Anti-Corrosion Methods and Materials

Latest advances in the understanding of acid dewpoint corrosion: corrosion and stress corrosion cracking in
combustion gas condensates
W.M.M. Huijbregts R.G.I. Leferink
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W.M.M. Huijbregts R.G.I. Leferink, (2004),"Latest advances in the understanding of acid dewpoint corrosion: corrosion and
stress corrosion cracking in combustion gas condensates", Anti-Corrosion Methods and Materials, Vol. 51 Iss 3 pp. 173 - 188
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R.G.I. Leferink, W.M.M. Huijbregts, (2002),"Nitrate stress corrosion cracking in waste heat recovery boilers", Anti-Corrosion
Methods and Materials, Vol. 49 Iss 2 pp. 118-126 http://dx.doi.org/10.1108/00035590210419362
J. Bordzilowski, K. Darowicki, (1998),"Anti-corrosion protection of chimneys and flue gas ducts", Anti-Corrosion Methods and
Materials, Vol. 45 Iss 6 pp. 388-396 http://dx.doi.org/10.1108/00035599810236243

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Latest advances in the
understanding of acid
dewpoint corrosion:
corrosion and stress
corrosion cracking
in combustion gas
condensates
W.M.M. Huijbregts and
R.G.I. Leferink
Downloaded by New York University At 17:17 16 April 2015 (PT)
The authors
W.M.M. Huijbregts is based at Huijbregts Corrosion
Consultancy, Arnhem, The Netherlands.
R.G.I. Leferink is based at KEMA, Arnhem, The Netherlands.
Keywords
Corrosion, Stress (materials), Gases
Abstract
Corrosion failures due to condensing flue gases containing H2O,
SO3, NOx and HCl still occur more often than might be expected.
The corrosion failures can be of several types: general corrosion,
pitting attack and stress corrosion cracking (SCC). The chemistry
of condensing gases is discussed, and some examples of
corrosion in large-scale installations are presented, including
blast stoves for steel production, heat recovery steam
generators, and waste incineration boilers. The use of thermal
insulation inside boiler casings can result in nitrate SCC when
the flue gas contains high concentrations of NOx. Nitric acid from
flue gas can react with carbon steel and insulation material
forming ammonium nitrate and calcium nitrate. Both materials
have hygroscopic properties and are very corrosive, even above
the water dewpoint of the gases.
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available at
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Anti-Corrosion Methods and Materials
Volume 51 · Number 3 · 2004 · pp. 173–188
q Emerald Group Publishing Limited · ISSN 0003-5599
DOI 10.1108/00035590410533129
173
1. Introduction
Corrosion arising from condensing gases has been
a problem in industry for many years. The basics of
corrosion due to condensing gases are well
understood, and it might be expected, therefore,
that this type of attack should not occur. However,
the many different combinations of operating
temperature and chemical stoichiometry of
combustion reactions, combined with
constructional features of a combustor design, can
lead to many possible corrosion reactions.
In recent years, many corrosion problems have
arisen from condensing gases. When there is a risk
of condensation, the designer should have the
answers on the following questions:
.
Which condensed liquid can be formed?
(The dewpoints of the various gases should be
calculated.)
.
What amount of condensed liquid can be
expected?
. What concentration of corrosive liquid can be
expected?
.
What is the corrosion resistance of the
material in the environment to be expected?
These aspects should be considered at an early
stage of a new or modified design as such
consideration will reduce drastically the likelihood
of premature failure or the necessity for later
modifications of the design.
A brief overview of the basic chemical and
physical processes taking place during
condensation is presented below; then some
examples and their analysis are discussed to
illustrate the types of situation in which
combustion gas condensation corrosion may occur
and what measures can be taken to avoid or
mitigate attack. Specific examples associated with
condensation in blast stoves for steel production,
heat recovery steam generators (HRSGs) and
waste incineration boilers are considered.
2. Dew points of H2O, NO2 and SO3
Descriptions and calculation methods of
condensation have been published quite
extensively in the works of: Hoftyzer and Kwanten
(1972), Kiang (1981), Land (1977), Perry and
Chilton (1973), Ullmann’s Encyclopaedia of
Industrial Chemistry (2001), Verhoff and
Banchero (1974), and Weast (1988).
The basis for all calculations is the definition of
the dewpoint: this is the temperature to which a
given parcel of air should be cooled, at constant
pressure and water content, to reach a state at
which the saturation vapour pressure is equal to
 Latest advances in the understanding of acid dewpoint corrosion
W.M.M. Huijbregts and R.G.I. Leferink
the actual vapour pressure. Any further cooling
will result in the formation of liquid (dew) or solid
(frost/ice).
In its simplest form, when dealing with clean air,
the dewpoint may be directly plotted from the
water vapour pressure tables ( Weast, 1988) as
shown in Figure 1.
When other gaseous species are present, such as
SO3, SO2, HCl or NO2, the dewpoint will deviate
from the ideal dewpoint line. Dewpoint in the
presence of these gases can be calculated by means
of the equations of Kiang (1981), Perry and
Chilton (1973), and Verhoff and Banchero (1974).
In Figures 2-5, examples of calculated dewpoints
are presented for SO3, SO2, HCl and NO2.
Only in cases of very low HCl and NO2 levels
can the calculated dewpoints be lower than the
water dewpoint. In practice, this does not
occur, and the water dewpoint should be used.
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This can be seen in Figures 4 and 5, where a
straight water dewpoint line is used for low
HCl and NO2 levels.
3. Amount of condensed acid
When the temperature drops below the dewpoint,
sulphuric acid, nitric acid and water begin to
condense, either as small fog droplets or as a film
(Land, 1977). In flue gas, condensation droplets
can be formed easily on particles that act as
condensation nuclei. A common example
of condensation nuclei that can cause mist
condensation in coal fired boilers and waste
incinerators are fly ash particles. If a mist is
formed, most of the droplets are carried away with
Figure 1 The water vapour pressures from the water vapour table
174
Anti-Corrosion Methods and Materials
Volume 51 · Number 3 · 2004 · 173–188
the flue gas. As a result, the corrosion rate of
steelwork and wall tubes will be low, even when the
droplets are acidic. However, if the gas velocities
become high, or local flow disturbances occur,
droplets may be pushed onto the metal walls and a
thin liquid film may be formed. On the other hand,
in a rather clean gas, such as in gas-fired units,
super-saturation can take place, resulting in film
condensation on cool walls or heat exchanger
tubes. Acid deposition can be quite high under
certain conditions.
To get an impression of the deposition rates
to be expected under mist formation conditions
and no supersaturating conditions, Land (1977)
produced Figure 6. The calculation method
of Land is based on heat transfer and mass
flow equations. As Land (1977) mentioned:
“In practice we may expect to find curves
laying anywhere between the two extremes”.
If calculations are to be made of the expected
corrosion rates for a new boiler design, it is
strongly advised that the worst case be assumed,
i.e. that film condensation will occur.
Following the Land calculation method,
deposition rates of sulphuric and nitric acids have
been calculated for the gas conditions presented in
Table I. The results of these calculations are shown
in Figures 7 and 8. As there are some uncertainties
in the exact figures for heat transfer coefficients of
sulphuric and nitric acids, the results should be
considered as estimations. Land compared his
calculations on sulphuric acid with experimental
measurements and the results were very
satisfactory.
The calculated deposition rate of sulphuric
and nitric acids for both gases A and B are 0.0073
 Latest advances in the understanding of acid dewpoint corrosion Anti-Corrosion Methods and Materials
W.M.M. Huijbregts and R.G.I. Leferink Volume 51 · Number 3 · 2004 · 173–188

