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Electrochemical Noise Monitoring
Electrochemical Noise Monitoring
a
Tianjin Key Laboratory of Composite and Functional Materials, School of Material Science and Engineering, Tianjin University, Tianjin, P.R. China;
b
CAS Key Laboratory of Nuclear Materials and Safety Assessment, Institute of Metal Research, Chinese Academy of Sciences, Shenyang, Liaoning,
P.R. China; cDepartment of Chemical and Materials Engineering, University of Alberta, Edmonton, Alberta, Canada
Introduction
spectroscopy (EIS) and electrochemical noise (EN) have
Atmospheric corrosion of metal is one of the most common been applied to on-line corrosion monitoring. Yadav et al.
and important corrosion degradation processes. This kind of [8] and Thee et al. [9] used EIS measured at 105–0.01 Hz to
corrosion is an electrochemical corrosion process under a study the simulated atmospheric corrosion of galvanised
thin electrolyte film [1]. The atmospheric corrosion of metals steel and weathering steel in a wet–dry cycling condition.
is mainly determined by the relative humidity, wetting time, One of the pitfalls of EIS measurement is that it usually
temperature, light irradiation time, impurity ions, pH, acid takes some time to complete the data acquisition process at
fog, ion concentration, among other factors [2–4]. It has the whole frequency range. In view of this, Nishikata et al.
been reported that the global economic losses caused by [10] proposed to use impedance at 10 mHz (Z10mHz) to on-
atmospheric corrosion is up to US$100 million each year line monitor the atmospheric corrosion of weathering steel
[5], and there is a need to on-line monitor atmospheric cor- and found that Z10mHz correlated well with the weight loss
rosion of metallic materials for service life evaluation and safe data. EIS has been successfully used in atmospheric corrosion
operation [6]. monitoring, but its setup is usually complicated. To make the
To achieve the on-line corrosion monitoring of metal, the on-line monitoring device more portable and light in weight,
measurement technique must be reliable and can be applied investigators began to use EN for on-line corrosion monitor-
in an outdoor atmosphere for a long time. Traditional ing in recent years [11–15]. The advantages of using EN to
methods such as weight loss can obtain the average corrosion monitor atmospheric corrosion are as follows: (1) EN exper-
rate for a certain time, but the instant corrosion behaviour iments are easy to set up, (2) EN is an in situ electrochemical
cannot be acquired. In addition, weight loss is not very suit- method that eliminates the need to apply an external signal
able for identifying the early stage corrosion because the for the collection of experimental data (this is big different
weight loss has very small level [7]. In recent years, electro- from EIS), (3) EN can obtain the instant corrosion process
chemical methods including electrochemical impedance rapidly and (4) EN can analyse the corrosion mechanism of
CONTACT Da-Hai Xia dahaixia@tju.edu.cn Tianjin Key Laboratory of Composite and Functional Materials, School of Material Science and Engineering, Tianjin
University, Tianjin 300072, P.R. China
© 2017 Institute of Materials, Minerals and Mining Published by Taylor & Francis on behalf of the Institute
CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY 433
an electrochemical system without establishing its electroche- mechanism of the reaction process. The position of the maxi-
mical model in advance. mum relative energy in the EDP corresponds to the dominant
For on-line atmospheric corrosion monitoring using EN, process in the corrosion processes, and a change in the pos-
the measurement is usually conducted at zero resistance ition can reflect evolution of the corrosion process [20,21].
ammeter (ZRA) mode under which the electrochemical This work aims to establish a suitable electrode system for
potential noise (EPN) and electrochemical current noise atmospheric corrosion monitoring and to identify the cor-
(ECN) can be recorded synchronously. In atmospheric con- rosion process by statistics and wavelet transform. Two elec-
ditions where the corrosion is proceeding under an extremely trochemical probes were used to monitor the atmospheric
thin electrolyte film, two major issues should be considered. corrosion of Q235B and T91 steels; subsequently, the cor-
One critical issue is to establish the electrode system under rosion form and corrosion process during early stage atmos-
the atmospheric condition for the EN measurement. For pheric corrosion were discussed.
example, Jamali et al. [16] used 0.5 M NaCl soaked filter
paper as the electrolyte to perform EIS and EN to evaluate
the corrosion resistance of paint coating. García-Ochoa Experimental procedure
et al. [12] used a copper electrode and a wetted cloth to per- Materials
form the EN test on copper surface in an outdoor atmos-
phere. Although these electrochemical measurements have The chemical compositions of Q235B and T91 steels are
been successfully set up, the soaked filter paper and cloth shown in Table 1. Q235B is a low carbon steel, and T91 is
would change the surface state and may accelerate the cor- a martensitic heat-resistant steel. The microstructures of
rosion rate of the tested materials. As a result, the corrosion Q235B and T91 are shown in Figure 1(a) and (b), respect-
tests were not conducted in the real atmosphere condition. ively. Q235B steel has a lamellar pearlite structure with a
Therefore, there is a need to establish a more suitable elec- small amount of ferrite. The T91 steel has a needle-like ferrite
trode system for atmospheric corrosion monitoring. structure.
