SPE 93056

Measurement of the Particle Deposition Profile in Deep-Bed Filtration During Produced

Water Re-injection
M.A.J. Ali and P.K. Currie, SPE, Delft U. of Technology, M.J. Salman, Kuwait Inst. for Scientific Research

Copyright 2005, Society of Petroleum Engineers Inc.

This paper was prepared for presentation at the 14th SPE Middle East Oil & Gas Show and
Conference held in Bahrain International Exhibition Centre, Bahrain, 1215 March 2005.
This paper was selected for presentation by an SPE Program Committee following review of
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presented, have not been reviewed by the Society of Petroleum Engineers and are subject to
correction by the author(s). The material, as presented, does not necessarily reflect any
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acknowledgment of where and by whom the paper was presented. Write Librarian, SPE, P.O.
Box 833836, Richardson, TX 75083-3836, U.S.A., fax 01-972-952-9435.

Abstract
An on-line linear X-ray apparatus has been used to
examine deep bed filtration during water injection in
Bentheimer sandstone core samples. Hematite particles
suspended in brine were injected at different flow rates and
concentrations to investigate the deposition profile. The X-ray
attenuation is strongly related to the density; and therefore the
amount of deposited material can quantitatively be estimated
at any time and distance along the core sample. Deep
penetration can be distinguished from external filtercake
buildup. Permeability decline as determined by the pressure
change and chemical analysis of hematite concentration were
used to confirm the X-ray analysis.

1. Introduction
Re-injection of produced water is of increasing
importance as watercuts continue to increase worldwide. It
provides an environmentally acceptable way of disposing of
the water, and contributes to pressure maintenance if injection
takes place into the reservoir itself. Injection can take place
under matrix injection or fracturing conditions. In both cases,
the performance of the injection well and the distribution of
the injected water are strongly influenced by the build up of
formation impairment around the wellbore or the fracture face.
Solid particles and small oil droplets in the injection water,
which are deposited in the formation by a process of filtration,
will cause this impairment.
As part of a study on filtration mechanisms, an online
single detector x-ray system was used to examine deep-bed
filtration during water injection in sandstone cores with
hematite particles suspended in the brine. The X-ray provides
a means of quantitatively measuring the deposition profile of
hematite as a function of time during the test.
This measurement of the deposition profile is not
normally available during such core tests, which usually

measure just the reduction in permeability. The measurement

offers a direct way of testing deep-bed filtration and filter-cake
build-up theories. Several models are available in the literature
for deep bed filtration. Most of these models are based mainly
on measurement of effluent concentration and only the final
deposition profile in the core, so the tests reported here
provide a more rigorous check of the models. The results of
the tests will be discussed, and the implications for the models
will be examined. Future work will be carried out to model the
filtration phenomena.
2. Literature Review: Deep-bed Filtration
Injectivity decline due to particles in the injection
water takes place to some degree in most injection wells. In
water injection projects, thousands of pore volumes typically
flow through the near well bore region where most particles
deposit. To understand and predict this decline requires the
knowledge of several parameters involving the water quality,
formation characteristics, and rate of deposition. The rate for
particle deposition is usually referred to as the filtration
coefficient. The filtration coefficient is a dynamic quantity
and changes with the number of previously deposited
particles. To determine the injectivity decline for an injection
well due to particles in the injected water (1-3), we need to:
Determine the concentration of deposited particles as
a function of time and distance from the well bore.
Determine the skin factor or (external filter cake)
distribution around the well bore.
Determine the injectivity decline with time, knowing
the skin factor and permeability change around the
well.
The permeability damage process can be divided into different
classes based on different mechanism of permeability
impairment (4). Many studies have shown that four processes
produce permeability damage: in-depth particle deposition by
surface deposition, pore-bridging, internal filter cake build-up,
and external filter cake build-up.
Pang & Sharma (5) demonstrated four types of
pressure build-up curve that characterise permeability
impairment. Type 1: straight-line pressure build-up observed
when incompressible external filter cake is formed or internal
cake is formed very close to the injection well. Type 2: curve
with increasing slope obtained in cases where a compressible
external filter cake or internal cake is formed. Type 3: curve
with decreasing slope obtained in cases where pore filling is
the dominant mechanism of particle capture or that particle

