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N21d
no. 1236

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National Research
Council Canada

Conseil national
de recherches Canada

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BLDG

EVALUATION OF TEST METHODS FOR ALKALI-AGGREGATE

REACTIVITY
*
NRC

by P.E. Grattan-Bellew

CISTI

BLDG. RES.
LIBRARY

84-

11- . O 6

BIBL~OTHZQUE
Reth. Bttim.
CNRC

Reprinted from
Danish Concrete Association
6th. International Conference
"Alkalis in Concrete: Research and Practice"
Technical University of Denmark
Copenhagen, 22-25 June 1983
Proceedings, p. 303 - 314

ICIST

DBR Paper No. 1236

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Les msthodes d ' e s s a i d e l a r h c t i o n a l c a l i - g r a n u l a t comprennent

celles q u i p e r m e t t e n t d e d'eterminer l a r ' e a c t i v i t ' e p o t e n t i e l l e
d'un g r a n u l a r ( l ' e s s a i chimique e t l a m6t hode p'et r o g r a p h i q u e
propos'ee
pour d'eterminer l ' a n g l e d ' e x t i n c t i o n o n d u l a t o i r e du
q u a r t z ) e t c e l l e s q u i v i s e n t 2 mesurer l ' e x p a n s i m d'un
g r a n u l a t d a n s l e b'eton (msthodes du prisme d e b'eton, du b a r r e a u
Plusieurs
d e mortier e t de l'gprouvette cylindrique).
m o d i f i c a t i o n s o n t 'et5 apport'ees B l a m'ethode chimique,
ASTM C289,
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ALKALIS IN CQMCRlETlE
Research and Practice
Paper reprinted from the
PROCEEDINGS

TECHNICAL UNIVERSITY of Denmark

COPENHAGEN J22.-25.
U N E - 1983

Editors: G. M. ldorn - Steen Rostam

EVALUATION OF TEST METHODS FOR ALKALI-AGGREGATE REACTIVITY

P.E. Grattan-Bellew
D i v i s i o n of B u i l d i n g Research, N a t i o n a l Research Council Canada
Ottawa, Canada K1A OR6
ABSTRACT
T e s t methods f o r a l k a l i - a g g r e g a t e r e a c t i v i t y c a n be d i v i d e d i n t o t h o s e t h a t
determine t h e p o t e n t i a l r e a c t i v i t y of an aggregate ( t h e chemical t e s t and t h e
proposed p e t r o g r a p h i c method f o r determining t h e undulatory e x t i n c t i o n a n g l e
of q u a r t z ) and t h o s e t h a t p u r p o r t t o measure t h e e x p a n s i 9 i t y of a n a g g r e g a t e
i n c o n c r e t e ( c o n c r e t e prism, mortar b a r , and rock c y l i n d e r methods).
Several
m o d i f i c a t i o n s have been developed f o r t h e chemical method, ASTM C289, t o t a k e
i n t o account r e g i o n a l v a r i a t i o n s i n aggregates. The main disadvantage of t h e
methods measuring expansion is t h a t they t a k e a long t i m e . To t r y t o overcome
t h i s problem, v a r i o u s methods of a c c e l e r a t i o n have been proposed, v a r y i n g from
immersion of t h e samples i n s a l t s o l u t i o n a t an e l e v a t e d temperature t o
autoclaving. Autoclaving methods must be regarded w i t h some c a u t i o n , however,
because a t e l e v a t e d temperatures and p r e s s u r e s hydrothermal r e a c t i o n s occur
t h a t do n o t t a k e p l a c e a t atmospheric pressure.
KEY WORDS:
1.

E v a l u a t i o n , T e s t s , A l k a l i , Aggregate.

INTRODUCTION

The i d e a l method of determining t h e p o t e n t i a l a l k a l i e x p a n s i v i t y of a n

aggregate i n c o n c r e t e should be a p p l i c a b l e t o a l l rock t y p e s , should be r a p i d ,
t a k i n g no more t h a n a few days t o complete, and must g i v e r e l i a b l e r e s u l t s .
The q u e s t f o r t h i s t e s t h a s k e p t a number of r e s e a r c h e r s busy f o r many y e a r s ,
b u t l i k e t h a t of t h e a l c h e m i s t s b e f o r e them i t w i l l n o t succeed. M v e r s i t y i n
t h e composition, g r a i n s i z e , and p o r o s i t y , and t h e presence o r absence of
secondary cementing m i n e r a l s i n r o c k s p r e d i c a t e s a g a i n s t t h e development of a
u n i v e r s a l l y a p p l i c a b l e , r a p i d t e s t method. Some t e s t s , f o r example t h e
c o n c r e t e prism method, a r e a p p l i c a b l e t o a l l rock t y p e s b u t may t a k e s o l o n g
t h a t t h e s t r u c t u r e w i l l be b u i l t b e f o r e t h e t e s t i s complete. Other tests,
l i k e t h e mortar b a r and t h e chemical methods, a r e s u i t a b l e f o r a g g r e g a t e s
e x h i b i t i n g c l a s s i c a l a l k a l i - s i l i c a r e a c t i v i t y but not f o r r e a c t i v e c a r b o n a t e
aggregates. A s a r e s u l t , a number of d i f f e r e n t t e s t methods have been, and
continue t o be, developed. This review w i l l examine t h e e f f e c t i v e n e s s and
l i m i t a t i o n s of e x i s t i n g and proposed t e s t methods.
2.

