Advances in Cement Research, 1994,6, No.
23, July, 127-134
Experimental procedure for the calculation of
chloride diffusion coefficients in concrete from
migration tests
C. Andrade* and M. A. Sanjuan*
INSTITUTE OF CONSTRUCTION SCIENCES 'EDUARDO TORROJA" (CSIC)
A decrease in the time required for testing the resistance
of concrete to chloride penetration is proposed, based on
the so-called rapid chloride permeability test developed
by Whiting. Numerous papers have been published
presenting results obtained by this method, which has
already been standardized by AASHTO, although its
interpretation is disputed. A previous paper presented a
theoretical basis to improve the Whiting set-up and to
convert it into a reliable method for the calculation of
chloride diffusion coefficients. The approach was based
on the fundamentals of electrochemistry regarding
transport in electrolytes, by use of the Nemst-Planck and
Nemst-Einstein equations. In this Paper preliminary
experimental results are presented and natural diffusion
and migration tests are compared. The results indicate
a satisfactory agreement of the two test types and the
soundness of the simplifying assumptions adopted. The
experimental procedure and possible improvements are
described.
Introduction
The 'rapid chloride permeability test' developed by
Whiting 1 attracted much criticism due to the high voltage
drop (60 V) used to shorten the test duration. However,
now that it has been approved as a standard by
AASHT0 2 and ASTM3 an increasing number of
researchers are using it as a routine test. 4-8 The users
report high reproducibility, although uncertainties persist
as to whether this type of test really measures concrete
permeability to chlorides or whether it gives only a rough
estimation of the concrete's electrical resistance. 9
In a recent paper by one of the Authors 10 the errors
inherent in the actual AASHTO test were enumerated and,
after a description of the electrochemical basis of the
processes developed under an electrical field applied to
* Institute of Construction Sciences 'Eduardo Torroja' (CSIC), Madrid,
Spain.
Paper received 29 October 1993.
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the concrete, a method was proposed to calculate the
chloride diffusion coefficient from a migration experiment
with an arrangement similar to the AASHTO one,
provided steady-state conditions are reached.
The previous paperlO demonstrated in detail that the
rapid chloride permeability test contains the following
defects: (1) it does not measure 'permeability', because
it deals with coulombs, which are not related to this
concept; (2) in measuring the integral amount of electricity
passing, it does not discriminate for chlorides; (3) it gives
erroneous results when other electrolytes (admixtures) that
can also carry the current are added to the concrete.
In order to overcome these shortcomings, the
theoretical approach considered in Ref. lOis based on
the use of the Nernst - Planck equation 11 (which models
in general mass transport in electrolytes) or of the
Nernst- Einstein equation 11 (a particular case of the
Nernst- Planck equation, using electrolyte equivalent
conductivity as the main parameter).
Nemst-Planck: total flow = diffusion + migration +
convection.
x
-J(x) = D
J J
a9
ax
) +
ZjF aE(x)
- DC - - + CV(x) (1)
RT J J a(x) J
where J(x) is the unidirectional flux of species j
(mol/cm 2 per s), Dj is the diffusion coefficient of species
j (cm 2/s), ac is the variation of concentration (mol/cm3),
ax is the variation of distance (cm), Zj is the electrical
charge of species j, F is Faraday's number (callY
equivalent), R is the gas constant (cal/mol per K (1 cal
= 4 19 J)), T is the absolute temperature (K), Cj is the
bulk concentration of species j (mol/cm3), aE is the
variation of potential (V) and V is the artificial or forced
velocity of an ion (cm/s)
Nemst- Einstein
---.!!L ZF aE
= -J-DC (2)
~F RT J J ax
127
 Andrade (Ifill Sanjuan

where i i tht: current den ity pas. ing or applied between

electrode (A/cOl 2) and I) is the tran ference number of
species j .
Simplifying assumption ' were propo cd lO in order to
make bot h equat ions of practical interest for the particular
ea e of ch loride transport in onc rete . The expre sions
for the calcu lation of the effective chloride diffu ion
coefficient Derr in a traditiona l 'diffu ion cdI' were as
follow . . IO
Nernst- Planck

