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During the past decades extensive research has been dedicated to degradation phenomena
of concrete and reinforced concrete structures in order to reveal the governing mechanisms,
and explain and quantify the deleterious effects of aggressive substances. For structures under
service conditions, the environment, i.e. the natural atmosphere, soil, water or user-made
conditions, imposes sustaining actions on the surfaces of structural members. The durability
of a concrete or reinforced concrete member is then controlled by the resistance of the
outermost layers or concrete skin of a cross section to the external attacks [2.1].
The external attacks may cause a deterioration of the skin of a member which is
immediately exposed to the actions, and with prolonged exposure the corrosion front
progresses deeper into the section. Assuming that the already corroded material in the surface
layer is instantaneously removed, the progress of the corrosion front is controlled by the
reaction rate of deleterious species with concrete compounds. If, however, the reaction
products remain in place, the attacking species have to penetrate the corroded concrete zone
before they can reach and react with non corroded material either concrete compounds or
steel. In this case the progress of the corrosion front is controlled by the rate of transfer of
aggressive species to the reaction front.
The second case includes the penetration of deleterious substances which do not cause a
degradation of the concrete surface zones directly, e.g. the ingress of chloride ions, or do not
immediately cause degradation of the concrete integrity, but they result in changes of the
physical-chemical properties, e.g. carbonation. These processes, however, may initiate further
corrosive actions in deeper sections of a structural member, such as the anodic dissolution of
embedded steel reinforcement. Also in these cases the external reactants associated with a
corrosion reaction have to penetrate a concrete section of a given thickness first. Thus, the
corrosive action is controlled by the availability of reactants, i.e. their rate of transfer.
The first case of a purely reaction-rate controlled degradation is not usually of importance
for concrete structures under typical service conditions, except in rare cases of acid attack in
flowing media, to soft water attack accompanied by erosion, or mechanical wear. Most
corrosive actions on concrete and reinforced concrete members are encountered when
aggressive species penetrate the concrete surface zone, i.e. the concrete cover of the
reinforcement. Examples of such degradation mechanisms are [2.2]:
13
the corrosion of the steel reinforcement by anodic dissolution of the iron, initiated
by the ingress of chloride ions which depassivate the steel surface after a critical
threshold concentration has been reached. The rate of transfer of chloride ions
controls the time to corrosion.
the corrosion of the steel reinforcement by anodic dissolution of the iron after
depassivation of the steel surface as a consequence of the loss of alkalinity due to
carbonation. The penetration of carbon dioxide determines the depth of
carbonation at a given time t.
the formation of secondary ettringite from calcium aluminate hydrates (hydration
products of the cement) with sulphate ions penetrating from external sources. The
availability of sulphate ions is rate-controlling, provided the internal reactants are
available.
expansive alkali-aggregate reactions supported by the ingress of external alkalies
and/or water. Although all necessary reactants for AAR may be introduced into the
concrete by the concrete making materials the penetration of alkali ions and water
into deeper concrete sections increases the severity of the attack.
frost action, eventually enhanced by de-icing agents, which cause disruptive forces
upon freezing of water in a water saturated pore system. Saturation of the pore
system is attained only by up-take of water from the exposed surfaces.
Based on these considerations the transport properties of concrete for water, gases and
dissolved species have attracted increasing interest during recent years in order to analytically
explain, quantify or predict a corrosive action on a concrete structure or describe the
perviousness of a concrete section to various media [2.3-2.5].
In addition to durability considerations, the imperviousness of concrete sections to liquids
and gases is often a service requirement for advanced structures in the nuclear energy sector,
for retaining or barrier structures, and for underground or underwater infrastructure [2.6-2.8].
Some related tasks associated with the transport properties of concrete are:
-
14
For an analytical treatment of these tasks the transfer of mass either in a gaseous state,
liquid state or dissolved state, must comply with the physical model describing a transport
process in which the mechanism of transfer is characterized by a driving force, by properties
of the moving species as well as by properties of the penetrated material. Under simplifying
assumptions the transport properties of the penetrated material are taken as a materials
characteristic or intrinsic value, which is often regarded as a constant but indeed may be a
function of several internal and/or external parameters. Consequently, apparent or effective
transport parameters are then often defined as a simplification of the real process.
