CEMENT and CONCRETERESEARCH. Vol. l ] , pp. 395-406, Ig81.

Printed in the USA

0008-8846/81/030395-12502.00/0 Copyright (c) 1981 Pergamon Press, Ltd.

DIFFUSION OF CHLORIDE IONS IN HARDENED CEMENT PASTES

C.L. Page, N.R. Short and A. E1 Tarras

Department of Construction and Environmental Health
University of Aston, Birmingham, England

(Communicated by A.J. Majumdar)

(Received Jan. 13, 1981)

ABSTRACT
Kinetics of diffusion of chloride ions in hardened cement
pastes have been investigated. For Portland cement pastes
of fixed type, made with various water-cement ratios (w/c),
activation energies for the diffusion process have been
measured and the results have been related to the pore
structures of the materials. The influence of certain
other factors, including the curing conditions~ the
presence in the samples of interfacial zones of segregation
and the use of several other types of cement, have also
been examined.

La cin4tique de diffusion des ions de chlorure darts les p~tes

durcies de ciment a 4~4 Etudi4e. On a mesurE, pour des
pates de ciment Portland d'un type constant prEparEes en
utilisant diverses proportions eau-ciment, les Energies
d'activation des processus de la diffusion. Les rEsultats
ont 4tE discutEs en termes de structures des pores des
mat~riaux. Les effets de quelques considerations, qui
comprennent le r4gime de traiter les p~tes, l'existence dans
les Echantillons de zones interfaciales de sEgr4gation et
l'emploi de ciments de plusieurs autres types, ont 4t4
examin4s aussi.
Introduction
The diffusion of chloride ions in hardened concrete is widely recognised
as being of importance in relation to the corrosion of reinforcing bars.
It is significant as a process by which chlorides from external sources
penetrate normal thicknesses of concrete cover in the cases of structures
exposed to seawater (i) or deicing salts (2,3). More generally, whenever
chloride ions are present in concrete, their influence on passivity and
anodic dissolution of embedded metals must depend on their mobility in
the vicinity of the metal~concrete interface (4,5), ionic mobility being
lifted to diffusivity by the Nernst-Einstein relationship (6).
The work to be described in this paper represents the initial phase of a
continuing study of the effects of cement matrix variables on diffusion of

395
396 Vol. I I , No. 3
C.L. Page, et al.

chloride ions in concrete. Its principal aims were to establish a

convenient technique for study of chloride diffusion kinetics in mature
cement pastes and to elucidate the effects on diffusion of the following
factors:
(i) w/c and temperature for specimens of constant cement composition,
(ii) curing conditions and interfacial segregation for specimens of fixed
cement composition and w/c at constant temperature,
(iii) variations in cement composition for specimens of fixed w/c at
constant temperature.
Experimental
The work was conducted in three series of experiments, the scope of which
corresponded with the factors outlined previously.
Throughout series (i) and (ii), the cement used was a variety of Ordinary
Portland Cement (OPC), whilst for series (iii) Sulphate Resisting Portland
Cement (SRPC) was used and blended cements were prepared from OPC and 65%
ground granulated blast furnace slag (BFS) or 30% pulverised fuel ash (PFA).
The compositions of the various materials, expressed in percentages by
weight of the constituent oxides, are shown in Table i.
TABLE 1
Chemical Analyses

Material CaO SiO 2 AI203 Fe203 SO 3 MgO Na20 K20 Ign~tionboss

OPC 63.0 20.3 7.1 2.7 3.3 1.3 0.47 0.60 0.8
SRPC 64.0 20.2 4.1 5.3 2.6 1.4 0.28 0.39 l.l
BFS 42.37 33.30 10.77 0.33 8.74 0.37 0.50 -
PFA 2.9 46.6 24 .O 9.5 0.9 2.1 2.0 3.8 3.3
Samples of cement pastes were made up with distilled water to desired w/c in
the range 0.4 to 0.6. After being mixed thoroughly they were cast into
cylindrical PVC moulds, 4.9mm diameter x 75mm length, and compacted by means
of vibration. The completely filled moulds were tightly sealed and subjected
to continuous rotation at 8rpm about a horizontal axis; this served to prevent
significant segregation within the pastes whilst their condition remained fluid.
For series (i) and (iii) experiments, the specimens were demoulded after 48
o
hours and cured under saturated Ca(OH) 2 solution at 22 C for 60±3 days. As a
non-destructive measure of quality, ul~ra-sonic pulse velocity (UPV)
determinations were then made along the axis of every cylinder. The values
obtained are recorded in Table 2.