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SPE 93056

capture results in an increase in the interstitial velocity to the

point where no further deposition of particles can take place.
Type 4: curve with S shape observed when several mechanism
of deposition occurs simultaneously.
Several researchers have established different models
(6-8)
for deep bed filtration, with or without external cake build
up. The aim of the tests reported here is to test such models.
The advantage of conducting the tests in an X-ray apparatus is
that the internal deposition processes in the core can be studied
independently of the build-up of the external filter cake.
3. Core tests
All core samples used in these experiments were
plugged from a block of Bentheimer sandstone with an
average porosity 22% and permeability 1200md, grain density
2650 kg/m3, pore throat 10-30 m, pore size 100 m, and
grain diameter 100-300 m. Core diameter is 38 mm (1
inches) and length 72mm. The density of hematite is 5400
kg/m3, grain diameter 2 m, and porosity of the packed dry
material 27%.
Brine is prepared by adding 2% KCl to deionized
water. The brine is filtered using filter paper type 40M to
remove any undissolved salt particles. To add hematite, the
sample is put in a high shear mixer 3000RPM for 10 minutes,
and the hematite is added gradually until a completely
homogenous solution is achieved which usually takes another
5 minutes. A sample of the filtered brine containing hematite
is analyzed for suspended solids using the Coulter-Counter
and Wet-Chemistry analysis for dissolved iron.
The tests were conducted in an on-line linear X-ray
apparatus. This enables the hematite particle deposition in the
core to be measured in real-time, rather than just at the end of
the experiment. Al-Abduwani et al (9) have reported on a
similar experiment carried out in a CT-scanner. A
disadvantage of the apparatus we used is that it is only
possible to measure the total pressure drop over the whole
core. Multiple pressure tap core holders, as commonly used to
measure permeability impairment, cannot be accommodated.
Fully brine-saturated core samples are placed in the
X-ray apparatus in the special 300mm core holder and
38.1mm diameter Viton sleeve. The core holder has a window
for the X-ray beam. The X-ray source and detector move
automatically along the length of the coreholder during a scan.
All tests were performed at confining pressure of 2000 psi and
temperature 33oC. A high accuracy, dual-piston, diaphragm
pump was used to inject both brines (clean, and containing
hematite) into the core sample. A backpressure regulator was
not used and therefore the downstream pressure is atmospheric
(16.23psi).
Approximately 200 pore-volume of clean brine was
injected to give the baseline permeability. The hematite
solution is then injected. Four flow rates (15, 30, 60, and
90cc/min) and 3 concentrations of hematite (50, 100, and
200ppm) were used. The average pore volume was measured
to be 19cc, and 250 pore volumes were injected for each
sample. The effluent fluid coming out of the end of the core
was monitored. Hematite was not detected in the effluent in
any of the tests, so all hematite was deposited in the cores.

Once the test was over, chemical analysis was

performed to check on the final hematite deposition profile
and to compare this with the profile predicted from the X-ray
measurement. This analysis is a destructive method and
therefore all required information from the core must be taken
in advance. The procedure for chemical analysis is described
in Appendix A.
4. X-Ray Measurements
X-rays have been used over the past 50 years to
measure fluid saturation in core samples (10-11). When a beam
of x-ray passes through a material, that material becomes the
source of secondary x-rays and electrons and, because of these
secondary processes, a portion of the primary beam is
absorbed .
The X-ray apparatus (HRC-069) (12) is designed to
measure fluid saturations during multiphase core flooding
experiments. It contains an X-ray source and an X-ray
detector. The X-ray detector is an integrating, not a countingtype detector. It cannot be used to determine the spectrum of
incident X-rays without an elaborate test and calibration
procedure The detector comprises a wafer of CsI (Tl), 10 mm
x 10 mm x 2.5 mm thick, optically coupled to a 10 mm x 10
mm Si p-n photodiode. The stopping power (detection
efficiency) of the crystal is close to 100% over the entire range
of X-ray energies generated by the source.
Lambert's equation is recognized as the basis for Xray absorption (13-14). When a beam of monochromatic X-ray
goes through matter, the intensity drops exponentially with
distance if the material is homogenous. Lambert related the
intensity (E) of an X-ray beam that generates from an absorber
of known thickness (z, mm) and linear absorption coefficient
(, mm-1) to the incident beam intensity (Eo):
E = Eo exp[-(z)]

(1)

When several absorbers are placed in the beam, then the

intensity can be rewritten as:
E = Eoexp [-(1z1 + 2z2 + 3z3 + )]

(2)

where 1,2,3,..are different absorbers within the beam path. The

mass absorption coefficient (/) is a property of each
substance that is independent of the state of physical
aggregation (11). For a mixture of absorber materials, the
average mass absorption coefficient can be calculated if the
relative weight (Wi), density, and absorption coefficient of the
mixture, for each compound, in solution are known:
(/)average = W1(/)1 + W2(/)2 + .