CHEMICAL TEST

The chemical method, ASTM C289 111, was developed a s a r a p i d means of

d i f f e r e n t i a t i n g between p o t e n t i a l l y r e a c t i v e and non-reactive s i l i c a - b e a r i n g
aggregates. The c r i t e r i a f o r e v a l u a t i o n were developed from t h e r e s u l t s of
p a r a l l e l s e t s of mortar b a r and chemical t e s t s on many a g g r e g a t e s from t h e
United S t a t e s 121. The r o c k s t e s t e d included some c o n t a i n i n g o p a l , c h e r t o r
chalcedony a s t h e r e a c t i v e component and o t h e r s i n which v o l c a n i c g l a s s was
t h e r e a c t i v e component. A s t h e two main r e a c t i v e components, o p a l and
v o l c a n i c g l a s s , c o n s i s t of c r y p t o c r y s t a l l i n e S i 0 2 and an a l u m i n o s i l i c a t e
g l a s s , r e s p e c t i v e l y , i t i s s u r p r i s i n g t h a t one s e t of c r i t e r i a were found t o
be a p p r o p r i a t e f o r e v a l u a t i o n of b o t h types.
The problem of o b t a i n i n g meaningful v a l u e s f o r t h e d i s s o l v e d s i l i c a (Sc) and
t h e r e d u c t i o n i n a l k a l i n i t y (Rc) a r e complicated i f c a r b o n a t e s o r s u l p h a t e s ,
e.g., gypsum 131, a r e p r e s e n t i n t h e a g g r e g a t e because t h e y r e a c t w i t h NaOH t o

reduce its a l k a l i n i t y . The v a l u e s of Sc and Rc a r e a l s o very s u s c e p t i b l e t o

o p e r a t o r influence. For example, i f t h e sample i s n o t properly s i z e d and a
s i g n i f i c a n t amount of -150 um m a t e r i a l is included i n t h e test, t h e value of
Sc w i l l be markedly increased.
Grinding q u a r t z t o s i z e s less t h a n about
100 u m g r e a t l y i n c r e a s e s i t s s o l u b i l i t y (Figure 1).
The phenolphthalein i n d i c a t o r does n o t g i v e a s h a r p end p o i n t and t h e v a l u e
of Rc determined is t h u s , t o some e x t e n t , dependent on t h e judgement of t h e
operator. Soaie of t h e p r o b l e m i n h e r e n t i n t h e chemical test were d i s c u s s e d
by Dent G l a s s e r and Kataoka 141. Their main conclusion i s t h a t t h e value of
Rc, as c u r r e n t l y determined, i s r a t h e r meaningless s i n c e i t i n c l u d e s
reductions i n both OH- and t h e c o n c e n t r a t i o n of ~ a i+n t h e s o l u t i o n . They
suggested t h a t t h e method should be a l t e r e d s o t h a t O H can be determined by a
pH meter and ~ a by
+ a s p e c t r o s c o p i c method.
The q u e s t i o n a r i s e s a s t o t h e need t o d e t e r d n e t h e reduced a l k a l i n i t y , Rc;
is determination of Sc alone s u f f i c i e n t f o r p r e d i c t i n g t h e p o t e n t i a l
r e a c t i v i t y of a n aggregate? To i n v e s t i g a t e t h i s , test r e s u l t s f o r a s e r i e s of
q u a r t z sands containing varying amounts of opal 121 were p l o t t e d i n Figure 2;
i t is e v i d e n t t h a t expansion of mortar b a r s c o r r e l a t e s b e t t e r w i t h t h e f a c t o r
Rc/Sc than with Sc alone, i n d i c a t i n g t h a t f o r t h e s e aggregates i t i s b e t t e r t o
determine both Rc and Sc.
I t has been e s t a b l i s h e d t h a t t h e c r i t e r i a given i n C289 a r e n o t adequate f o r
the e v a l u a t i o n of I c e l a n d i c sands containing volcanic g l a s s o r of Danish f l i n t
g r a v e l s , f o r which l o w v a l u e s of t h e amount of d i s s o l v e d s i l i c a are i n d i c a t i v e
of p o t e n t i a l r e a c t i v i t y .
New c r i t e r i a were developed f o r t h e i r e v a l u a t i o n a s
follows ( p e r s o n a l comnunication, Hakon Olaf sson) :
I c e l a n d i c sands:
non-reactive
Sc <I00 nsnol/L
Sc 100 t o 200 mmol/L
potentially reactive
reactive
Sc s200 mmol/L
Danish g r a v e l s :
non r e a c t i v e
Sc <50 mmol/L
potentially reactive
Sc 50 t o 200 mmol/~
Sc >200 mmol/L
reactive

I n c o n t r a s t , i n B r i t a i n t h e Thames Valley f l i n t g r a v e l s y i e l d e d v a l u e s of Sc
i n excess of 100 mmol/L y e t caused no problems i n concrete 131. It appears
t h a t s e p a r a t e s e t s of c r i t e r i a need t o be developed on a r e g i o n a l b a s i s , even
f o r e v a l u a t i o n of what a r e nominally t h e same rock types.
I n t h e late-expansive a g g r e g a t e s of t h e Malmesbury Formation i n t h e
Cape Peninsula of South Africa, i n which s t r a i n e d q u a r t z is t h e r e a c t i v e
component, t h e c r i t e r i a s p e c i f i e d i n C289 a r e e f f e c t i v e f o r d i f f e r e n t i a t i n g
r e a c t i v e and non-reactive aggregates; but i n t h e Tygerberg Formation from t h e
same r e g i o n lower v a l u e s of Sc were obtained from r e a c t i v e aggregates. The
r e s u l t s of the chemical t e s t on t h e s e aggregates, reported by Brandt,
It i s e v i d e n t t h a t t h e
Oberholster and Westra 151, a r e r e p l o t t e d i n F i g u r e 3.
d i v i d i n g l i n e between r e a c t i v e and non-reactive aggregates must l i e a t a value
of Sc between 35 and 50 nnnol/L.
I n S e r b i a t h e chemical method, ASTM G289, used by MitroviE and
~ u r i EI61 i n d i c a t e d t h a t t h e aggregates a r e p o t e n t i a l l y r e a c t i v e ( a s d i d t h e
mortar bar t e s t ) , although no problems have been observed i n concrete. There
a p p e a r s t o be some doubt concerning t h e v a l i d i t y of both methods f o r
e v a l u a t i n g t h e s e p a r t i c u l a r aggregates.
I n A u s t r a l i a , t h e c r i t e r i a s p e c i f i e d i n C289 a r e e v i d e n t l y s a t i s f a c t o r y ;
they have been adopted as an A u s t r a l i a n standard, AS 1141 Section 39, 1954.