TABLE 2
UPV Determinations
Cement w/c UPV (km s -1)
OPC 0.4 3.66±0.05
OPC 0.5 3.40±0.05
OPC 0.6 3.17±O.O3
OPC/30% PFA 0.5 3.18±O.01
OPC/65% BFS 0.5 3.31±O.01
SRPC 0.5 3.17±O.O5
From the central regions of each of the cylinders at least four, but normally
five or six, circular discs of convenient thickness (~3mm) for subsequent study
were cut by means of a diamond saw, the blade of which was lubricated with
distilled water. The surfaces of the discs were then lightly ground on
Grade 600 emery paper, rinsed with distilled water and dried with lens
tissue before being fitted into diffusion cells of the type shown in Fig.l.
Vol. I I , No. 3 397
CHLORIDE, DIFFUSION, CEMENT PASTES, WATERCONTENT, CURING

CEMENT PASTE DISC

Fig. 1

Diffusion Cell

I M NmCI In SATURATED Ca(OH)=

SATURATEDC~OH~

For series (ii) experiments, OPC pastes of w/c 0.5 were cast into PVC moulds
fitted with flat PTFE base-plates. They were compacted and rotated for 48
hours as described previously, but thereafter the pastes were allowed to remain
o
in their moulds and were stored for 60 days at 22 C in saturated alr. At the
end of this period of curing, the specimens were demoulded and discs, 3mm thick,
were cut both from the central regions of the cylinders and from the ends which
had been separated from the PTFE plates. The cut surfaces were lightly ground,
washed and dried in the usual way before the discs were mounted in diffusion
cells; the 'as-cast' interfaces were then in contact with compartment 2 of the
cells.
The experimental arrangements under which diffusion of chloride ions was
studied are depicted fully in Fig. i. For every set of conditions examined,
four to six replicate cells were placed in a water bath, the temperature of
which was adjusted to values within the range 7 to 47°C for series (i)
experiments and fixed at 25°C for series (ii) and (iii) experiments. The
concentrations of chloride ion in compartment 2 of the cells after various
diffusion times were determined by withdrawing IOOul aliquots of the solutions
and analysing them by a standard spectrophotometric technique ( 7 ) . Samples
were tested in this way over a period of up to 3 weeks, depending on the rate
of diffusion. Their combined volume was negligible in comparison with the
total volume of solution in compartment 2 of the cells and so no
corrections for errors arising from this source were required in subsequent
calculations.
On completion of each set of diffusion measurements, the thicknesses of the
discs of cement pastes were determined by means of a micrometer gauge.
Specimens were then dried in vacuo and subjected to differential thermal
analysis (DTA) or dried in an oven at iO5°C and subjected to mercury
intrusion porosimetry (MIP). The results were compared with data obtained
for similarly cured cement pastes which had not been exposed to the effects
of chloride diffusion. In all cases, the MIP results showed that no
significant alterations in pore structure had occurred during the diffusion
periods. Certain changes in the DTA traces were, however, recorded and
these will be referred to in subsequent discussion.
Results and Discussion
A typical set of results from a diffusion experiment is shown in Fig.2.
After an initial delay ( t ) , during which chloride diffusion becomes
established across the thickness of the disc, there is a linear increase with
time in the chloride concentration (C 2) of the solution in compartment 2 of
398 Vol. I I , No. 3
C.L. Page, et al.

