i on of th e g l ass. Aft er the ro d ti p i s wet t ed by

Th e t i mer sh al l be co rrect ed for sys t emat i c errors g reat er t h an

the g l ass, i t i s d r awn u pwar d s ( s ee n o t e to 7. 1 ) . Th e rod m ay be

0, 2 %.
d r awn by h an d or an y su i t abl e d evi ce.

5
I S0 78 8 4- 3 : 1 9 8 7 ( El

7. 3 Fi n i sh i n g th e test speci men respect to th e wal l of th e fu rn ace. Obse rve as soon as po ssi bl e

th e posi ti on of th e i n d i cator by m e an s of th e cath etometer.

Th e l en g th of th e test spe ci m e n s sh ou l d be between 50 an d Assi g n th i s posi ti on to th e ori g i n al l en g th /, , of th e test

1 00 mm before beg i n n i n g th e me asu re me n t. A su i tabl e pi ece of spe ci me n .

th e d rawn fi bre ( se e 7. 1 or 7. 2) , 20 to 30 mm l on g er th an th e

d esi red fi bre l en g th of th e test spe ci me n , is sel ected on th e

8. 2. 2 Wh e n vi sco si ti e s fro m 1 08 to 1 0s d Pas are to be d eter-

basi s of u n i form d i ameter an d rou n d n ess. By fl ame - worki n g ,

mi n e d by u si n g th e l oad i n g d e vi ce d escri bed in 6. 3. 4, wai t u n ti l

both en d s are me l ted d own to bal l s abou t 2 mm in d i ameter.

th ere i s a n earl y co n stan t el on g ati on rate an d take th at val u e for

Take care th at th e bal l s are cen tred on th e fi bre axi s.

th e vi sco si ty cal cu l ati on . Th e fi bre sh ou l d n ot el on g ate by mo re

th an 2 % d u ri n g on e test.

After th e test spe ci me n h as cool ed , th e l en g th of th e fi bre ( bet-

we en th e bal l s) is d etermi n ed to th e n earest 0, 2 mm. Gen eral l y, N OTE - Du ri n g a 2 % el on g ati on of th e fi bre, th e i n stan tan eou s speed

th e d i ameter sh al l be between 0, 6 an d 0, 8 mm. For me asu ri n g of th e d escen d i n g i n d i cator i n crease s by 4 %. Th e ti me for a 2 % fi bre

el on g ati on i s esti mated in th e se co n d co l u mn ( for a l oad m = 1 g) of

vi sco si ti e s ran g i n g fro m 1 0 s to 1 0s d Pas, d i amete rs up to 1 mm

th e tabl e.
are acceptabl e. A n u mbe r of d etermi n ati on s of th e d i ameter

sh al l be mad e , eq u al l y d i stri bu ted over th e l en g th of th e fi bre, in

Establ i sh th e n e xt measu ri n g temperatu re as so on as possi bl e.
d i recti on s perpen d i cu l ar to th e fi bre axi s. Th e m a xi m u m an d
Wai t o n ce mo re u n ti l th ere is a n earl y con stan t el on g ati on rate,
mi n i mu m d i ame ters sh al l n ot d i ffer by m o re th an 2, 5 % of th e
an d so on . Wh e n vi sco si ti e s l e ss th an 1 09 d Pas are to be d eter-
me an . Th e ari th me ti c m e an of th e d i ame ters me asu re d sh al l be
mi n e d by u si n g th e l oad i n g d e vi ce d escri be d in 6. 3. 3 wi th ou t
u sed for cal cu l ati on of th e vo l u me V.
l oad i n g pi e ce s [see th e th i rd co l u m n ( for a l oad m = 4 g) of th e

tabl e] , u se th e sam e proced u re as d escri bed above.