(3)
ZdFC,.(yA

where 'Y is the activity coefficient. Ii ' the conc ret di 'c
thi kness (cm) and J I is the ch loride now (mol/cm 2 per
s) .
Nel'llsl- inSlein
Joo nt
RT ilc i
(4)
--;;FT A A CO'YZcI

where ACI is the equivalent conductivity of chloride ioris Distilled waler 05 M NaCI
(n - Icm - 2equ ivalent - I). lo i the transference number of
chloride ions and A is the cro -sectiona l area of conc rete
A nolyte "
disc ( '111 2) .
The previous paper lO was purely theoretical : although
num erical exam ple we re presented. ex perimental
evidence is necessary to va lida te the approach. i.e. to Fi8. I . Cell lIsed i" liIe //Iil:l rtllioll mill dij}il.l'io/l eX{J{'/';lIl el/l.\
veri fy the reliability of the theoretical implifying a sump-
tions and that the equatio ns deduced really can be applied
to a porous . olid material contai ning an electrolyte .
Thi Paper pre 'en t the results of an experimen tal trial
undertaken to ex plore the proposed methods . Although
numerous preli minary experiments were carried out. on ly
a few had va lid re ults. because the exper imental condi -
tions were critical in obtaining app roximate va lue of
Den. Therefore. only one of the trials compari ng Dcf!'
va lues obtained from natural diffusion in teady- ta te
conditions and those obtained from migration test (a l 0
in st ady- tate condition) i used here to illustrate the
proper experimenta l procedure for migration experiment .

Experimental details
The general et-up of the exper iment wa simi lar to that
of the AASHTO test. in order to profit as much a ' po sible
from testing equ ipment already developed which is widely
u ' d.
Cel/lype
The appearance of the cel l used for the ex perimen t and
the arrangement of the electrodes are hown in Fig. I .
Although th is cell is slightly differen t to the AASHTO
one, any arrangement with two chamber ' is feasibl .
The th ic kne ' of the concrete di c was 05 cm (Fig.
2) in order to achieve steady -state condit ion rapidly . Any
thickness is feasible provided stationary condition are
reached . These condition are establi hed as oon a the
chloride content in the ano lyte pre ents a traight inc reas-
128
Fig. 2. COli erNe disc 5 //1//1 Ilrick /I I'd ;/1 Ihl' Irials
ing lope wi th ti me (constant flow) . The cro - ection of
the concrete di e used in the trial. was 283 cm 2
The eatholyte u ed wa 05 M ae l olut ion. which
simulate the ch loride content in sea water. Any con-
centration i possible. although it i important that acti ity.
and not concentration. be u ed in the equation '. Therefore.
highly co ncentrated olution ' are not recommended
because the chloride activ ity decreases. On the other hand.
exce ively dilute so lutions will produce a weaker driving
A,II""/( ,',, ill eel/It' ll I Res,'arch . )1)94 . 6 . 0 . 1.,