2.1

Discussion

The c h e d c a l test i s t h e only rapid, currently a v a i l a b l e method, t h a t has

been thoroughly evaluated.
With some m d i f i r a t i o n of t h e c r i t e r i a used t o
d e f i n e r e a c t i v e aggregates, and i n co-njuaction w i t h a p e t r o g r a p h i c
examination, it can be used t o e v a l u a t e t h e p o t e n t i a l r e a c t i v i t y of a wide
range of s i l i c e o u s aggregates. Improvements might be made i n t h e a n a l y t i c a l
procedures s o t h a t t h e r e d u c t i o n s i n OH- and i n ~ a a+r e determined s e p a r a t e l y .
There is some evidence t h a t determination of d i s s o l v e d s i l i c a a l o n e i s
sufficient t o d i f f e r e n t i a t e between r e a c t i v e and non-reactive aggregates.
Owing t o t h e wide d i v e r s i t y i n the conpositlo-n g r a i n s i z e and p e r m e a b i l i t y of
rocks, it is most u n l i k e l y t h a t u n i v e r s a l l y a p p l i c a b l e c r i t e r i a can be
developed t o d i f f e r e n t i a t e between r e a c t i v e and non-reactive aggregates;
i n s t e a d , c r i t e r i a a p p l i c a b l e t o s p e c i f i e d rock t y p e s should be developed.
2.2

Modified chemical test

A d i f i e d c h e d c a l t e s t was developed f o r e v a l u a t i n g t h e p o t e n t i a l

r e a c t i v i t y of a g g r e g a t e s i n she Schleswig-lblstein region of Germany. The

1-2 mm and 2-4 mm.
These a r e
aggregate i s d i v i d e d i n t o two s i z e f r a c t i o n s :
The samples are washed, d r i e d ,
d i g e s t e d f n NaOH s o l u t i o n f o r 60 d n a t BO'C.
and weight l o s s determined; t h i s r e p r e s e n t s t h e amount of s i l i c a d i s s o l v e d o u t
and g i v e s , i n p r i n c i p l e , a measure of t h e p o t e n t i a l r e a c t i v i t y of t h e
by N&H
aggregate. The l i m i t a t i o n s of t h i s test have been d i s c u s s e d by Jensen,
C h a t t e r j i , Christensen, Thaulow and Gudmndsson 171. It would be a p p l i c a b l e
only t o a g g r e g a t e s c o n t a i n i n g r e a c t i v e silica, i.e., opal, c h e r t o r chalcedapy
and p o s s i b l y a l s o t o aggregate composed of v o l c a n i c g l a s s .
3.

MORTAR BAR METHOD

The mortar b a r t e s t , ASTM C227-8 / 8 / , i s t h e most widely used method of

e v a l u a t i n g t h e p o t e n t i a l a l k a l i - r e a c t i v i t y of aggregates. A number of
v a r i a t i o n s i n t h e method of e v a l u a t i n g t h e t e s t r e s u l t s a r e i n u s e by
d i f f e r e n t o r g a n i z a t i o n s . Despite t h e almost u n i v e r s a l acceptance of t h e
mortar bar method, i t h a s s e v e r a l shortcomings: It u s u a l l y t a k e s from s i x
months t o a y e a r t o complete, except w i t h some opal-bearing aggregates t h a t
c a n be e v a l u a t e d i n about t h r e e months. Such l o n g l e a d times f r e q u e n t l y do
not e x i s t before c o n s t r u c t i o n is s t a r t e d , even i n major s t r u c t u r e s f o r which
t h e d u r a b i l i t y of t h e c o n c r e t e i s of c r i t i c a l importance.
The e v a l u a t i o n of t h e r e a c t i v i t y of c o n c r e t e aggregate by t h e mortar b a r
method assumes t h a t expansion of concrete i n t h e f i e l d c o r r e l a t e s w i t h
expansion of test mortar bars. Although t h i s holds t r u e f o r some aggregates,
t h e r e a r e exceptions. The carbonate aggregate from Kingston, Ontario, f o r
example, shows much g r e a t e r expansion i n c o n c r e t e prisms than i n mortar b a r s ,
a s do late-expansive quartz-bearing aggregates such a s Malmesbury aggregate
from t h e Cape Peninsula i n South A f r i c a and a greywacke from Nova S c o t i a ,
Canada 191 ( s e e Figure 4, #73-50).
3.1

I n t e r p r e t a t i o n of observed expansion

Recommended c r i t e r i a f o r e v a l u a t i o n of t h e r e s u l t s of t h e mortar b a r t e s t
It must be s t r e s s e d t h a t
a r e given i n ASTM C33-82, Appendix XI.1.3 /lo/.
t h e s e a r e recommendations, n o t a mandatory p a r t of t h e standard. Although
they a r e f r e q u e n t l y i n t e r p r e t e d a s "limits," t h i s i s i n c o r r e c t .
According t o C33, expansions a r e t o be considered e x c e s s i v e i f they exceed
0.05% a t t h r e e months o r 0.10% a t s i x months; t h e three-month d a t a should only
be used, however, when a six-month t e s t i s n o t possible. The a l k a l i c o n t e n t
of t h e cement should be 0.6%, pr p r e f e r a b l y 0.8%. With t h e h i g h a l k a l i
cements now commonly i n use, an a l k a l i l e v e l of 1.0% o r g r e a t e r would be more

a p p r o p r i a t e . The problem w i t h t h e s e recommended maximum p e r m i s s i b l e