Figure 2 Dewpoint behaviour of SO3 at various water contents of the gas, calculated from the formula of Verhoff
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Figure 3 Dewpoint behaviour of SO2 at various water contents of the gas, calculated from the formula of Kiang. The SO2 dewpoints for
all gases are lower than the water dewpoint of the gases

175
 Latest advances in the understanding of acid dewpoint corrosion Anti-Corrosion Methods and Materials
W.M.M. Huijbregts and R.G.I. Leferink Volume 51 · Number 3 · 2004 · 173–188

Figure 4 Dewpoint behaviour of HCl at various water contents of the gas, calculated from the formula of Kiang and the water
vapour table
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Figure 5 Dewpoint behaviour of NO2 at various water contents of the gas, calculated from the formula of Perry and the water
vapour table

176
 Latest advances in the understanding of acid dewpoint corrosion
W.M.M. Huijbregts and R.G.I. Leferink
Figure 6 Theoretical curves for the rate of acid deposition according to the calculations of Land (Perry and Chilton, 1973; Land, 1977)
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Table I Conditions assumed for the calculation of acid
deposition: gas flow, 4 m/s; tube diameter, 4 m; gas temperature,
1308C
Gas A Gas B
SO3 (vppm) 0.15 – pressure is equal to 1,316 vppm or
NO2 (vppm) – 200
H2O (volume per cent) 6.5 6.5
and 9.7 mg/m2/s, respectively, in case of film flow.
At a lower NO2 content, e.g. 20 vppm NO2 the
deposition rate of nitric acid is proportionally
lower and lies at a level of maximum 0.97 mg/m2/s
in case of film flow. Additionally, note that at a
temperature near the dewpoint of 388C the
deposition rate is minimal.
4. Concentration of the first condensed
liquid
The concentration of the sulphuric acid can be
derived from the boiling lines in the phase diagram
of SO3-H2O in Figure 9.
At a dew point of 958C, the condensed
sulphuric acid has a concentration of 67 per cent.
At lower temperatures, the concentration
decreases according to the boiling line, but at 608C
the concentration is still 43 per cent, a very
corrosive liquid that will result in uniform
corrosion of carbon steel.
It is more complicated to determine the
concentration of the condensed nitric acid.
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Anti-Corrosion Methods and Materials
Volume 51 · Number 3 · 2004 · 173–188
The equilibrium vapour pressure diagram of
Hoftyzer and Kwanten (1972) can be used,
as shown in Figure 10. The gas pressures are
given in mm Hg. A pressure of 1 mm Hg
0.13 volume per cent.
Nitric acid is in equilibrium with NO and NO2
according to the formula:
NO þ NO2 þ H2 O þ O2 $ 2HNO3
When 200 vppm NO2 and 200 vppm NO are
present, the reaction will result in 400 vppm
(0.305 mm Hg) HNO3. The water dew point and
the NO2 dewpoint of the gas are 38 and 408C,
respectively. In the range of 10-200 vppm NO2
(0.015 and 0.305 mm Hg HNO3 vapour pressure),
the concentration of the condensed HNO3 will be
in the range of 17-40 per cent. These figures can be
derived from Figure 10 by following the 408C line
until it intersects with the mentioned HNO3
vapour pressures.
The nitric acid concentration in the liquid
will be high, even at low NO2 concentrations
(17 up to 40 wt per cent). Such concentrations
result in extremely acidic conditions with pH values
of 20.4 and 20.8, respectively. Fortunately, at
low NO2 contents (as usual in modern HRSGs)
the deposition rate will be rather low. For a
gas with 10 vppm NO2 the deposition rate of
17 per cent nitric acid will be 0.45 mg/m2/s. At a
temperature of 388C (near the dewpoint) the
deposition rate will be minimal, as can be seen in
Figure 8.
 Latest advances in the understanding of acid dewpoint corrosion Anti-Corrosion Methods and Materials
W.M.M. Huijbregts and R.G.I. Leferink Volume 51 · Number 3 · 2004 · 173–188

