13th ICC Paper 150 Page 1

INITIATION OF FLOW INDUCED LOCALIZED CORROSION

IN OIL AND GAS PRODUCTION.
HYDRODYNAMIC FORCES VS. MECHANICAL
PROPERTIES OF CORROSION PRODUCT SCALES
G. Schmitt, U. Pankoke, Ch. Bosch,
T. Gudde#, E. Strobel-Effertz#, M. Papenfuss# & W. Bruckhoff *
Laboratory of Corrosion Protection, Iserlohn Polytechnic
#Institute of Technical Chemistry, Aachen University of Technology
*BEB Erdgas und Erdl GmbH
SUMMARY: Wall shear stresses encountered in technical flow systems, e.g. in oil and gas
production wells, proved to be too small to initiate flow induced localized corrosion (FILC) by
destruction of corrosion product scales. Therefore, the fracture mechanical properties of scales
from CO2 and H2S corrosion of carbon steel were investigated with respect to FILC inititiation.
Failure mode diagrams for iron carbonate and iron sulfide together with experimental data from
corrosion products revealed that iron carbonate scales can build up intrinsic growth stresses
comparable with critical stresses for fracturing and spalling. Inhibitors improve the fracture
mechanical properties of these scales by reducing their thickness, porosity and intrinsic stress.
Using the submerged jet impingement method the FILC resistance of iron sulfide scales were
quantified in terms of critical wall shear stresses which however seem to be relatible to
microturbulence induced dynamic mechanical loading of the scales. The FILC resistant type of
sulfide scale was significantly thinner than the FILC susceptible type and exhibited better fracture
mechanical properties.
Keywords: carbon steel, carbon dioxide, hydrogen sulfide, sour gas, elemental sulfur, polysulfide,
iron carbonate, iron sulfide, corrosion product scales, oil and gas production, corrosion, flow, jet
impingement, wall shear stress, fracture mechanics
1. INTRODUCTION
The initiation of flow induced localized corrosion (FILC) is generally explained by hydrodynamic destruction of corrosion
product scales. However, recent experimental results demonstrated (1, 2) that hydrodynamic forces expressed in terms of wall
shear stresses, are orders of magnitudes to small to be made responsible for the destruction of e.g. iron carbonate scales.
Therefore, other influences, e.g. the fracture mechanical properties of the scale (specifically the intrinsic growth stress), must be
involved in the initiation step of the mechanism of FILC.
Experimental work was carried out both in sweet and sour systems. This paper reports first on the quantification of intrinsic
growth stresses and critical fracture strains of iron carbonate scales from CO2 corrosion of carbon steel, including effects of
corrosion inhibitors. The second part will describe results from submerged jet experiments designed to quantify critical flow
intensities for FILC initiation on iron sulfide covered carbon steel under conditions of high pressure hydrogen sulfide corrosion.
13th ICC Paper 150 Page 2
2. EXPERIMENTAL
2.1 CO
2
Corrosion
2.1.1 Rotated cage experiments
Coupons (50 x 10 x 2 mm) of the same heat of a carbon steel type 38 Mn6 (C 0.4; Si 0.25; Mn 1.26; P 0.016; S 0.005; Al 0.005;
Cu 0.04; Cr 0.03; Ni 0.01; Mo 0.04) were tested with as-rolled (ferritic-pearlitic) microstructure (API-J55) and with
quenched-and-tempered (martensitic-bainitic) microstructure (API-C75; in some experiments also API-C90) in the 'rotating cage'
arrangement (3) in brine with 10 g/L NaCl under 5 bar (0.5 MPa) CO2 at 50 and 80C with a rotation speed at the outer coupon
surface of 2 and 4 m/s. The exposure time was generally 96 h (4 days). Inhibitor effects were studied with n-dodecylamine, n-
octadecylamine, n-dodecyltrimethylammonium chloride, and n-octadecyltrimethylammonium chloride. The inhibitor
concentration generally was 1 mmole/L. No measures were taken to adjust the pH of the solution. Prior to the experiment the
coupons were degreased in an ultrasonic bath for 5 min. in a low boiling hydrocarbon mixture and subsequently 5 min. in
acetone. The coupons were then pickled with 10% hydrochloric acid, neutralized with alkali and air-dried after rinsing in water
and finally with methanol.
2.1.2 Evaluation of results
To estimate critical fracture strains of iron carbonate scales produced under a given set of environmental conditions the scales of
the 20 x 2 mm cross section of corroded test coupons were completely photographed with a magnification of 100. Ten
characteristic areas were then selected and photographed again with a magnification of 500. These photos were used to estimate
the scale thickness h, the porosity p and the weakening factor f. The porosity p was calculated according to Eq. 1 from the ratio of
the area Ad of the sum of all small defects identified in a defined area At in the cross section.
p = Ad/At [1]
In pratice, each single defect was circumscribed by the required rectangle, and the resulting areas of the rectangles were summed
up to give Ad. The weakening factor f was defined as the ratio of the composite defect length td (perpendicular to the metal
surface) and the total scale thickness h (Eq. 2)
f = td/h [2]
The composite defect length was estimated according to a graphical procedure proposed in the literature (4) using standard
techniques generally applied to determine the interaction of defects in welds (5). In practice, each defect was circumscribed by
the required rectangle and the rules of interaction were applied as detailed in lit. (4).
Critical fracture strains
crit were estimated according to Eq. 5 (6). The surface fracture energy was calculated according to Eq.
3 with
o = 3.0 N/m as assessed from literature (6). The numerical factor F was chosen as 1 assuming only burried defects in the
scale. The Young's modulus was calculated according to Eq. 4 with
o = 150 GN/m
2
(2,6). Eq. 4 shows that thinner scales
crack at higher straines than thicker scales.
=
o(1-p)
3
[3]
=
o (1-p) [4]

