High sensitivity electrical resistance sensors

for indoor corrosion monitoring

M. Kouril*, T. Prosek, B. Scheffel and F. Dubois
It is essential that corrosion monitoring of indoor atmospheres be highly sensitive, especially when
corrosion rates corresponding to the lowest standard corrosivity categories are supposed to be
identified within one or a few days. The electrical resistance (ER) technique in combination with
high sensitivity ER sensors enabled detection of corrosion loss on an atomic scale. The
magnetron sputtering method was used to produce sensors equipped with 50 to 800 nm metallic
track. The set of developed sensors represent a wide range of materials, e.g. copper, silver, iron,
lead and bronze. Laboratory experiments have proven that copper and silver sensors respond to
changes in relative humidity and temperature within minutes. Bronze and copper sensors are able
to detect changes in concentrations of volatile organic acids, which are common pollutants of
indoor atmospheres in museums.
Keywords: Electrical resistance, Corrosion monitoring, Thin film sensor, Magnetron sputtering, Corrosivity classification

Introduction needs for the anticipated corrosion conditions. As to

The electrical resistance (ER) technique is one of the
methods used for corrosion monitoring. It records
corrosion loss in metal thickness in time, and the slope
of the curve corresponds to the corrosion rate.
Deviations from the curve slope indicate changes in
corrosion conditions, whose information is effectively
used to identify the causes of corrosion aggressiveness
elevation and to verify the effectiveness of the respective
corrosion measure, i.e. it acts as an early warning. The
method is especially recommendable for the detection of
the onset of corrosion.1 Another advantage of the ER
technique is that in contrast to electrochemical methods
the presence of an electrolyte layer on the metal surface
is not inevitable. In that sense, there are no problems
with the method being used is atmospheric conditions
even at a low relative humidity (RH) of atmosphere.1
Moreover, it is used for corrosion monitoring of high
temperature corrosion, erosion corrosion or in non-
conductive environments. Despite other methods2–9
used for monitoring atmospheric corrosion, the resisto-
metric method provides information directly about the
metal corrosion loss.
The sensors for corrosion rate testing using the
resistometric method must comply with certain sensitiv-
ity and service life requirements. High sensitivity is
achieved by a small thickness of the sensor metallic
track. Compared to a less sensitive sensor, the dis-
advantage of a thin metallic track is its shorter service
life. The appropriate thickness of the metallic track thus
depends on what sensitivity and service life the user
Milan Kouril Institute of Chemical Technology, Prague, Czech
*Corresponding author, email kourilm@vscht.cz
indoor conditions with the corrosivity ranging from IC1
to IC5,10 metallic track thicknesses tend to be opted in
the order of tens and hundreds of nanometres. For
outdoor conditions with corrosivity category C2,11 it is
recommendable to use sensors with the metallic track
ranging within the orders of units and hundreds of
micrometres so as to ensure their functioning for at least
1 year.
Monitoring of the corrosion rate corresponding to the
lowest corrosivity categories of indoor atmosphere
corrosion aggressiveness is inevitable to make sure that,
for instance, sensitive electronic equipment is protected
and that metallic artefacts are treated right and safely
when exhibited, transported or stored in depositories.9
The atmosphere corrosivity category is determined on
the grounds of the corrosion rate of steel, zinc, copper
and silver. Corrosion rates ranging within the order of
hundreds of mg m22 a21 correspond to the second
lowest corrosivity category IC2. Expressed by the loss in
metal thickness in time, corrosion rates in IC2 atmo-
sphere correspond to the order of tens of nm a21.
Hence, should the corrosion monitoring system be able
to provide an early warning, i.e. within 24 h, that
corrosivity increased by one category, the corrosion
sensor must be able to detect the change on the metallic
track thickness within the order of tenths of nanometres.
Such sensitivity was approached by Cai and Lyon12 with
their zinc and steel based resistometric sensors.
Standards for corrosivity classification introduce four
metals only, although other metals may differ in their
response to a great extent. Whereas zinc and steel or iron
are very sensitive to sulphur dioxide, silver in contrast to
iron is highly sensitive to sulphane.13 Compared to all
the other common metals, lead is the most sensitive to
organic acids.13,14 Especially for its specific corrosion

