Materials Transactions, Vol. 57, No. 2 (2016) pp.

148 to 155
© 2016 The Japan Institute of Metals and Materials

Weathering Steel in Industrial-Marine-Urban Environment: Field Study

P. Dhaiveegan1, N. Elangovan2, T. Nishimura3 and N. Rajendran1,+
1
Department of Chemistry, Anna University, Chennai-600025, India
2
Department of Chemistry, A. M. Jain College, Chennai-600114, India
3
Material Recycling Design Group, Research Center for Strategic Materials,
National Institute for Materials Science, Tsukuba 305-047, Japan

In the present field study, we report the exposure of weathering steels in the industrial-marine-urban environment at Ennore, located near
the east coast of India for 3 years. The Corrosion products viz., iron oxyhydroxides and oxides present in the rust layers were characterized using
ATR-FTIR, XRD studies and quantified using TGA analysis. The specific surface area of the rust particles formed during the corrosion process
were determined using N2 adsorption isotherm studies. The morphology of the corrosion products were elucidated using SEM. ATR-FTIR and
XRD studies showed that the corrosion products formed on the skyward surfaces were highly more crystalline than those on the the earthward
surfaces. TGA showed that the iron oxyhydroxides were major corrosion products. N2 adsorption-desorption studies confirmed the formation of
compact inner rust layers with high specific surface area (SA). SEM analysis revealed that the skyward surface was smooth and compact while
the earthward surface were cracked and porous. SEM images confirmed the formation of characteristic morphological structures such as sandy
crystal (lepidocrocite), needle-like (goethite), cotton ball (goethite) and cigar shaped (akaganeite) structures. Further, it revealed the formation of
goethite on the skyward surface as a major constituent phase in the rust layer, which was influenced by the presence of SO2 content in the
environment. [doi:10.2320/matertrans.M2015345]

(Received September 7, 2015; Accepted November 12, 2015; Published January 18, 2016)
Keywords: weathering steel, X-ray diffraction (XRD), scanning electron microscope (SEM), brunauer-emmet-teller (BET), atmospheric
corrosion, rust and goethite