As flow paths for transport through concrete, the capillary porosity of the matrix, the
paste/aggregate interface as well as microcracks are considered. Concrete is an aging material:
due to on-going hydration of the cement the porosity as well as the continuity of the capillary
porosity decreases with time, microcracking may increase due to drying shrinkage, and corrosive
interactions with the environment may increase or decrease the porosity of the matrix. Similar
considerations must be taken into account for the interaction of the penetrating species with the
porous material, i.e. the degradation process itself may change the porosity. Therefore, the
transport characteristics also change with time, i.e. aging is considered by time functions. This is
of considerable importance when transport properties are assessed in laboratory experiments on
young concrete specimens to provide input data for a long term assessment of structures, e.g. a
service life prediction. Sensitivity analyses on prediction models have demonstrated the
dominating effect of ageing parameters on the final result of the modelling [2.9].
Also the selection in isolation of a single transport mechanism for the ingress of a particular
substance may represent an over-simplification of the real transport process since more than one
transport mechanism may be active at a given time, either in parallel or in different sections
along the flow paths, so called mixed modes of transport. They play an important role in the
ingress of dissolved species, e.g. chloride ions, when capillary suction takes place in nonsaturated surface zones, whereas in deeper sections diffusion governs their transport.
It is common practice to distinguish those transport mechanisms which are important for
the above mentioned performance characteristics of concrete structures as diffusion,
permeation, capillary suction and migration. The distinction between these mechanisms
depends on the driving forces for the transport.
2.1
Diffusion
Brownian free motion of atoms, ions or molecules results in a net flow of mass from regions
of higher concentration to regions of lower concentration. The flux per unit area of a plane
perpendicular to the flux, q,
q=
dm 1
dt A
(2.1)
15
q is proportional to the concentration gradient dc/dx as the driving force for the transport, and
to the diffusion coefficient D. This relation is expressed in Ficks first law of diffusion [2.10]
q = D
dc
dx
(2.2)
The application of Ficks first law of diffusion to non-steady state transport processes leads
to the mass balance equation which describes the change of concentration in a unit volume
with time, i.e.
Change of concentration c with time = flux into element minus flux out of element (Fig. 2.1):
16
Fig. 2.1 - Mass balance for volume element in non steady state transport condition
flux into element:
c
q x = D
x x
(2.4a)
c
q (x +x) = D
x x +x
(2.4b)
change of concentration:
c
c
c
x = D
+ D
t
x x +x
x x
(2.4c)
or
c
c
+ D
D
c
x x +x
x x
=
t
x
(2.4d)
and for x 0
2c
c
= D 2
t
x
(2.5a)
Equation (2.5a) is valid for D=const. If D is a function of the local concentration c or the
space variable x or time t then
17
c
c
= D
t
x
x
(2.5b)
The mass balance equation (2.5a) is usually referred to as Ficks second law of diffusion
[2.12]. Explicit solutions exist for this partial differential equation (PDE) for simple
geometries and constant boundary conditions as well as constant material properties, in
particular D = const. For instance
x
c(x, t) = c0 1 erf
2 Dt
(2.6)
where erf is the error function and the initial conditions (t = 0):
c = 0 for x > 0
c = c0 for x = 0
Equation (2.6) is often used to evaluate observed concentration profiles on laboratory test
specimens as well as on real structures after an exposure time t by means of a regression
analysis with respect to D, e.g. a least squares fit.
The ingress of ions into concrete is treated in general as a diffusion process. Nilsson [2.11]
points out that in this process, not only a transfer of mass occurs but also a transport of
electrical charge. In order to maintain electro-neutrality in the system the flow of anions must
be balanced by a corresponding flow of cations. If the transfer of charges cannot be balanced
a voltage difference will build up. In this electrical field one type of ion may be accelerated
while others can be slowed down in their movement. In this state the diffusion of ions will
overlap with migration as described in section 2.4 .
2.2
Permeation
Liquids and gases can percolate through interconnected pore spaces or crack networks of
cementitious materials under the driving force of an absolute pressure gradient [2.13, 2.14].
2.2.1 Gas permeability
18
p1
p2
= time (s)
There is experimental evidence, however, that eq. (2.7) does not account for all mechanisms
acting in a porous solid, since the observed coefficient of permeability kobs will depend on the
pressure level used in the experiments. Additional effects such as non-Newtonian fluid
characteristics, inertia effects causing turbulent flow patterns and Knudson or slip flow are
discussed in [2.15-2.17]. While non-Newtonian behaviour is not considered to have a major
effect on the flow volume [2.16], a turbulent flow pattern is likely to occur in the capillary pore
system due to the pore sizes, the tortuosity and the roughness of the pore walls. If the size of the
pores percolated is in the range or smaller than the mean free path length of the gas molecules
an additional flow component occurs, i.e. slip flow or Knudson flow. The mean free path length
of gas molecules at ambient temperature and atmospheric pressure is in the range of 10-7 m, and
it is inversely proportional to the gas pressure. In particular test methods applying pressures less
than 1 atmosphere should be affected more by slip flow than tests in the high pressure range,
since the free path length of the gas molecules then extends more into the range of capillary
pores contributing to the flow. In any case the observed coefficient of permeability kobs depends
on the applied pressure and it is no longer a material constant.