Figure 7 Acid deposition rates in case of sulphuric acid condensation of gas A

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Figure 8 Acid deposition rates in case of nitric acid condensation of gas B

5. Stress corrosion cracking in blast stoves temperatures may be as high as 1,5508C.

of blast furnaces in the steel production
industry
In steel production, combustion air for a blast
furnace is preheated in a blast stove. The stove is
filled with bricks that are heated with the natural
gas burners. Air for the blast furnace is preheated
by passing it over the hot bricks. Typical
dimensions of modern blast stove are a diameter of
10.7 m and a height of 46.4 m. Maximum dome
178
NOx formation is a particular concern at these
high temperatures.
In older blast stoves where the dome
temperature was below 1,3408C, NOx was
not formed in large amounts. However, as a
result of the high levels of NOx in modern
blast stoves, nitrate stress corrosion cracking
(SCC) has been identified as the cause of
several failures (Blekkenhorst et al., 1980;
Bohnenkamp et al., 1983; Buhler and Kalfa, 1981;
 Latest advances in the understanding of acid dewpoint corrosion Anti-Corrosion Methods and Materials
W.M.M. Huijbregts and R.G.I. Leferink Volume 51 · Number 3 · 2004 · 173–188

Figure 9 Phase diagram of sulphuric acid (Land, 1977) (PH2O+PH2SO4 ¼ 0.1 atm)
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Figure 10 Vapour pressures of nitric acid and water as a function of acid strength and temperature