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force and a small difference in concentration between
catholyte and anolyte, which could introduce inaccuracies
to the results.
The activity coefficient used for the 05 M NaCl was
o.68, calculated previously. II The initial volume of each
chamber was about 300 m!.
The anolyte was distilled water instead of the NaOH
solution recommended by Whiting. This is based on the
need to develop an active dissolution of the anodic
electrode. If non-oxidable electrodes or alkaline solutions
that passivate the steel are used, water electrolysis and
CI 2 evolution from migrating CI- are developed due to
the level of voltage reached in the anodic electrode. In
consequence, anolyte volume (important for chloride con-
centration calculations) changes continuously and chloride
analysis may give erroneous results if CI 2 is being
evolved. In addition, chlorides are consumed and cannot
be analysed accurately. On the other hand, if corrodible
electrodes are used the potential reached by the anode
forestalls the water electrolysis and therefore CI 2
evolution, and no anolyte volume changes occur with
increasing time, due to the passage of the current.
Therefore, a piece of rebar (steel) was used as an anodic
material, and distilled water as the anolyte, in order to
induce an immediate oxidation when current is applied.
Steel, graphite, platinum and titanium were also tested
as anodic electrodes but, as described above, Cl 2
evolution was detected.
The anolyte finishes 'dirty' because of the ferrous ions
produced during the trials. A steel rebar was also
employed as the cathodic electrode.
A voltage drop of 12 V was used in all the experiments.
This is high enough to accelerate the process significantly,
but low enough to avoid undesirable heating. In any case,
the real voltage drop near the concrete surfaces was
measured in each experiment because, although it could
be assumed that no voltage drop was produced across the
liquid of the two chambers (as the distilled water has a
low conductivity), the real M may be less than 12 V (this
was found to be the case). Therefore the voltage drop was
measured by means of two reference electrodes contacting
the concrete surfaces, just before the end of each trial.
Parameters measured
The only parameter that needs to be monitored during
the experiment is the variation of Cl- concentration in
the anolyte, because from the plot of this concentration
against time it is possible to calculate Deff using equation
(3). Nevertheless, in the present trials other parameters
were also measured in order to follow chemical changes
in both chambers, namely pH, conductivity, current across
the cell and chloride depression in the catholyte. Chloride
proportion in both chambers was measured by periodically
extracting aliquots of 5 ml whose chloride concentration
was obtained by titration with a Mettler DL40RC auto-
matic titrator, using AgN0 3 as the indicator.
In the preliminary trials, an ion-selective electrode was
tried in order to avoid the need to take aliquots of the
Advances in Cement Research, 1994, 6, No. 23
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Chloride diffusion coefficients in concrete
electrolyte. However, the need for previous calibration
of the chloride-selective electrode in blank solutions of
similar concentration made it unsuitable for the procedure,
due to the progressive unforeseen concentration changes.
A final detail to be considered is the calibration of
volume in both chambers in order to calculate precisely
the chloride contents after each aliquot is taken for
analysis. Volume also changes in the cathodic compart-
ment due to the water electrolysis.
The pH value was measured by the periodic introduc-
tion of an Orion electrode of range 0-14 previously
calibrated in solutions of pH 7 and 13. The pH-meter was
a Crison model 501. Conductivity (J was monitored using
a conductimeter Crison model 522 with a standard cell.
The current flowing through the cell was recorded
throughout the experiment by means of an electrometer
(Keithley model 197 Autoranging Microvolt DMM).
Electrical resistance of the concrete disc was also
measured in order to check the reliability of equation (4).
It was measured directly on the concrete disc before and
after each trial. It was also measured when the concrete
disc was in the cell and already in contact with both
electrolytes. In all cases the electrical resistance was
measured by means of the positive feedback of an Amel
potentiostat model 551. The temperature of the trials was
20 2C.
Diffusion cell
The cell used for the natural diffusion experiments is
exactly the same as that for migration experiments, but
without the electrodes. In order to avoid Ca(OH)z
leaching, 01 M NaOH was used in this case instead of
distilled water in the compartment initially without
chlorides.
Concrete characteristics
For these preliminary trials a conventional concrete was
fabricated as cylindrical specimens 75 cm in diameter
and 15 cm high. The cement used was a rapid hardening
OPC with the Spanish denomination 'type I155A'. The
aggregate was siliceous. The concrete mix per m3 was:
cement, 300 kg; water, 150 I; sand, 860 kg; aggregate
(maximum size 12 mm), 1100 kg; slump, 6 cm.
After the specimens were cast, they were cured under
water for 24 h. After demoulding they were submerged
in a solution of saturated Ca(OH)2 in order to avoid
leaching prior to testing.
The concrete discs for the trials were prepared by
careful dry cutting into slices 5 mm thick. Slices used for
the natural diffusion test were 6 mm thick.
Results
Migration test
Figures 3 and 4 show the evolution with time of
conductivity, pH, intensity, and chloride content in anolyte
and catholyte for two duplicate migration tests. The evolu-
tion of pH was as expected, i.e. the pH increased with
129
 Andrade and Sanjuan