Th at en d of th e fi bre wh i ch h as th e l arg er d i ameter sh al l be

ch o se n as th e u pper ( fi xed ) en d of th e test spe ci me n . Th e test

8. 2. 3 For me asu ri n g vi sco si ti e s n ot l e ss th an 1 0s d Pas, th e

spe ci m e n sh al l be free from scratch e s, stri ae, d evi tri fi cati on s or

l oad i n g pi ece s h ave to be u sed ( see th e fou rth to si xth co l u mn s

oth er i n h omog en ei ti es. Th ere sh al l be no n ecki n g of th e fi bre at

of th e tabl e) . Fi rst h eat th e spe ci m e n to th e req u i red

ei th er en d ad j acen t to th e bal l s.

temperatu re wi th ou t l oad i n g it wi th th e l oad i n g pi ece s. Wh e n

th e i n d i cator is d escen d i n g at n earl y con stan t speed , or d oe s

7. 4 Etch i n g of th e test speci men

n ot apparen tl y ch an g e i ts posi ti on , attach th e l oad i n g pi e ce s

an d d etermi n e th e rate of el on g ati on on ce an approxi mate l y

Th e su rface l ayer resu l ti n g fro m th e d rawi n g pro ce ss of th e

con stan t el on g ati on rate is observed . Th e el on g ati on sh al l n ot

g l ass fi bre sh al l be re mo ve d by etch i n g th e test spe ci m e n in an

e xce e d 2 % in on e test. By preferen ce smal l e r el on g ati on s, as

aq u eou s sol u ti on of h yd roch l ori c, su l fu ri c or n i tri c aci d [c( H CI ) ,

d etermi n ed by m o re se n si ti ve measu ri n g d e vi ce s, sh ou l d be

c( 1 /2H2S04) , or c( H N 0 . J = 2 mol /l l , con tai n i n g 3 % h /m) of

d etermi n ed if possi bl e. Re m o ve th e l oad i n g pi e ce s d u ri n g e ve ry

h yd rofl u ori c aci d , for 0. 5 to 1 mi n at ro o m temperatu re. Th e

ch an g e of th e me asu ri n g temperatu re.

test spe ci m e n sh al l be ri n sed wi th d i sti l l ed water, th en d ri ed .

If vi sco si ti e s n ot l e ss th an 1 01 1 d Pas are to be measu re d , th e

d el ayed el asti ci ty of th e g l ass u n d er test h as to be taken i n to

7. 5 Speci al treatmen t
con si d erati on . Th erefore, wai t o n ce mo re for a con stan t rate of

el on g ati on after attach i n g th e l oad i n g pi ece s.

For g l asse s wh o se properti es mi g h t be al tered ve ry e asi l y,

con d i ti on s sh ou l d be ag reed for th e treatmen t of th e sampl e ,

e. g . th e type of bu rn er fl ame , e xcl u si o n of th e appl i cati on of 8. 3 Determi n ati on of th e vi scosi ty at i n creasi n g

an y fl ame in th e preparati on of th e test spe ci me n , th e u se of an temperatu re

i n ert g as atmosph ere.

Wh e n a h eati n g rate of AO/At (i n d eg rees Ce l si u s per mi n u te) is

provi d ed , bri n g th e fu rn ace to a temperatu re wh i ch is l e ss th an

th e d esi red starti n g temperatu re of th e i n crease by an amou n t

8 Pro ce d u re
eq u al to fi ve ti mes th e val u e of ABl At. Th en i n trod u ce th e test

spe ci me n , te mper for 1 0 mi n , l oad an d start th e temperatu re-

8. 1 Cal i brati on ti me pro g ramme . After 5 mi n beg i n to me asu re th e el on g ati on

an d repeat th e me asu re me n t at eq u al ti m e i n terval s. Me asu re

Gen eral l y, th e fi bre el on g ati on me asu re me n t is an absol u te th e temperatu re u si n g th e sam e i n terval s bu t d i spl aced ag ai n st

d etermi n ati on of th e vi sco si ty, i . e. th e vi sco si ty is cal cu l ated th e el on g ati on read i n g s by h al f an i n terval . ( Th e con ti n u ou s

( se e 5. 1 an d 9. 2) fro m th e d i me n si o n s of th e fi n i sh ed test reg i strati on of both read i n g s m ay be preferred . )

spe ci me n . Th e th ermoco u pl e s sh al l be cal i brated by co m -

pari son wi th a certi fi ed stan d ard th ermocou pl e. Repeat th e Th e meth od appl i es to i n i ti al temperatu res eq u al to or so m e

cal i brati on reg u l arl y. d eg rees h i g h er th an th e tran sformati on temperatu re or th e an -

n eal i n g poi n t.