crit
F f Eh
=

2
2
1
2
[5]
Critical fracture strains calculated for iron carbonate scales grown under different environmental conditions were introduced into
a failure mode diagram (Fig. 1) showing the regimes of elastic adherence, brittle spalling and ductile adherence of iron carbonate
scales, if =
o = 3.0 N/m, =
o = 150 GN/m
2
, F = 1 and f = 0.1 in Eq. 5. The boundary lines between brittle spalling and
ductile adherence are limited by the yield
y of the iron carbonate which was estimated from literature data (6) to be approx. 1.4
GN/m
2
. In this regime the scale remains attached to the substrate and protective. The strain where the carbonate scale reaches the
yield strenght is 9.33 10
-3
for the above given set of data (Eq. 6).
=
y/
o = 9.33 10
-3
[6]
The limiting scale thickness is 1.46 m for these conditions. Fig. 1 gives the boundary lines for 1.0 , 0.5 and 0.2 to show
the scatter band if 50% or 20% instead of 100% of the surface fracture energy would be needed for scale cracking.
13th ICC Paper 150 Page 3
Figure 1: Failure mode diagram for iron carbonate scales.
Data points obtained from corrosion experiments (steel 38
Mn6, 1 % NaCl, 5 bar CO
2
, 1 mM inhibitor (if present), 50
and 80C, 2 and 4 m/s) were inserted into calculated
diagram.
2.2 H2S Corrosion
2.2.1 Submerged jet experiments
A submerged jet cell (Fig. 2) was integrated into a high pressure flow loop (Fig. 3) designed for experiments up to 180C and
100 bar hot pressure under sour gas conditions. All medium-contacted materials were made of Hastelloy C4 (2 ltr. heated
autoclave), Hastelloy C22 (jet cell, tubings, fittings), PTFE filled with synthetic mica (gears in gear pump), TORLON (a
polyamideimide; used for electrical insulation purposes) and peroxidically linked EPDM (O-rings).
Figure 2 - Submerged jet cell Figure 3 - High pressure loop for jet cell
In the jet cell (Fig. 2) the finely ground surface of a cylindrical steel probe (a manganese steel type 39 Mn 5/API-C75/2,
chemical composition: C 0.39; Si 0.09; Mn 1.38; P 0.016; S 0.0039; Al 0.017; Cu 0.04; diameter: 20 mm; height: 8 mm) was
centrically exposed to a liquid jet stream from a nozzle with 1 mm inner diameter. The distance between the nozzle and the
specimen's surface was 5 mm. Under experimental conditions both the specimen's surface and the mouth of the nozzle were
submerged in the test liquid which was heated in the 2 ltr. autoclave and circulated with a gear pump. The flow velocity at the
nozzle exit was measured by a mass flow meter. Provisions were made to vibrate the probe with frequences up to 100 Hz and
amplitudes up to 120 m if desired.
The corrosion system tested correlated with the downhole conditions in north German sour gas fields which are produced by
continuous injection of aqueous monoethylamine MEA regenerate to prevent plugging of production strings by elemental sulfur
(7-9). The corrosion liquid consisted of an aqueous, polysulfide containing MEA solution with MEA concentrations of 2.4 and
5.0 moles/ltr. saturated at test temperature with 23 to 45 bar (2.3 to 4.5 MPa) hydrogen sulfide. In the 2.4 M MEA solution 28.8
g/ltr. elemental sulfur were dissolved as polysulfide, while the 5 M MEA solution contained 60 g/ltr. polysulfide. Jet
experiments were run at 110 and 130C with jet exit flow velocities of 1.4 to 11.5 m/s. The exposure times were 42 to 120 h.
The surface preparation of the specimen's surface followed the same procedure as described in chapter 2.1.1.
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2.2.2 Evaluation of results
In submerged jet streams oriented perpendicular to a solid surface the flow pattern can be described according to Fig. 4 (10).
The lowest thickness of the hydrodynamic boundary layer is found in region B. For this region (3 x/d 5) the wall shear stress