14 I I I I l I I

DISC T M I C K N E S S
- 12 • 301 mm
• 313ram

E
E ~o
G

I I J I
2 4 6 10 12
11M| t ~ x lOJ|

Fig. 2
Chloride diffusion through OPC paste of w/c 0.4 at 25°C

the cell, the concentration (CI) in compartment 1 remaining effectively

constant over the period of measurements. This is consistent with conditions
of quasi-steady-state diffusion across the disc and implies that the flux
through all sections normal to the diffusion direction is constant and that
the activity of chloride ion is effectively unchanging at all points in the
disc.
-2 -i
The flux (J) in mole cm s of chloride ion entering compartment 2 is
then given by:

j = Z dC 2 = £ (~-Cl-C
2-
A 1
dt
wh~relD is the effective diffusivity of chloride ion through the disc in
cm s (assumed to be independent of concentration), V is the volume of
3 2
solution in compartment 2 in cm , A is the cross-sectional area in cm , 1 is
the thickness of the disc in cm and C 1 and C^, the solution concentrations,
are3assumed to be equal to the surface activities of chloride ion in moles
cm
Hence : [ ]
log e l+ C2 DA(t-t )
Cl-C----
~ = V--~ o

For t>to,Cl>>C2: C2 ~ DACI(t-t O)

Vl
.Thus D may be calculated from the slope of the rectilinear plot of C 2 versus t.
Series (i)
The'values of effective diffusivity of chloride ions at various temperatures in
OPC pastes of three w/c ratios are shown in Table 3.
From these data, best-fit Arrhenius plots, which are illustrated in Fig.3,
were constructed by means of linear regression analysis.
Vol. I I , No. 3 399
CHLORIDE, DIFFUSION, CEMENT PASTES, WATERCONTENT, CURING

TABLE 3
Effective Diffusivlties of Chloride Ion in OPC Pastes
w/c 0.4 w/c 0.5 w/c 0.6
Temperature Dx~091 Temperature Dx½091 Temperature Dx½091
°C cm s °C cm s °C cm s-
8.94 18.6 58.2
11.88 22.0 56.4
7 14.15 7 22.3 7 5O.9
8.17 20.3 46.5
12.02 20.2 47.5

Ave. 11.03 Ave. 20.7 Ave. 51.9

13.5 22.9 88.4

13.5 24.5 86.4
14.5 9.5 13.5 14.7 14.5 83.8
14.4 31.7 79.6
12.4 24.4
Ave. 84.6
Ave. 12.7 Ave. 23.6

24.9 40.6 120

19.9 44.2 129
25 25.2 25 48.2 25 115
28.6 44.0 156
27.7 47.8 iiO
29.6 43.4 iii

Ave. 26.0 Ave. 44.7 Ave.123.5

43.2 98.4 180

49.2 92.5 156
35 49.5 33.5 91.7 35 164
39.3 99.9 166
39.9 91.3 160
47.0
Ave. 94.8 Ave.165.2
Ave. 44.7

90.7 201 321

91.1 152 299
44 89.0 45 190 47 328
75.1 186 344
74.1 189 299

Ave. 84.0 Ave.183.6 Ave.318.2

The correlation coefficients for the lines obtained at w/c 0.4, 0.5 and 0.6
were calculated to be -0.97, -0.97 and -0.98 respectively and the slopes
corresponded to activation energies (U) of magnitudes ShOWn with 95%
confidence limits in Table 4.

The effective dlffusivities shown in Table 3 are in reasonable accord with

results obtained by previous workers for comparable systems. As an
indication of this, the data of Collepardi et al (8) relating to the
400 Vol. l l, No. 4
C.L. Page, e t a l .

1 0 -a J I J I I 1 I

W/C
• 06
• 05
: 04
0 4 Ref 8

10.7 FIG. 3
U
u.. Arrhenius plots
u.

Z
_o
p.