1. Introduction
Weathering steel is widely used as a construction material
due to its low cost and high corrosion resistance. The high
corrosion resistance of weathering steel is attributed to the
formation of dense and adherent rust layer.1) Atmospheric
corrosion studies of weathering steels in various environ-
ments such as marine, urban and industrial areas were
reported.2) The corrosion parameters like chloride (Cl¹),
sulphur dioxide (SO2), relative humidity (RH), temperature
and composition of alloying elements play a crucial role in
the formation of rust products during the period of exposure
in different environments.3­5) The characteristic nature of the
rust layer were well studied by several researchers over the
last few decades. 6­8)
Asami et al.9) investigated the weathering carbon steels
exposed to industrial and marine environments for 17 years
and concluded that the distributions of ¡-FeOOH phase in the
inner rust layer was uniform and served as a barrier layer in
the rust. Fuente et al.10) studied the morphology of corrosion
products formed on mild steel, which was exposed for 13
years in various environments such as marine, industrial, rural
and urban. It was found that the skyward facing surface had
smooth and uniform structure with low aggressivity, whereas
the earthward facing surface had irregular cracked structure.
Thermogravimetric analysis were used to identify and
quantify the composition of the rust and this can be achieved
with a small amount of sample.11) Yuxi et al.12) quantitatively
analysed the composition of the rust formed in various
environments using thermal analysis. Ishikawa et al.13)
assessed the specific surface area of the rust layer by N2 and
H2O adsorption studies and related this to the extent of
corrosion and type of steel exposed. They showed that
+
Corresponding author, E-mail: nrajendran@annauniv.edu
compact rust layers with high SA or small particle size exhibit
a high corrosion resistance. Singh et al.14) have studied the
long term corrosion behaviour of low alloy and plain carbon
structural steel exposed to different climatic conditions for 2
years and reported the nature of rust formed, which revealed
that the presence of SO2 played a vital role in reducing the
corrosion rate at Chennai site when compared to other sites.
Ennore is situated in the northern part of Chennai city at
the east coast of South India near Bay of Bengal. Thermal
power plants, petrochemical plants, ports, refineries, pharma-
ceutical companies and residential buildings are situated in
Ennore and it is a marine-industrial-urban environment.
There are no reports on the detailed field study of rust layers
formed on weathering steels subjected to long term exposure
in an industrial-marine-urban environment in India. In the
present investigation, thermo gravimetric analysis and N2
adsorption studies were used to understand the nature of
corrosion products formed on the skyward and earthward rust
layers of weathering steel exposed at Ennore, Chennai, India.
2. Experimental Procedure
2.1 Preparation and exposure of specimen
The composition of the exposed weathering steel is
presented in Table 1. The chemical composition of alloying
elements was confirmed by inductively coupled plasma
optical emission spectroscopy (ICP-OES). The specimen
dimensions are 100 mm © 50 mm © 3 mm. The specimens
were abraded with 800 # SiC paper, rinsed with water and
acetone, dried, weighed and kept in a moisture free
Table 1 Chemical composition of the weathering steel (mass%).
Elements C Si Mn P S Cu Cr Ni Fe
Composition 0.08 0.25 0.33 0.07 0.01 0.44 0.51 0.25 Balance
 Weathering Steel in Industrial-Marine-Urban Environment: Field Study
Table 2 Environmental conditions of exposure site (yearly average values for the period 2009­2012).
Temperature
Test site Environment
(T/K)
Ennore Industrial-Marine-Urban 307
Fig. 1 Topography of the location of atmospheric corrosion exposure site
of Chennai, India.
desiccators for 3 days prior to exposure. ASTM G 50-9715)
standard was followed and the specimens were exposed to
environment for 36 months (January 2009-Dec 2012). The
exposure distance was 100 m from the marine and 200 m
from the industrial environment. The topography map of the
exposing the site is given in Fig. 1.
The climatic and environmental parameters viz., relative
humidity, temperature were obtained from Regional Mete-
orological Centre, Chennai. The amounts of atmospheric
deposition of Cl¹ and SO2 content in the field were estimated
using wet candle and sulphonation plate procedures pre-
scribed in ASTM G 140-9616) and ASTM G 91-9717) were
followed. The 3 years average environmental parameters are
listed in Table 2.
2.2 Rust separation and its analysis
The easily peelable rust layers from the skyward and
earthward facing surfaces were collected and labelled as
skyward outer rust layer (SOL) and earthward outer rust layer
(EOL). The adherent rust layers were carefully scrapped from
the specimen using a sharp cut knife and were designated
similarly as skyward inner rust layer (SIL) and earthward
inner rust layer (EIL). The collected rust was ground and kept
in a desiccator for 3 days before analysis. The attenuated total
reflection fourier transform infrared (ATR-FTIR) spectra of
rusts were recorded in the 2000­400 cm¹1 range on a Perkin
Elmer Spectrum Two instrument with UATR as accessory
and KBr window. A maximum of 200 scans were
accumulated for each sample. X-ray diffractograms (XRD)
were recorded using a PANalytical X’Pert PRO diffractom-
eter in the 2ª range from 10° to 70° at a step size of 5°/min
using CuK¡ (­ = 0.154 nm) as X-ray Source The micro-
structure and elemental distributions in the rust layers were
analysed using a Quanta 200 FEG Scanning Electron
Microscope equipped with energy dispersive X-ray analysis
(SEM-EDAX). Thermo gravimetric analysis (TGA) of the
149
Relative humidity Cl¹ deposition SO2 deposition
(%) (mg/cm2/day) (mg/cm2/day)
98 62 85
rust were carried out using a TA SDT Q600 thermal analyser
at a heating rate of 5°C/min from room temperature to
1000°C in an air atmosphere. The specific surface area SA of
the rust were determined using N2 adsorption/desorption
studies with quanta chrome system at 77 K. Before the
adsorption studies, the samples were degassed with N2 at
100°C for 12 hours. The SA and pore size distributions were
calculated by using Brunauer-Emmet-Teller (BET) and
Barret-Joyner-Halenda (BJH) methods, respectively.
3. Results and Discussion
3.1 Corrosive agents and environmental characteristics
in the exposure site
The ISO 9223-2012 classification can be used to predict
the nature of aggressiveness environment by determining the
atmospheric pollutant parameters viz., SO2 and Cl¹. In our
case study the atmospheric corrosion exposure location is
closer to the industrial environment, the SO2 deposits are
observed in higher amount compared to the Cl¹. The
determined values of Cl¹ and SO2 by wet candle and
sulphonation plate confirmed the presence of SO2 (85
mg/cm2/day) (P3) in the higher amount when compared to
Cl¹ (62 mg/cm2/day) (S2). Based on the measured values
of SO2 and Cl¹ at our location, our site can be classified as
C5 with reference to ISO 9223-2012 classification.18) The
average temperature (36°C) and RH (98%) remain through-
out the year with high values. The temperature and RH varied
from 30°C to 39°C, 60 to 98% respectively throughout the 3
years of exposure period. The major rainfall was observed in
the months of June to December during the southwest and
northeast monsoon period.
3.2 Characterization of rust layers and their products
3.2.1 Surface appearance of WS after 3 years of
exposure
The physical appearance of WS surface of the skyward
(Fig. 2(a)) rust layer was light red brown, adherent, compact
and more uniform, whereas the earthward (Fig. 2(b)) surface
of the specimens was dark brown and uneven. Also the
surface was rougher and high porous in nature with the looser
rust particles in EOL; but in the SOL the surface was
smoother with less porous nature.
3.2.2 ATR-FTIR spectroscopic studies
The skyward (Fig. 3(a)) and earthward (Fig. 3(b)) facing
rust layers were analysed using ATR-FTIR. All the ATR-
FTIR spectra display the characteristic absorption peaks
for water insoluble corrosion rust products namely lepidoc-
rocite (£-FeOOH-1020 cm¹1), goethite (¡-FeOOH-890 and
790 cm¹1), (akaganeite) (¢-FeOOH-680 cm¹1) maghemite
(£-Fe2O3-560 cm¹1).19) Water-soluble iron chloride and
sulphate as residual concentration in the rust layers are hard
to be detected.20) In all the spectra, the absorption peak
150 P. Dhaiveegan, N. Elangovan, T. Nishimura and N. Rajendran