(3)

Lambert's equation may be difficult to apply because of the

difficulties in measuring incident beam intensity (11). If the
incident intensity remains constant or corrected for minor
changes in flux and spacing between the tube, sample, and
detector, then Lambert's equation can be rewritten as:

www.petroman.ir

I = Ioexp [-(1z1 + 2z2 + 3z3 + )]

(4)

SPE 93056

Io is the X-ray beam intensity at reference conditions, (in our

experiments Io is the X-ray signal emerging from a brinesaturated sandstone core), while I is the intensity after a
change in the absorption characteristics or change in thickness
of absorber within the beam path, (in our case, I is the X-ray
signal emerging from the core with the accumulation of
hematite particles). The thickness variable z represents the
effective change in thickness of an absorber compared to its
thickness when Io was measured. Io takes into account photon
absorption by the coreholder, insulating material, rock matrix,
confining oil, rubber sleeve, and any other materials within the
beam path that are expected to retain consistent absorption
properties throughout the test.
To calibrate the X-ray signal, samples were prepared
with a known amount of hematite. Lambert's equation in the
form of Eq.4 will be used to measure the absorption
coefficient for each material or absorber (ex. rock material,
fluid in pores, and hematite). Once the absorption coefficient
for each compound is known, then the effective thickness (and
thus deposition density) of the tested material (hematite) can
be calculated. Details are given in Appendix A. As shown
there, the following correlation is an excellent fit to the data
obtained from these specially prepared samples, and is used to
calculate the amount of hematite deposited in the core flow
tests. The volume of hematite deposited at a given point in
the core, as a fraction of the dry rock volume, is predicted
using
= 0.169 ln(3.23/I).
(5)
5. Results of the core tests
This section presents the test results of hematite
deposition profile and permeability decline on 12 core
samples. Four flow rates of 15, 30, 60, and 90cc/min and 3
concentrations of hematite of 50, 100, and 200ppm were used.
5.1 Deposition profile from the X-ray measurement
Fig.1 shows the time-behaviour of the X-ray signal
for a typical test. Although there is some noise in the signal,
there is a clear trend with time as more and more hematite
particles are deposited. This demonstrates clearly that the
linear X-ray apparatus can provide valuable information about
the deposition profile. For clarity, the data has been smoothed
using modified exponential fit
I= Io /{1 + exp(a-bX)}

(6)

where the two parameters (a and b) change with time. Figs. 2 4 show the smoothed X-ray signals for selected tests. Figs. 5-7
show the final X-ray signals for all tests after injecting 250
pore-volumes (at the termination of the experiment).
These figures can be converted to the percentage of
hematite deposited per unit volume in the core, as a function
of time and distance along the core using the empirical
correlation given by Eq. (5). The final X-ray signal given in
Fig. 6 is converted in this way and shown in Fig. 8. Also
shown on Figs. 9 is the percentage of deposited hematite
determined from the chemical anlaysis after the testing weight
percentage, (each segment is approximetly 12mm, the first
segment was 8mm). The measured data was converted to

volume percentage to compare it with the X-ray data, (density

of hematite 5400kg/m3, and sandstone 2650 kg/m3). Fig. 10 is
a comparison between the measured hematite deposition from
chemical analysis and the estimated from X-ray data as a
fraction of the dry rock volume. It is seen that the chemical
analysis is in good agreement with the X-ray prediction for
deposition of hrmatite. The chemical analysis for the first
section of the core (which has more deposition) did not match
well with the X-ray analysis, which probably is due to loss of
hematite cake build up at core inlet during removing the core
from the core holder.
5.2 Permeability change
As noted above, in the X-ray apparatus it is only possible to
measure the total pressure loss across the core. It is therefore
impossible to locate the damage by looking at the varying
pressure profile along the core. Figs. 11-14 show the decline in
permeability as a function of the amount of hematite injected.
The inverse of the normalized permeability is plotted (initial
permeability/impaired permeability). For each flow rate, a
consistent curve is obtained, although there is some variation
at the lowest flow rate, as we discuss below. The rate at which
impairment occurs increases with increasing flow rate.
However, it is clear that the sensitivity of the permeability
impairment due to the concentration change is higher than that
due to flow rate change.
Table 2 lists the permeability damage after 250 porevolumes. Also indicated is the strength of the X-ray signal at
the entrance to the core at the end of the test, taken from Figs.
5-7.
6. Discussion of results
The type curves introduced by Pang & Sharma (5)
were discussed above in Section 2. Looking at Figs. 11-14 we
see that at the flow rate 15cc/min, a Type-3 curve was
obtained for all concentrations indicating pore filling is the
dominant mechanism of impairment. When the flow-rate
increased to 30cc/min, a Type-2 curve was obtained for the
lower concentration indicating compressible external filter
cake or internal cake build up. A Type-3 curve was obtained
for the higher concentration indicating continous pore filling.
Increasing the flow-rate to 60cc/min gave a Type-1 curve for
most samples. A straight line slope at early time then a
decreasing slope at later time indicating incompressible
external cake or pore-throat blocking. At flow rate of
90cc/min, a Type-4 curve, or combination of Type-1 and
Type-3 curves would best describe the impairment. External
cake build up for the 200 and 100-ppm concentration samples
was established earlier than that for the 50-ppm sample.
These conclusions are generally confirmed by the Xray signals for hematite deposition
50-ppm samples: Looking at Fig. 5, it is seen that the highest
build-up at the entrance to the core was for the 30cc/min
sample. A flow rate of 15cc/min was too slow to invade the
sample and therefore only external cake with minimum
invasion. Flow rates of 60, and 90cc/min were high enough to
penetrate the core sample, forming smaller external cake but
rather deeper.