179
 Latest advances in the understanding of acid dewpoint corrosion
W.M.M. Huijbregts and R.G.I. Leferink
Harp et al., 1985, 1990; Kalfa and Buhler, 1985;
Sucker et al., 1981).
The blast stoves are insulated on the inside of
the casings by means of a brick lining. No
insulation is used on the outside of the stove shells.
Buhler and Kalfa (1981) noticed the first failures
in the blast stoves cause by nitrate SCC in as far
back as 1965. Initially the cause of the cracking
was ascribed to the formation of nitric acid
because of the high amounts of NO2 in the gas.
Blekkenhorst et al. (1980) described the conditions
and the corrosion process in the stoves as follows.
During the firing of the stove, the NO
concentration increases by the endothermic
reaction:
N2 þ O2 , 2NO
Pressurising the stove at the beginning of the blast
period causes diffusion of NO into the insulation
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towards the steel shell. During the blast period,
the NO concentration will decrease, due to the
oxidation of NO2 and its diffusion back into the
combustion chamber. At the start of the next blast
period, the NO2 concentration will increase
because of the higher NO concentration and the
build-up of pressure according to the reaction:
1 Cathodic reaction: NO2
NO þ O2 , NO2
2 3H2 O þ NH3
Below 6508C the rate of NO2 formation is
significant. The formation of NO2 is fastest in the
coldest area of the stove, e.g. on the steel shell.
During the blast period, the temperature of the
steel shell will easily fall below the water dewpoint
and NO2 will dissolve in the water and form nitric
acid in the reaction:
1 week. In gas with dewpoints of 45 and 608C,
2NO2 þ H2 O þ O2 ) 2HNO3
2
According to Blekkenhorst, the formation of nitric
acid and the dissolution of various compounds
from the insulation material into the acidic
condensate, yield a nitrate solution causing SCC of
the stove shell. Although Blekkenhorst mentioned
that reaction products of nitric acid with the
insulation could be responsible for the nitrate
solution that causes SCC, he did not mention
which cations might be present. However, because
of the presence of a brick line in the stove, calcium
nitrate solution, a well-known test environment for
SCC experiments, could be one of the products.
The experience with the hot blast stoves is that
the NO2 content in the gas would be expected to
be approximately 80 vppm (Blekkenhorst et al.,
1980; Harp et al., 1985, 1990). Nitrate
concentrations in the condensed liquid would
range from 1 to 100 g/l. In the insulation layer near
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Anti-Corrosion Methods and Materials
Volume 51 · Number 3 · 2004 · 173–188
the shell, nitrate levels of 4.5 g/kg were found.
Sulphate and chloride were also present, however,
though their levels were considerably lower, at 0.6
and 0.1 g/kg, respectively. Near the gas side, the
amounts of nitrate, sulphate and chloride in the
bricks reached levels of 0.7, 5.6 and 0.1 g/kg,
respectively (Buhler and Kalfa, 1981).
In literature references, the composition of the
blast-stove environment regarding SO2, SO3 and
H2O levels was not mentioned. The dewpoint in
all relevant references is 678C. Because sulphates
are found in the deposits it is most likely that
sulphuric acid will condense in the insulation near
the gas side at first. In the cooler locations near the
shell, NO2 will condense as nitric acid below the
nitric acid dewpoint, or it may dissolve in the
condensed water below the water dewpoint.
Harp et al. (1985) analysed the condensed
liquid and the deposits at the stove shell. In the
condensed liquid both ammonium and nitrate ions
were found even though the gas itself did not
contain ammonium ions or ammonia. They
concluded that the ammonium must have been
formed from the reduction of nitrate when steel
corrodes in the concentrated nitric acid
environment according to the following reactions:
Anodic corrosion reaction: Fe ! Fe2þ þ 2e2
þ
3 þ 9H þ 8e !
2
To prove this hypothesis, Harp exposed steel
samples in wet NO and NO2-containing gas at
temperatures above the dewpoint. The gas
atmospheres he used contained 75 vppm NO and
25 vppm NO2 and dewpoints of 30, 45 and 608C
were created by using different amounts of water.
Carbon steel samples were exposed in these
gases at temperatures of 64, 80 and 1258C for 1
ammonium nitrate deposits were formed on the
specimens exposed at 648C. No deposit formation
occurred at 80 and 1258C. Figure 11 was
constructed on the basis of these results.
When the shell is warmed above the water
dewpoint, the ammonium nitrate will still contain
water, because of its hygroscopic properties. In dry
conditions, ammonium nitrate is not corrosive, but
below 1608C it starts to absorb water and highly
concentrated nitrate liquid films can be formed.
Figure 12 shows the solubility of ammonium
nitrate at increasing temperature (Ullmann’s
Encyclopaedia of Industrial Chemistry, 2001).
According to Harp et al. (1985) above 1208C, the
water content is too small (less than 5 per cent) to
cause SCC. Therefore, the ammonium nitrate
saturation line in Figure 11 is drawn as a dotted
line above 1208C.
As the blast stoves are filled with bricks and
there is a cemented brick lining at the shell, the
 Latest advances in the understanding of acid dewpoint corrosion
W.M.M. Huijbregts and R.G.I. Leferink
presence of calcium nitrate cannot be excluded.
Calcium nitrate has hygroscopic properties similar
to those of ammonium nitrate. However, contrary
to the behaviour of ammonium nitrate, the
Ca(NO3)2 will absorb specific quantities of water
according to the specific hydrate proportions.
Data for the system Ca(NO3)22 X H2O) are
Figure 11 Conditions for the formation of ammonium nitrate containing liquid
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Figure 12 Solubility of ammonium nitrate versus temperature
181
Anti-Corrosion Methods and Materials
Volume 51 · Number 3 · 2004 · 173–188
shown in Table II and Figures 13 (Ullmann’s
Encyclopaedia of Industrial Chemistry, 2001).
Thus, if calcium nitrate hydrate is heated from
room temperature it will lose a discrete number of
water molecules per molecule of calcium nitrate.
The solubility of calcium nitrate is very high, as can
be seen in Table III.
From these data, it can be calculated that if
water is released as a liquid, the associated calcium
nitrate will dissolve easily, creating a highly
concentrated calcium nitrate solution. For
instance: Ca(NO3)2·2H2O will loose two
molecules of H2O at 51.68C (Table II), and in this
small amount of water, very much Ca(NO3)2 can
be dissolved (Table III).
With regard to SCC, it is known that it is not
really important which cations of nitrate are
present. Nitrate SCC is known to occur in
solutions containing calcium nitrate, ammonium
nitrate, potassium nitrate, sodium nitrate, lithium
nitrate and nitric acid (ASM Handbook, 1986).
Thus, if nitrates are present in combination
with stressed carbon steel there is a high risk
of SCC.
6. SCC in HRSGs
In the early 1990s, several HRSGs of combined
cycle power plants in The Netherlands, suffered
tube failures. Cracks were mostly found in the low-
temperature heat exchangers (typically operating
at temperatures between 70 and 908C). In general,
the exchangers had been fabricated from steel
St35.8, a standard low-carbon steel for
construction purposes. Most cracking occurred in
bends and finned tubes where mechanical stresses
were relatively high. Microscopic analysis of
samples revealed that intergranular corrosion had
occurred and it was frequently reported that
complete grains of material had become detached.
Nitrate SCC was identified as the cause of the
failures (Figure 14).
On an average, the gas composition in a HRSG
around 1990 was: 18 volume per cent CO2,
50 vppm NO2 and 6.5 volume per cent H2O.
In general, a small amount of sulphur-containing
odorant, tetrahydrothiofene (THT) is added to
natural gas for safety reasons. In addition, small
amounts of sulphur-containing components also
can be present in the combustion air. This will
cause a small content of SO3 in the flue gas of at
least 0.15 vppm. From Figure 2 it can be
concluded that the dewpoint for a gas containing
6.5 per cent water will be 958C.
Thus, small amounts of sulphuric acid can
condense in the HRSG. In most installations
keeping the temperature above the sulphuric acid
dew point as much as possible prevents the
 Latest advances in the understanding of acid dewpoint corrosion Anti-Corrosion Methods and Materials
W.M.M. Huijbregts and R.G.I. Leferink Volume 51 · Number 3 · 2004 · 173–188

