SPE 80372
Real-time and In-Situ Detection of Calcium Carbonate Scale in a West Texas Oilfield
J.K. Smith; M. Yuan, SPE; T.H. Lopez, SPE; Mitch Means; and John L. Przybylinski; Baker Petrolite
Copyright 2003, Society of Petroleum Engineers Inc.
th
This paper was prepared for presentation at the SPE 5 International Oilfield Scale
Symposium held in Aberdeen, Scotland, U.K., 29-30 January 2003.
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Abstract
A novel technique has been developed to detect the onset and
increase of calcium carbonate scale deposition from oilfield
production fluids. This method utilizes an attenuated total
reflectance (ATR) probe, called the scale sensor, to detect
scale formation in-situ. Because this method is based on
existing technology and requires little supporting equipment, a
simple cost-effective monitoring device could be placed in
many locations within a production system. This method could
provide a system wide, in-situ, real-time response to calcium
carbonate scale formation at its earliest stages.
As a first step towards evaluating the effectiveness of
this new technology, the scale sensor was field tested at a west
Texas oilfield. The scale sensor was observed to detect the
deposition of calcium carbonate under static and flowing
conditions in actual produced fluids. In the static tests, crude
oil, suspended solids and other endogenous materials did not
affect the scale sensor response. Under flowing conditions,
like those found in the production flow lines at the west Texas
oilfield, scale sensor response was observed to correlate to the
chemical injection rate of both the scale inhibitor and
dispersant. Based on the results from the scale sensor, the
scale inhibitor injection point will be moved to the wellhead
shortly.
Introduction
Calcium carbonate scale commonly occurs in multiple
locations within a production system. These locations include,
but are not limited to, production wells, injection wells,
flowlines, valves, vessels, separators, and pumps. Scale may
form as a result of commingling, depressurization, or heating
of the produced fluids contained therein. The result of scale
deposition in oil and gas production systems is increased costs
due to equipment failures, manpower-related maintenance of
scaled equipment, and lost production. Application of a
reliable real-time and in-situ sensor that could detect the onset
and rate of calcium carbonate scale deposition could greatly
reduce equipment failures by informing operators of an
imminent scale problem. Corrective actions prompted by such
an early warning would prevent excessive scale build-up on
production equipment, thus reducing the rate of scale related
failure rates.
At present, scaling tendency and scale occurrence in
oilfield produced fluids are typically assessed by relying on
analysis of produced water samples and/or using an in-situ
scale coupon. Laboratory determinations of real-time scale
deposition were recently reported using a rotating disk
electrode (RDE) technique1, tapered optical fibers,2-4 and a
“near real-time” sensor.5 Recent literature regarding the on-
line real-time detection of oilfield scale in actual production
systems has included pulse neutron measurements, 6 gamma
ray attenuation, 7 ultrasonic, 8 nuclear attenuation, 9 and a dual-
energy-venturi multiphase flow measurement.10
Attenuated total reflection (ATR) spectroscopy is a
direct measurement surface analysis technique well suited for
oilfield use. This technique is ideally suited for obtaining
spectroscopic information in direct contact with samples,
which are either too thick or opaque for transmission
spectroscopy. ATR is an energy-loss mechanism wherein
incident light energy strikes the crystal-sample interface at
such an angle that total internal reflection occurs. While a
great proportion of the energy is reflected back into the
crystal, a small portion of the energy is transferred from
crystal surface to the sample medium.11 Because this
technique requires that the measurement surface referred to as
the crystal surface is in contact with the sample, this technique
is also ideally suited for process type environments such as
those found in oilfield production tubulars. Unlike the other
aforementioned methods, ATR devices require very little
supporting equipment. For example, the scale sensor used for
this study was powered by a 5V-power supply.
Preliminary laboratory investigations with the scale
sensor response as a function of the calcium carbonate scaling
tendency in a series of stirred beaker tests revealed that this
technique is suitable for field use.12 In that study, synthetic
brine was prepared based on the water analysis from the west
Texas oilfield. The brine constituents were separated into the