8. 2 Determi n ati on of th e vi sco si ty at co n stan t N OTE - Wh e n th e vi sco si ty- te mperatu re beh avi ou r is co mpl e te l y

temperatu re u n kn own , m ake a pre l i mi n ary d etermi n ati on , ch oosi n g h i g h er rates of

temperatu re i n crease, starti n g fro m th e tran sformati on temperatu re or

an n eal i n g poi n t.

8. 2. 1 Heat th e vi sco m e te r fu rn ace to th e d esi red me asu ri n g

temperatu re. Su spe n d th e spe ci me n an d th e l oad i n g l i n kag e

Wh e n th i s meth od is appl i ed , a d i fferen ce between th e read i n g

fro m th e su pport, cen tre an d ad j u st for free h an g i n g wi th

an d th e tru e temperatu re of th e test spe ci m e n is possi bl e,

6
 I S0 78 8 4- 3 : 1 9 8 7 ( E)

d epen d i n g on th e rate of h eati n g . Wi th i n th e ran g e of 9. 3 Eval u ati on of th e measu remen ts at con stan t

eq u i l i bri u m vi sco si ty, i . e. be l ow 1 01 2 d Pas, th e d i fferen ce can temperatu res

be d etermi n ed experi men tal l y by th e proced u res d escri be d in

8. 2, an d th e me asu re me n ts sh al l be corrected for th i s pu rpose. I n sert in eq u ati on ( 3) th e val u es of th e fi bre vo l u m e V in cu bi c

Wi th i n th e ran g e in wh i ch n on - eq u i l i bri u m vi sco si ti e s occu r, m i l l i me tre s, of th e ti m e i n terval At in se co n d s, of th e rel ated

i . e. above 1 01 2 d Pas ( see n ote 1 to cl au se 21 , di fferen t l abora- el on g ati on AI in mi l l i me tre s, an d of th e i n i ti al l en g th II in

tori es sh al l ag ree on th e ti me- temperatu re pro g ramme ch osen . mi l l i me tre s. Appl y th e co rrecti on s expl ai n ed in 9. 2 if n e ce ssary.

9. 4 Eval u ati on of th e measu remen ts at i n creasi n g

8. 4 Termi n ati on of th e tests
temperatu re

Fi n i sh th e test (i f n ot termi n ated before) wh en th e fi bre h as

Th e el on g ati on Z( t) - /( t = 01 , an d th e temperatu re ti are pl ot-

el on g ated by m o re th an 1 0 % of i ts ori g i n al l en g th 1 0. Re m o ve

ted ag ai n st th e ti m e as reg i stered , or taken fro m th e read i n g s.

th e test spe ci m e n from th e fu rn ace, al l ow it to coo l an d i n spect

Se l e ct so m e el on g ati on s Al an d assi g n th e respe cti ve i n i ti al

it for d evi tri fi cati on , stri ae, scratch e s, an d n e cki n g s. Dete rmi n e

l en g th I t. Take th e me an of th e temperatu re for th e rel ated ti me

on ce mo re th e l en g th as we l l as th e d i ameter an d i ts

i n terval At. Eval u ate th ese d ata as in 9. 3.