ß 2013 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 11 September 2012; accepted 25 November 2012
282 Corrosion Engineering, Science and Technology 2013 VOL 48 NO 4 DOI 10.1179/1743278212Y.0000000074
 Kouril et al. High sensitivity ER sensors for indoor corrosion monitoring

behaviour and its frequent presence among metallic

artefacts, lead would deserve a separate and standar-
dised atmosphere corrosivity assessment.
The corrosivity classification has a relatively universal
application. As the ISO 11844 standard or the Sacchi
and Muller classification15 not only describes corrosivity
category determination on the basis of corrosion rate
but also enables estimating the corrosivity category
according to the conditions (type of indoor atmospheric
environment, temperature, RH, etc.), the corrosivity
categories can be used to describe the quality of
atmosphere from the perspective of materials other than
metals.16 Air reactivity monitoring is a method of
evaluating the quality of makeup and recirculation air
characterising the museum or archive environment and
evaluating the effectiveness of chemical filters.17
This paper presents a set of new corrosion sensors that
can be used for high sensitivity corrosion monitoring,
and extends the portfolio of high sensitivity sensors by
materials that are common in historical artefacts, but
whose corrosion rates are not registered in corrosivity
classification standards. The sensors’ design has been
innovated so as to avoid inaccuracies in thickness loss
testing caused by non-uniform corrosion on the interface
of the sensing and reference parts of the sensor.
1 Traditional concept of atmospheric corrosion sensor
Experimental
of identical thicknesses. We have adjusted the relation so
Electrical resistance technique that the assumption of a known initial thickness is always
The traditional ER technique is based on identification met. The thickness of the reference part, which does not
of the change in electric resistance of a thin layer of essentially change throughout the sensor’s service life,
metal in time. The thinner the layer of metal as a result acts as the initial thickness in relation (2). Should the
of corrosion, the higher the electric resistance of the sensor be used repeatedly, the user must remember the
metallic track. Moreover, the electric resistance of initial resistance of the sensing part that has not been
metals depends on temperature because of its positive affected by corrosion when using relation (1). The new
temperature coefficient. Therefore, a compensation of relation (2) eliminates this limitation
the temperature dependent drift of ER is a must. This  
compensation is realised by a division of sensor into Rref,0 Rref
Dh~h0,R : { (2)
corroding and non-corroding parts by measurement Rsens,0 Rsens
of both resistances and calculation of their ratio. The where h0,R is the initial thickness of the reference part.
corroding part of the sensor is called a coupon or Precision of the method depends on the accuracy with
a sensing part, and the non-corroding part acts as a which electric resistances are determined. The most used
reference part. The reference part of the sensor has a method is the four-wire resistance measurement. The
similar shape to that of the sensing part but is covered ratio of electric resistances of reference and sensing parts
with a protective coat to be separated from the corrosion can be measured by an ac bridge network.1 The loss of
environment. The traditional relation for calculating metal thickness or the corrosion rate can be expressed as
corrosion loss based on the ratio of real time resistances, a ratio of resistances of the corroding track at the start
initial resistances and initial thickness of the metallic of exposure and at a given time.12,19 Figure 1 shows the
track has the following form18 traditional shape of atmospheric corrosion sensors,18,20
 
Rref : Rsens,0 where the testing current passes between two terminal
Dh~h0 : 1{ (1) circuit contacts with the voltage that let the current pass
Rsens Rref,0
through the metallic track being measured between two
where h0 is the initial thickness of the sensor’s metallic other spots on the sensing and reference parts.
track, Dh is the mean thickness loss, Rref is the ER of the
reference part, Rsens is the ER of the sensing part, Rref,0 Sensor’s design
is the initial ER of the reference part and Rsens,0 is the The coat protecting the reference part from corrosion is
initial ER of the sensing part. usually applied so as to have the edge pass through the
This relation anticipates the same initial thickness for symmetry axis of both parts of the sensor (Fig. 1).
both sensing and reference parts. However, this assump- However, the organic coat and metal interface tends to
tion is not always lived up to, which is demonstrated by be a weak point in terms of corrosion protection. The
the fact that the initial resistances of the sensing and protective coat may be undercorroded, and the metallic
reference parts are never ideally identical. The testing track on the sensing and reference part interface may be
itself in the corrosion environment is often preceded by intensively attacked. The original thing about the
restoration of the sensing part surface by smooth structure of sensors designed and used by us is that the
grinding or pickling, which abandons the assumption sensor’s sensing and reference parts are connected by an