9
10.11 - -

30
I
-3.1
~
3.2
]
3.3
1
3.4
I
3.5
RECI~OCALOFABSOLUTETEMPERA~RE(xl~)
1
3.6
1
3.7 3.8
I
TABLE 4
Activation Energies for Diffusion of Chloride Ions
in OPC Pastes

w/c Activation Energy (U)

kJ/mole

0.4 41.8±4.0
0.5 44.6±4.3
O.6 32.0±2.4

diffusion of chloride ions in mature Portland cement pastes of w/c 0.4 have
been plotted in Fig. 3. The closeness of these points to the corresponding
line obtained from the present work is notable, bearing in mind that the
results had been acquired by an independent technique (based on a solution
of Fick's second law applied to unsteady diffusion) and with somewhat
different materials.
Since each set of effective diffusivities could be fitted to a unique straight
line on the Arrhenius plots (Fig.3) it is clear that, for a given paste,
diffusion kinetics were under the control of a single dominant process over
the temperature range considered. The activation energies recorded in
Table 4 are all considerably in excess of values characteristic of the
diffusion of chloride ions in normal electrolyte solutions, which are
typically in the region of 17.6 kJ/mole ( 9 ) . This therefore indicates that
the rate-limiting process governing the diffusion of chloride ions in mature
Portland cement paste involves some form of surface interaction, as others
have suggested (8). The precise nature of this interaction is, however,
uncertain as desorption of the diffusing ions from binding sites on the pore
walls and/or structural rearrangements necessary to accommodate ion
migration through surface-bound water may be involved. Essentially similar
considerations apply as for the interpretation of activation energies for
ionic transport in clay/water systems - see for example (iO, ii).
Vol. ] l , No. 4 401
CHLORIDE, DIFFUSION, CEMENT PASTES, WATERCONTENT, CURING

0.3
I I

WlC

o
FIG. 4
0.2
Pore size distribution
curves for OPC pastes. o
o>
z

4(
0C

z o.1

10 J 10 a 10
PORE G4AMETERInm)

The results given in Table 4 indicate also that whilst the activation
energies for chloride diffusion in pastes of w/c 0.4 and 0.5 were not
significantly different one from another, they were higher than the value
obtained for specimens of w/c 0.6. This interesting trend in behaviour
is probably a consequence of differences in pore structure of the three
materials. According to the classic model of Powers et al (12, 13), all
capillary pores in 60 day-old cement pastes of w/c 0.4 and 0.5 would be
expected to have become subdivided by gel, whilst in similar paste of w/c 0.6
a residue of capillary pores might still be expected to remain unsegmented.
Some indication of the relative pore size distributions for the three pastes
investigated in the present work may be obtained from the MIP data presented
in Fig.4.

It is of course recognised that these results do not accurately represent the

condition of the pastes as studied in the diffusion experiments since drying
would have caused modifications to the pore structure in all cases.
Treating the data in Fig. 4 therefore simply as a means of comparison, it
appears that the paste of w/c 0.6 contained a substantial volume of
continuous pores with minimum effective neck diameter greater than iOOnm.
The pastes of w/c 0.5 and 0.4, however, had minimal porosity in this range
and their pore size distributions were generally very similar in form down
to pore diameters of around 4Ohm. Thus, assuming that diffusion occurs most
readily within the largest continuous channels, the diffusion paths of the
majority of chloride ions in pastes of w/c 0.6 would tend to by-pass the
more constricted pores in the size range which is most significant both for
pastes of w/c 0.4 and 0.5. The predominant interactions between diffusing
chloride ions and the pore surface/bound water layer might therefore be
somewhat different in character and more easily overcome, implying a lower
activation energy, in pastes of w/c 0.6.
Estimation and a n a l ~ of pre-exponential constants (A) in the diffusion
coefficients (D=Ae .... ) would have been of interest since these constants
are compounded of several terms dependent on the effective porosity, path
tortuosity and entropy of activation (iO). On the basis of the present
results, however, this was not considered worthwhile as measurements of D had
been confined to a fairly small range of temperatures such that large errors
402 Vol. 11, No. 3
C.L. Page, et al.

would have been incurred in making the necessary extrapolation of the

Arrhenius plots to the axis i=0.
T
The results for pastes of w/c 0.4 and 0.5, which had very similar activation
energies, could be compared on the basis that the ratio of diffusivities
(D_ ~:D_ _) at a given temperature would be approximately equal to the ratio
or pre-exponential constants for the two materials (A -:A ). The values
O-5 0 .4
obtained for this ratio at various temperatures were all wlthin the range
1.96±O.25 and thus could be largely attributed to the relative total
porosities of the pastes (see Fig.4).