w [N/m
2
] can be calculated for a given flow velocity uo at the exit of the nozzle using Eq. 7 (10),

w
u
x
d
=

0 0447
0
2 0 182
2
, Re
,
[7]
with = density [kg/m
3
], Re = Reynolds number = uo d/, = kinematic viscosity [m
2
/s] d = inner diameter of jet nozzle [m], x
= radial distance [m] from centre of nozzle.
If corrosion product layers are destroyed at a critical wall shear stress
w(crit) the mass transfer coefficient k which is effective at
the site of scale destruction can be calculated using Eq. 8 for mass controlled corrosion on scale-free surfaces (D = diffusion
coefficient [m
2
/s]).
k
u D
x
d
w
=

2
3
0 8 ,
[8]
The density and kinematic viscosities of the polysulfide containing MEA solutions at 110 and 130C estimated in (12) are listed
in Table 1. If
w from Eq. 7 is inserted into Eq. 8 the mass transport coefficient at 3 x/d 5 (region B in Fig. 4) can be
assessed with Eq. 9 if the Schmidt number Sc (Gl. 10) can be approximated with 10
3
for aqueous media (Table 2).
k u
D
x
d
=

0 0447
0 182
2
3
1 2
, Re
,
,

[9]
Sc = /D 10
3
[10]
Figure 4: Flow pattern at submerged jet (10)
Table 1 - Density and kinematic viscosity of polysulfide containing 2.4 and 5.0 M MEA solutions at 110 and 130C
(12)
MEA-Concentration
[mole/ltr.]
Temperature
[C]
Density
[kg/m
3
]
Kinematic
Viscosity
[m
2
/s]
2.4 110 951.4 3.44 10
-7
130 929.5 2.62 10
-7
5.0 110 949.1 4.19 10
-7
130 926.6 2.90 10
-7
3. RESULTS
3.1 CO2 Corrosion
In the absence of inhibitors the iron carbonate scale thicknesses ranged in the order of 40 to 100 m depending on the corrosion
conditions. Addition of fatty amines and quats as inhibitors (1 mM) reduced the scale thickness (2 to 5 m) by more than one
order of magnitude. A small effect of steel microstructure was observed. The inhibitors tested generally produced slightly thinner
scales on steel with ferritic-pearlitic microstructure (J55) than on steel with quenched-and-tempered microstructure (C75).
13th ICC Paper 150 Page 5
However, in the absence of inhibitors J55 coupons yielded thicker scales than C75 samples. Incomplete inhibition and higher
flow intensities resulted in thicker scales which could then exceed 100 m.
When critical strains for brittle spalling of the scales were estimated with the procedure described in detail in the experimental
part, it appeared (Fig. 1) that in the presence of no or poor inhibitors the critical strains ranged in the order of 5 10
-4
to 4 10
-3
while in the presence of effective inhibitors the critical straines were close to 10
-2
. This yields according to Eq. 11 critical
stresses for the iron carbonate scales in the range of 75 to 600 N/mm
2
in uninhibited or poorly inhibited solutions and 1000 to
1250 N/mm
2
in effectively inhibited media.

crit =
crit [11]
As spalling of iron carbonate scales was observed to occur with topotactic scales (formed at the beginning of corrosion) at
thicknesses in the range of 10 to 20 m, it must be assumed that (according to Eq. 12 with =
o = 150 GN/m
2
, Poisson number
= 0.3 [2,6]) intrinsic stresses in the order of 550 to 770 N/mm
2
(assuming 100% ) can be built up in carbonate scales which is
in the same order of the critical stresses for fracturing and spalling of iron carbonate scales formed under conditions of
uninhibited CO2 corrosion.

intr = /(1-)
[12]
These findings support the hypothesis that initiation of FILC in CO2 corrosion of steel is caused by cracking and subsequent
spalling of iron carbonate scales rather than by hydrodynamic scale destruction. Inhibitors improve the fracture mechanical
properties of scales by reducing their thickness (which increases their critical strains), their intrinsic growth stress and their
porosity.
Table 2 - Correlation between flow velocity u at the nozzle exit, wall shear stress
w
and mass transport
coefficient k according to Eq. 7 and 8
Flow velocity
u [m/s]
Wall Shear Stress