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SPE 93056

100-ppm samples: Fig. 6 shows higher cake built for

30cc/min, and less external cake built for the 60 and 90cc/min
samples. The small invasion for the 15cc/min sample was not
expected. A flow-rate at 30cc/min was critical causing less
invasion but higher cake build up, yet permeability was not
affected as for the higher flow rates.
200-ppm samples: Fig. 7 shows higher external cake for lower
flow rate 15, 30cc/min, but less invasion deep in the samples.
A flow-rate of 60cc/min caused higher concentration and
deeper invasion than the 90cc/min sample, but less
permeability damage.
The availability of the X-ray results, which visualize
tha amount of deposition inside the core, thus enables us to
distinguish between the internal and external damage
processes. A strong relationship between the flow rate and the
nature of the impairment (external or internal filter cake) was
found. With higher flow rates, smaller external filter cakes
were built and deeper invasion occured. Eylander (15) made the
same observation. He used two types of sandstone cores,
Bentheimer and Brent with suspended latex particles in the
injected water. He found that with high flow rate, he obtained
a decreasing slope type indicating deeper particle invasion,
and at low flow rate, he obtained an increasing slope
indicating compressible external filter cake. Eylander
concluded that as depth invasion increases the injectivity
decline increases. Koorosh (16) observed that increasing the
flow-rate accelerates face plugging. Tran (17) and Bruin (18)
observed that an increase in flow rate leads to a more rapid
permeability decrease. They also concluded that an increase in
the particle concentration and size leade to rapid permeability
decline. Shirzadi (20) and Al-Abduwani et al (21) performed
similar experiments on Bentheimer cores and hematite
suspended in water and concluded that increasing the flow rate
and the solid concentration would increase the internal
permeability damage to the formation.
The sensitivity of formation damage due to particle
concentration is more than that for flow rate has also been
observed. Cruesbeck (22) made a similar observation that
agrees well with our analysis. He found that a critical velocity
or flow-rate exists, below which entrainment of fines does not
occur and above which the rate of entrainment increases
linearly with flow-rate.
Conclusion
An online X-ray apparatus was used to test deep bed filtration
during water injection on Bentheim sandstone core samples. In
addition to the X-ray signals, permeability measurements and
chemical analysis were performed. It has been found that at a
given flow rate, the total amount of hematite injected
determines the drop in permeability. However, the amount and
type of permeability damage is dependent on the rate of
injection. At low flow rates, external filtercake build-up and
damage close to the entrance of the core are the dominant
mechanisms. At higher flow rates, smaller external filter cakes
are built-up and deeper invasion occurs.
Further work will be carried on to investigate
dynamic filtration modeling and to assess the controlling
factors of depth of impairment since it forms an important
factor in the prediction of the injectivity decline rate.