Another critical issue is how to extract useful information
from the EN spectrum by using signal processing methods
Atmospheric corrosion probes and EN measurement
[17]. Generally, time domain (mainly refers to statistical
methods), frequency domain (such as fast Fourier transform, Two modified time of wetness probes were used in the atmos-
FFT) and time–frequency domain (such as wavelet trans- pheric corrosion monitoring, and one of the probe is shown
form) are three major analysis methods. Although FFT is a in Figure 2. For each probe, three nominally identical
common method of EN data analysis, one of the pitfalls of Q235B or T91 electrodes were embedded into the poly-
FFT is that it has a fixed resolution caused by the width of urethane sealant. The electrode on the left was used as the
the windowing function [18]. A wide window gives better fre- reference electrode (RE), and the other two electrodes were
quency resolution but poor time resolution. A narrow win- used as working electrodes (WEs), marked as WE1 and
dow gives good time resolution but poor frequency WE2. Each Q235B or T91 electrode had an exposed area of
resolution [17]. EN signals are frequently non-stationary; 4.2 cm2; non-working surfaces were covered with a poly-
wavelet transform is more suitable for analysing non-station- urethane sealant. A thin polyethylene terephthalate (PET)
ary signals [19]. Wavelet transform can transform the EN film with a thickness of 0.2 mm was placed between adjacent
data into a series of signals with different frequencies. The electrodes, and insulating glue was painted between them.
energy distribution of each signal can be calculated, and The two atmospheric corrosion probes were exposed to the
then the energy distribution plot (EDP) of all signals can be outdoor atmosphere without a cover in Tianjin. Tianjin is
obtained. EDP contains the information about the located at east longitude 117°38′ , latitude 38°98′ and 5 m
Figure 1. Microstructure of the metal materials used as electrodes in the atmospheric corrosion probe (a) Q235B steel and (b) T91 steel.
434 C. MA ET AL.
Wavelet analysis
To identify the corrosion form, the EN data were decomposed
to wavelet crystals at different levels and wavelet approxi-
Figure 2. (a) Electrochemical probe for atmospheric corrosion monitoring (the mation. The energy contribution of a wavelet crystal, which
three electrodes are made of Q235B or T91); (b) a schematic diagram of EN
measurement using a ZRA (WE, working electrode, RE, reference electrode, ‘E’ is commonly used in EN analysis, is defined below. The energy
means potential, ‘I’ means current). contribution of each crystal to the overall signal is given by
1 2 J 2
N
Ejd = d
k=1 j,k
(j = 1, 2, . . . , J), (3)
above sea level. The probes were placed at 45° angles to the E
floor during the atmospheric corrosion monitoring 1 2 J 2
N
experiments. EJs = s ,
k=1 J,k
(4)
E
The EN system comprised a Compact FieldPoint (CFP)
industrial controller module (National Instruments, NI), a where SJ,K and dj,k are the wavelet coefficients. The orthogon-
Field-Point analog input module CFP-AI-118 (NI) and a ality of the wavelets allows calculation of the overall energy
ZF3 Potentiostat (Shanghai Zhengfeng Company), which using
was used to constitute the ZRA test circuit [19]. The CFP sys- J
tem was used to acquire potential and current data. The E = EJs + Ed .
j=1 j
(5)
potential and current were amplified and digitised by using
The number of iteration steps J is defined by the user. It is
a 16-bit A/D converter with a resolution of 0.03 mV and
experimentally determined that for a level J = 7, the valu-
0.3 nA. A low-pass filter of 10 Hz was applied during data
able mechanistic information is captured in detail crystals
recording [22]. EN was measured under ZRA mode, the
D1–D7 and wavelet approximation A7 [25,26]. The type
EPN was recorded between RE and WE1 and the ECN was
of the used wavelet transformation was db4, which is a
recorded between the two working electrodes (WE1 and
Daubechies wavelet [26]. Short timescale crystals, typically
WE2). The test frequency of EN was set at 2 Hz, because
D1 and D2, are associated with uniform corrosion. Long
EN in corrosion reaction is considered to be noise at low fre-
timescale crystal A7 provides information on localised
quency, as claimed by Cottis in his review paper [23].
corrosion.