It is proposed to correct the observed coefficient of permeability kobs by the Klingenberg
term, to yield the intrinsic coefficient of permeability kint as follows [2.15, 2.17]:
kobs = kint (1+ /pm)
with
(2.8)
kobs
pm
= Klingenberg number
19
kobs
non-viscous flow
. kint
kint
viscous flow
1/pm
Fig. 2.2 - Relationship between mean pressure pm and observed coefficient of permeability
kobs. [2.17]
In addition to the above mentioned influences from the pore structure and/or fluid
characteristics, the flow of gases through the pore spaces depends on the water content in the
pore system, since only the empty free pore space is available as flow paths. Therefore, the
apparent coefficient of permeability still depends on the degree of saturation of the pore
system. Since the slip flow is also affected by the water content, the Klingenberg number
depends on the degree of saturation as well. Both effects must be assessed experimentally.
The effect of the degree of saturation on the coefficient of gas permeability has been
investigated in numerous experiments: In the moisture range of oven dried specimens to
specimens in equilibrium with air of r.h.> 95 %, a variation of kobs and kapp has been observed
over three orders of magnitude [2.16, 2.18-2.20]. The effect of the water content on the
Klingenberg number is less pronounced: Carcasses et al. [2.20] reported a decreasing
contribution of the slip flow to overall flow with increasing water saturation.
The experimental assessment of the moisture effect on the gas permeability of concrete
relies on the assumption that the moisture is uniformly distributed in the volume of concrete
under test, i.e. no moisture gradients prevail along the flow paths. Therefore, in the past
different methods for preconditioning of test specimens were proposed aiming at a
homogenization of the water held in the specimens [2.16, 2.19, 2.21]. Concrete sections that
were subjected to drying will always exhibit moisture profiles, e.g. the near surface regions of
a concrete member, and the observed flow of gas by permeation will not be equal to the
volume flowing through a corresponding concrete section with the same mean moisture
20
concentration but uniformly distributed [2.16, 2.22]. Verdier and Carcasses [2.22] considered
the physical analogy of permeation with electrical conductance in order to analyze the effect
of known moisture profiles on the overall gas flow with the help of moisture dependent
coefficients of permeability. Tauscher [2.16] also found that the gas flow through sections of
variable moisture concentrations cannot be described by the flow parameter at a mean
moisture concentration but is strongly affected by the highest moisture content prevailing.
Drying may also induce microcracking: If cracking shows a preferential orientation, e.g.
perpendicular to the prevailing stresses, concrete sections will exhibit an anisotropic
behaviour with respect to gas permeability: Microcracks in parallel to the flow direction
drastically increase the volume flow while crack opening normal to the direction of gas flow
has a far lesser effect [2.23]. This effect must be addressed in gas permeability tests on
concrete surfaces exposed to drying conditions.
2.2.2 Water permeability
QL
t A p
(2.9)
QL 1
t A h
(2.10)
21
By equating (2.9) and (2.10) a relation can be found between the coefficient of permeability K
and DArcys coefficient as shown in equation (2.11):
Kw = K
(2.11)
Capillary Suction
Even in the absence of an external absolute pressure, porous media such as concrete can
take up liquids by the action of capillary forces. Surface forces of the liquids and solids are
responsible for this action which leads to a wetting of the internal solid surface in the capillary
pores (Fig. 2.3). The capillary pressure of the liquid (pore water pressure) is described by the
Laplace equation
2
(2.13)
pca p = pl pg =
r1
and r1 = r/ cos , then
pca p =
2 cos
r
(2.14)
22
= wetting angle
2 cos r 2
= 2 r cos
r
(2.15)
23
fa = external force
fg = force induced by mass of liquid column
fr = force caused by friction at pore wall
fi = inertia force
fcap= capillary force
h = height of liquid level outside specimen
z = penetration depth
z = velocity in direction z
z = acceleration in direction z
r = capillary radius
= viscosity of liquid
liq= density of liquid
Fig. 2.4 - Forces acting in capillaries
The balance of forces in a capillary results in
(2.16)
fa + fg fr fi + fcap = 0
and
fa = liq a h r2
(2.16a)
fg = liq a z r2
(2.16b)
fr = 8/r2 z z r2
(2.16c)
fi = liq r2 z z
(2.16d)
In equations (2.16c) and (2.16d) z and z represent the first and second derivative of z
with time t.