Nomenclature
E
x-ray intensity
Eo incident beam intensity
I
emergent intensity
initial emergent intensity
Io
z
thickness of material, cm
h hematite porosity
rock porosity , %

absorption coefficient,cm-1

f
fluid absorption coefficient,cm-1
h hematite absorption coefficient,cm-1
r
rock absorption coefficient,cm-1
density kg/m3

References
1

10

11
12
13

K.E. Wennberg, M.M. Sharma: "Determination of the

filtration Coefficient and the Transition Time for Water
Injection Wells", SPE 38181, European Formation Damage
Conference, The Hague, The Netherlands, 2-3 June, 1997.
R.W. Paige & L.R. Murray: "Re-injection of produced water
Field experience and current understanding", SPE 28121,
August, 1994.
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Under Particle Cake Buildup and Particle Invasion". SPE
15073, April, 1986.
G. Chauveteau, L. Nabzar: "Physics and Modeling of
Permeability Damage Induced by Particle Deposition". SPE
39463, International Symposium on Formation Damage
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Decline in Water Injection Wells". SPE 28489, 69th Annual
Technical Conference & Exhibition, New Orleans, Louisiana,
25-28 September, 1994.
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Blocking Mechanisms on Formation Damage". SPE 16233,
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Marchesin, E. Rezende, A. Siqueira, A.L. Souza, F. Shecaira ,
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W.M.G.T. van den Broek, P.L.J. Zitha. Filtration of micronsized particles in granular media revealed by X-ray computer
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Company catalog description www.detectorportal.net
Silicon photodiodes and charges sensitive amplifiers for

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SPE 93056

16

17

18

19

20

21

3.3
3.25
3.2

X-ray Signal (kV)

15

scintillation Counting and High Energy Physics, Hamamatsu

Photonics K.K., Solid state Division, Catalog
#KOTH0002E02, June, 1993.
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February, 1987.
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by Fine Particle Movment- AWater Injection Problem". SPE
29006, International symbosium on Oil Field Chemistry, San
Antonio, Texas, 14-17 February, 1995
T.K. Tran: "Permeability decrease of sandstone as a result of
injection of oil-and-sand-containing water", MSc thesis from
Delft University of Technology, Jauary 1998.
J.N. Bruin: "Permeability decline caused by simultaneous
invasion of soild particles and oil droplets", MSc thesis from
from Delft University of Technology, October 1998.
A. Shirzadi, "Detailed investigation of formation damage due
to hematite suspension injection", MSc thesis from from Delft
University of Technology, August 2002
F.A.H. Al-Abduwani, Van den Broek, P.K. Currie: Visual
Observation of produced water Re-injection under laboratory
conditions", SPE 68977. European Formation Damage
Conference, Hague, the Netherlands, 21-22, May 2001
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Fine particles in porous media", SPE 8430, Annual Technical
Conference and Exhibition, Las Vegas, 23-26, September
1997.

3.15
12:19 PM
12:30 PM
12:40 PM
12:51 PM
1:12 PM
1:22 PM
1:33 PM
1:59 PM
2:10 PM

3.1
3.05
3
2.95
0

10

20

30

40

50

60

70

80

Core Length (mm)

Fig.1: Original X-ray signal for the 50ppm-90cc/min sample.

3.2

3.15

X-ray signal

14

12:09 PM
12:19 PM
12:30 PM
12:40 PM
12:51 PM
1:01 PM
1:12 PM
1:22 PM
1:33 PM
1:43 PM
1:59 PM
2:10 PM

3.1

3.05

2.95
0

10

20

30

40

50

60

70

Core Length mm

Fig.2 Smoothed X-ray signal for the 50ppm-90cc/min sample.

3.24

Table 1: X-ray signal at varying potential (kV) for

calibration samples with different saturation and
thickness of hematite
75Kv
3.82

65Kv
1.48

55Kv
0.39

50Kv
0.16

Saturated core

3.23

1.19

0.3

0.13

Dry concentric core

2.15

0.90

Saturated concentric core (not

filled)
Saturated concentric core
(filled)
Dry concentric core filled with
dry hematite
Saturated concentric core filled
with dry hematite
Dry core wrapped with 1mm
dry hematite foil
Saturated core wrapped with
1mm dty hematite foil
Empty sleeve with no core

1.89

0.76

4.49

1.21

0.49

0.93

0.34

0.09

0.04

0.60

0.22

0.06

0.02

0 min
8 min
17 min
26 min
35 min
44 min
52 min
61 min
70 min
79 min
88 min
97 min
105 min
114 min
121 min

3.20
3.18

xra signal kV

X-ray potential
Dry solid core

3.22

3.16
3.14
3.12
3.10
3.08
3.06
3.04
0

20

40

60

80

100

120

140

160

180

200

core length mm

Fig.3 Smoothed X-ray signal for the 100ppm-90cc/min sample

3.20
3.15
3.10

1.42

0.37

0.15

2.77

1.02

0.27

0.11

x-ray signal

3.69

0 min
6 min
12 min
18 min
24 min
30 min
36 min
42 min
48 min

3.05
3.00
2.95
2.90
2.85

2.68

2.80
2.75
0

10

20

30

40

50

60

70

80

90

core length mm

Table 2: Permeability damage after 250 pore-volumes.