Corrosion Engineering, Science and Technology 2013 VOL 48 NO 4 283

Kouril et al. High sensitivity ER sensors for indoor corrosion monitoring
2 New concept of atmospheric corrosion sensor
H shaped bridge, and the protective coat borderline
passes approximately in the middle of the bridge
(Fig. 2). Despite the traditional design (Fig. 1), the
borderline of the protective coat is a part neither of the
sensing nor the reference part as the bridge serves only
as a conductor for passage of testing current, and the
voltage scanning points are placed in a safe distance
from the coat edge.
Manufacturing of sensor
The indoor sensors were produced by means of
magnetron sputtering, a technology that is referred in
some recent studies.19,21 Manufacturing comprises of the
deposition of contacts, a thin film deposition by vacuum
technology and vapour mask structuring. A fine grained
Al2O3 alumina was used as substrate material. Copper,
silver, bronze (CuSn8), lead and iron sensors were
prepared. Examples of sensors without the reference
part protection are shown in Fig. 3.
3 Examples of high sensitivity atmospheric corrosion sensors: Pb–400 nm (left), Fe–800 nm, CuSn8–400 nm, Cu–50 nm,
Ag–50 nm (right)
284 Corrosion Engineering, Science and Technology 2013
Loggers
AirCorr I and AirCorr I Plus loggers (NKE electronics)
were used to measure and record the corrosion losses of
high sensitivity corrosion sensors. They are autonomous
battery driven loggers equipped with a built in connector
providing connection to corrosion sensors. The AirCorr
I version employs one corrosion sensor within a given
period of time, while the AirCorr I Plus version works
with two sensors, recording concurrently the RH and
temperature. Results are recorded by WinAirCorr soft-
ware (NKE electronics).
Results and discussion
Sensitivity and reproducibility tests of corrosion
sensors
A great advantage of laboratory tests is the possibility
to control exposure conditions with a relative accu-
racy. Corrosion sensors were thus exposed to various
regimes under changing conditions, response of corro-
sion sensors to the changed conditions was monitored
and reproducibility of the response was assessed.
Temperature and relative atmospheric humidity were
the only features changed during the first experiment,
without any corrosion stimulator being added to the
corrosion atmosphere. The curves of RH and tempera-
ture in time are described in Fig. 4.
Figure 5 records corrosion loss (reduction of metallic
track thickness in the sensing part of the sensor) in time
for four concurrently exposed copper sensors. The initial
thickness of the sensor metallic track was 500 nm. The
design of the sensor was meant to ensure that the
sensor’s service life was at least 2 years under the
conditions of a medium corrosivity indoor atmosphere
that corresponds to the corrosivity category of IC3
according to the ISO 11844-1 standard. The overall view
(Fig. 5) shows that the sensors react to the increase in
RH from 50 to 85% at 20uC. The increase of tempe-
rature by 10uC immediately accelerates the corrosion
rate. The corrosion loss versus time curve during one
24 h period of time has a parabolic shape, which is typi-
cal for copper corrosion under atmospheric conditions.13
The total corrosion losses assessed after six daily cycles
were 6?6, 5?2, 5?8 and 6?1 nm. The deviation of ex-
treme values from the mean value does not exceed 12%.
Such reproducibility can be considered excellent in the
VOL 48 NO 4