Initial distilled water Initial 05 M NaCI

80 13 13

70 12 12

60 11 60

50 10 pH 50
(fJ

E
E 40 a9 40 -'-'
i:i

30 8 30

20 7 20

10 6 10

(a)

130

35 120

30 110

25 100

l5
~ 20 90
E
15 80

10 70

5 60

10 20 30 40 50 10 20 30 40 50
Time: h Time: h
(0; (e)

Fig. 3. Evolution with time of (a) conductivity a, pH, intensity of ions passing through the cell; chloride
concentration in (b) anolyte and (c) catholyte in the migration cell when 12 V was applied across the electrodes

time in the catholyte due to the production of hydroxides
from the water electrolysis
while it decreased in the anolyte due to acidification
resulting from the hydrolysis of water by the ferrous ions
generated by oxidation of the steel
Fe - Fe2+ + 2e-
Fe+ 2 + 2H 20 - Fe(OHh + 2H+
The initial pH in both anolyte and catholyte was not
neutral, but around 10. This was attributed to leaching
of OH- from the concrete disc during the time required
to fill the chambers with solution, install the electrodes
and carry out other operations before the electrical field
was connected.
130
The conductivity a increased in parallel with the pH
in the catholyte, due to the generation of OH -. It also
increased in the anolyte due to the acidification and the
generation of Fe2+ ions from the anode.
The current increased to a maximum, after which a
slight decrease was recorded, as was reported in many
experiments of the AASHTO test. This was due to the
changes in total electrical resistance that occurred during
the experiment. The value of !::.E measured beside the
concrete disc was 8 5 V, compared with the 12 V applied
between electrodes.
Figures 3 and 4 show the change in molarity of
chlorides. After an initial delay in the passage of these
ions from the catholyte, they were detected in the anolyte
in amounts that increased approximately linearly with
time. This is consistent with steady-state conditions, and
Advances in Cement Research. 1994, 6. No. 23

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 Chloride diffusion coefficients in concrete

Initial distilled water Initial 05 M NaCI

80 13 13
pH
70 12

60 11 11 60

(]
50 10 10 50
en
E I
0.
ti 40 9 9 40 ~

30 8 8 30

20 1- 20

10 10
(J

(a)

35 120

30 110

25 100
I

(320 90
~
E
15 80

10 70

5 60

20 30 40 50 60 70 20 30 40 50 60 70
Time: h Time: h
(b) (e)

Fig. 4. As Fig. 3, for a twin concrete disc (duplicate experiment)

the shape is similar to that reported for natural It can be deduced from these results that the value of
diffusion. 4 ,7,12 When the slope of the straight lines in the Rohm from the Fig. 3 test is erroneous; however, the test
Nernst-Planck equation was used? the values found for shown in Fig. 4 gives a very similar value for Deff to that
8 2
Deff were 193 X 10- cm /s (Fig. 3) and 149 X obtained by the use of the Nernst-Planck equation. Also,
8 2
10- cm /s (Fig. 4). transference numbers are of a reasonable magnitude.
For the calculation of Deff from the Nernst-Einstein
equation, it is necessary first to calculate the transference Natural diffusion test
number of chlorides tCi from 10 Only one natural diffusion experiment was carried out
lCiF Table 1. Values of parameters in Nemst-Einstein equation
tCi = -.- (5)
It from Figs 3 and 4
Equation (4) is then used for further calculations, provided Nernst-Einstein Fig. 3 test Fig. 4 test
the electrical resistance Rohm of the concrete disc has also
been measured. It was decided to use the value of electrical lel.mig: mol/em2 per s 441 10- 9
X 327 X 10- 9
resistance Rohm measured (before testing) directly on the tCl 030 037
disc placed between two metallic plates acting as Rohm: n 4200 152
electrodes (Table 1). Deff,mig: em 2/s 009 x 10- 8 3 44 x 10- 8