(++), (+), (-), (--) indicate the strength of the X-ray signal at
the entrance to the core in descending order
15cc/min
30cc/min
60cc/min
90cc/min

50ppm
0.70
0.48
0.34
0.25

(+)
(++)
(--)
(-)

100ppm
0.38
(--)
0.32
(++)
0.10
(+)
0.05
(-)

Fig.4 Smoothed X-ray signal for the 200ppm-90cc/min sample.

200ppm
0.12 (+)
0.12 (++)
0.05 (--)
0.03 (-)

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SPE 93056

60
3.3

50
3.2

Hematite deposition Wt%

0.34
3.1

0.25

X-Ray kV

50-15-sw
50-30-sw
50-60-sw
50-90-sw

0.7

2.9

0.48

2.8
2.7

40

30
100/15/sw Chemical
100/30/sw chemical
100/60/sw chemical
100/90/sw chemical

20

10

2.6

0
0

2.5
0

10

20

30

40

50

60

Core Segment

70

Core Length (mm)

Fig.9 Chemical analysis for hematite deposition at 100ppm

Fig.5: X-ray signal after 250-pore volumes at various flow rates
and 50ppm concentration. Numbers refer to the sample
permeability reduction, given in Table 2

0.0350

0.0180

100-30-Sw Xray

100-15-Sw X-ray

0.0160

0.0300

100-30-Sw Chem

100-15-Sw Chem

0.0140

0.0250

0.0120
0.0200

0.0100
0.0080

0.0150

3.3

0.0060

0.38

0.0050

0.0020

0.05

3.1

0.0000

0.0000
0

0.1

3
X-Ray kV

0.0100

0.0040

3.2

20

40

60

80

20

40

60

80

Core Length (mm)

Core Length (mm)

2.9
100-15-sw
100-30-sw
100-60-sw
100-90-sw

2.8

2.7

0.32

0.0250

0.0160

10

20

30

40

50

60

0.0100

70

Core Length (mm)

0.0080

0.0100

0.0060

Fig.6: X-ray signal after 250-pore volumes at various flow rates

and 100ppm concentration. Numbers refer to the sample
permeability reduction, given in Table 2

100-90-Sw Chem

0.0150

0.0200

100-60-Sw Chem

0.0120
2.5

100-90-Sw Xray

100-60-Sw Xray

0.0140
2.6

0.0040
0.0050
0.0020
0.0000

0.0000
0
3.3

20

40

60

80

20

40

60

80

Core Length (mm)

Core Length (mm)

3.2

0.05

3.1

Fig.10 Comparison between the X-ray predicted

deposition and the chemical analysis at 100ppm

X-Ray kV

3
0.03

hematite

2.9

2.8
0.12

200-15-sw
200-30-sw
200-60-sw
200-90-sw

2.7
0.12

2.6

0.00

0.20
2.5
10

20

30

40

50

60

70

permeability impairment K/Ki

Core Length (mm)

Fig.7: X-ray signal after 250-pore volumes at various flow rates

and 200ppm concentration. Numbers refer to the sample
permeability reduction, given in Table 2.
0.030

0.40

0.60
50/15/sw
100/15/Sw
200/15/Sw

0.80

1.00

100-15-sw
100-30-sw
100-60-sw
100-90-sw

0.025

0.00
1.20

0.020

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

injected amount of hematite (gm)

Fig.11 Decline in inverse normalized permeability (15cc/min)

0.015

0.010

K/Ki
0.38 @ 15cc/min
0.32 @ 30cc/min
0.10 @ 60cc/min
0.05 @ 90cc/min

0.005

0.000
0

10

20

30

40

50

60

70

Core Length (mm)

Fig.8 X-ray predicted hematite (Vol.%) at 100ppm

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SPE 93056

8. Dry solid core with 1mm thick dry hematite foil wrapped all
around it
9. Saturated core with 1mm thick dry hematite foil wrapped all
around it

0.00

permeabilitry impairment K/Ki

0.20

0.40

0.60

0.80

50/30/Sw
100/30/Sw
200/30/sw

1.00

0.00
1.20

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

injected amount of hematite (gm)

Fig.12 Decline in inverse normalized permeability (30cc/min)

0.00

50/60/Sw
100/60/Sw
200/60/Sw

permeability impairment K/Ki

0.20

0.40

0.60

0.80

1.00

0.00
1.20

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

injected amount of hematite gm

Fig.13 Decline in inverse normalized permeability (60cc/min)