anion water (brine containing all scaling anions) and the cation
water (brine containing all the scaling cations). Sodium
chloride was evenly distributed in each brine portion to effect
efficient mixing. Tests were initiated by combining the anion
water with the cation water. In cases where crude oil was also
added, it was added last. In each test, the bicarbonate
concentration in the anion water was changed to effect a
change in the scaling tendency, referred to here as the
2 SPE 80372
saturation index (SI), and probe response was monitored.
Experiments conducted in the presence and absence of crude
oil gave similar results. In both experiments, scale sensor
response was observed to track the SI of the solution.
In another stirred beaker test conducted during the
course of this previous study, the effects of scale inhibitor on
scale sensor response were monitored. The results from these
tests suggest that the scale sensor response is inversely related
to the concentration of scale inhibitor present in the combined
brine-crude oil mixture. Based on these results a field trial
was initiated in west Texas.
Currently, the produced fluid at the oilfield in west
Texas is being treated with a phosphate ester scale inhibitor
which is injected at the production headers at the tank batteries
and battery extensions. This field has been on an alternating
water and CO2 gas (WAG) injection for a decade. This
current treatment regiment had been effective at controlling
scale deposition in the production system for nine years.
Approximately a year ago, increases in scale deposition,
predominantly calcium carbonate, were observed on valves at
the outlets of the water injection stations. Since then, scale
occurrence on the injection well screens and in the flow
meters has increased in frequency.
Prior to the field test, water analyses from the past
decade were examined to identify the cause in the recent
increase in calcium carbonate deposition. Scale modeling was
performed with all water analyses contain herein using
Scalesoft Pitzer 3.0.13 The modeled results are expressed as SI,
which is defined as the logarithm of the ratio of the scaling ion
concentration product over their solubility product. The sign
and magnitude of the SI is an indication of the thermodynamic
driving force for scaling ions to precipitate out of solution.
When the SI<0, the scaling ions are undersaturated at the
experimental conditions. If the SI=0, the scaling ions are at
equilibrium at the experimental conditions. Precipitation of
scale is predicted when the SI>0, indicating that the scale ions
are oversaturated at the experimental conditions. It should be
noted that the calculation of the SI does not take into account
the kinetic forces for scale precipitation.
Before the initiation of the WAG program,
bicarbonate concentrations were approximately 317 ppm,
analyzed on September 30, 1992, and the most recent water
analysis, October 30, 2002, showed the bicarbonate ion
concentration to be 2957 ppm, while the calcium
concentration increased from 1800 ppm to 4806 ppm (Table
1). Based on the water analyses from these two dates, the
calculated SI was determined to be 1.36 and 2.38 respectively,
at 43oC and 12 psig. Since the inception of the WAG
program, the calcium carbonate scaling potential had
increased by approximately 10.5 times. Over the same time
period, oil cut had remained roughly constant at 0.5% in the
produced water going into the settling tanks for re-injection.
Common to this west Texas oilfield was the rapid
depressurization of the produced fluids from the wellhead to
the collection tanks. Table 2 lists each pressure change and
the associate change in the SI of the produced fluid at each
point. This table clearly indicates that the scaling potential for
calcium carbonate deposition increases approximately 126
times from wellhead to the water collection tank. The row
titled header represents the point in the system where scale
inhibitor and dispersant are injected, where the SI is calculated
to be 6.6 times greater than at the wellhead.
Identified within this field was a produced water
collection station, which was fed by two production batteries
that were physically isolated from the rest of the field. The
isolation of the produced fluids within these batteries from the
rest of the field provided a unique opportunity to precisely
control the scale inhibitor injection rate and thus the inhibitor
concentration in the produced water at the water collection
station.
Experimental
Side stream. A side-stream flow loop running from the inlet
line of the water station to the overflow tank was constructed
to house the testing apparatus for the scale sensor. There was
concern that placement of the scale sensor directly in the inlet
line to produced water collection station would not yield