Series (ii)
Values of effective diffusivity of chloride ions obtained at 25°C for discs
cut from the central (D-bulk) and PTFE interface (D-interface) regions of
pastes of w/c 0.5 which had been cured in saturated air were as follows :
-7 2 -i
D-bulk = 1.14xlO cm s
D-interface = 4.27xlO-8cm2s -1

Comparison of D-bulk with the result obtained for paste of the same w/c, which
had been cured in saturated Ca(OH) 2 solution (see Table 3), indicates that
curing in air led to a markedly higher effective diffusivity.
The fact that D-interface was substantially lower than D-bulk is in accordance
with suggestions made previously by one of the present authors (4, 14) that
the portlandite-rich interfacial zone of segregation formed between Portland
cement paste and embedded materials (15, 16) may constitute a significant
diffusion barrier which tends to stabilise the passive oxide film on steel
reinforcement. This finding is paralleled by the results of independent
investigations, which have shown that the rate of diffusion of dissolved
oxygen through water-saturated concrete is considerably lower for specimens
with 'as-cast' surfaces than for similar ones with cut surfaces (17).

Series (iii)
In Table 5 are recorded values of effective diffusivity of chloride ions
measured at 25°C for pastes of w/c 0.5 manufactured from various types of
cement.
TABLE 5
Effective Diffusivity of Chloride Ions at 25°C
in Various Cement Pastes of w/c 0.5
Type of Cement D ~ !~ 9
Cm s
OPC 44.7
OPC/30%PFA 14 .7
OPC/65%BFS 4.1
SRPC iOO.O

The results indicate that diffusion of chloride ions in hardened cement

paste is strongly influenced by the type of cement used. They confirm the
conclusions of previous investigations, which have shown that blended cements
containing slags (18) or pozzalanas (8) limit chloride diffusion more
effectively than Portland cements. They show also that the particular SRPC
studied was somewhat less effective in this respect than the OPC but, whilst
this is consistent with the results of certain other workers (18), it does
not necessarily imply that the low C_A content of the SRPC was solely
responsible for the difference in be~aviour as subsequent discussion will
show. A further note which should be added to Table 5 is that the results
Vol. I I , No. 3 403
CHLORIDE, DIFFUSION, CEMENT PASTES, WATER CONTENT, CURING

0.3

O~ °°'*°
o~c . ~ ~s .....'~__
......... 0~¢ 3o~ PfA x:~""

~ 0.2 ......-" i ~
FIG. 5
Pore size distribution
curves for cement
pastes of w/c 0.5

io,

10' 10 m 10
P O l l [ [ X 4 M k ' T ~ (rim)

quoted refer to diffusion at a single temperature and it is known that the

temperature dependence of effective diffusivities may vary from one type of
cement to another (8).

To gain insight into factors underlying the different performance of the

various cements, their pore size distribution curves, recorded in Fig. 5,
may be compared. Examining first the data for OPC and SRPC pastes of w/c
0.5, it is clear that the pore structures of the two materials were
dissimilar. The SRPC paste of w/c 0.5 was actually more nearly comparable
with OPC paste of w/c 0.6 (see Fig.4) in terms of total porosity and pore
size distribution. Correspondingly, the UPV values recorded in Table 2
for SRPC paste of w/c 0.5 and OPC of w/c 0.6 were similar. It is therefore
reasonable to account provisionally for the fact t~at ~heleffective diffusivity
of chloride ions in SRPC paste o~ w~c 9.5 (l.OxlO - cm s -) was7cl~se~ to that
of OPC paste of w/c 0.6 (1.2xlO -cm-s -) than w/c 0.5 (O.45xlO cm s -) in
terms of physical pore-structure characteristics rather than chemical effects
ascribable, for example, to the different C3A contents of the two materials.
This conclusion, which requires confirmation, does not imply that there was
no complexation of diffusing chloride ions by the aluminate phases in the
cement pastes. This would be contrary to the findings of other workers
(19, 20) and would also conflict with the apparent indications of DTA analysis
obtained for OPC and SRPC pastes before and after diffusion experiments had
been performed. The appearance of an endothermal peak at around 350°C in the
post-diffusional trace for OPC (Fig.6) signifies the presence of calcium
chloroaluminate hydrate (21) which must have been formed either during the
diffusion experiment or during subsequent manipulation and drying of the
specimen.