Table II Data for the system Ca(NO3)2-X H2O

Transition point
and temperature (8C) Content of Ca(NO3)2 (wt per cent) Range Stable hydrate formula mp (8C)
a
E 2 28.7 42.9
E– A Ca(NO3)2·4H2O 42.7
A þ 42.6 70.8 –
A –B Ca(NO3)2·3H2O 51.1
B þ 50.6 77.2
B–C Ca(NO3)2·2H2O –
C þ 51.6 78.1
above C Ca(NO3)2 561
bpb þ151 79.0

Water vapor pressure over saturated solution with solid Ca(NO3)2·4H2O

Temperature (8C) 0 10 20 30 40
Pressure (kPa) 0.36 0.69 1.25 1.99 2.63
Notes: aE ¼ cryohydric point; bBoiling point (101.3 kPa) of the saturated solution
Source: Ullmann (2001) see chapter Nitrates and nitrites, 3, calcium nitrate, Table 6
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Figure 13 Properties of a saturated solution of calcium nitrate in water

formation of sulphuric acid. However, during start
up and shutdown operations, the temperature will
inevitably fall below the sulphuric acid or water
dew points and condensation will occur.
As a consequence, a small amount of uniform
corrosion by the sulphuric acid cannot always be
avoided. In addition, in the case of high NOx
contents, nitric acid and concentrated ammonium
nitrate liquid films will be formed in a way that is
very similar to the case in blast furnace stoves.
It was discovered that in deposits found near
cracked pipes on failed exchangers, both sulphates
and nitrates were present. The large amount of
sulphate in the deposits was explained by the
182
presence of sulphur salts in the intake air. If air filters
are fitted, these salts can be removed from the air.
However, during atmospheric fog conditions, small
moisture droplets precipitate onto the filters. Salts
in the air filter dissolve in these droplets. If the fog
conditions persist for a longer period, the air filter
will become saturated with water and salt-
containing droplets can be sucked into the
combustion air entering the gas turbine.
In a gas, containing 50 vppm NO2 and
6.5 per cent water (a typical high NO2-containing
GT exhaust composition) the calculated NO2
dewpoint (32.78C) is lower than the water
dewpoint (388C). Hence, the water dewpoint
 Latest advances in the understanding of acid dewpoint corrosion
W.M.M. Huijbregts and R.G.I. Leferink
Table III Solubility of calcium nitrates
Solubility (g/l)
Temperature (8C) Ca(NO3)2·4H2O
0 2,660
18 – 1,210
30 6,600
100
Source: Weast (1988)
should be considered as the temperature at which
the first condensation takes place (Figure 5).
During the operation of HRSGs, the temperature
at the flue gas stack should be at least 708C, which
will preclude the condensation of water and nitric
acid. Only during shutdown conditions can gas
dissolve in the water droplets to form nitric acid,
but in this case, the concentration of the nitric acid
will be about 25 per cent (Figure 10).
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Therefore, the most realistic mechanism for
nitrate SCC in the HRSGs in The Netherlands
before 1995 was the dissolution of NO2 in
condensing sulphuric acid and in aerosols. By
increasing the inlet temperature above the
sulphuric acid dewpoint, formation of sulphuric-
nitric acid mixtures was more or less prevented.
In 1999, a number of new failures occurred in
HRSGs (Leferink and Huijbregts, 2002).
Ammonium nitrate was found in large amounts in
the HRSGs in the eastern part of The
Netherlands. The combustion air for affected gas
turbines was filtered before it was used to burn the
fuel and to cool turbine components. However,
Figure 14 Overview of an area where SCC occurred
Anti-Corrosion Methods and Materials
Volume 51 · Number 3 · 2004 · 173–188
small particles (aerosols, smaller than 5 mm in
diameter) could slip through the filter. The major
Ca(NO3)2 components of aerosols in The Netherlands,
monitored over a 10-year period, were reported as
–
being: 7 mg/m3 SO22 3 2
4 ; 3 mg/m NO3 ; 3 mg/m
3
þ 3 2
–
NH4 and 2 mg/m Cl (present as NaCl). These
3,760 amounts were low. However, gas turbines use vast
quantities of air for cooling and burning the
natural gas. This means that a considerable
amount of ammonium nitrate can enter the
recovery boiler in some of the Dutch HRSGs
(in rural regions of The Netherlands).
Ammonium nitrate deposits have been found in
the cooler parts of recovery boilers, close to the
stack. Under normal conditions, the flue gas will
be cooled to about 808C. However, at 1708C,
ammonium nitrate is already solid and is most
likely to be deposited on the tube walls. Because
ammonium nitrate will not leave the recovery
boiler in a vapour state, it will accumulate over
time on the heat exchanger surfaces near the
discharge to the stack. Ammonium nitrate is
hygroscopic and is easy soluble in water (1.183 kg/l
at 08C and 8.710 kg/l at 1008C) (Figure 12).
According to Harp et al. (1985), and as per the
experiences in the blast stoves, ammonium nitrate
with more than 5 per cent water (below 1208C) can
be assumed to be corrosive.
At the water dewpoint (388C) a liquid film
containing up to 75 per cent ammonium nitrate can