Temperature and relative humidity were recorded every
In the present paper, energy values of D1 and A7 are
10 min with a DL-WS20 data recorder. Weight loss data at
calculated every 1 h, and the cumulative probability curves
10 and 20 days were obtained and were converted to polaris-
for D1 and A7 are used as indicators for corrosion process
ation resistance according to the following equation:
identification. The cumulative probability, p, was plotted as
ba bc B a function of the wavelet energy D1 or A7. To obtain the
Rp = = , (1)
2.303(ba + bc ) · icorr icorr cumulative probability, the parameter values were sorted
into ascending order and p was derived as n/(N + 1),
where Rp is polarisation resistance and ba and bc are Tafel
where n is the value rank in the sorted list, and N is the
constants for anodic reaction and cathodic reaction,
frequency of occurrence of the value. The results have
B = ba bc /2.303(ba + bc ).
been presented to clearly show the distribution of the
values and allow for easy comparisons with previous
results.
Statistics and wavelet analysis of the electrochemical
noise spectrum
Corrosion morphology
Statistics analysis
The EN data were batch processed using Labview 8.6. First The morphology of Q235B and T91 after exposure to the
the direct current (dc) component was removed from original Tianjin urban atmosphere was observed by a KEYENCE
EN data by a five-order polynomial fitting, a frequently used VHX-5000 microscope.
CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY 435
Results and discussion over 20 days, the standard deviations of ECN and EPN
decrease with time. For instance, after 16 days, the standard
EN monitoring results of Q235B steel
deviations of ECN and EPN are lower than those at the initial
Figure 3(a,b) shows the EPN and ECN measured by a Q235B couple of days. This implies that the rust layer would protect
steel probe that was exposed to an outdoor atmosphere in the metal from corrosion to some extent.
Tianjin over 20 days. Figure 3(c,d) shows relative humidity To study the atmospheric corrosion process of Q235B in
and temperature values during a 20-day exposure. The rela- detail, three groups of EPN and ECN data obtained on day
tive humidity and temperature fluctuate in opposite direc- 3, day 9 and day 19 in the same weather conditions (i.e. on
tions over the 20-day period: when the temperature rises, rainy days when the metal surface is totally wetted) are com-
the humidity falls; when the temperature is low, the humidity pared in Figure 4. The reason for selecting these three data is
is high. The temperature ranges from 8 to 30.6°C, and the that we have to compare the EN data in the same humidity,
relative humidity ranges from 13.4% to almost 100%. because the humidity would affect the amplitudes of EPN
Figure 3(a,b) shows that EPN and ECN fluctuate around and ECN. These EPN and ECN data are selected from
0 mV and 0 nA, respectively. The EPN and ECN have the Figure 3 on day 3, day 9 and day 19, respectively. It can be
same variation trends: (1) When the humidity is low, the seen from Figure 4 that, at the beginning stage of atmospheric
ECN and EPN amplitudes are very small, only a few exposure, the amplitudes of ECN and EPN of Q235B are lar-
nanoamps and millivolts, respectively, indicating that the cor- ger than those on day 9 and day 19. On day 3, the maximum
rosion rate is significantly low. (2) When the relative humid- amplitudes of ECN and EPN are 19.1 nA and 4.6 mV,
ity is increased to 65% or even higher, the fluctuation respectively; however, maximum amplitudes of ECN and
amplitudes of the ECN and EPN increase obviously; there- EPN decrease to 3 nA and 2.3 mV, respectively, on day
fore, the corrosion rate of the Q235B steel is significantly 9. These two values continue to decrease to 0.58 nA and
increased accordingly. 0.96 mV, respectively, on day 19. The decrease in ECN and
Figure 3(f,g) shows the calculated standard deviation of EPN amplitudes is due to the formation of a rust layer on
ECN and EPN, respectively. The maximum value of the stan- the Q235B surface. As the exposure time is prolonged, the
dard deviation of the ECN is 35.4 nA cm−2, and the maxi- formation of rust layer may retard the mass transfer process
mum value for EPN is 7.88 mV. As the relative humidity of the anodic reaction.