w(x=3d)[N/m
2
]
Mass Transport Coefficient
k [m/s]
1.4
2.3
4.6
11.4
1.9
4.7
16.6
87.9
3.59 10
-5
5.37 10
-5
9.47 10
-5
19.90 10
-5
Figure 5: Effect of temperature and MEA-concentration on
integral corrosion rate and FILC of steel 39 Mn5/C75-2 in
polysulfide containing MEA-solution under sour gas
pressure (Rotating cage experiments with 50 x 20 x 2 mm
coupons; 15 - 60 g/ltr. S
x
; 30 - 90 bar H
2
S; 2.2 - 4 m/s
rotation speed in rotating cage; 93-96 h; I
max
= max. local
penetration)
3.2 H2S Corrosion
It has been shown in previous investigations (13) that the corrosivity of polysulfide (Sx) containing MEA solution depends at and
above 130C primarily on the MEA concentration (Fig. 5). While no significant effect of the MEA concentration was observed
at 110C, a sharp increase in corrosion rate and severity of localized attack was encountered if the MEA-concentration was
increased at and above 130C from 4.0 to 5.0 moles/ltr.. The increase in corrosion attack was accompanied by a different
appearance of the corrosion product scales. The more protective and flow resistant sulfide scales (observed at 110C at all
MEA-concentrations and at 130C at MEA-concentrations below 4.7 M) were obviously rather thin and adherent and exhibited a
13th ICC Paper 150 Page 6
dark-purple/magenta colour, while the less protective and flow susceptibel sulfide scales were thicker and spongy-like with poor
adherence and showed a grey/graphite-like appearance.
A threshold temperature for the transition of protective to non-protective iron sulfide scales had been found already in earlier
investigations on the corrosivity of polysulfide-free MEA regenerates in the annulus of concentrically completed sour gas wells
with MEA injection (7,8). Between 115 and 123C the properties of the sulfide scales changed in the same way as described
above, i.e. from protective, thin, dark-purple/magenta sulfide films to non-protective, thick, grey/graphite-like sulfide scales.
This was attributed to morphology changes of the sulfides involved (troilite, hexagonal and monoclinic pyrrhotite and pyrite)
which are known to occur in this temperature range (14), but was also shown to be influenced by the presence of MEA and
polysulfide (7,8).
It was now decided to quantify the FILC resistance of the different types of sulfide scales formed under the environmental
conditions presented in Fig. 5. Experimentally the sugmerged jet was used to evaluate critical flow intensities in terms of critical
wall shear stresses
w(crit) for the initiation of FILC. These data for inhibitor-free systems are needed for later comparison with
inhibited media for ranging corrosion inhibitors by their critical wall shear stresses for FILC initiation.
Figure 6: Effect of flow velocity at the nozzle exit and of
MEA concentration on integral corrosion rate (28.8 resp.
60 g/ltr. S
x
; 33-45 bar H
2
S (hot); (130C; 96; l
max
= max.
local penetration)
Figure 7: Effect of wall shear stress at a distance of 3d
from jet centre and of MEA concentration on FILC (28.8
resp. 60 g/ltr. S
x
; 33-45 bar H
2
S (hot); 130C, 96h)
The effect of flow velocity on the corrosion rate of carbon steel (calculated from mass loss data) at 130C in polysulfide
containing 2.4 and 5.0 M MEA solution is shown in Fig. 6. In the 2.4 M MEA solution the increase of the flow velocity had only
minor effects. After 4 days at 11.4 m/s only a faint indication of a first start of FILC was visible on the coupon surface. The
corresponding wall shear stress of 88 N/m
2
(calculated according to Eq. 7) was therefore taken as the threshold wall shear stress
under these corrosion conditions. However, in 5 MEA solution the initiation of FILC was already observed at a flow velocity of
2.3 m/s. The intensity of FILC increased significantly with increasing flow velocity. Only at a flow velocity of 1.4 m/s no FILC
was found within the exposure time.
The dependence of FILC intensity from the wall shear stress at a distance of 3d from the jet centre is seen in Fig. 7. At this
