Heat Exchanger Fouling and Cleaning – 2022

CHARACTERIZING FOULING TENDENCY OF CRUDE OIL ON A SURFACE USING A

HIGH TEMPERATURE VARIABLE SHEAR COUPON TEST RIG

P. Singh1, *S. Krishnaswamy1, K. Ponnani2, A. Verma3 and J. Rawat3

1
Centre of Excellence in Process Engineering & Intensification (COE-PE&I),
Department of Chemical Engineering, BITS-Pilani K K Birla Goa Campus, Goa, India
*E-mail address: srinivas@goa.bits-pilani.ac.in
2
15/151 (old 7/383) Sreenivas, Sivan Kovil Street, Tharakkad, Palakkad, Kerala-678001, India
3
Bharat Petroleum Corporation Limited, Corporate R & D Center, Greater Noida, India

ABSTRACT studies [3], [7]–[15]. Heat transfer investigations

The present study experimentally and deposit characterization in several of these
demonstrates the ability of a High Temperature studies has been based on the flow of multiple
Variable Shear (HTVS) coupon test rig to streams over surfaces under varying operating
characterize fouling under dynamic flow conditions. conditions. A deeper insight into refinery fouling
Experiments were conducted in a 2-litre batch can be obtained by testing an individual stream
autoclave system with provision to immerse metal under a specific operating condition of interest. This
coupons into the stream. Experiments were formed the genesis of the present work.
conducted covering bulk temperatures and stirrer This study demonstrates the potential of a High
speeds (which incorporated a shear effect) ranging Temperature Variable Shear (HTVS) coupon test rig
from 250 oC to 300 oC and 100 to 600 RPM in understanding fouling due to sulfidic corrosion
respectively. Parts of the foulant deposits collected over a wide range of temperature and rotational
were found to strongly (hard) and weakly (soft) speeds. A custom design setup was built for this
adhere to a coupon surface. These deposits were purpose. The use of HTVS was earlier demonstrated
subsequently characterized independently using for a limited temperature range at a fixed rotational
Thermogravimetry (TGA), Elemental analysis, speed by Singh et al. [18]. The setup design was
Scanning Electron Microscopy (SEM) and X-Ray based on an approach adopted by Wang and
Diffraction (XRD). The nature of soft deposits was Watkinson [11], [16], [17] who studied fouling on a
found to be distinct from the nature of crude oil used. cylindrical surface immersed in a rotating fluid at
Corrosion was found to be the dominant fouling temperatures greater than 350 oC. The rig facilitates
mechanism in this work. The results obtained easy removal of deposits for further analysis and
confirm the potential of this test rig in understanding characterization. Details of the rig, experiments
fouling tendency of liquid refinery streams on a performed and results are reported herewith. The
surface. temperature range covered in this study corresponds
to that prevalent in the crude Pre-Heat Exchanger
INTRODUCTION Train (PHT) in a refinery. The effect of rotational
Petroleum refining has long been the primary speed not included in [18] is also reported.
backbone for meeting global energy demands,
producing fuels that have been used in industry, EXPERIMENTAL SETUP AND PROCEDURE
transportation and homes. Fouling from light and Fouling experiments were carried out in a
heavy crude oil streams during processing has been custom-made test rig comprising of a 2-liter
identified as a major cause of suboptimal operation stainless steel autoclave (120 mm ID and 300 mm
in refinery systems resulting in plant downtime and height) surrounded by a 2.5 kW ceramic band heater
production loss [1], [2]. Several studies have been fitted with a controller. A schematic of the autoclave
carried out over the years to better understand the internals is shown in Fig. 1. The controller was
complex mechanisms associated with fouling in driven by a temperature sensor that measured the
refinery equipment ranging from molecular to lab outer surface temperature of the autoclave. This
and plant scale. Several of these studies were mainly facilitated maintaining the fluid temperature at a
concerned with examining the impact of fouling on desired value during the test runs. The autoclave and
heat transfer, particularly on tubular test surfaces heater assembly were insulated using glass wool. A
[3]–[6]. Attempts have also been made to head assembly enabled closing of the system when
characterize foulant deposits in some of these