4 Temperature and relative humidity variations during
laboratory corrosion testing
area of corrosion monitoring. Another question is
whether the recorded corrosion loss corresponds to the
corrosion loss of the metal bulk, i.e. what is the accuracy
of corrosion rate determination by copper resistometric
sensors. For that purpose, corrosion copper coupons
were exposed with the sensors, and their corrosion was
coulometrically evaluated after exposure. A negligible
layer of corrosion products was galvanostatically re-
duced, and the amount of copper that converted in an
oxidised form during the corrosion test was calculated
from the charge necessary for reduction. This amount
recalculated to the loss of thickness of three coupons
exposed in parallel corresponded to 5?2, 6?2 and 6?3 nm.
The coulometrically specified average loss of thickness of
cooper is equal to the mean value of the loss of thickness
identified by the resistometric sensor.
Copper sensors react to the increase in RH from 50 to
85% almost immediately. The time to respond was
shorter than the selected sampling period of 15 minutes.
The sensor with a 500 nm metallic track is not able to
detect corrosion at RH lower than 50%. In spite of that,
the sensor’s sensitivity is sufficient for detecting pro-
cesses on an atomic level, where corrosion converts one
layer of metal atoms, i.e. on the level of tenths of
5 Corrosion depth record of four parallel Cu–500 nm sen-
sors exposed to varying temperature and RH
Corrosion Engineering, Science and Technology
Kouril et al. High sensitivity ER sensors for indoor corrosion monitoring
6 Corrosion depth record of three parallel Cu–50 nm sen-
sors exposed to varying temperature
nanometres. A copper sensor with a 50 nm metallic
track provides even higher sensitivity (Fig. 6).
For a cut of the graph of the corrosion loss of three
copper sensors exposed in parallel with a metallic track
thickness of 50 nm, see Fig. 6. Reproducibly recorded
thickness losses on the level of hundredths or even
thousandths of nanometres may be merely considered a
conversion of a specific amount of metal atoms on
the cross-section of the metallic track in an oxidised
form, i.e. corrosion products rather than a uniform
loss of metal over the entire exposed surface. Such
high sensitivity is essential for corrosion monitoring
that must be able to detect a change of corrosivity
category from IC1 (very low corrosivity) to IC2 (low
corrosivity) as defined by the ISO 11844-1 standard
within 1 day, yet ensure at least 1 year service life for
corrosivity IC2.
From a practical point of view, silver sensors with a
50 nm metallic track show the same sensitivity as Cu–
50 nm copper sensors. The corrosion loss is again
recorded reproducibly with accuracy on the level of
hundredths and thousandths of nanometres (Fig. 7).
Moreover, the change of RH from 30 to 50% did not
cause any change of the slope of the corrosion loss
versus time curve, which confirms a well known fact that
silver sulphide developing in indoor atmospheres due to
the presence of traces of sulphane at low RH is formed
as a result of direct chemical reaction with silver, and the
slope is thus not much dependent on the presence of
water.22
The response of lead and iron sensors was tested the
same way. As shown in the graph (Fig. 8), reproduci-
bility of the measurements of the loss of thickness of
these materials is remarkably lower than in the case of
sensors made from silver and copper. It is probably
given by more frequent localised attacks in the starting
phases of corrosion of these metals, namely, iron.
However, it is obvious that corrosion losses of iron
and lead are higher by an order under the same
conditions than those of silver and copper, with lead
being specifically sensitive to volatile organic substances
in the atmosphere. Therefore, it may be advisable to use
sensors made from lead and iron for corrosion
monitoring of these metals instead of deriving their
corrosivity from the responses of silver and copper.
2013 VOL 48 NO 4 285
Kouril et al. High sensitivity ER sensors for indoor corrosion monitoring
7 Corrosion depth record of three parallel Ag–50 nm sen-
sors exposed to varying temperature
Laboratory tests in air contaminated with
organic acids
A chamber allowing for corrosion measurements in air
with low and well controlled concentrations of gaseous
pollutants was designed. A setup consisting of an air
dehumidifier, air filter, gas generator, humidifier, expo-
sure chamber and exhaust air treatment unit has been
built. A polluted air generator produces the target
pollutant level. This gas generator includes an oven with
temperature precisely controlled between 30 and 100uC
(¡0?1uC) and a mass flow controller. It is possible to
reach any concentration to ,1500 ppb of acetic acid and
to ,3000 ppb of formic acid in the outlet air.
A measurement performed in humid air at an RH
range from 15 to 80% containing acetic acid at
concentrations from 0 to 870 ppb on a bronze thin film
sensor with a thickness of 500 nm (CuSn8–500 nm) is
given in Fig. 9. The experiment was carried out at 20uC
in the chamber described above.
It is obvious that the corrosion rate of bronze increased
with both RH and acetic acid concentration. The
corrosion depth started to increase rapidly after the
introduction of the pollutant into the air, which shows the
rapid response of the sensor. On the contrary, it took
several days until the corrosion rate started to decrease
after a decrease in pollutant concentration. This was
observed even under conditions where the RH was also
8 Total corrosion depth of three parallel sensors after
test cycle at varying temperature and relative humidity
286 Corrosion Engineering, Science and Technology 2013
9 Corrosion depth measured in air containing acetic acid
using CuSn8–500 nm sensor: numbers give concentra-
tion of acetic acid and relative humidity
reduced to low levels, see e.g. the transition 870 ppb–80%
RH to 0 ppb–15% RH in Fig. 9. Since the air in the
chamber is exchanged within ,15 min, this indicates that
a film of the adsorbed pollutant was present on the metal
surface long after the pollutant was removed from the air.
A simple model for the effect of the acetic acid air
concentration and RH on the corrosion rate of bronze
was proposed. The corrosion rate rcorr can be expressed as
rcorr ~RH(AzB cAA ) (3)
where cAA is the concentration of acetic acid in ppb, RH
is the relative humidity in % and A and B are constants.
A similar experiment was carried out in air containing
formic acid at concentrations from 0 to 1590 ppb and at
RH from 15 to 80%. However, the air corrosivity was
increased systematically in this experiment in order to
establish a threshold level of the formic acid concentra-
tion, which leads to an unacceptable corrosion rate of
the materials tested. Cu–500 nm, Pb–800 nm and Fe–
800 nm sensors were tested in three replicates.
The corrosion depth record for a Cu–500 nm sensor is
plotted in Fig. 10. The experiment started in clean air at
15% RH. The corrosion rate was below the detection
limit until the RH was increased to 70%. It stabilised
after ,4 days at 4–5 nm a21 and did not change
10 Corrosion depth measured in air containing formic
acid using Cu–500 nm sensor: numbers give concen-
tration of formic acid and relative humidity
VOL 48 NO 4