adequate information pertaining to the effectiveness of this
device to detect scale because of the high fluid velocity
environment, 3.65 m/s. It was ascertained that the shear
velocity of the fluid would preclude any definitive results
involving the scale sensor, as in the field no scale deposition
was evident at high velocity locations. Therefore, use of the
side stream would reduce the fluid velocity to approximately
0.3 m/s, which is low enough to allow scale to adhere to the
probe surface. Additionally, the lower flowrate would more
closely mimic the conditions in the produced water collection
tanks where measurable amounts of scale are formed then
transferred to equipment downstream. The side stream flow
loop was also ideal for installing an assembly of monitoring
devices, namely two scale sensor probes, a scale coupon, an
absolute pressure transducer, an online flow meter, a
thermocouple for measuring fluid temperature, and two water
sampling ports (Image 1 and in schematic form in Figure 1).
These additional monitored parameters were observed to
monitor any changes in the system condition and provide
supporting evidence on whether scale was occurring in the
flow line.
Chemical injection at the side stream. Two production
batteries, A and B, fed the produced water collection station
chosen for this study. Two scale inhibitor injection pumps
were located at battery A. Four scale inhibitor and two
dispersant injection pumps were located at battery B. For the
experiments contained herein, scale inhibitor and dispersant
concentrations were calculated based on the chemical pump
rate and total daily production of the two production batteries.
Changes instituted at each chemical pump during the course of
this study were followed by a four-hour equilibration period
prior to the initiation of the next experiment. Each experiment
was conducted for duration of approximately 18 hours.
Scale Sensor. Each ATR probe used for this study consists of
a crystalline end, which is housed, in a protective stainless
steel collar. Perforations in the collar provide effective fluid
contact with the crystal surface (Image 2). The crystal design
is trapezoidal in shape (Image 3). A light emitting diode
provided the narrow band light source. An integrated
source/detector card (Image 2) converted the reflected light
intensity to a millivolt output signal as log Io/I. Hence, energy
SPE 80372
losses are observed as apparent increases in reflected energy.
It was the authors’ opinion that the scale sensor response
should be proportional to scale thickness on the crystal
surface. The millivolt output of the source/detector card was
collected by remote data logging devices. All data collected
by these data loggers was transferred daily to computer for
analysis.
Static tests with the scale sensor. In addition to the scale
probe experiments that were carried out in the side stream
flow loop. Scale detection tests in static produced fluid were
also conducted in the field. Produced fluid was obtained
upstream of the scale inhibitor and dispersant chemical
injection points. For each test, approximately 3.78 L of
produced fluid was collected and chilled on ice until used.
The collected produced fluid was processed prior to each
experiment by either triple filtering it through cotton,
acidifying it with a 2% (vol/vol) addition of 15% HCl, or
adding phosphonate scale inhibitor. After processing, the
produced fluid was placed in a reservoir and allowed to warm
to room temperature (~30◦ C). Each test was initiated by
submerging the probe in the processed produced fluid and data
was collected for an 18-hour period. A computer collected
scale sensor data for these tests via an A/D card.
Results
Static tests. Under laboratory conditions, scale sensor
response was observed to be only affected by the deposition of
calcium carbonate scale on the crystal surface. It was unclear
whether any endogenous materials (such as crude oil,
suspended particulates or any organic materials) present in the
west Texas oilfield would affect the scale sensor response.
Therefore, a series of static tests were devised where, under
controlled conditions, scale sensor response could be
compared to several different produced fluid samples which
had been
1. Filtered and acidified: To remove any suspended solids,
oil, and calcium carbonate scale.
2. Not filtered, but acidified: To remove any calcium
carbonate scale allowing the evaluation of the scale sensor
response in the presence of suspended solids and oil.
3. Not Filtered, Not acidified: The “as is” brine where scale
sensor response was evaluated in the presence of
suspended solids, oil, and calcium carbonate. The
calculated SI for this solution was determined to be 2.46.