Advances in Cement Research, 1994,6, No. 23 131

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 Andrade and Sanjuan

170

160

50 150

25 140

'- 20 130
()
~
E 15 120

110

100

20 40 60 80 100 20 40 60 80 100
Time: days Time: days
(a) (b)

Fig. 5. Evolution with time of chloride concentration in the diffusion cell: (a) initial 0] M NaOH; (b) initial 05 M NaCI

for these preliminary trials. The results obtained for the 80

evolution of chloride with time in both compartments of
70 Fig. 3 (migration)
the cell are shown in Fig. 5. A slow linear increase in
chlorides was noticed in the compartment from which 60
chlorides were initially absent. Fig. 4 (migration)
50
The effective diffusion coefficient obtained from these
results using the procedure described by Page et al. 12
was
Deff.dif = 79 X 10-
8

which is higher than those obtained from the migration

tests, but nevertheless satisfactory considering the
cm 2/s 20 -------... Fig. 5 (diffusion)

differences between individual samples reported by Page 10 30 50 70 90 110

et al. 12 for replicate experiments. The value of the Time: h (migration); days (diffusion)
chloride steady-state flow from this experiment is
Fig. 6. Chloride apparently taken up by the concrete disc
JCI,dif = 758 X 10-
11
mol/cm 2 per s during the experiment