be expected on the wall. At 608C, the ammonium
nitrate concentration of the liquid can increase to as
much as 80 per cent (10 mol/l). In these
environments intergranular corrosion of carbon
183
 Latest advances in the understanding of acid dewpoint corrosion
W.M.M. Huijbregts and R.G.I. Leferink
steel and low alloyed steel will occur, initiating the
stress-assisted intergranular corrosion or SCC.
In some HRSGs, thermal insulation material is
mounted on the inside of the casing. The
advantage is a lower metal temperature of the
casing. This will reduce the risk of creep damage to
casing steel, and hence less expensive materials can
be used. However, there is a temperature gradient
between the inside and outside of the insulation, as
shown schematically in Figure 15. The dewpoints
of water and of gases containing NO2 and SO3 are
shown. From their locations, the dewpoints of
sulphuric acid, nitric acid and water can be found
graphically. In Figure 15, the location of the dew
points for start-up and for normal operation are
plotted for an insulation layer 25 cm in thickness.
.
In the startup situation, the temperature at the
casing will be below the water dewpoint.
At NO2 contents lower than 150 vppm, NO2
Downloaded by New York University At 17:17 16 April 2015 (PT)
and NO will dissolve in water, forming nitric
acid. At very high NO2 contents, nitric acid
will start to form above the water dewpoint in
the insulation at a depth from the casing of
about 3 cm. The SO3 present in the gas will
start condensing as sulphuric acid is at a depth
of 16.3 cm (at 0.15 vppm SO3) or 21.3 cm (at
1.5 vppm SO3). NO2 can dissolve in the
sulphuric acid, resulting in sulphuric-nitric
acid mixtures.
.
At normal operations, the casing temperature
will be above the dewpoints of water and NO2
and condensation will not occur.
Figure 15 Schematic view of the condensation processes in the insulation for a startup and a normal operation condition
184
Anti-Corrosion Methods and Materials
Volume 51 · Number 3 · 2004 · 173–188
The sulphuric-nitric acid mixture will still be
formed in the insulation at a depth of 13.8 and
20 cm.
.
Because the operational conditions are not
stable (gas and casing temperatures will move
within a certain range dictated by the actual
operating conditions), the temperature decay
lines through the depth of the insulation will
change as well. Over time, the insulation
material will accumulate sulphuric and nitric
acids and their reaction products with carbon
steel and with insulation material itself.
The most likely reaction products to be found
include nitrate and sulphate salts of iron,
calcium and ammonia.
According to Harp et al. (1985), ammonium
nitrate will no longer be corrosive above a
temperature of 1208C because the water content is
too low (i.e. less than 5 per cent). Calcium nitrate
will lose all its water of crystallisation at
temperatures greater than 51.58C. However,
because temperatures in the insulation are as low
as 508C (Figure 15), even during normal operating
conditions, the acidic nitrate salt solutions can
corrode the outer shell continuously.
7. Corrosion in a waste incineration plant
In a newly build waste incinerator the waste
(Refuse derived fuel) was burnt on a discontinuous
 Latest advances in the understanding of acid dewpoint corrosion
W.M.M. Huijbregts and R.G.I. Leferink
moving grate. Because of the variable fuel
composition the occurrence of overpressure peaks
can be considered unavoidable. However, because
the casing of the boiler was not completely airtight,
flue gas and flyash was pushed into the boiler
house (de Weijer and Huijbregts, 2003). During
the start-up period of the plant a seal in a water-
feed pipeline broke and a large amount of
condensed steam entered the boiler house.
The seal was repaired and the plant started
operation again. After approximately 2 weeks of
further operation, very severe corrosion was
noticed on the galvanised gangways, steel building
components, aluminium sheetings and processing
lines. The spring discs, from which the boiler was
suspended, suffered from SCC because of the acid
mist in the top of the boiler house directly after the
steam leakage. All springs had to be replaced.
Downloaded by New York University At 17:17 16 April 2015 (PT)
The normal condition in the boiler house is a
dry warm atmosphere and condensation is not
noticeable. Figure 16 shows some photographs
taken just after the incident in the new plant.
Figure 16 Corroded aluminium isolation plates and steel valves
185
Anti-Corrosion Methods and Materials
Volume 51 · Number 3 · 2004 · 173–188
The whole building was cleaned with water to
remove the acid products.
The flue gas concentration in the building
because of the leakage in the casing and the
overpressure peaks can be approximated with
some calculations. In these calculations, the
following parameters were considered: under
pressure in the boiler, the value of the pressure
peaks and the period of the overpressures, the