increases, both of the standard deviations of ECN and EPN To identify the corrosion process more visually, the prob-
increase, illustrating that the corrosion reactions are acceler- ability density distribution of EPN and ECN shown in
ated. The obtained noise resistance Rn is shown in Figure 3(e). Figure 4 is analysed by statistical analysis. The probability
The evolution of Rn is closely linked to the humidity: Rn and density distributions are plotted as a function of the EPN
humidity have the same variation trends. As the humidity and ECN amplitudes, as shown in Figure 5. The probability
increases, Rn decreases accordingly; as the humidity density distribution curve shows that, for Q235B steel, the
decreases, Rn increases accordingly. EPN and ECN distributions are mainly concentrated around
Q235B is a kind of low carbon steel, which shows poor 0, and the maximum density values are located at the centre.
corrosion resistance in the atmosphere, a layer of rust As the rust layer becomes thicker and the EPN and ECN dis-
forms on the surface of the electrode in a short time. The tribution becomes narrower, the corrosion rate of Q235B is
impact of this rust layer on the corrosion resistance in the decreased. The probability density distribution curve implies
early stage can be reflected in the EN. Observing the data that both EPN and ECN fluctuate around 0, and there is no
Figure 3. EN monitoring results of Q235B steel exposed to Tianjin urban atmosphere over 20 days. (a) Relative humidity; (b) temperature; (c) EPN; (d) ECN; (e) noise
resistance; (f) ECN standard deviation and (g) EPN standard deviation (some data are lacking in Figure 3 due to a power outage).
436 C. MA ET AL.
Figure 4. Typical EN spectrum of Q235B steel on rainy days. (a–c) EPN spectrum on days 3, 9 and 19, respectively; (d–f) ECN spectrum on days 3, 9, and 19,
respectively.
apparent transient peaks existed in the EN spectrum. This EN monitoring results of T91 steel
correlates well with the characteristic of EN during uniform
Figure 6(a,b) shows EPN and ECN data of T91 steel probe
corrosion [27].
exposed to the Tianjin outdoor atmospheric environment
for 20 days. Figure 6(c,d) shows the relative humidity and
temperature values during a 20-day exposure. The tempera-
ture and relative humidity fluctuate in opposite directions
over the 20-day period. The temperature ranges from 10.5
to 30.1°C, and the relative humidity ranges from 20.5% to
almost 100%.
The ECN and EPN of the T91 steel fluctuate around
0. When the temperature is relatively high and the humidity
is relatively low (in dry condition), fluctuation of the ECN
and EPN amplitudes is small: 0.5 nA and 4.9 mV, respect-
ively. ECN and EPN amplitudes remain basically unchanged
during the dry condition. Under this condition, the corrosion
rate is extremely low because there is no continuous thin elec-
trolyte on metal surface. However, when the relative humidity
increases (i.e. on rainy days), the ECN amplitude fluctuation
significantly increases, reaching to 100 nA. The increased
ECN amplitude indicates that the corrosion rate of T91
steel in the high humidity condition is accelerated. The
EPN of T91 steel also changes with the change in relative
humidity and temperature, and the trend of the EPN changes
are consistent with the trend of the ECN fluctuation.
Figure 6(f,g) shows the calculated standard deviations of
ECN and EPN, respectively. The maximum values of the stan-
dard deviations of the ECN and the EPN are 22.6 nA and
11.10 mV, respectively. It is generally accepted that EPN is
related to the type of corrosion whereas ECN is associated
with corrosion intensity [27]. At dry conditions with lower
humidity, the ECN standard deviation value is low, leading
to a very low corrosion rate of T91 steel. On rainy days with
high relative humidity, the corrosion rate is increased, as indi-
cated by the increased standard deviation of ECN.
Figure 5. Probability density distribution plot of EPN and ECN shown in Figure 4;
(a) probability density distribution of the EPN of Q235B on days 3, 9 and 19; (b) To further study the atmospheric corrosion process of T91,
probability density distribution of the ECN of Q235B on days 3, 9 and 19. EPN and ECN data were collected on day 8, day 10 and day 19
CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY 437
Figure 6. EN monitoring results of T91 steel exposed to Tianjin urban atmosphere over 20 days. (a) Relative humidity; (b) temperature; (c) EPN; (d) ECN; (e) noise
resistance; (f) ECN standard deviation and (g) EPN standard deviation. (Some data are lacking in Figure 3 due to a power outage.)