Chlorides held in the concrete disc
The amount of chlorides taken up by the concrete disc
was calculated from the mass balance between those
passing to the anolyte and those remaining at the catholyte.
This mass balance for the three experiments described
here is shown in Fig. 6.
Figure 6 shows that the amount of chlorides apparently
held in the concrete disc during the migration tests is about
three times as high as that held in the diffusion trial. These
results are surprising and need clarification, although a
possible interpretation is given below.
Discussion
The importance of obtaining values of the chloride
diffusivity across the concrete in a very short time was
pointed out by Whiting 1 when he proposed his test. In
addition, he tried to keep the testing procedure simple so
that it would be suitable for practical purposes. Various
workers have modified the Whiting test with a view to
132
improving its reliability. The preliminary results presented
here appear very promising; also, the values of Deff and
of other fundamental parameters such as chloride trans-
ference number derived here are theoretically well sup-
ported and are linked to the intrinsic microstructural
characteristics of concrete.
Although complete accordance between migration and
diffusion results is not obtained, the differences are
considered insignificant for a preliminary trial in com-
parison with the advantage that a Deff value can be
obtained in about 48 h of testing. However, further
improvement of the testing procedure and more careful
consideration of the mass balance between the migrating
chloride ions and those held in the concrete disc are
necessary before this methodology can be proposed for
standardization. In any case, the use of an electrical field
to accelerate chloride diffusion across concrete, with
reference to either the Nernst- Planck or the Nernst-
Einstein equation, is confirmed here to be theoretically
well-founded.
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The simplifying assumnptions used in the previous
theoretical paperlO in order to solve the difficulties
associated with such a complicated phenomenon are con-
firmed here to have a negligible effect on the diffusion
chloride flux compared with that due to migration. The
results obtained indicate that diffusion flow (considered
simultaneously to migration, by the Nernst-Planck
equation) is about two orders of magnitude smaller than
that due to migration, and therefore comparatively
negligible. The confirmation of this simplifying assump-
tion is critical for the validation of the present approach
and its possible future use as a standard method for
concrete.
Possible ways to improve the testing procedure
In the application of the Nernst-Planck equation, the
differences found between diffusion and migration indicate
that the value of Deff.mig was smaller than that of Deff.dif'
Assuming this is due not to normal scatter but to experi-
mental errors, the following improvements could be made
(see equation (3)).
(a) It might be better to use a mesh rather than a steel
rod in order to introduce a more efficient current
distribution.
(b) The activity factor used for the NaCI solution was
o.68, as calculated in a previous paper. II Perhaps an
adjustment is needed, since conductivity changes as
the experiment progresses and therefore the ionic
strength of the solution also changes.
(c) The chloride content at the catholyte was not constant
throughout the experiment. Perhaps this is another
source of error, due to a significant decrease in
chloride in the catholyte. It might be better to provide
a constant chloride concentration by periodic
adjustment.
(d) The adsorption of Cl- ions by the ferrous-ferric
products produced from the oxidation of the anode
in the anolyte during the experiment may give rise
to error (it is known that the akaganeite may take up
chloride ions I7 ). This adsorption might explain the
higher proportion of chlorides measured in the
concrete discs subjected to migration. In fact the
chlorides would be in the anolyte, but not as free
species: analysis of the iron products is one way to
check this hypothesis. If this is confirmed, the cell
type should be modified in order to avoid the effect
of contact between iron products and chlorides. This
could be achieved by means of a three-compartment
cell using a chloride-selective membrance to stop the
passage of chlorides into the anolyte, or using non-
polarizable electrodes.
Regarding the Nernst-Einstein equation, the values of
tCiwere within the expected order of magnitude for an
electrolyte of the type 02 M NaOH + 05 M NaCl (tCi
= 0 34). On the other hand, only one of the two migration
experiments gave the correct value of concrete electrical
resistance Rohm ' This indicates that this measurement is
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Chloride diffusion coefficients in concrete
subject to experimental errors. The value of concrete
resistivity p, taking account of the geometry of the disc,
was 20 MO cm in the case of the correct value.
As was pointed out in the previous papers,IO,14 the
possibility of using resistivity values to characterize
concrete mass transport properties is of great practical
interest because it would allow on-site measurement of
chloride diffusivity. If concrete resistivity could also give
an indication of concrete porosity, 16 this parameter might
become a universal parameter l3 to characterize concrete
durability, when the deteriorating mechanism is based on
the transport of aggressive substances from the exterior.
Another improvement in the experimental procedure
would be to work galvanostatically instead of potentio-
statically, in order to improve the value of tCi'
Conclusions
The results presented are only of preliminary trials, and
further experiments are being developed in order to
determine more precisely the accuracy of the migration
method to measure the diffusion coefficient of chlorides.
However, although a perfect accordance was not found
between migration and natural diffusion tests, some
important conclusions could be drawn.
1. Migration tests theoretically described in a previous
paper lO have resulted in a practical method of
accelerating chloride diffusion across concrete, and
therefore of shortening considerably the testing time to
calculate the effective chloride diffusivity D eff . Either the
Nernst- Planck or the Nernst-Einstein equation can be
applied to the method.
2. The Deff values calculated from migration experi-
ments were about three to four times (Planck) and twice
(Einstein) as small as those calculated from natural
diffusion tests. The discrepancy needs to be reduced by
optimization of the experimental conditions and a more
careful study of chloride mass balances.
3. The diffusion flow resulting from the electrical field
is about two orders of magnitude smaller than that due
to migration, and can therefore be regarded as negligible.
4. Concrete resistivity appears promising as a universal
parameter with which to characterize the mass transport
properties of concrete and thus certain aspects of its
durability.
Acknowledgement
c. Andrade would like to thank Dr C. Page of Aston
University for the explanation of fundamentals and the
description of testing procedures of natural diffusion given
some years ago.
References
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2. AASHTO. Standard method of test for rapid determination of
133
 Andrade and Sanjuan
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Discussion contributions on this Paper should reach the Editor by
27 January 1995
Advances in Cement Research, 1994, 6, No. 23