cross-sections of the leaks and the ventilation in the
building. In the direct neighbourhood of the
leakage a higher flue gas concentration will be
present than at the walls of the building.
The increase of the flue gas concentration in the
building can be calculated by means of the
equation:
C ¼ leakage=ventilation £ ðt=ð1 þ tÞÞ
The ultimate composition of the flue gas in the
building, together with the various dewpoints, are
presented in Table IV.
In the thickness of the insulation layer between
the membrane wall and the aluminium sheeting,
the temperature decreased from about 3008C to
about 458C. The temperature in the boiler hall was
about 308C when the boiler was in operation. SO3
and HCl in the escaped flue gas were the corrosive
gases to be considered (Figure 17).
The SO3 concentration decreased because of
dilution in the isolation area from a maximum of
18 vppm at the membrane wall down to the
calculated value of 0.033 vppm (diluted flue gas in
the boiler house). The calculated dewpoints for
these concentrations are 146 and 588C,
respectively. Because of the temperature decay and
the more or less linear dilution in the insulation,
the sulphuric acid droplets could be formed at
about 758C and at a depth of 3 cm in the
insulation. From Figure 9, it can be found that the
sulphuric acid concentration at 758C is 60 per
cent. Thus, condensation of sulphuric acid could
occur readily before the flue gas reached the
aluminium sheeting.
The dewpoints of the hydrochloric acid in the
flue gas at the casing (membrane wall) and in the
Table IV Composition of the boiler gas, the environment in the boiler house and
various dewpoints
Gas Waste incineration plant Boiler house
SO3 (vppm) 18 0.033
SO2 (vppm) 140 0.260
HCl (vppm) 871 1.6
H2O (volume per cent) 125 mbar (12.5 per cent) 7.2 mbar (0.72 per cent)
Dewpoint H2O (8C) 54 4.5
Dewpoint SO3 (8C) 146 58
Dewpoint SO2 (8C) 48 2
Dewpoint HCl (8C) 42 1
 Latest advances in the understanding of acid dewpoint corrosion
W.M.M. Huijbregts and R.G.I. Leferink
Figure 17 Temperature decay over the insulation outside the membrane wall with the various dewpoints
Downloaded by New York University At 17:17 16 April 2015 (PT)
boiler house were very low. The hydrochloric acid
concentrations in undiluted flue gas on an average
were about 871 and 1.6 vppm in the boiler house
atmosphere. The dewpoints at the corresponding
water vapour pressures were 58 and 18C.
Hydrochloric acid would not condense in the
insulation beneath the aluminium sheets. Dry
hydrochloric acid was present in the boiler house
as gas and was removed by the boiler house
ventilators.
However, as soon as the boiler house was filled
with steam the escaped hydrochloric acid could
dissolve instantaneously in the water droplets.
The ventilators would not remove these acid
droplets. The acid remained in the boiler house
and condensed as a film over the entire installation
inside the boiler house. This explained the severity
of observed corrosion damage.
8. Material choice in relation to nitrate
stress corrosion cracking
The use of carbon steels in conditions where there
is a risk of condensation in the presence of nitrates
or NOx means that there is a substantial
probability that SCC is likely to occur sooner or
later. SCC due to nitrates is nearly always
associated with intergranular corrosion. Leferink
and Huijbregts (2002) studied the resistance of
several ferritic steels to intergranular corrosion
in ammonium nitrate solutions in the range of
2-35 wt per cent at 908C for a period of 100 h.
186
Anti-Corrosion Methods and Materials
Volume 51 · Number 3 · 2004 · 173–188
After exposure, the steels were examined with an
optical microscope. When the intergranular
corrosion was more than three grains deep, the
steel was considered to be sensitive for
intergranular corrosion in the environment.
A clear correlation was found between the
steel composition and the molar ammonium
nitrate in which the corrosion became three
grains deep.
For all tested steels, C-steel, 15Mo3,
13CrMo44, 10CrMo910 and 12 per cent Cr steel
the correlation was:
Critical percentage ammonium nitrate
¼ 6Mo þ 2Cr þ 1Mn þ 8 2 12Si 2 8Cu 2 1C
ðR2 ¼ 0:85Þ
The correlation between the measured and
calculated critical nitrate percentages is given in
Figure 18.
After the results of this study were published,
samples steels that had failed due to nitrate SCC
were obtained from several sources. The steels
were analysed for their chemical composition, and
critical ammonium nitrate concentrations were
calculated. The results of these calculations appear
in Table V.
It is obvious that all the steel samples from the
failed constructions had a low resistance to
intergranular corrosion according to the
ammonium nitrate correlation formula.
Additionally, the difference in resistance between
 Latest advances in the understanding of acid dewpoint corrosion Anti-Corrosion Methods and Materials
W.M.M. Huijbregts and R.G.I. Leferink Volume 51 · Number 3 · 2004 · 173–188