expansions i s t h a t they assume a f a s t r a t e of expansion w i t h a s h o r t
i n i t i a t i o n period. A slowly expanding aggregate may show mortar b a r
expansions w e l l below t h e v a l u e s considered t o be d e l e t e r i o u s , according t o
C33, but t h e continuing slow expansion w i l l e v e n t u a l l y l e a d t o e x c e s s i v e
s t r e s s and cracking.
A t y p i c a l example of expansion of a mortar b a r made w i t h Malmesbury
aggregate and a cement c o n t a i n i n g 0.82% a l k a l i i s shown i n Figure 5 ( p e r s o n a l
comnunication, R.E. O b e r h o l s t e r ) . T h i s a g g r e g a t e i s known t o cause
d e l e t e r i o u s expansion i n c o n c r e t e made w i t h a high a l k a l i cement. The problem
of e v a l u a t i n g t h e r e s u l t s of expansion of mortar b a r s made w i t h l a t e e x p a n s i v e
aggregates has a l s o been discussed by Kennerly e t a l . 1111 and by Sims 131.

3.2

Corps of Engineers

The Corps of Engineers c r i t e r i a f o r e v a l u a t i o n of t h z r e s u l t s of t h e mortar

bar t e s t a r e p o s s i b l y more a p p r o p r i a t e than t h o s e recommended i n C33.
EM 1110-2-2000 1121 s t a t e s t h a t expansion of 0.10% o r more a t any a g e should
be considered d e l e t e r i o u s . An expansion of 0.05% o r more a t s i x months may
a l s o be considered d e l e t e r i o u s . When expansions c l o s e t o t h e s e l i m i t s a r e
recorded, t h e t r e n d of t h e time-expansion curve should be taken i n t o account.
T h i s i s i n l i n e w i t h t h e concept of determining t h e r a t e of expansion proposed
by Grattan-Bellew 191. Cracking of mortar b a r s i s g e n e r a l l y observed when
expansion exceeds about 0.04%; i f c r a c k i n g i s accepted a s evidence of
d e l e t e r i o u s r e a c t i o n , expansions of l e s s than 0.10% must i n d i c a t e p o t e n t i a l
a l k a l i - a g g r e g a t e r e a c t i v i t y . The problem i s t h a t a t p r e s e n t n o t enough
information on t h e c o r r e l a t i o n between expansion of mortar b a r s and f i e l d
c o n c r e t e e x i s t s t o s e t r e a l i s t i c s a f e l i m i t s of expansion f o r mortar bars.
3.3

Canadian Standards Association

The Canadian s t a n d a r d (CAN3.A23.1-M77,

Appendix B3.4 1131) s t a t e s t h a t
expansions i n excess of 0.04% a t any age a r e t o be considered d e l e t e r i o u s .
It a l s o n o t e s t h a t t h e shape of t h e expansion curve i s o f t e n of importance i n
making a judgement.
The 0.04% l i m i t f o r expansion i s i n agreement w i t h
f r e q u e n t o b s e r v a t i o n s of c r a c k i n g when t h i s l e v e l of expansion i s exceeded;
t h e l i m i t may, however, be too r e s t r i c t i v e f o r some aggregates f o r which
expansion may j u s t exceed t h i s v a l u e and t h e n l e v e l o f f .
3.4

Accelerated Danish mortar b a r t e s t

T h i s t e s t , d e s c r i b e d by Jensen e t a l . 171, i s an a c c e l e r a t e d v e r s i o n of t h e
mortar bar method C227 and i s used f o r Danish f l i n t g r a v e l s . The mortar b a r s
a r e made i n t h e u s u a l way and cured i n a f o g room a t 23OC f o r 27 days. They
a r e then placed i n s a t u r a t e d NaCl s o l u t i o n a t 50C and expansion i s monitored
w i t h time. No l i m i t s have been proposed. T h i s method i s r e p o r t e d t o be
s a t i s f a c t o r y f o r t h e aggregates t e s t e d i n Denmark, but t h e r e a r e no r e p o r t s of
i t s use elsewhere.
3.5

Chinese autoclaved mortar bar t e s t

T h i s i s a n o t h e r a c c e l e r a t e d mortar b a r t e s t . Mortar b a r s 1 x 1 x 4 cm a r e
prepared and cured f o r one day i n a fog room. Following t h i s , they a r e steam
cured a t 100C f o r 4 h and then immersed i n 10% KOH s o l u t i o n and autoclaved a t
150C f o r 6 h. Expansions a r e recorded a f t e r each phase of t h e c u r i n g cycle.
A l a r g e number of a l k a l i - s i l i c a r e a c t i v e a g g r e g a t e s were t e s t e d i n t h i s way by
Ming-shu, Su-fen and Shi-hua 1141, who concluded t h a t t h e method i s capable of
d i f f e r e n t i a t i n g between r e a c t i v e and non-reactive aggregates. More t e s t i n g
should be c a r r i e d out t o e v a l u a t e i t s e f f e c t i v e n e s s f o r a wider v a r i e t y of
rock types. Hydrothermal t e s t s must, however, be regarded w i t h some c a u t i o n

because of the possibility that the observed expansion might be distorted by

hydrothermally induced reactions that would not occur in concrete under normal
conditions.
3.6

Discussion

No firm limit of expansion can be specified that is applicable to all rock

types. Cracking of mortar bars is frequently observed when expansion exceeds
about 0.04%, and this value might be considered indicative of potentially
deleterious expansion. In some cases, however, this could result in
classification of some aggregates that perform satisfactorily in concrete as
deleterious. It would be desirable to have a time limit for the mortar bar
test; owing, however, to wide divergences in initiation periods and in rates
of expansion it is not possible to establish a universally applicable time
limit. It is possible that regionally applicable time-expansion limits such
as those proposed in C33 may be established for some suites of aggregates.
Accelerated tests have so far not been evaluated for a wide enough range of
aggregates to permit conclusions to be drawn as to their applicability.
4.