4. Filtered, not acidified and spiked with 300 ppm of a scale
inhibitor: To remove suspended solids, oil, and calcium
carbonate scale. This test was designed to determine if
any acid soluble suspended solids were affecting the scale
sensor response.
Examination of the data listed in Table 3 and Figure 2 reveals
several interesting points. First, scale sensor response does
not appear to be affected by the crude oil. Second, probe
response is only affected by acid soluble suspended solids that
are present in the aqueous phase in the non-acidified
experiments. The calcium carbonate scale that is affecting
probe response in this non-acidified and non-filtered
experiment is diminished in the presence of scale inhibitor.
3
Therefore, it was concluded that the scale sensor is responding
primarily to scale deposition and not to some unknown
material present in the produced fluids at this west Texas
oilfield. Furthermore, solution pH was determined not to
affect probe response.
Side stream tests. To confirm the conclusions from the static
tests, similar tests were performed under flowing condition in
the side stream. Probe responses in the absence of scale,
called the control test, was measured while by pumping 15%
HCl solution into the injection point at the head of the side
stream (Figure 1), where the fluid pH was depressed to
approximately 1.0, way below the calcium carbonate scale-
forming pH range. For the blank test, both the scale inhibitor
and dispersant injection were turned off to provide the
maximum amount of scale deposition on the probe surface.
Comparison of the data presented in Figure 3 along
with the cumulative ∆mV from the control and blank
experiments of 6.9 mV (control, no scaling) and 98.1 mV
(severe scaling blank) corroborates the earlier conclusions
from the static tests. The scaled probes from the blank test are
presented in Image 4. More supporting evidence is provided
by analysis of the coupon data, in which 136.4 mg and 0.5 mg
of scale had deposited on the coupon present during the blank
and control tests, respectively. Inductively coupled plasma
(ICP) analysis of the dissolved cations contained in the acid
washes from the coupons placed in the side stream flow loop
during the blank and control tests were determined to be
comprised of 96.5% and 12.8% calcium, respectively. ICP
analysis of the probe washes from these tests also identifies
calcium as the primary cation deposited. The probe washings
were determined to contain 91.5% and 79.1% calcium from
the blank and control tests, respectively.
Comparisons between scale sensor response and
scale inhibitor effectiveness were accomplished by monitoring
scale sensor response while changing the scale inhibitor
concentration. The data presented in Figure 4 shows a
relationship between scale sensor response and scale inhibitor
concentration. The cumulative ∆mV for each experiment
listed in Figure 4 is tabulated in Table 4 and compared to the
scale coupon data. Comparison of the scale inhibitor
concentrations with scale sensor response reveals a trend.
Clear differentiations can be made between the blank, 15 ppm
of scale inhibitor, and the remaining scale inhibitor
concentrations. When the scale inhibitor concentration was
set to 15 ppm, the current treatment rate, a moderate response
(20.9 mV) was still observed from the scale sensor. Whilst
this response was meager compared to the blank (98.1 mV),
the deposition rate in this test is based on a total of 18,511 L of
produced fluid passing by the scale sensor. If this value is
compared to the total water production rate of this water
station, 378,541 L/day, calcium carbonate deposition could
still be a problem over time, as evidenced in the field.
Examination of the scale sensor response when the
scale inhibitor concentration is changed from 7.5 ppm, 3.75
ppm and 1.88 ppm reveals a non-linearity in scale sensor
response. This non-linearity could be caused by the resolution
of the scale sensor or scale sensor response could be affected
by the daily system fluctuations inherent in this west Texas
oilfield. These fluctuations could include, but are not limited
4 SPE 80372
to amount of dissolved CO2, concentration of dissolved solids,
total number of wells producing, or the operational integrity of
the production equipment. The ∆mV between the lowest scale
sensor response, 3.75 ppm, and the highest 7.5 ppm, was
determined to be 23.5 mV.
Dispersant injection in produced fluids at this west
Texas oilfield was employed to reduce the presence of
suspended solids. From careful analysis of Millipore data
over the past year, clear correlations between dispersant rates
and suspended solids amounts present in the produced fluids
was apparent. The effectiveness of the dispersant to alleviate
scale deposition was tested with the scale sensor. Although