Figure 18 Correlation between the measured and calculated critical nitrate concentrations of steels tested in ammonium nitrate
solutions of varying nitrate concentrations
Downloaded by New York University At 17:17 16 April 2015 (PT)

Table V Steels from in service failures

Chemical analysis of the steels Calculated critical

Number Steel Cr Cu Mo C Mn Si per cent nitrate
1a C-steel 0.08 0.21 0.02 0.11 0.61 0.31 3.4
2 15Mo3 0.08 0.14 0.25 0.17 0.67 0.22 6.4
3 15Mo3 0.14 0.18 0.27 0.15 0.61 0.23 6.2
4 C-steel 0.07 0.2 0.02 0.12 0.46 0.22 4.4
5 C-steel 0.06 0.04 0.01 0.11 0.48 0.25 5.2
6a 15Mo3 0.08 0.32 0.33 0.12 0.61 0.21 5.6
7 C-steel 0.07 0.14 0.01 0.08 0.49 0.15 5.7
8 C-steel 0.08 0.52 0.03 0.05 1.17 0.14 3.6
9 C-steel 0.058 0.42 0.052 0.05 1.09 0.17 4.1
10 C-steel 0.036 0.44 0.03 0.05 1.11 0.17 3.9
11 C-steel 0.036 0.44 0.03 0.05 1.12 0.17 4.0
12 C-steel 0.036 0.48 0.03 0.06 1.16 0.15 3.8
13 C-steel 0.036 0.33 0.03 0.06 1.23 0.19 5.8
14 C-steel 0.036 0.25 0.03 0.07 1.07 0.34 3.2
15 C-steel 0.02 0.021 0.002 0.13 0.959 0.342 4.6
16 C-steel 0.03 0.024 0.006 0.111 1.19 0.193 6.7
17 C-steel 0.1 0.11 0.03 0.07 0.49 0.17 5.9
Note: aSteels were tested in ammonium nitrate

the carbon steels and 15Mo3 steel to intergranular which generate condensing gases makes it
corrosion in nitrate solutions was minimal. necessary to think carefully about the
operational regimes (both on and off line), and
of the possible risk of acid condensation
9. Conclusions attack.
.
Even though knowledge on condensation of
.
Condensation of nitric acid can cause SCC of
corrosive gases is well available in literature, carbon steel. However, reaction products of
design failures due to condensation nitric acid with the steel or insulation also can
phenomena still occur in technical result in the formation of corrosive
installations. The operation of equipment, ammonium or calcium nitrates.
187
 Latest advances in the understanding of acid dewpoint corrosion
W.M.M. Huijbregts and R.G.I. Leferink
.
Both calcium and ammonium nitrates are
hygroscopic materials that can take up water
even above the dewpoint of a gas. Up to a
temperature of 1208C this can create a very
corrosive environment and may result in a
severe risk of nitrate SCC to susceptible
materials.
.
As nitrate SCC is often a precursor to
intergranular corrosion, SCC is particularly
influenced by chemical corrosion. Annealing a
material, or the selection of a higher strength
material, will be of minimal help in preventing
SCC on the longer term. The selection of a
low-alloyed 2 per cent chromium steel as a
replacement for carbon steel in critical
locations is a better choice for preventing the
intergranular corrosion in dissolved nitrate
environments.
Downloaded by New York University At 17:17 16 April 2015 (PT)
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Nitratkonzentration und Potential sowie molydangehalt
und Gefugezustand auf die Spannungsrisskorrosion von
Kohlenstoffstahlen”, Werkstoffe und Korrosion, Vol. 38,
pp. 243-59.
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Wendler-Kalsch, E. (1991), “Potentialabhangigkeit der
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calciumnitrat-Losung und natronlauge”, Werkstoffe und
Korrosion, Vol. 42, pp. 128-38.
Krautschick, H.J., Bohnenkamp, K. and Grabke, H.J. (1987),
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corrosion cracking of carbon”, Werkstoffe und Korrosion,
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stress corrosion cracking of mild steels in nitrate
solutions”, Corrosion Science, Vol. 28 No. 3, pp. 251-8.
Mazille, H. and Uhlig, H.H. (1972), “Effect of temperature and
some inhibitors on stress corrosion cracking of carbon
steels in Nitrate and Alkaline Solutions”, Corrosion, Vol. 28
No. 11, pp. 427-33.
McEvily, A.J. Jr (1990), “Atlas of stress corrosion and corrosion
fatigue curves”, in McEvily, A.J. (Ed.), Ohio 44073, ASM
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