CONCRETE PRISM TEST

The concrete prism test (CSA A23.2-14A 1151) was developed in Canada for
evaluating the expansivity of reactive dolomitic limestones that do not cause
significant expansion in mortar bars. The test has also been used successfully for late-expansive siliceous aggregates and limestones containing
reactive silica. Similar tests have been used in New Zealand and
South Africa. The criteria for evaluation of the test results are specified
in CSA A23.1.M77, Appendix B3.5. Linear expansions of more than about 0.03%
indicate potentially deleterious expansion. Appendix 3.5 concludes that some
aggregates expand beyond the three-month period and that, where possible, the
test should be continued until expansion has virtually ceased. This is sound
advice, but it may often not be practical since with some late-expansive
aggregates it may take up to two years for expansion to taper off.
The use
of the rate method of evaluating expansivity of aggregates 191 may help in
evaluating the expansivity of concrete prisms before expansion tapers off.
It is very desirable to carry out a petrographic examination in conjunction
with the concrete prism test so that the type of reactivity to be expected can
be determined; this helps in the correct evaluation of early test results if
it is not possible to wait until the expansion has tapered off.
The concrete prism method may be the most reliable test for all types of
aggregate. In it, the aggregate is tested in the same size range and with the
same cement:aggregate ratio that is used in field concrete. For some l a t e
expansive siliceous aggregates and for carbonate reactive aggregates such as
those from Kingston, Ontario, the concrete prism test is the only satisfactory
method since these aggregates do not cause significant expansion in mortar
bars. Expansion can be significantly accelerated by storage of the prisms at
38C and 100% RH instead of at 23C as specified. A few preliminary
experiments to try and accelerate expansion by immersion of the prisms in NaCl
solution, after the method of the Danish accelerated mortar bar test, were not
very successful, but more research is needed before any firm conclusions can
be drawn.

5.

CONCRETE CUBE TEST

This test was developed in Germany 1161, and cracking is the criterion used
to determine whether a cement-aggregate combination is reactive. There are
two versions of it. In the first, 30-cm cubes are made and expansion is

Other exposure c o n d i t i o n s a r e
a c c e l e r a t e d by s t o r a g e i n a f o g room a t 40%.
a l s o used, f o r example, s t o r a g e on t h e roof of t h e r e s e a r c h l a b o r a t o r y .
I n t h e second v e r s i o n of t h e test, 10-cm cubes a r e s t o r e d a t 65% RH, with t h e
bottom 1 c m immersed i n water a t 20C. I n some samples c o n t a i n i n g r e a c t i v e
a g g r e g a t e marked c r a c k i n g was observed j u s t above t h e w a t e r l i n e .
I n B r i t a i n , a t t h e Cement and Concrete Association, a modified v e r s i o n of
the 10-cm cube t e s t is being i n v e s t i g a t e d (D.W. Hobbs, personal communicat i o n ) . Cubes a r e immersed i n a water b a t h a t 23'C and crack formation i s
observed. A temperature of 23'C i s reported t o be t h e optimum f o r s o l u b i l i t y
of s i l i c a .

I
I

I n South A f r i c a , 30-cm cubes a r e used a t outdoor exposure s i t e s where they

may be submitted t o v a r i o u s moisture and weather exposure conditions.
T e s t s involving t h e o b s e r v a t i o n of cracking have a major advantage over
tests r e q u i r i n g a c c c u r a t e measurement of l e n g t h change i n t h a t no e l a b o r a t e
This means t h a t t h e c o n c r e t e cube t e s t could r e a d i l y
a p p a r a t u s i s required.
be c a r r i e d o u t by p i t , quarry o r ready-mix operators. The disadvantage i s
t h a t u n l e s s r a p i d l y expanding aggregates a r e being e v a l u a t e d i t would t a k e a n
unacceptably long time f o r v i s i b l e cracks t o develop. From l a b o r a t o r y
o b s e r v a t i o n s by t h e a u t h o r i t is known t h a t a c o n s i d e r a b l e amount of expansion
can f r e q u e n t l y be observed before cracks become v i s i b l e t o t h e unaided eye.
6.

ROCK CYLINDER METHOD

The rock c y l i n d e r method (ASTM C586-69 1171) was designed t o e v a l u a t e t h e

p o t e n t i a l r e a c t i v i t y of a l k a l i r e a c t i v e carbonate aggregates, but it has a l s o
been used w i t h varying degrees of success t o e v a l u a t e t h e r e a c t i v i t y of
a l k a l i - s i l i c a r e a c t i v e aggregates /5, 10, 18, 191. Paragraph 9.3 of C586
s t a t e s t h a t expansive behaviour of aggregate (carbonate) i n c o n c r e t e i s
q u a l i t a t i v e l y p r e d i c t e d by t h e r e s u l t s of t h e rock c y l i n d e r t e s t .
Grattan-Bellew 1191 found moderate c o r r e l a t i o n between expansion of c o n c r e t e
made with s i x samples of Kingston aggregate and expansion of miniature rock
prisms made w i t h t h e same aggregates. Much poorer c o r r e l a t i o n was observed
f o r expansion of c o n c r e t e prisms and t h a t of miniature rock prisms made with
late-expanding s i l i c e o u s aggregates. Kennerley e t a l . 1111 found t h a t some
prisms of New Zealand greywacke expanded e x c e s s i v e l y i n NaOH, but t h a t t h e
same rock caused no expansion i n concrete.
It is concluded t h a t t h e rock c y l i n d e r t e s t , o r v a r i a t i o n s of i t , can only
be used t o e v a l u a t e t h e r e a c t i v i t y of c e r t a i n rock types. Its optimum u s e
would probably be f o r e v a l u a t i n g t h e p o t e n t i a l e x p a n s i v i t y of i n d i v i d u a l horizons i n a quarry containing a rock type f o r which c o r r e l a t i o n of expansion of
rock c y l i n d e r s and t h a t of c o n c r e t e prisms has previously been demonstrated.