the dispersant was believed to be reducing the agglomeration
and adhesion of suspended solids by dispersion mechanism, it
was not clear how significantly scale deposition rates were
also affected by the presence of dispersant. Comparing scale
sensor response from tests with varying concentrations of
dispersant and scale inhibitor, reveal that the dispersant is
significantly contributing to scale deposition abatement
(Figure 5 and in tabulated form in Table 5). The first set of
comparisons can be made between those tests where the scale
inhibitor/dispersant concentrations were: 15 ppm/0 ppm, 15
ppm/6.7 ppm, and 0 ppm/6.7 ppm. These tests compare the
extremes between treatment regimens at this west Texas
oilfield, dispersant only, scale inhibitor only, and scale
inhibitor/dispersant (the current treatment program). In these
tests, scale inhibitor/dispersant concentrations of 15 ppm/0
ppm, 15 ppm/6.7 ppm, and 0 ppm/6.7 ppm showed minimal
response. Interestingly when compared to the blank, those
from the 15 ppm/0 ppm, 15 ppm/6.7 ppm, and 0 ppm/6.7 ppm
tests suggest noticeable control of scale deposition with only
dispersant treatment or scale inhibitor. Differences in the
scale sensor response when the scale inhibitor/dispersant
concentrations were 3.75 ppm/6.7 ppm and 3.75 ppm/0 ppm
showed noticeable changes between these tests. Essentially, a
∆mV of 24.0 mV was observed between the scale sensor
responses between those tests where the scale inhibitor
concentration was 3.75 ppm and the dispersant concentrations
were 0 ppm and 6.7 ppm. The results from tests where the
scale inhibitor/dispersant concentrations were 3.75 ppm/6.7
ppm and 3.75 ppm/0 ppm corroborates the previous
conclusions that the addition of dispersant does alleviate scale
deposition.
Conclusions
The data presented herein suggests that the ATR scale sensor
is a device that is capable of detecting calcium carbonate in
mixed production fluid systems. These results suggest that the
scale sensor is not affected by crude oil, suspended solids,
solution pH, or any other unidentified materials present in the
production fluids at this west Texas oilfield. During this test,
the scale sensor provided valuable information on the real-
time effectiveness of the scale inhibition program. Based on
this information, a new product was formulated and it will be
injected at the wellhead. The results of these changes will be
presented in forthcoming articles.
Acknowledgements
The authors would like to thank Baker Petrolite for permission
to publish the data included in this paper. In particular, James
Ripley of Baker Petrolite was acknowledged for his valuable
assistance with the field test of the scale sensor.
References
1. Morizot, A.P. and Neville, A.: “A Novel Approach for
Monitoring of CaCO3 and BaSO4 Scale Formation,” paper
SPE 60189 presented at the SPE Second International
Symposium on Oilfield Scale, Aberdeen, UK., 26-27
January.
2. Moar, P.N. et al.: “Fabrication, modeling, and direct
evanescent measurement of tapered optical fiber sensors,”
Journal of Applied Physics (April 1999) 3395.
3. Love, J.D. et al., IEE Proc. (1999) 343.
4. Black, R.J. et al., Applied Physics Letters (1991) 355.
5. Emmons, D.H. et al.: “On-Site, Near-Real-Time
Monitoring of Scale Deposition,” paper SPE 59776
presented at the 1999 SPE Annual Technical Conference
and Exhibition, Houston, 3-6 October.
6. Wyatt, D.F., Jr. et al.: “Use of Supplemental Curves from
Pulsed Spectral Gamma Logs to Enhance Log
Interpretation,” paper SPE 28410 presented at the 69th
Annual Technical Conference and Exhibition, New
Orleans. Louisiana, 25-28 September.
7. Bamforth, S. et al.: “Revitalizing Production Logging,”
Oilfield Review 8, no. 4 (Winter 1996): 44-60.
8. Gunarathne, G.P.P. and Keatch, R.W.: “Novel
Techniques for Monitoring and Enhancing Dissolution of
Mineral Deposits in Petroleum Pipelines,” paper SPE
30418 presented at the Offshore Europe Conference,
Aberdeen, Scotland, 5-8 September.
9. “Nuclear Technique Grabs Gold Metal,” article in NST
Quarterly (July 1999), on-line report at
http:\\www.mint.gov.my/PAPERS/DEFAULT.HTML
10. Theuveny, B. et al.: “Detection and Identification of
Scales Using Dual Energy/Venturi Subsea or Topside
Multiphase flow Meters,” paper OTC 13152 presented at
the 2001 Offshore Technology Conference, Houston,
Texas, 30 April-3 May.
11. Urban, M.W.: Attentuated Total Reflectance
Spectroscopy of Polymers, American Chemical Society,
Washington, D.C. (1996).
12. Smith, J.K. et al.: “Real-Time and In-Situ Detection of
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80248 presented at the 2003 SPE International
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7.
13. Tomson, M.: Scalesoft Pitzer ver3.0, Rice University,
Houston, TX. (2000).
SPE 80372 5