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 Heat Exchanger Fouling and Cleaning – 2022

in operation. A photograph of the test unit is shown Carbon steel (AISI 1060) coupons with
in Fig. 2. dimensions of 7.5 cm (length)  1.2 cm (width)  0.1
Pressure was measured using a Bourdon cm (thickness) were used for experimentation.
pressure gauge (WIKA make, range: 0 – 100 bar, These coupons were fixed vertically at two
accuracy: ± 1.0% of full scale) and also using a prescribed levels on a solid central shaft which could
WIKA make pressure transmitter (range: 0 – 150 be rotated up to 1450 RPM. A maximum of 6
bar, accuracy: ± 0.5% of full scale). A reflux numbers of coupon (at 60o positions on a discs)
condenser was used to condense any low boiling could be anchored at a particular level. Fig. 3 shows
vapors arising from the sample which were directed the photograph of a test coupon. A SCADA based
Data Acquisition System (AMAR DAS 4.0)
provided by Amar Equipment Pvt. Ltd. (Mumbai,
India) was used to record data.

Fig. 3. Test coupon.

The experimental procedure was initiated by

measuring the coupon surface roughness using a
surface roughness tester (Surftest SJ-410 Series
Mitutoyo make, Japan). Before measurements, the
coupons were polished with emery paper of 180 grit
to eliminate surface flaws if any. The coupons were
then independently weighed and anchored to the
Fig. 1. Schematic of autoclave internals. shaft. The autoclave was filled with the 1.8 liters of
test fluid and closed. The system was pressurized to
back into the autoclave by gravity. A vent valve at 30 bar (g) with nitrogen and leak tested for 2 hours.
the condenser outlet was used to depressurize the The system was then depressurized to ~8 bar (g).
system at the end of every run. The fluid temperature The nitrogen purging also ensured removal of air
was measured using two Nickel-chromium/Nickel- from the vapour space of the autoclave.
aluminum (K type) thermocouples positioned at a The fluid was first heated to attain a desired
distance of 135 mm and 290 mm from the head bulk temperature at a prescribed RPM. Tests showed
assembly. Samples were discarded after each run that no significant deposition occurred during this
using a Flush Bottom Valve. heating process. The system was allowed to operate
for 80 hours following which the heater was
switched off. The system was then cooled and
depressurized. The head assembly along with
coupons attached to the shaft was removed and kept
on a side seat (see Fig. 2) for 8 hours. This ensured
gravity draining and removal of any excess amount
of the test fluid which would have adhered to the
coupons during experimentation.
Each coupon with accumulated foulant deposits
was detached from the shaft, washed using 100 ml
of n-heptane, dried for 1 hour at room temperature
and weighed. Deposits washed away with n-heptane
were collected in a petri dish. The petri dish and its
contents were weighed after evaporating the solvent
in an oven for 8 hours.

RESULTS AND DISCUSSIONS

Fig. 2. Photograph of coupon test rig A crude oil sample provided by BPCL
(Reproduced from [18]) Corporate R&D Centre was used for

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 Heat Exchanger Fouling and Cleaning – 2022

experimentation. The important properties of the oil the corrosion rate increasing above this temperature
are listed in Table 1. [16], [17].
The higher temperature also promotes chemical
Table 1 Properties of crude oil# reactions among organic species in the soft deposit.
Element Result These reaction rates dominate the rate of formation
API 30.87 of FeS at higher temperatures (> 275 oC). These soft
Viscosity (cP) @ 38 oC 2.631 deposits will subsequently adhere to the FeS layer
Viscosity (cP) @ 200 oC 0.843 due to change in surface characteristics. This will
C (wt. %) 84.22 result in a higher organic content in hard deposit (as
H (wt. %) 12.13 confirmed by TGA).
N (wt. %) 1.33
S (wt. %) 1.83 35
Saturates (wt. %) 25.58 Hard Deposit
30 Soft Deposit
Aromatics (wt. %) 44.38

Wt. of deposits, mg
Resins (wt. %) 27.37 25
C7-Asphaltenes* (wt. %) 1.76
CII 0.38 20
Fe (ppm)** 2.31 15
Mg (ppm)** 1.26
Na (ppm)** 7.16 10
Ni (ppm)** 6.95
5
Si (ppm)** 86.54
V (ppm)** 17.7 0
# Reproduced from [18]; *Estimated using ASTM D 6560 240 250 260 270 280 290 300 310
protocol. **Elemental analysis done using ICP – AES.
Fluid bulk temperature (oC)
Foulant deposit was collected from each coupon
post washing with n-heptane. A part of the deposit Fig. 4. Effect of bulk temperature on formation of
formed was carried away by n-heptane, while a hard and soft deposits at 100 RPM after 80 hours
portion remained strongly adhered to the coupon
surface and could only be removed by scraping. The effect of temperature on hard and soft
These are henceforth referred to as soft and hard deposits was also investigated at 250 RPM and is
deposits respectively. shown in Fig. 5.
In the subsequent sections, influence of bulk
temperature and rotational velocity on the amount of 160
hard and soft deposit formed on a coupon surface is Hard Deposit
140 Soft Deposit
discussed.
Wt. of deposits, mg