(a) (b) around 1620 cm¹1 corresponds to physisorbed water. The

difference in the band intensities between 890 cm¹1 and
1020 cm¹1 in the skyward rust layer is attributed to the
formation of goethite over lepidocrocite. The formation of
goethite in the SOL is thermodynamically favourable at
lower pH in the presence of sulphur dioxide which is
observed at 1460 cm¹1. Figures 3(a) and (b) reveals the
presence of chloride ion favours the formation of akaga-
neite.21­24) The formation of stable goethite in the skyward
outer rust (SOL) layer suppresses the penetration of chloride
ions to the skyward inner layer (SIL) and hence less intense
peak is observed for akaganeite at 680 cm¹1 in the SIL. The
protective ability index (PAI) of the rust is determined by the
peak intensity ratio of the ¡-FeOOH and £-FeOOH.22) The
skyward rust layers show the higher PAI value of 1.7 whereas
the earthward rust layer shows a value of 0.98. PAI value
indicates the high corrosion resistance nature of SOL when
Fig. 2 Surface appearance of (a) skyward and (b) earthward specimens compare to EOL.
exposed for 3 years at industrial-marine-urban environment.
3.2.3 XRD analysis
Figures 4(a)­(d) shows the XRD patterns of the rust layers

EIL
A
M
Transmittance (a.u.)
Transmittance (a. u.)

SIL L
G
G
SOL EOL
A A
M SO42-
H L M
G L
M
G (a) G
G (b)
500 1000 1500 2000 500 1000 1500 2000
Wavemumber, υ / cm-1 Wavemumber, υ / cm-1

Fig. 3 ATR-FTIR spectra; (a) SOL and SIL, (b) EOL and EIL (G-Goethite, A-Akagagenite, L-Lepidocrocite, M-Maghemite,
H-Hematite).