Ion Water Analysis from Water Analysis from

September 30, 1992 October 30, 2002
Cl 18500 41000
HCO3 317 2957
SO4 450 289
*
Na 9793 20000
Mg 243 941
Ca 1800 4806
pH 6.5 6.1
SI 1.36 2.38
Figure 1. Side stream schematic.
Table 1. Comparison between water analyses from present
and a decade ago at the west Texas oilfield. * Sodium
calculated by difference.

Location Temperature Pressure SI

o
( C) (psig)
High Pressure 43 300 1.38
Production Well
Low Pressure 43 100 1.84
Production Well
Header 43 42 2.2
Transfer Line from 43 32 2.31
Batteries to Water
Station
Inlet to Water 43 12 2.71
Station
Collection Tank 43 1 3.48

Table 2. Positions in the isolated portion of the west Texas Image 2. Scale sensor (left) and source/detector card (right).
oilfield where the scale sensor field trial was conducted where
changes in the system conditions increase the SI.

Image 3. Scale sensor crystal surface. The left probe is the 1”

crystal and the right probe is the ¾” crystal.
Image 1. Side stream apparatus at the west Texas oil field.
6 SPE 80372

100
Not Filtered/Not Acidified (1) Filtered/Acidified (4)
Blank (1) 1
Crude (2) Spiked with 300 ppm of Scale Inhibitor (5)
Not Filtered, but Acidified (3) Control (2)
100
80
1

Scale Sensor Response (∆mV)

80
60
∆mV)

60
40
Scale Sensor Response (

40
2 20

3 2
20
4 0

0 5 0 5 10 15

Time (hr)
0 5 10 15
Time (hr)

Figure 2. Scale sensor response in produced fluids under Figure 3. Scale sensor response under flowing conditions
static conditions. comparing the blank and control experiments.

Experiment Scale
Sensor
Response
( ∆mV)
Filtered and Acidified 14.7
Not Filtered, but acidified 30.3
Crude Oil 20.4
Not Filtered/Not acidified 95.1
Spike with 300ppm of a Scale 4.9
Inhibitor

Table 3. Comparison of the scale sensor response under static

conditions.

Image 4. Crystal surfaces of both the 1” and ¾” probes after

the blank test.
SPE 80372 7

100
Blank (1) 1 Scale Dispersant Scale Sensor Coupon
7.5 ppm of Scale Inhibitor (2) Inhibitor Conc. (ppm) Response Weight
1.88 ppm of Scale Inhibitor (3) Conc. (ppm) (∆mV) (∆mg)
Scale Sensor Response (∆ mV)

75 3.75 ppm of Scale Inhibitor (4)

15ppm of Scale Inhibitor (5)
Control (6) 2 Blank 98.1 136.4
Control 6.9 0.5
50 3
15 6.7 18 0.3
15 0 15.7 0.5
4 0 6.7 24.2 4.6
25
3.75 0 32.1 0.9
5
3.75 6.7 8.1 0.5
0 6
Table 5. Comparison of the scale sensor response to scale
5 10 15 coupon data for those experiments where the scale inhibitor
Time (hr) and dispersant concentrations were varied.

Figure 4. Scale sensor response to produced fluids where the

scale inhibitor concentration was varied in the absence of
dispersant.

Scale Inhibitor Scale Sensor Coupon

Conc (ppm) Response Weight (∆mg)
(∆mV)
Control 6.9 0.5
Blank 98.1 136.4
15 20.2 0.5
7.5 58.6 0.9
3.75 35.1 0.9
1.88 55.6 1.1

Table 4. Comparison of the scale sensor response to scale

coupon data for those experiments where the scale inhibitor
concentration was varied and the dispersant concentration was
0 ppm.

100
Blank (1) 1
Scale Inhibitor/Surfactant=0 ppm/6.7 ppm (2)
Scale Inhibitor/Surfactant=3.75 ppm/0 ppm (3)
Scale Inhibitor/Surfactant=15 ppm/6.7 ppm (4)
Scale Sensor Response (∆mV)

75 Scale Inhibitor/Surfactant=15 ppm/0 ppm(5)

Control (6)
Scale Inhibitor/Surfactant=3.75 ppm/6.7 ppm (7)

50

5
2

25
3
4
6
7
0
5 10 15

Time (hr)

Figure 5. Scale sensor response to produced fluids where both

scale inhibitor and dispersant concentrations were varied.