120
Effect of bulk temperature 100
The impact of fluid bulk temperature at 100
RPM on the amount of hard and soft deposit is 80
shown in Fig. 4 at 250, 275 and 300 oC. The results 60
presented are for a single representative coupon (C1)
immersed in the test fluid during the above runs. The 40
average coupon surface roughness (Ra) across these 20
three runs was 1.584 μm. The variation in coupon
0
surface roughness between 250 and 300 oC was
0.059 μm. 240 250 260 270 280 290 300 310
The amount of hard and soft deposit formed on Fluid bulk temperature (oC)
the coupon surface increases with temperature. At
250 oC, the soft deposit is one order of magnitude Fig. 5. Effect of bulk temperature on formation of
higher in amount than the hard deposit. The orders hard and soft deposits at 250 RPM after 80 hours.
are comparable at 275 and 300 oC due to increase in
the rate of FeS formation (via a corrosion The trend in hard deposit was found to be similar.
mechanism) at these temperatures. The FeS formed However, a significant increase in amount of hard
is part of the hard deposit (confirmed later by deposit was observed beyond 275 oC. This is due to
characterization). Sulfidic corrosion based fouling the increased attachment of organic content in soft
on carbon steel has been reported as a predominant deposit to the FeS layer formed. At these
mechanism in past works at 260 oC and above with temperatures, the attachment is also preceded by
increased rate of chemical reactions of FeS

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 Heat Exchanger Fouling and Cleaning – 2022

formation and chemical species in the soft deposit. of decrease in amount of hard deposit. The
The soft deposit is found to decrease with increase discrepancy in soft deposit values for the two
in temperature. coupons at a shear stress of 0.18 Pa can be attributed
to flow conditions being laminar and applicability of
Effect of RPM equation 1 in this flow regime.
The effect of RPM at a constant temperature on
the amount of hard deposit formed on a coupon 40 C1
surface after 80 hours is shown in Fig. 6. The results
are presented for 2 representative coupons (C1 and 35 C2

Wt. of hard deposit, mg

C2). Apart from 100 RPM at 275 oC, test runs were 30
also conducted at 250, 400 and 600 RPM without
changing the bulk temperature. The range of shear 25
stress and Reynolds number (Re) corresponding to 20
these RPM values is 0.18 to 3.88 Pa and ~2100 to
~16000 respectively. The shear stress was estimated 15
using the correlation [17], [19] 10

𝜏c = 0.079  𝑅𝑒c−0.3  𝜌  𝑢c2 (1) 5

0
The coupon Reynolds number was calculated using 0 1 2 3 4
Shear Stress (Pa)
Ω𝑅C 𝐿
𝑅𝑒c = (2)
𝜐 Fig. 6. Effect of shear stress on formation of hard
deposit at 275 oC after 80 hours
The angular velocity was calculated from
40
2π𝑁 C1
Wt. of soft deposit, mg