(a) (b)

(c) (d)

Fig. 4 XRD patterns of powdered rust layers of weathering steel after 3 years of exposure; (a) SOL, (b) SIL, (c) EOL and (d) EIL.
 Weathering Steel in Industrial-Marine-Urban Environment: Field Study 151

present in SOL, SIL, EOL, EIL of the exposed weathering (a) (c)
steel. The presence of iron oxides viz., maghemite (£-Fe2O3),
magnetite (Fe3O4) and hematite (¡-Fe2O3) and oxyhydrox-
ides viz., lepidocrocite (£-FeOOH), goethite (¡-FeOOH),
akaganeite (¢-FeOOH) and ferrihydrite (¤-FeOOH) with
varying intensities in all the rust layers are observed. The
relative peak intensity of goethite (2ª = 21°) in the skyward
surface was stronger than the earthward surface which is 200 μm
attributed to the presence of higher sulphur content which
in turn enhances the transformation of lepidocrocite into (b) (d)
thermally stable goethite.14) In the case of EOL relative peak
intensity of lepidocrocite (2ª = 14°) is much stronger than
the skyward surface. The relative peak intensity of akaganeite
in the earthward layer is lower than the skyward layer due to
the spallation of the earthward rust layers.25) Exogeneous
silica (SiO2) is observed in all the rust layers. The cation
selective ability of goethite enhances the corrosion resistance 200 μm
of the steel which retards penetration of chloride from the
environment.26) From the above results, it is inferred that the Fig. 5 SEM/EDAX micrographs of the rust layers on weathering steel:
skyward surface is more corrosion resistant than the earth- (a), (c) skyward surface and (b), (d) earthward surface.
ward surface. These results are in agreement with the ATR-
FTIR studies. surface. The presence of chloride influences the formation of
cracks which are evident from the difference in the skyward
3.3 Morphology of corrosion products and earthward micrographs. Chloride ion influences the
Scanning electron micrographs (SEM) of the skyward and formation of flaked rust in the earthward surface whereas,
earthward surfaces of exposed weathering steel are shown SO2 plays a crucial role in the formation of less rougher
in Fig. 5. The presence of voids and micro cracks are morphology in the skyward surface.9,27) Figures 6 and 7
significantly higher in the earthward surface when as show the typical morphologies of the rust products formed on
compared to the skyward surface (Fig. 5(a) and (b)). SEM- the skyward and earthward surfaces respectively after 3 years
EDAX results for both skyward and earthward surfaces are of exposure in the marine-urban-industrial environment. Fine
represented in Fig. 5(c) and (d). It is inferred from the SEM­ plate-like structure is present in the skyward surface
EDAX mapping that the distribution of relative sulphur (Fig. 6(a) and (b)) and the crystalline globule (sandy crystals)
content in the skyward rusted surface is higher than in the structure is present in the earthward surface (Fig. 7(a)). These
earthward surface. Further, it is inferred that the chloride structures account for the presence of lepidocrocite (£-
content in the skyward surface is lower than the earthward FeOOH). The cotton ball (Fig. 6(c)) and needle-like

(a) (c) (e)

(b) (d) (f)

Fig. 6 SEM micrograph of typical morphologies of skyward surface corrosion products of rusted weathering steel: (a) and (b)
lepidocrocite, (c) and (d) goethite and (e) and (f ) akaganeite.
152 P. Dhaiveegan, N. Elangovan, T. Nishimura and N. Rajendran

(a) (b) (c)

Fig. 7 SEM micrograph of typical morphologies of earthward surface corrosion products of rusted weathering steel: (a) lepidocrocite,
(b) goethite and (c) akaganeite.