distance also the start of local penetration was observed. Here the integral penetration rate reached 33 mm/a already at a wall
shear stress of only 4.7 N/m
2
. At a wall shear stress of 1.9 N/m
2
no FILC could be detected. Therefore, 2 N/m
2
were taken as the
threshold value of the wall shear stress for these corrosion conditions.
The findings that the critical wall shear stress for FILC initiation in 2.4 MEA solution at 130C is approx. 90 N/m
2
, but only 2
N/m
2
in 5.0 M MEA solution demonstrate the great difference in FILC susceptibility of the sulfide scales formed under those
conditions. Even at 110C the critical wall shear stress increased only to 10 N/m
2
for the 5 M MEA solution. This proves in
accordance with earlier results (7,8) that high MEA concentrations initiate the formation of non-protective iron sulfide scales,
even in the presence of polysulfide. Once the sulfide scale is locally destroyed mass transfer coefficients in the distance of 3d to
5d from the jet centre range between 3.6 10
-5
m/s (u = 1.4 m/s) and 19.9 10
-5
m/s (u = 11.4 m/s) (Table 2).
The fact that critical wall shear stresses, i.e. critical hydrodynamic forces for FILC initiation could be quantified for these iron
sulfide scales seems to contradict the results obtained with iron carbonate scales found to be destructed by intrinsic mechanical
forces rather than hydrodynamic forces. However, it had already been suggested (2) that dynamic mechanical loading of the
scales by hydrodynamic forces, e.g. by dynamic pressure changes at microturbulences, could also contribute to the initiation of
FILC in the sense of fatique loading of the scale. In case of the submerged jet stream it seems also possible that dynamic
mechanical loading can be exerted onto the scaled surface. Therefore, the submerged jet cell was equipped with a vibrator which
13th ICC Paper 150 Page 7
allowed to vibrate the test specimen in order to simulate fatigue loading and thus initiate FILC under conditions under which no
FILC would occur without additional vibrations.
Indeed, it could be shown (Fig. 8) that FILC is initiated by additional vibration (frequency: 35 Hz; amplitude: 100 m) of the
coupon at 110C in the presence of polysulfide containing 5 M MEA under a jet flow velocity of 4.6 m/s. While pratically no
FILC was observed without additional vibration, the vibration enhanced the mass loss rate and the intensity of FILC significantly.
This influencing parameter will be studied further in detail with the aim of finding critical dynamic loading conditions for
destruction of corrosion product layers and FILC initiation.
For comparison with the iron carbonate scales also the question of iron sulfide scale destruction by mechanical forces was
investigated by means of failure mode diagrams. Fig. 9 shows the failure mode diagram for iron sulfides calculated according to
Eq. 5 using the data collected in Table 3 based on assessments from literature data (6). The scale thickness was measured in the
scanning electronic microscope (SEM) and the porosity p was assessed from cross sections investigated in the SEM. The iron
sulfide scales proved to be much thinner than the iron carbonate scales. However, it agrees with the previous experience that the
nonprotective sulfide scales formed in 5 M MEA (approx. 10 m) are about three times thicker than the protective scales grown
in 2.4 M MEA solution (3 m).
Figure 8 Effect of mechanical vibrations (frequency: 35 Hz;
amplitude: 100 m) on initiation of FILC 23-26 bar H
2
S
(hot); flow velocity at nozzle exit: 4.5 m/s; wall shear
stress at x = 3d: 14.4 N/m
2
(assuming Eq. 7 is still valid
under these conditions) ; 66.5h)
Figure 9 Comparison of experimental with calculated data
in the failure mode diagram for iron sulfide scales
(experimental conditions: steel 39 Mn 5; 2.4 or 5 M
MEA; 28.8 or 60 g/ltr. S
x
; 29-34 bar H
2
(hot); 130C; 4 m/s
(jet), 44-96 h)
Table 3 - Data used to calculate the failure mode diagram in Fig. 9 and the experimental data points for sulfide
scales in 2.4 and 5 M MEA solution at 130C
Parameter 5 M MEA 2.4 M MEA