Ω = (3)
60 C2

The amount of hard deposit is initially found to 30

increase with rotational velocity (till 400 RPM) and
subsequently decreases. The consistency in the trend
obtained was confirmed using another Coupon (C2).
At a given bulk temperature, an increase in 20
RPM promotes increased mixing of the fluid
resulting in more foulant precursors or foulant being
transported from the bulk to the coupon surface by
advection / diffusion. However, the higher RPM will 10
also promote removal rate of deposit from the 0 1 2 3 4
vicinity of the coupon surface. This can be attributed Shear Stress (Pa)
to the increase in shear stress at the coupon surface
when new and later at the deposit fluid-interphase. Fig. 7. Effect of shear stress on formation of soft
As the RPM increases the corresponding shear stress deposit at 275 oC after 80 hours.
increase will reduce contact or residence time for
deposit adhesion to occur on the surface [1]. The Characterization of hard deposit
trends obtained in Fig. 6 can be due to the competing Hard deposits were collected after 80 hours
effects of transport and adhesion with the former from test runs carried out at 275 oC at 100 and 250
dominating over the shear stress at RPM below 400. RPM. These deposits were scraped from both
Such a trend where the fouling rate goes to a surfaces of a single coupon using a stainless-steel
maximum has been reported in earlier work [17], scalpel and cumulatively collected from 8 coupons.
[20]. The deposits were characterized using TGA, CHNS
The effect of RPM on soft deposit formed was and XRD. The TGA (Make: TA Instruments
also investigated and is shown in Fig. 7. Both (Waters), Model: Discovery SDT 650) was used to
coupons show similar trends from 250 RPM determine volatile, combustible and ash content in
(corresponding shear stress: 0.88 Pa) onwards. The the sample, the weight percentage of which is given
trend in soft deposit also exhibits a maxima at 400 in Table 2. At 275 oC, the deposit is inorganic in
RPM (corresponding shear stress: 1.95 Pa) due to nature with a high ash content (>75%).
the dominating effect of transport over shear. The The TGA results for hard deposits collected at
rate of decrease in amount of soft deposit beyond 300 oC and 250 RPM is shown in Table 3. The
400 RPM is relatively lower as compared to the rate organic material content is found to increase with

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 Heat Exchanger Fouling and Cleaning – 2022

temperature. The increase in volatile fraction is as compared to FeO. Similar spectra were obtained
relatively higher as compared to the increase in for hard deposit samples collected at other
combustible fraction. The organic content is likely temperatures and RPMs’.
to originate from the soft deposit.

Table 2 TGA result of hard deposit at fixed

temperature and varying RPM
Hard deposit composition
Components (wt. %)
275 oC, 275 oC,
100 RPM* 250 RPM
Volatiles 8.4 13.03
Combustibles 7.3 11.42 Fig. 8. XRD spectra of hard deposit at 275 oC and
Ash 84.3 75.55 250 RPM
*reproduced from [18]; shown for comparative purposes
Surface morphology of coupon surface
Table 3 TGA result of hard deposit at fixed RPM Fig. 9 shows the morphology of a coupon
and varying temperature surface with hard deposit at 275 oC and 100 RPM.
Hard deposit composition The micrograph indicates agglomeration of deposit
Components (wt. %) structures on the coupon.
250 RPM, 300 oC
Volatiles 25.45 275 oC
Combustibles 14.50
Ash 60.00

The sulfur content in the deposits was estimated

using a CHNSO analyzer (Make: Perkin Elmer,
U.S.A, Model: 2400 Series II). This analysis also
helped quantify the content of Carbon (C),
Hydrogen (H), and Nitrogen (N) in the deposits. The
results are tabulated in Table 4.
The results confirm a relatively high content of
sulfur in the deposit samples. The hydrogen to Fig. 9. SEM image of coupon surface with deposit
carbon (H/C) ratio was found to be 1.73 and 1.10 at at 275 oC and 100 RPM
100 and 250 RPM respectively. These H/C values
are indicative of the fact that the organic content in Elemental mapping of hard deposits on a
the deposit at the two temperatures investigated has coupon surface at 300 oC and 100 RPM is shown in
degraded less with time to form coke-like material. Fig. 10. The presence of sulfur at this temperature
The sulfur content at 300 oC at the two RPMs’ was was consistent with the XRD spectra obtained for
29.77 and 26.02 respectively. this element at the same temperature reported in
[16].
Table 4 CHNS analysis data for hard deposit
Composition Composition
(wt. %) (wt. %)
Elements (275 oC, 100 (275 oC, 250
RPM)* RPM)
C 7.84 10.53
H 1.13 0.97
N 0.01 0.07
S 32.34 32.97
*reproduced from [18]; shown for comparative purposes

The XRD spectra of a hard deposit sample at

275 oC and 250 RPM is shown in Fig. 8. The
analysis was carried out for 2θ values from 10 to 80° Fig. 10. Elemental mapping on coupon surface with
using an X-Ray Diffractometer (Model: Bruker D8 hard deposit at 300 oC, 100 RPM
Advance). The spectra show characteristic peaks of (Reproduced from [16])
iron sulphide and iron oxide. The peak intensities
confirm the deposit samples to mainly contain FeS

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 Heat Exchanger Fouling and Cleaning – 2022

Characterization of soft deposit deposit. Therefore, it is likely that iron naphthenate