0.00

permeability impairment K/Ki

0.20

50/90/Sw
100/90/Sw
200/90/Sw

Samples were inserted in the coreholder and

pressured to 6900 kPa (1000psi). Tests were performed at
different input potentials 75, 65, 55 and 50kV. At higher
potentials, the X-ray attenuation in some samples was too low,
and the attenuated signal exceeded the limit of the detector.
The entries for these tests are shown empty in Table 1.
We note first from Table 1 that for any two samples
the ratio of their respective X-ray signal is approximately the
same for all values of the potential. This confirms that the
linear absorption coefficients ()in Eq.(4) are constant,
independent of the incident potential. This means that we can
calculate the absorption coefficients at one potential, and use
them at the higher potential of 75kVat which we perform the
core tests.
We assume in all cases that the X-ray signal passes
through the thickest part of the samples, along the diameter.
For most samples a reasonably constant X-ray signal was
found. For the sample with 1mm thickness of hematite foil,
some non-uniformity was observed, presumably due to small
variation in hematite thickness. Average values have been
taken in this case.
According to Eq. (4), the X-ray signal for a
calibration sample will be given by :
I = Ioexp [-(rzr + fzf + hzh)]

0.40

(A1)

0.60

0.80

1.00

0.00
1.20

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

injected amount of hematite (gm)

Fig. 14 Decline in inverse normalized permeability (90cc/min)

Appendix A. Calibration of the X-ray signal

To calibrate the X-ray signal, samples were prepared
with a known amount of hematite. The sample preparation is
critical. The adsorption coefficient is very sensitive to sample
thickness and fluid saturation, and therefore precise
measurements of total thickness and saturation are necessary.
The calibration measurements are listed in Table 1. All 9
samples had a diameter of 38mm and were plugged from the
block of Bentheimer sandstone described in Section 3. Some
were tested dry, others saturated with 2% KCl brine. The 9
samples were as follows:
1. Dry solid core
2. Saturated solid core
3. Dry concentric core: a core with a centred concentric hole
of 21mm diameter
4. Saturated concentric core (not filled): inside empty of brine
5. Saturated concentric core (filled): inside filled with brine
6. Dry concentric core filled with dry hematite
7. Saturated concentric core filled with dry hematite

where Io is the same for all samples but varies with the input
potential, r , f , h are the absorption coefficients of the rock,
fluid (brine) and hematite, and zr , zf , zh are the effective
thicknesses of rock, fluid and hematitie in the sample. We take
these effective thicknesses to be the centerline thicknesses,
along the diameter lying in the path of the X-ray.
The difference in signal between the dry solid sample
and the empty sleeve is caused just by the extra dry rock in the
solid sample, for which the extra zr = 38(1-) mm. Hence from
the measurements at 50kV in Table 1 and (A1), it follows that
r is given by
(1-r) r = ln(2.68/0.160)/38= 0.074

(A2)

The difference in signal between the saturated solid

sample and the sleeve is caused by the saturated rock in the
solid sample, for which the extra zr = 38(1-r) mm and the
extra zf = 38r mm. From the measurements at 50kV in Table
1 and (A1) it follows that
(1-r)r+rf = ln(2.684/0.127)/38 = 0.081 mm-1 (A3)
The difference in signal between the saturated sample and the
dry sample is caused by the fluid in the center for which zf =
21 mm.

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f = ln(.160/0.127)/38 = 0.021 mm-1

(A4)

SPE 93056

12.0%
100-15-Sw X-ray
100-30-Sw Xray
100-60-Sw Xray
100-90-Sw Xray

10.0%

Change in Porosity

Note again that taking the values for 55kV potential will give
the same result, since the ratios of the signals are the same.
The values given by (A2)-(A4) are consistent only if the
porosity r has the value 22%, exactly that measured
independently by standard methods. This remarkably accurate
agreement, gives confidence in the X-ray measurements.
In principle the measurements of dry and saturated
hematite samples can also be used to give estimates for the
absorption coefficients for the rock and fluid. However these
signals are less suitable, because of the lower intensity in the
case of the 21mm sample or the uncertainty in the repeatability
of thickness of the 1mm sample. These measurements are
therefore used only to estimate the hematite absorption
coefficient. From the measurements at 50kV of the dry core
and the dry concentric core filled with hematatite with zh =
(38-21)(1-h) mm, we find from (A1) that

8.0%

6.0%

4.0%

2.0%

0.0%
0

10

20

30

40

50

60

70

80

Core Length (mm)