l on g i tu d i n al an d ci rcu mfere n ti al vari ati on s. Th e d i fferen ce be-

tween th e m a xi m u m an d mi n i mu m d i ameters sh al l n ot excee d

4 % of th e mean .
9. 5 Represen tati on of th e resu l ts; preci si on

Th e resu l ts co n si st of a n u mber of temperatu res an d th e rel ated

vi sco si ti e s, cal cu l ated accord i n g to 9. 3 or 9. 4. Th e vi sco si ty-

9 Expressi o n of resu l ts

temperatu re rel ati on sh i p an d th e temperatu re coeffi ci en t of th e

vi sco si ty are represen ted ( n u me ri cal l y or g raph i cal l y) accord i n g

to I S0 7884- l .
9. 1 Fi bre vo l u me

Th e preci si on is i n fl u en ced mai n l y by th e fol l owi n g i tems :

Th e i n crease in th e fi bre vo l u m e by th ermal expan si on n ever e x-

ce ed s 2 %. Wi th respe ct to th e preci si on of th e temperatu re

a) scatter of read i n g s;
measu re men t, th i s error in vo l u m e of th e fi bre can be

n eg l ected .

b) d evi ati on of th e parti cu l ar measu ri n g poi n ts fro m th e

fi tti n g cu rve;

9. 2 Correcti on of th e l oad
c) u n certai n ty of th e fi bre vo l u me , i n i ti al l en g th , correcti on

of th e l oad .
Wh e n th e l oad i n g mass is l e ss th an 4 g, correcti o n s sh al l be

mad e, to take i n to con si d erati on th e i n fl u en ce of th e d ead -

Erro rs sh ou l d be represen ted accord i n g to I S0 78941 .
wei g h t an d th e su rface ten si on of th e g l ass, u si n g eq u ati on s ( 5)

to ( 8) :

1 + ( Al l /, ) 1 0 Test report

q = 3 2 7 OOxAt x; x x m* . . . ( 5)

Al /l ,
Th e test report sh al l i n cl u d e :

wh ere
a) referen ce to th i s part of I S0 7884;

m* = m+ fQ- f. . . . ( 6)
b) d escri pti on of th e sampl e ;

fe = 0, 000 5 x @ x v . . . ( 7)
c) meth o d of sampl i n g ;

f, = 0, 0001 8 x o x . * . ( 8)
d) n u mbe r of test spe ci m e n s;

e) meth o d of preparati on ;
wh ere

f) test proced u re ( 8. 2 or 8. 3) ;

Q is th e d en si ty of th e g l ass, in g ram s per cu bi c cen -

ti metre;
g) ti me- temperatu re pro g ramme of th e me asu reme n t;

~7 is th e su rface ten si on of th e g l ass, in mi l l i n e wto n s

h) co rrecti on s appl i ed ;

per metre;

i) vi scosi ty- temperatu re rel ati on sh i p of th e test sam pl e as

II, At, I t, V an d Al are expl ai n ed in 5. 1 . d escri bed in I S0 7884- l ;

Wh e n th e val u e of th e su rface ten si on is u n kn own , e sti mate i ts j) an y ch an g e in th e g l ass, observed d u ri n g an d /or after

i n fl u en ce by pu tti n g cr = 300 m N /m . th e test.

7
I S0 78 8 4- 3 : 1 9 8 7 ( El

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 . )

P OOLE , J . P. I mpr o ve d appar atu s fo r me asu ri n g vi sco si ty of g l asse s in an n e al i n g ran g e of tempe ratu re . J. Ame r. Ce r am. So t. , 1 9 49

( Vol . 321 , pp. 21 5220.

ZI J LSTRA, A. L. Th e vi sco si ty of some si l i cate g l asse s in co n n e cti o n wi th th ermal h i sto ry. Ph ysi cs an d Ch e mi str y of G /asse s, Au g u st

1 963 ( Vol . 4, No. 41 , pp. 1 43 - 1 5 1 .

8
I S0 76 6 4- 3 : 1 9 6 7 ( E)

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

De scri ptors : g l ass, tests, vi sco si ty me asu reme n t, vi sco si ty.

Pri ce based on 8 pag es