o[N/m]
1.2 1.2
Eo [GN/m
2
] 67 67
p 0.5 0.3
[N/m]
0.15 0.41
E [GN/m
2
] 8.4 23
f 0.1 0.1
h [m]
10 3

crit
3.37 10
-3
6.16 10
-3
4. CONCLUSIONS
In CO2 corrosion of steel FILC is initiated by cracking and subsequent spalling of iron carbonate scales due to high intrinsic
stresses. Inhibitors improve the fracture mechanical properties by reducing their thickness, porosity and intrinsic stress. Critical
13th ICC Paper 150 Page 8
wall shear stresses for FILC initiation measured with the jet impingement method at iron sulfide scales with different FILC
resistivity seem to be relatible to microturbulence induced dynamic mechanical loading of the scales. The information on the
fracture mechanical properties of corrosion product scales is essential to assess their FILC resistivity.
5. REFERENCES
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CORROSION'95, NACE International, Houston/Texas(USA), 1995, Paper 95102.
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Relation to Localized Corrosion", CORROSION'96, NACE International, Houston/Texas(USA), 1996, Paper 96009.
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Werkstoffe und Korrosion 28 (1977) 597.
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(National Association of Corrosion Engineers), Houston/ Texas (USA), 1990, Paper 90013.
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Scales under Sour Gas Corrosion Conditions" (in german), Diploma Thesis, University of Dortmund, March 1996.
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Gas" (in german), Dissertation, Aachen University of Technology, June 1996.
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