Fig.1A Change in porosity for the 100ppm samples

9.0%
8.0%

3.0%
2.0%
1.0%

200-15-Sw Xray

200-60-Sw Xray

100-30-Sw Xray

200-30-Sw Xray

50-15-sw (X-ray)

100-60-Sw Xray

100-90-Sw Xray

0.0%
200-90-Sw Xray

(A6)

4.0%

50-30-sw (Xray)

h = 0.22, f = 0.021, r = 0.0956 mm-1

5.0%

50-60-Sw (Xray)

A similar calculation using the saturated signal values gives

(1-h)h = 0.159, which is reasonably consistent. We take the
average value 0.162 Then, from (A3) (A4), taking h = 27%,
as measured, we find values for the absorption coefficients

6.0%

50-90-Sw (Xray)

(A5)

100-15-Sw X-ray

(1-h)h=[ln(2.684/0.0121)-r(17)(1-r)]/21=0.164mm

Change in porosity

7.0%

-1

Fig.2A Average change in porosity at 10mm calculated from

We can now check the consistency of these results with the

measurements found using the 1mm layer of hematite. The
agreement is not good. This is thought to be because the
measured X-ray signals are very sensitive to small changes in
the thickness layer, and this is difficult to control accurately.
Knowing the values for the absorption coefficients, it
is now possible to quantify the deposition of hematite inside
the cores during the flow tests. Let be the amount of
hematite deposited at a given cross-section along the core,
expressed as a fraction of the dry rock volume. Compared with
a fully saturated core, the hematite deposition gives an
increase in zh = 38(1-) mm (the core diameter is 38mm),
and an equal decrease in zf. From material balance, the volume
of particles filling the pores is equal to the volume of fluid loss
so that zh = zf at maximum deposition. The boundry conditions
for is zero for no deposition and r/(1-r) for complete
blocking on pores, (0.282 0). At the potential 75kV used
for the core tests, the X-ray signal of the saturated core is 3.23
(see Table1). Thus, from (A1), if I is the X-ray signal,
=ln(3.23/I)/[ D(1-r)(h-f )]= 0.169 ln(3.23/I). (A7)
The change in porosity can also be estimated if the values of
are known at different X-ray signals.
(1 r )
(A8)
=

Fig.1A illustrate the change of porosity from A8. Note again

that a crtitical flow rate exists at which higher deposition
occurs. Fig.2A illustrates the change in porosity for the first
10mm sections of the cores.

Appendix B. Procedure for chemical analysis

The core samples were slabbed into two halves along
the entire length of the core samples. One-half was used for
chemical analysis while the other half was kept for later
analysis. Each half-slabbed core was cut into six segments to
approximately 12mm thickness. The core segments were
crushed to increase the exposure to chemical reaction, and the
weight of each segment was taken. Each core segment was
placed in a flask and 40ml of 37.7% hydrochloric acid (HCl)
was added. Each flask was covered with foil to facilitate the
condensation of any escaping vapor. The mixture was placed
on heated sonic bath at 65oC for 1 hour. The flask was allowed
to cool down to room temperature and the solution was
separated using filter paper size 0.4micron. Only the acid was
drained carefully into a 100ml graduate cylinder while keeping
the sand in the flask. A 30ml of de-ionized water was added to
the remaining sand and kept in sonic bath for 30 minutes at
65oC to remove any residual acid in the sample. The mixture
was filtrated and the solution was added to the 100ml
graduate. Cylinder. The remaining sand in the flask was
washed with another 30ml of de-ionized water and filtered to
make a 100ml of acidic solution (40ml acid and 60ml deionized water). The solution is used for iron concentration
using the ICP test analysis and the weight of the sand is
measured to quantify the amount of dissolved solids.
The background amount of iron present in native
Bentheimer sandstone must be determined in advanced. Tests
showed 3% dissolved iron. Subtracting the background
amount from the measured concentration yields the actual
concentration of deposited hematite. Since the ICP gives the

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SPE 93056

total Fe concentration in the sample, this measured value must

be converted to Fe2O3 by multiplying by molecular weight
ratio of 2.8958, [(2Fe+3O)/(2Fe)]. Finally, the percentage of
hematite per volume of dry rock in each segment was taken by
dividing the measured concentration of hematite by ICP from
each segment by the original weight of each segment before
dissolving in acid.
We note that the total amount of hematite in the core,
which would give a check on how much has entered the core
during the test and how much was deposited in the external
filter cake, cannot be estimated because large amount was lost
during slabbing and cutting the core samples to small
segments.

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