Fig. 8 Schematic illustrations for the formation of various rust layers on weathering steel and its microstructure.

structures (Fig. 6(d)) in the skyward surface and whiskery
cotton ball structure (Fig. 7(b)) in the earthward surface can
be regarded as the structures of goethite (¡-FeOOH).23)
Akaganeite (¢-FeOOH) is present in the form of cigar
shaped crystals (Fig. 6(e)) and rosette morphology
(Fig. 6(f )) in the skyward surface and whiskery rod shape
structures (Fig. 7(c)) in the earthward surface.
It is accepted that rusting is a heterogeneous process and
results in different phases.27,28) The different morphological
structures of the iron rust corrosion products with same
phases are attributed to the time of exposure.29) Based on
Evans30) and Misawa’s Model,31) the corrosion processes and
the formation of rust layers are depicted in Fig. 8. In the
initial stage of rusting lepidocrocite is formed and further the
presence of sulfur dioxide favors the formation of goethite
through solid-state transformation.
3.3.1 Cross-sectional morphology of rust layers
The cross-sectional morphology of rust layers are depicted
in (Fig. 9(a)­(b)) and their EDAX spectra (Fig. 9(c)­(d))
show the Cl¹ and SO2 enrichment. The rust layers are wavy
and undulating with distinguishable outer and inner layers.
Among the two rust layers, the corrosion products in the
skyward inner layer (SIL) is compact, dense and adherent
The Earthward inner layer (EIL) is thinner than the skyward
inner layer (SIL), cracked due to spallation.32) The average
thickness of the skyward and earthward rust layers are 92 and
62 µm respectively. Figure 9(b) shows that the earthward rust
layers have larger number of pores and cracks through which
penetration of deleterious species such as Cl¹ and SO2 are
possible. From the cross section morphological studies, it is
seen that the earthward surface were highly influenced and
affected by corrosive agents than the skyward surface.
Figure 9(c) and (d) EDAX spectra shows the presence of
chloride, sulphur and exogenous silica along with alloying
elements in the rust layers. Exogenous silica also enhances
the corrosion protection of the steel. Further, skyward rust
layer is enriched with Cr, Mn and Ni but the earthward rust
layer is enriched with Ni only. The enrichment of Cr and Ni
enhances the formation of stable goethite in the skyward rust
layers when compared to the earthward rust layers.33,39)
 Weathering Steel in Industrial-Marine-Urban Environment: Field Study 153

3.4 Thermal analysis of rust
Figure 10(a) shows the thermogram of the rust layers. The
study reveals that weight loss of iron oxyhydroxides and
oxides at different temperatures for skyward and earthward
rust layers are distinct. The significant loss of weight in the
temperature range 20­220°C is attributed to desorption of
(a)
Outer Layer
physisorbed water molecules. subsequently, the second
weight loss occuring at 370°C is due to the accelerated
transformation of oxyhydroxides to iron oxides, with the
varying weight loss (%) corresponding to their relative
amounts present in the skyward and earthward rust layers.12)
It is evident from Fig. 10(b). that the amount of oxy-
hydroxides in comparison to iron oxides present in skyward
surface is higher than the earthward surface. Higher amounts
(b) of oxyhydroxides enhance the corrosion protection ability of
Outer Layer the skyward rust layers.34)

Inner Layer 3.5 N2 adsorption studies of rust layers

Inner Layer N2 adsorption desorption isotherms of powedered rust
layers of SOL, SIL, EOL, EIL are shown in Fig. 11(a) and (b)
Substrate Substrate respectively. From the Fig. 11(a) and (b) it is inferred that the
adsorption and desorption behaviour of rust layers shows
typical mesoporous material type IV isotherm which is
(c) (d)
attributed to the capillary condenstion in mesoporous rust
channels.
SOL and EOL shows the H2 type hystersis loop indicating
the porous nature of the rust which were substantiated by the
SEM results. SIL and EIL show typical H4 type hysteresis
loop attributing to the less porous nature of rust which also
accounts for the morphological structures as revealed by
SEM analysis. The hysteresis loop in the relative pressure
Fig. 9 Cross-sectional morphologies of rusted surface of weathering steel:
(P/Po) range between 0.4 to 0.8 and this can be attributed to
(a) skyward, (b) earthward surfaces and their corresponding EDAX the pores with narrow and wide sections and possible
spectrum (c) and (d). interconnecting channel in the rust layers.35) From, the BET