Soft deposit collected at 275 oC and 250 RPM thermally decomposes into FeO.
was analyzed using a TGA and found to be largely FeO is however thermodynamically unstable and
organic in nature. The composition of volatiles and forms Fe2O3/Fe3O4 along with iron (Fe). The Fe then
combustibles was more than 95%. Past works have reacts with H2S to form FeS. The formation of the
reported this part of the deposit to contain trapped sulfide layer promotes further fouling with organic
crude oil [4]. Subsequently, a TGA analysis of fresh species in the soft deposit increasingly adhering to
and used crude oil was carried out. Fig. 11 shows the the FeS or iron oxide layers. The organic content in
thermal behavior of soft deposits collected along the hard deposit subsequently increases which then
with that of the crude samples taken before and after inhibits the formation of FeS and iron oxides.
the test run at 275 oC.
CONCLUSIONS
The feasibility and potential of a custom
designed coupon test rig has been experimentally
demonstrated to study fouling in refinery streams.
The test rig facilitates the use of coupon strips of
simple geometry instead of the normally adopted
tubular and annular surfaces, which greatly
enhances the ease of operation during
experimentation. The coupons represent differential
surface elements of fouling heat transfer surfaces at
constant temperature and near uniform shear stress
[19]. The test rig enables studies to be made of the
effect of varying bulk temperature on foulant
deposition and subsequent collection and
characterization of deposits using a consistent
Fig. 11. Thermal analysis of crude oil, soft deposit repeatable and reproducible analytical protocol.
and C7 asphaltenes at 275 oC, 250 RPM Both bulk temperature and RPM were found to
have an effect on the amount of foulant deposited on
The figure also includes the thermal history of C7 a coupon. The deposits formed were found to
asphaltenes extracted from fresh crude using ASTM strongly or loosely bound to a coupon surface and
D 6560. It is observed that the crude oil before and are classified as hard and soft deposits respectively.
after use loses appreciable weight (~96%) as the Studies conducted using a representative
temperature is ramped up from 30 to 475 oC. The refinery stream indicated FeS based corrosion to be
nature of crude changes to a small extent. No weight the primary cause of fouling at the temperature and
loss was observed in the soft deposit sample up to RPM levels investigated. The corrosion process is
160 oC. initiated via naphthenic acid attack on a metal
The weight loss in soft deposit is ~10.31% and surface leading to formation of oxides of iron and
~83.91% at temperatures up to 300 and 475 oC subsequently FeS. Organic species from soft deposit
respectively. This indicates the presence of heavier adhere to the FeS/iron oxide layer depending on
material in soft deposit which are potentially formed temperature and stream velocity. The increase in
via chemical reactions of precursors transported organic content in the hard deposit inhibits the
from the bulk or in the crude sample near the coupon corrosion rate. Thus, both hard and soft deposit
surface. The combustible component in soft deposit contribute to the fouling phenomena.
is also higher, i.e. ~8.5% as compared to ~2.5% in The rig can be used to study and understand
the crude. relative impact of operating conditions on fouling at
The characterization of hard deposits presented temperatures greater than 300 oC which is the scope
in the preceding sections leads to the conclusion that of future work that includes understanding the
fouling is corrosion-based at the temperatures and contribution of soft deposit to the fouling process
RPMs’ investigated. This conclusion is in agreement and estimate activation energies.
with fouling results reported in past studies [14],
[16], [17]. NOMENCLATURE

Proposed Mechanism of fouling 𝜏 shear stress, Pa

At temperatures greater than 220 oC, naphthenic Re Reynolds number
acid in crude oil leads to the formation of iron 𝜌 fluid density, kg/m3
naphthenate. The iron naphthenate can directly react 𝑢 linear velocity, m/s
with H2S to form FeS on the surface. This reaction Ω angular velocity, s-1
is however unlikely due to the presence of oxides of R𝑐 distance between the shaft and coupon surface,
iron being detected in the XRD spectra of hard 0.017 m

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 Heat Exchanger Fouling and Cleaning – 2022

L width of the coupon, 0.012 m temperature crude oil fouling, Heat Transf.
𝜐 kinematic viscosity of the fluid, m2/s Eng., vol. 30, no. 10–11, pp. 794–804, 2009.
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sulphide and coke fouling from sour oils:
Review and initial experiments, in Proc.
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c coupon surface Exchanger Fouling and Cleaning IX, pp.
23–30, 2011.
[12] Saleh, Z. S., Sheikholeslami, R., and
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