6.1

Accelerated rock prism test

An a c c e l e r a t e d rock prism t e s t f o r e v a l u a t i o n of t h e p o t e n t i a l r e a c t i v i t y of
carbonate aggregates has been developed by Kazimir 1201 and adopted a s
Czechoslovakian s t a n d a r d CSM 72 1160. Rock prisms 1 x 1 x 3 cm a r e prepared
and autoclaved i n NaOH s o l u t i o n a t 215OC and 2.1 MPa f o r 6 h. This t e s t i s
r e p o r t e d t o be s u c c e s s f u l i n d i f f e r e n t i a t i n g between expansive and nonexpansive carbonate aggregates. Some r e s e a r c h was conducted by t h e author on
t h e a p p l i c a b i l i t y of t h i s t e s t t o late- expanding s i l i c e o u s aggregates, but i t
was discontinued a f t e r a f e l d s p a r - l i k e phase was found t o have formed i n t h e
prisms. Expansions occurred, but a s r e a c t i o n s were t a k i n g p l a c e ( t h e s e do n o t
occur a t one atmosphere) i t seemed most u n l i k e l y t h a t t h e observed expansions
would c o r r e l a t e w i t h expansions of t h e same prisms under atmospheric
conditions. More r e s e a r c h should probably be done a t various temperatures and
p r e s s u r e s t o see whether an a c c e l e r a t e d t e s t could be developed f o r l a t e expansive s i l i c e o u s aggregates.

308

7.

GEL PAT TEST

This test was developed in England as a rapid method of identifying

potentially deleterious minerals such as opal or chert in mortar samples.
It does not give any indication of the expansivity of the aggregate.
As reported by Sims 131, a smoothed, sawn surface of the mortar is prepared
and immersed face down in alkali for three days. Gel forms on the reactive
particles, which can thus be readily identified and counted to yield a measure
of the percentage of reactive component in the aggregate.
A somewhat similar test, CSN 72-1162 1211, is used in Czechoslovakia to
accelerate rim development around prisms of siliceous aggregates embedded in
mortar. It is useful for preliminary screening of potentially alkali-silica
reactive aggregates, but additional tests would be necessary to obtain a
measure of the expansivity of the aggregate in concrete.
8.

PETROGRAPHIC EXAMINATION

Petrographic examination, ANSIIASTM C595 1221, has been changed from a

technique for determining the mineralogical composition of a rock to a
semi-quantitative method of determining the potential reactivity of certain
rock types by Dolar-Mantuani's development of a technique for determining the
undulatory extinction angle, UE, and relating it to the expansivity of
aggregate 1231. Following on earlier work 124-261, describing the development
of the technique for measuring strain in the quartz lattice by means of the
undulatory extinction angle, Dolar-Mantuani suggested that aggregates with
undulatory extinction angles of less than 15 deg may be characteristic*
nowreactive aggregates.
Recent unpublished results obtained by the present author show that some
South African aggregates (a quartzite from the Witwatersrand, a greywacke, and
a spotted slate from the Malmesbury Formation in the Cape Peninsula, all of
which cause excessive expansion in concrete) have UE angles of 36, 36 and
43 deg, respectively, indicating that there is some correlation between high
UE angle and the reactivity of the aggregates. More research into this method
should be carried out. It has great potential as a rapid method of evaluating
the potential reactivity of quartz-bearing aggregates, particularly the lateexpansive types common in Precambrian terrains. It would be useful to conduct
a series of interlaboratory measurements of UE angles on reference samples so
that participants could adjust their measuring techniques to ensure results
consistent with those of other operators. In a limited test carried out in
Ottawa, a variation of 10 deg was found among measurements made by three
participants on the same quartz grains in a thin section. Such a wide
variation may have resulted because one or more of the participants measured
the extinction range, ER, rather than the undulatory extinction angle, UE, as
defined by DolarMantuani.
8.1

Use of scanning electron microscope

Use of the scanning electron microscope (SEM) to extend the scope of the
petrographic method by permitting characterization of texture and composition
of fine argillaceous rocks may, in due course, make it possible to distinguish
between expansive and non-expansive horizons in a particular deposit.
Figure 6 shows micrographs of two rocks from the Pittsbury quarry near
Kingston, Ontario. Figure 6a shows the highly expansive dolomitic limestone
characterized by isolated dolomite rhombs in a matrix of calcite; Figure 6b
shows a dolostone, which is non-expansive. This sample is composed almost
entirely of a more coarse grained dolomite. Electron probe analysis showed
that the Ca/Mg count rate ratio was different in the two samples
(6a: Ca/Mg = 3.6;
6b: Ca/Mg = 3.01, indicating a higher percentage of Ca

i n t h e r e a c t i v e dolomite; i t i s , t h e r e f o r e , a m e t a s t a b l e protodolomite 1271.

The SEM h a s one g r e a t advantage over o t h e r techniques, (e.g., p e t r o g r a p h i c
microscopy), t h a t i s , t h e speed w i t h which o b s e r v a t i o n and a n a l y s i s can be
done; i n about h a l f a n hour a c h i p of rock can be coated, examined, and
analysed by an expqrienced o p e r a t o r .
9.