The differential equation (2.16) can be solved for time t and penetration depth z and
subsequent integration yields
2
2 cos
r
+ pa
z=
t
r
(2.17)
24
In equation (2.17) an external pressure pa is considered for the liquid, e.g. given by the
density and the height of the liquid level.
Eq. (2.17) does not serve directly for the evaluation of a suction experiment although the
influencing parameters are demonstrated. However, the equation postulates a square root of
time relation for the development of penetration depth, or, assuming a homogeneously
distributed porosity, a square root of time relation for the absorbed volume of liquid. The
proportionality factors may represent
z(t) = B t
(2.18)
with
or
Ml(t) = C
(2.19)
Ml (t) = mass of liquid absorbed at time t per unit area of surface exposed to liquid
(g/m2)
C
In experimental studies with water as absorbed liquid it has often been observed that the
penetration depth or absorbed water Ml does not strictly follow a square root of time relation.
Empirical corrections are made then [2.19, 2.28] with
Ml(t) = D + C t
(2.20)
n < 0,5
(2.21)
Hall et al [2.29] have compared the capillary suction behaviour of cementitious materials
for water and a number of organic liquids that pose environmental risks and therefore are of
interest for retaining structures. Their results clearly indicate that the penetration of organic
liquids follows the expected square root of time relation with the surface tension and the
viscosity of the liquid as rate controling parameters, i.e (/ )1/2. However, water exhibited
the above mentioned anomalous penetration behaviour. They conclude that chemomechanical interactions of water with the cement paste occur, causing microstructural
changes in the paste: for pre-dried or re-saturated specimens on-going hydration of cement
particles may account for some changes in the pore system, as well as swelling of the paste.
25
Migration
In section 2.1 it was pointed out that the diffusion of ions in a liquid provokes an electrical
field if the transport of cations is not balanced by a corresponding counter flow of anions.
Considering that in natural conditions as well as in most experimental set-ups not only one type
of ion is moving, and different ions have different mobilities, the build up of an voltage
difference is likely to occur. These phenomena are of particular interest in studying the ingress
of chloride ions into concrete, with a concrete pore solution containing various ions.
It has been claimed that in these cases simple diffusion tests evaluated on the basis of
Ficks diffusion laws do not reflect the transport mechanism prevailing in the actual process
and thus do not yield a valid material characteristic. The Nernst Planck equation (2.22)
describes the flow of mass due to the simultaneous action of a concentration gradient, an
electrical field and a flow of the solvent, i.e. convection [2.11, 2.30, 2.31]. The simultaneous
transport of multiple species and their charges in an arising electrical field has been studied
therefore, and a set of equations known as the Nernst-Planck equations must be solved for the
individual ions i participating in the transport process:
c z F
q i = D i i + i ci
+ cv
x RT x
(2.22)
with
q = mass flux (g/m2s)
D = diffusion coefficient (m2/s)
c = concentration (g/m3)
x = distance (m)
z = electrical charge
F = Faraday constant (J/V mol)
R = gas constant (J/mol K)
T = absolute temperature (K)
= electrical potential (V)
v = velocity of capillary flow (m/s)
26
Aside from the claimed shortcoming in the description of the real transport process, natural
diffusion tests in the diffusion cell require long test durations, especially when steady state
transport conditions are to be reached on concrete specimens with a relevant thickness.
Accelerated test methods impose an external electrical field as an additional driving force
for the transport of ions and the evaluation of the materials transport properties is performed
on the basis of the Nernst Planck equation. Water saturated specimens are used and the
convection term in equation (2.22) can then be omitted. This issue is further discussed in
Section 5.2: Ion Migration Methods.
2.5
Reference tests
Due to the increasing interest in transport phenomena in concrete, transport processes have
been extensively studied in recent decades. Following the distinction of processes according
to the driving forces the investigations were focused on diffusion processes, permeability
studies and capillary suction tests. The interest in migration processes in cement based
materials has arisen only recently.
Although the general principles of test methods were available from other disciplines, e.g.
ceramic industry, soil sciences, petrochemical industry, hydraulics etc. their application to
concrete involved a number of additional problems due to the specific properties of concrete, e.g.:
- the ageing of concrete due to on-going hydration
- reactivity of concrete with penetrating substances studied, for instance water,
carbon dioxide, chloride ions etc.
- variability of concrete properties with moisture content of concrete
- sensitivity of concrete pore structure to preconditioning, e.g. micro cracking upon
drying
- pore water composition, its effect on, and interaction with, transport processes.