Table 1 Estimated threshold levels of formic acid concentration in air leading to change in corrosivity category
according to ISO 11844-1
Corrosion rate threshold according
Change in corrosivity category to ISO 11844-1/nm a21
IC1RIC2 6 220,cFA,460
IC2RIC3 22
IC3RIC4 101
although the RH was further increased to 80%. No
dramatic effect of formic acid on copper corrosion was
observed at concentrations from 10 to 220 ppb. When
the formic acid concentration increased to 460 ppb, the
corrosion rate changed to ,20 nm a21. It stayed at this
level at 1000 ppb as well.
A further increase in corrosion rate to ,50 nm a21
was noted at the maximal formic acid concentration of
1590 ppb. When the concentration was dropped to 190,
80 and 0 ppb, the corrosion rate decreased gradually to
low values.
Based on the conducted experiments, the threshold
levels of formic acid in air at 80% RH and at 20uC for
corrosivity categories defined by the ISO 11844-1
standard can be estimated (see Table 1). Such a formic
acid concentration has been reported in museums,
churches and other cultural heritage premises by several
authors.23–26
Conclusions
1. Magnetron sputtering enables the production of a
wide range of metals with a precisely controlled
deposition of the metal layer thickness that determines
the sensitivity of the resistometric sensor for measuring
corrosion loss.
2. The sensitivity of sensors on an atomic level was
identified under the conditions of changing temperature
and RH when corrosion changes one layer of metal
atoms, i.e. on the level of tenths of nanometres.
Reproducibly recorded thickness losses of very sensitive
sensors on the level of hundredths of nanometres may be
merely considered a conversion of a specific amount of
metal atoms on the cross-section of the metallic track
into corrosion products rather than a uniform loss of
metal over the entire exposed surface. Such high
sensitivity is essential for corrosion monitoring that
must be able to detect a change of a corrosivity category
from IC1 (very low corrosivity) to IC2 (low corrosivity)
as defined by the ISO 11844-1 standard within 1 day, yet
ensure at least 1 year service life for corrosivity IC2.
3. The recorded corrosion loss versus time curves
confirm the well known facts about the corrosion
processes kinetics in atmosphere and the different
sensitivities of various metals to different pollutants.
High sensitivity resistometric sensors may thus be used
for studying the kinetics of corrosion processes.
4. The reproducibility of measurements of corrosion
losses of copper and silver is high compared to the
reproducibility identified for lead and iron sensors.
Acknowledgements
The authors gratefully acknowledge the financial sup-
port by the European Commission under the Seventh
Framework Programme (contract no. 226539) and by
Corrosion Engineering, Science and Technology
Kouril et al. High sensitivity ER sensors for indoor corrosion monitoring
Corresponding threshold concentration
of formic acid cFA/ppb
460,cFA,1000
cFA.1590
the Czech Ministry of Education under special purpose
support to college research programmes (resolution
no. 21/2011).
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