CONCLUSION

There i s a d e f i n i t e t r e n d towards m o d i f i c a t i o n of t h e s t a n d a r d ASTM t e s t s

f o r use i n c e r t a i n r e g i o n s and f o r s p e c i f i e d types of aggregate. This h a s
come about a s a r e s u l t of inadequacies i n t h e s t a n d a r d t e s t methods, e i t h e r
because they f a i l t o p r e d i c t c o r r e c t l y t h e r e a c t i v i t y of an aggregate o r
because t h e t e s t t a k e s t o o long t o complete. The t e s t methods have been
modified i n two ways: expansion h a s been a c c c e l e r a t e d , a s i n t h e Chinese
autoclaved mortar b a r t e s t ; t h e c r i t e r i a f o r t h e chemical t e s t , a s
recommended, have been modified t o p r e d i c t t h e r e a c t i v i t y of l o c a l a g g r e g a t e s
more a c c u r a t e l y , a s i n I c e l a n d and Denmark where s p e c i f i c l i m i t s on t h e
d i s s o l v e d s i l i c a have been proposed.
Modified c r i t e r i a f o r e x i s t i n g t e s t methods may be l i m i t e d t o s p e c i f i e d
aggregates i n c e r t a i n regions. For example, t h e proposed Danish c r i t e r i a f o r
e v a l u a t i n g t h e r e s u l t s of t h e chemical t e s t of f l i n t a g g r e g a t e s , t h a t
Sc values between 50 and 200 mmol/L a r e i n d i c a t i v e of p o t e n t i a l r e a c t i v i t y ,
would be q u i t e u n s u i t e d f o r t h e e v a l u a t i o n of Thames Valley f l i n t s , which a r e
non-expansive i n c o n c r e t e d e s p i t e having Sc v a l u e s i n excess of
100 mmol/L.
There i s s t i l l a g r e a t need f o r b e t t e r , more r a p i d methods of diagnosing
p o t e n t i a l l y r e a c t i v e aggregates. For reasons a l r e a d y o u t l i n e d t h e new t e s t s
w i l l probably be developed f o r t h e e v a l u a t i o n of c e r t a i n a g g r e g a t e s i n
s p e c i f i c regions. The most promising f o r f u t u r e development a r e t h e chemical
method, i n conjunction w i t h improvements i n techniques f o r p e t r o g r a p h i c
e v a l u a t i o n , and p o s s i b l y some type of a u t o c l a v e a c c e l e r a t i o n f o r mortar o r
c o n c r e t e expansion t e s t s .
Acknowledgement
The a u t h o r i s indebted t o P.J. Lefebvre f o r h i s enthusiasm f o r t h e work and
t h e p r e c i s i o n w i t h which he c a r r i e d o u t t h e experiments r e p o r t e d i n t h i s
paper. T h i s i s a c o n t r i b u t i o n from t h e D i v i s i o n of B u i l d i n g Research,
National Research Council Canada, and i s published w i t h t h e approval of t h e
D i r e c t o r of t h e Division.
References

/1/

/2/

/3/
/4/

ASTM C289-81, P o t e n t i a l R e a c t i v i t y of Aggregates (Chemical Method),

Annual Book of ASTM Standards, P a r t 14, Concrete and Mineral Aggregates.
American S o c i e t y f o r T e s t i n g and M a t e r i a l s , 1916 Race S t . , P h i l a d e l p h i a ,
PA 19103, U.S.A.,
1982, 198-205.
MIELENZ , R.C., GREENE, K.T and BENTON, E .J , Chemical T e s t f o r
R e a c t i v i t y of Aggregates w i t h Cement A l k a l i s ; Chemical Processes i n
Cement-Aggregate Reaction. J o u r n a l of t h e American Concrete I n s t i t u t e ,
19(3), 1947, 193-221.
EMS,
I., The A p p l i c a t i o n and R e l i a b i l i t y of Standard T e s t i n g Procedures
f o r Potential Alkali Reactivity.
Proc., 5 t h I n t e r n a t i o n a l Conference on
Alkali-Aggregate Reaction, Cape Town, S252/ 13, 1981, 12 p.
DENT GLASSER, L.S. and KATAOKA, N., Some Observations on t h e Rapid
Cement and Concrete
Chemical T e s t f o r P o t e n t i a l l y R e a c t i v e Aggregate.
Research, 11, 1981, 191-196.