It would seem, however, that, insofar as chloride diffusion kinetics are

concerned, the effect of chloroaluminate formation may be of secondary
importance compared with the influence of other factors determined by pore
structure. This perhaps explains why studies of the rate of penetration
of chloride ions into concrete immersed in seawater showed little dependence
on the C3A contents of the cements used (i, 19).
404 Vol. II, No. 3
C.L. Page, et al.

FIG. 6
3~C
! DTA curves for
OPC pastes of
ilg
w/c 0.4.
5

BEFORE DIFFUSION

SAMPLE TEMPERATURE

Examination of the pore size distribution data shown in Fig. 5 for the blended
cement pastes suggests that, in these cases, a quite different interpretation
is required of factors governing chloride diffusion kinetics. Pastes
containing OPC/30% PFA are substantially more porous than plain OPC pastes of
the same w/c, yet the effective diffusivity determined for the blended paste
has a value of approximately one-third that for the OPC paste. This suggests
that different mechanisms of diffusion rate control are applicable to the two
materials. Likewise in the case of the slag cement paste, the fact that the
effective diffusivity was an order of magnitude lower than that of the
corresponding OPC paste does not appear to be explicable purely in terms of
differences in the pore size distributions of the two materials.

Research aimed at establishing the activation energies for chloride diffusion

in the various systems is in progress and it is hoped that this may shed
further light on the mechanisms involved.

Conclusions.

The investigations have shown that the relatively simple techniques used in
this work for study of chloride diffusion kinetics in hardened cement
pastes yield reproducible effective diffusivity values that compare well with
similar data obtained independently by alternative methods. The assumptions
inherent in the approach are therefore validated and its practical
advantages, in terms of speed, non-destructive nature and small specimen
requirement, may be exploited with reasonable confidence.
For diffusion of chloride ions in mature OPC pastes, the activation energy
was shown to be substantially higher than that for diffusion of the ions in
normal aqueous solutions. Its magnitude was practically constant for pastes
of w/c 0.4 and 0.5 but at w/c 0.6 a significantly lower value was obtained.
This is thought to be associated with the availability in pastes of w/c 0.6
of relatively large unconstricted capillaries which were absent from the
pastes of lower w/c.
Curing conditions had a marked effect on the transport properties of mature
cement pastes, the effective diffusivity of chloride ions being dependent
Vol. I I , No. 3 405
CHLORIDE, DIFFUSION, CEMENT PASTES, WATER CONTENT, CURING

on whether the material had been cured in saturated air or limewater. It was
also found that specimens, in which one surface had been cast against an
unreactive substrate to form an interfacial zone of segregation rich in
portlandite, limited diffusion of chloride ions more effectively than
specimens with two cut surfaces.
Investigations with various types of cement confirmed that diffusion of
chloride ions is strongly influenced by cement composition. Blended
cement pastes containing PFA or BFS sustained lower diffusion rates at 25°C
than OPC pastes of the same w/c and these differences could not be ascribed
simply to variations between the pore structures of the materials, The
effective diffusivity obtained at 25°C for the particular SRPC paste studied
was higher than that for OPC paste of the same w/c. In this case, however,
the difference appeared to be explicable mainly in terms of the coarser
pore structure of the SRPC paste and there was no clear evidence that the
lower C A content of the material had significantly affected chloride
diffusion kinetics.
The range of conditions that could be examined within the limited timescale
of the research reported in this paper is being extended by further work.
It is hoped that this will lead to conclusions of greater general
applicability and more detailed understanding of the mechanisms of chloride
diffusion in hardened cement pastes.
Acknowledgements
We wish to thank Professor A. W. Pratt for the provision of laboratory
facilities and Mr. C. Thompson for his excellent technical assistance.
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C.L. Page, et al.

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