4.0
(a) SOL (b)
100 SIL 3.5 Mass of hydroxy oxide
EOL Mass of oxide
80 EIL 3.0
Weight, (%)

2.5
60
Mass, mg

2.0

40 1.5

1.0
20
0.5

0 0.0
0 200 400 600 800 1000 SOL SIL EOL EIL
Rust layer
Temperature, T / K

Fig. 10 (a) TGA curves of powdered rust layers. (b) Relative abundance of iron oxy hydroxide and iron oxides within the various rust
layers of weathering steel.

SOL EIL
(a) SIL
(b) EOL
60 60
Voulme adsorbed, cm/g 3
Voulme adsorbed, cm/g 3

40 40

20 20

0 0
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Relative pressure, p/po Relative pressure, p/po

Fig. 11 N2 adsorption­desorption isotherms of powdered rust layers: (a) SOL and SIL, (b) EOL and EIL.
154 P. Dhaiveegan, N. Elangovan, T. Nishimura and N. Rajendran

8 3.0 110
SOL Average Pore size
(a) SIL
(b) Surface area
7 2.8 105
EOL
EIL 2.6 100
6

Average pore size, nm

2.4 95

dV/dD, cm 3/nm

Surface area, m 2 /g
5

2.2 90
4
2.0 85
3
1.8 80
2
1.6 75
1
1.4 70
0
1.2 65
0 5 10 15 20 25 30 35 40 SOL SIL EOL EIL
Rust layer
Pore Diameter, D/nm

Fig. 12 (a) Distribution of pore volume with respect to pore size as calculated by BJH method. (b) Correlation between the pore size and
specific surface area of weathering steel rust layers.

isotherm SA were calculated for the SIL, SOL, EIL and EOL surfaces exposed for 3 years in the industrial-marine-urban
rust layers which were found to be 107, 84, 92 and 74 m2/g environment led to better understanding of corrosion process
respectively. The SIL and EIL shows higher SA, higher leading to the formation of adherent protective layer on the
corrosion resistance which is due to the compact, adherent skyward surface when compared to earthward surface. The
and porous nature of rust layers. The higher SA results in results obtained from ATR-FTIR and XRD confirmed the
smaller rust particles of the agglomerates of iron oxide and formation of two distinct types of layers each having unique
iron oxyhydroxides with finer pore structure.13) EOL and oxides and oxyhydroxides on their surfaces. The formation of
SOL show less porous which is due to the low SA resulting goethite in the inner layer (SIL) as stable form of product
with poor adherent nature. The compactness and protective with needle like structures was influenced by SO2, which led
ability of the rust layers depend on the morphology of the rust to the formation of protective skyward rust layers along with
particles; smaller particles form more compact layers and other iron oxides. The BET isotherm studies confirmed the
sheet or plate ones make up less permeable layers by their compactness and densified nature of skyward inner rust
preferred orientation. layers which prevents the ingress of chloride ions. Corrosion
The relative difference in the specific surface area of SOL process with enrichment of Ni and Cr resulted in fine rust
and SIL can be inferred from the presence of a considerable particles in the skyward inner layer with higher surface area,
amount of akaganeite (¢-FeOOH) which has a tunnel thereby ensuring the corrosion protection of weathering steel.
structure and contributes to a high surface area and with
large pore size. The enrichment of Ni and Cr influences the Acknowledgement
reduction of particle size in the rust and its structure and
compostion.8,36­39) The SA above 50 m2/g has small pores The facilities provided by DST-FIST and UGC-DRS are
always filled with water by the adsorption and capillary gratefully acknowledged. The HR-SEM facility provided by
condensation. Further, it prevents the transfer of corrosive the SAIF-IIT, Madras is also acknowledged. The permission
agents into the pore thus leading to the high protective nature granted by Mr. P. Manikandan to expose the specimens in his
of weathering steels to atmospheric corrosion.37) From the place is gratefully acknowledged.
above results, it is clear that the SIL has a higher surface area,
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