/5/ BRANDT, M.P., OBERHOLSTER, R.E. and WESTRA, W.B., A Contribution to the
Determination of the Potential Alkali Reactivity of Tygerberg Formation
Aggregates. Proc., 5th International Conference on Alkali-Aggregate
Reaction, Cape Town, S,252/11, 1981, 6 p.
I61 MITROVIC, N. and DUCIC, V., Prilog, Zbornik, 1 MK-a, 10, 1981, 195-204.
/7/ JENSEN, A.D., CHATTERJI, S., CHRISTENSEN, P., THAULOW, N. and
GUDMUNDSSON, H., Studies of Alkali-Silica Reaction - Part 1, A Comparison
of Two Accelerated Methods. Cement and Concrete Research, 12, 1982,
641-647.
I81 ASTM C227-81, Potential Alkali Reactivity of Cement-Aggregate
Combinations (Mortar Bar Method).
Annual Book of ASTM Standards,
Part 14. American Society for Testing and Materials, 1916 Race Street,
Philadelphia, PA 19103, U.S.A., 153-158.
/9/ GRATTAN-BELLEW, P.E., A Review of Test Methods for Alkali Expansivity of
Concrete Aggregates. Proc., 5th International Conference on
Alkali-Aggregate Reaction, Cape Town, S25219, 1981, 12 p.
1101 ASTM C33-82, Appendix XI. Methods for Evaluating Potential Reactivity of
an Aggregate (Para. 1.2, Method C289). Annual Book of ASTM Standards,
Part 14. American Society for Testing and Materials, 1916 Race Street,
Philadelphia, PA 19103, U.S.A.,
13-22.
1111 KENNERLEY, R.A., ST. JOHN, D.A. and SMITH, L.M., A Review of Thirty Years
of Investigation of the Alkali-Aggregate Reaction in New Zealand.
Proc., 5th International Conference on Alkali-Aggregate Reaction,
Cape Town, S252112, 1981, 9 p.
1121 ENGINEER MANUAL EM 1110-2-2000, Engineering and Design Standard Practice
for Concrete, (Appendix B, 3C).
Department of the Army, Office of the
Chief of Engineers, Washington, D.C. 20314, 1971.
1131 CSA CAN3-A23.1-M77, Appendix B3, Tests for Alkali-Aggregate Reactivity
(3.4, ASTM Standard C227, Potential Alkali Reactivity of Cement-Aggregate
Combinations (mortar bar method).
3.5, CSA Test Method A23.2-14A,
Alkali-Aggregate Reaction, National Standard of Canada) : CAN3 AZ3.2-7 7,
Concrete Materials and Methods of Concrete Construction, Methods of Test
for Concrete. Canadian Standards Association, Rexdale Boulevard,
Rexdale, Ontario, Canada, 1977, 122-123.
1141 MING-SHU, Tang, SU-FEN, Han, and SHI-HUA, Zhen, A Rapid Method for
Identification of Alkali Reactivity of Aggregate. Cement and Concrete
1983, 417-422.
Research, 2,
1151 CSA A23.2-14A, Alkali-Aggregate Reaction (Concrete Prism Test).
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Standards of Canada, CAN3 A23.1-M77, CAN3 A23.2-M77, Concrete Materials
and Methods of Concrete Construction. Methods of Test for Concrete.
Canadian Standards Association, Rexdale Boulevard, Rexdale, Ontario,
Canada, 1977, p. 183-185.
1161 BONZEL, Von J. and DAHMS, J. , Alkalireaktion im Beton, Herstellung
Verwendung 23, 11, S4951500 und H.12, S5971554, 1973.
1171 ASTM C586-69, Standard Test Method for Potential Alkali Reactivity of
Carbonate Rocks for Concrete Aggregates (Rock Cylinder Method). Annual
Book of ASTM Standards, Part 14, Concrete and Mineral Aggregates.
American Society for Testing and Materials, 1916 Race Street,
Philadelphia, PA 19103, U.S.A., 1982, 357-360.
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Cement and Concrete Research, 2, 1973, 55-70.
I191 GRATTAN-BELLEW, P.E., Evaluation of Miniature Rock Prism Test for
Determining the Potential Alkali-Expansivity of Aggregates. Cement and
Concrete Research, 11,1981, 699-711.
1201 KAZIMIR, J., MoZnosE Skratenia Sk613ky Rozpinania Dolomitovy'ch ~ornl'ns
Alkaliami, Staveb. Cas. 25, c s. Veda Bratislava, 1977, 413-432.

1211 CSN 72 1162, Stanovenie Odolnostri Prirodnc$ho ~tavebnkhoI9me6a Proti

~ilicifikich. MDT 691.2.620.1 679.682.1, Ceskoslovenskti Stgtna Norma
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Part 14, Concrete and Mineral Aggregates. American Society for Testing
and Materials, 1916 Race Street, Philadelphia, PA 19103, U.S.A., 1982
218-229.
1231 DOLAR-MANTUANI, L.M.M., Undulatory Extinction in Quartz Used for
Identifying Potentially Alkali-Reactive Rocks. Proc., 5th International
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Some Chilean Granitic Rocks of Different Ages. Geological Society of
America, Bulletin 75, 1964, 363-366.
1251 DOLAR-MANTUANI, L.M.M.. Petrographic Aspects on Siliceous Alkali-Reactive
Aggregates. P;OC., ~ ~ ~ ~ o s i u m - o n ~ ~ l k a l iReaction,
~ ~ ~ ~ r eReykjavik,
~ate
1975. p. 87-100.
1261 M A ~ R ;K., Presentation at Symposium on Alkali-Aggregate Reactivity.
Annual Meeting of Transportation Research Board, Washington, D.C., 1976.
/27/ SWENSON, E .G. and GILLOTT, J.E , Alkali-Carbonate Rock Reaction. Highway
Research Record, No. 45, 1964, 21-40.

1000

-1

300

=-

-b

500

aoa 60 -

\'

30
15-

m 200 "

4 0' 0

"6 0 0 "

MEAN G R A l N S 1ZE,

800

L
,L

1000

F i g u r e 1 E f f e c t of g r a i n s i z e of q u a r t z on the a o u a t af d i s s o l v e d s i l i c a
determined by t h e chemical method, ASTM C289

12

16

24

20

% OPAL I N QUARTZ S A N D

Figure 2

P l o t showing v a r i a t i o n i n Sc and Rc/Sc determined by t h e chemical

t e s t , ASTM C289, and l e n g t h change of m o r t a r b a r s of q u a r t z sand
c o n t a i n i n g v a r i o u s amounts of o p a l

250

200

150

100

INNOCUOUS

DELETERIOUS

DISSOLVED SILICA Sc, mmolll

Figure 3

R e s u l t s of chemical t e s t , ASTM C289, f o r s o w r e a c t i v e and nonr e a c t i v e South A f r i c a n aggregates. Non-reactive:

No ( n o r i t e ) and
WS ( q u a r t z sand)

313

.-

- .

..

- . .. Y e ?-- . -;
-...-. ...
-

.:

=-

-5-

..-

The Fare Bridges

Construction site visited during the Conference Excursion
Trykt I Vejdlrektoratet
K~benhavn

T h i s paper, w h i l e being d i s t r i b u t e d i n
r e p r i n t form by t h e D i v i s i o n of B u i l d i n g
Research, remains t h e c o p y r i g h t of t h e
o r i g i n a l publisher.
It should n o t be
reproduced i n whole o r i n p a r t w i t h o u t t h e
p e r m i s s i o n of t h e p u b l i s h e r .
A l i s t of a l l p u b l i c a t i o n s a v a i l a b l e from
t h e D i v i s i o n may be o b t a i n e d by w r i t i n g t o
t h e P u b l i c a t i o n s S e c t i o n , D i v i s i o n of
Building Research,
National Research
C o u n c i l of
Canada,
Ottawa,
Ontario,
KIA 0R6.