It is evident that test methods must aim at controlling these effects, but also that
simplifying assumptions must be introduced and shortcomings will remain in the simulation
of the real process. The large number of influencing parameters may also be responsible for
the variety of test methods that have emerged each of them emphasizing some particular
aspects of transport by a special set up, test parameter or pre-treatment of the specimens,
while the general principles of the tests largely remain the same. In consequence, however, we
are far from having Reference Test Methods for the individual transport cases in a sense of
describing the true mechanism acting in reality, reflecting prevailing service conditions or
having a general acceptance in the research or engineering community. Despite these
limitations national and international standards and draft standards exist for some methods.
In RILEM Technical Committee 189-NEC, on-site test methods for transport mechanisms
were evaluated with regard to their suitability to indicate concrete durability characteristics,
taking into account their ease of handling, rapidity of performing a test as well as
uncertainties in the test conditions, in boundary conditions and in the state of the tested
concrete. In this context and for the purpose of comparison, reference is made to test methods
that draw on well defined test conditions and well known materials characteristics. However,
due to the additional efforts required, these are limited to laboratory application only. In [2.2]
a separate chapter presents well established laboratory test methods for transport parameters.
27
Furthermore, Alexander et al [2.32] have established a guide on the use and interpretation of
corresponding tests.
2.5.1 Diffusion tests
The general set-up of a diffusion test cell consists of a container which is separated by the
test specimen of given thickness into two chambers in such a way that the chambers contain
media of known concentrations c1 and c2 for the species under investigation, c.f. Fig. 2.5.
The test method developed by CEMBUREAU [2.35] is widely used for the measurement of the
gas permeability and procedures for the conduction of the test itself as well as for an appropriate
preconditioning of the test specimens have been developed, c.f. [2.16, 2.19, 2.21, 2.36].
Fig. 2. 6 gives an image of the set-up, with details of the pressure cell demonstrated.
28
Capillary suction experiments are designed in such a way that the driving force of an
absolute external pressure is excluded or minimized. Therefore, the test specimen is exposed
with the bottom end in contact with the liquid under investigation; the immersion is limited to
a few millimetres. The lateral sides of the test specimens are sealed in order to prevent
disturbances and evaporation; also the top surface of the specimen should be sealed to prevent
evaporation from the interior or condensation from the ambient atmosphere. However, the
sealing must not be rigid, thus no pressure in the capillaries can arise in front of the
penetrating liquid front due to compressed air.
A typical set-up is given in Fig. 2.8, a description of the test and recommendations on the
specimen preparation are given in [2.32, 2.36-2.38].
The layout of a migration test follows the same basic considerations as a diffusion test as
described in section 2.5.1, with the addition of an electrical field acting across the test
specimen. The electrical field is introduced into the test container by two electrodes which are
connected to a potentiostat. In chloride migration experiments the cathode is installed in the
up-stream cell and immersed in the catholyte, while the anode is immersed into the anolyte of
the down-stream cell. No general agreement has been reached on the voltage applied for the
electrical field: the desired accelerating effect of a high voltage is limited by possible heatbuild-up of the sample due to a high current. Voltages between 12 and 60 volts have been
recommended [2.32, 2.39-2.41].
The measurements during the operation of the test include monitoring of the flow of ions
by chemical analysis of the anolyte (and catholyte) or the conductivity of the anolyte as well
as the potential drop across the test specimen. In steady state conditions the diffusion
coefficient can be calculated according to the corresponding steady-state solutions of equation
(2.22). The ASTM C1202-97 method [2.42] measures the electrical charge passing the test
specimen.
With the same test set-up or at the termination of the migration experiment the resistivity
of the test specimen can be measured. The resistivity is related to the diffusion coefficient by
the Einstein relation
30
Deff =
k cl
= k cl
sa t
(2.23)
31
Fig. 2.10 - Migration cell with upstream and downstream compartment separated by the test
specimen.
Migration can also be studied in the non steady state condition, i.e. a penetration process is
monitored under the effect of an electrical field, and a penetration front is measured after a
test duration t. For chloride migration tests the penetration front of chlorides can be detected
by colorimetric tests after splitting the test specimens, e.g. spraying of silver nitrate. This
procedure is described in NT BUILD 492 [2.45].
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33
[2.28]
[2.29]
[2.30]
[2.31]
[2.32]
[2.33]
[2.34]
[2.35]
[2.36]
[2.37]
[2.38]
[2.39]
[2.40]
[2.41]
[2.42]
[2.43]
[2.44]
[2.45]
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34