under rainy days when the metal surface is totally wetted. distributions are plotted as a function of EPN/ECN ampli-
Figure 7(a–c) shows the EPN on day 8, day 10 and day 19, tudes. The probability density distribution curve of EPN pre-
and the corresponding ECN is shown in Figure 7(d–f), respect- sents several peaks, indicating that the EPN distribution of
ively. Many transient peaks can be seen in both EPN and ECN T91 steel is dispersed. The EPN probability densities of T91
spectra of T91 steel; such peaks are usually linked to passive steel are basically unchanged with a fluctuation amplitude
film breakdown and repassivation. On rainy days, ECN and of about 1.5 mV. The probability density distribution of
EPN amplitudes are 2.0 nA and 1.0 mV, respectively. Com- ECN is basically unchanged except on day 10 where it is
parisons of (a, d) with (b, e) and (c, f) in Figure 7 indicate slightly wider, indicating that the corrosion rate of T91 steel
that EPN and ECN amplitudes do not increase or decrease sig- in rainy conditions is basically unchanged. The probability
nificantly with the extension of time, revealing that the cor- density distribution curve implies that the dispersed distri-
rosion rate did not change remarkably on days 8, 10 and 19. bution is due to the transient peaks existed in the EN spec-
The statistical analyses of EPN and ECN shown in Figure 7 trum. This correlates well with the characteristic of EN
are presented in Figure 8, in which the probability density during localised corrosion.
Figure 7. Typical EN spectrum of T91 steel at rainy days. (a–c) EPN spectrum on days 8, 10 and 18, respectively; and (d–f) ECN spectrum on days 8, 10 and 18,
respectively.
438 C. MA ET AL.
Figure 11. Surface topography of the atmospheric corrosion probe after a 20-day exposure to an outdoor atmosphere; (a) Q235B and (b) T91.
where Rn is the noise resistance at the time of t, Dt is the data corrosion. The standard deviation of ECN and the noise
acquisition time and Dt is the total time. In this study, Dt resistance have direct relationships with the corrosion
= 10 and 20 days, because Rn of 10 and 20 days is needed. rate. As the exposure time is prolonged, the standard devi-
Correlation of the noise resistance and weight loss data is ation of the current noise decreases due to the formation
shown in Table 2. The weight loss data are converted to polar- of a rust layer.
isation resistance. The values of polarisation resistance and 3. The probability density distributions of EPN and ECN can
integrating–averaging noise resistance were in the same be used to illustrate a corrosion process visually. The prob-
order of magnitude, indicating that EN is effective for evalu- ability density distribution curves of EPN and ECN plots
ation of atmospheric corrosion. for Q235B steel became narrower as the atmospheric
In atmospheric conditions, the solution resistance may exposure time increased, but the probability density distri-
affect the calculation of noise resistance. However, the dis- bution curves of EPN and ECN plots for T91 steel showed
tance between the RE and WE is about 200 μm, and the sol- little change.
ution resistance has been estimated and found to be lower 4. Low-frequency and high-frequency wavelet energies can
than 1000 ohm [10]. Therefore, solution resistance can be be used to identify atmospheric corrosion form. The
negligent in calculation of noise resistance, because noise high-frequency energy D1 of Q235B steel was higher
resistance is usually 10 times higher than the solution than that of T91 steel, whereas the low-frequency energy
resistance. A7 of Q235B steel was lower than that of T91 steel.
5. Weight loss data obtained from 10 and 20 days correlate
well with the EN data, indicating that the EN can be
Conclusion used as an effective method to instantly evaluate the
atmospheric corrosion process.
In the present work, the atmospheric corrosions of Q235B
and T91 steels were monitored by atmospheric corrosion
probes, and the conclusions are summarised as follows:
Disclosure statement
1. This work implies that the atmospheric corrosion can be No potential conflict of interest was reported by the author(s).
successfully assessed by EN, and thus EN can be used as
a fast and economic method in atmospheric corrosion
detection. Funding
2. Standard deviations of EPN and ECN, and noise resist- The authors wish to acknowledge the financial support of the Major
ance can be used as corrosion process indicators. Q235B State Basic Research Development Program (973 Program) (grant no.
2014CB046805), the National Natural Science Foundation of China
steel undergoes uniform corrosion in Tianjin urban
(nos. 51131007, 51671144), National Natural Science Foundation of
atmosphere whereas T91 steel suffers from localised China (51471117) and Key Project of Tianjin Natural Science Foun-
dation (13JCZDJC29500).
Table 2 Correlation of the noise resistance and weight loss data of Q235B and
T91.
ORCID
Data obtained from
Data obtained from weight loss electrochemical noise Da-Hai Xia http://orcid.org/0000-0003-2336-8564
Corrosion Polarisation Integrating-averaging
Exposure current density resistance Rp noise resistance Rn
time Icor/(μA cm−2) (MΩ cm2) (MΩ cm2) References
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