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EVALUATION OF SCALE INHIBITORS

PERFORMANCE UNDER SIMULATED FLOWING
FIELD CONDITIONS...

Article in Journal of Chemical Sciences · January 2016

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 Int. J. Chem. Sci.: 14(1), 2016, 16-28
ISSN 0972-768X
www.sadgurupublications.com

EVALUATION OF SCALE INHIBITORS PERFORMANCE

UNDER SIMULATED FLOWING FIELD CONDITIONS USING
DYNAMIC TUBE BLOCKING TEST
M. RAMZIa, R. HOSNYa, M. El-SAYEDb*, M. FATHYc and
TH. ABDEL MOGHNYc

a
Production Department, Egyptian Petroleum Research Institute (EPRI), CAIRO, EGYPT
b
Analysis and Evaluation Department, Egyptian Petroleum Research Institute (EPRI), CAIRO, EGYPT
c
Applications Department, Egyptian Petroleum Research Institute (EPRI), CAIRO, EGYPT

ABSTRACT

Formation scales considered harmful and expensive problem in the the oil and gas industry. The
most common solutions to reduce and preventing scales deposition is the use of scale inhibitors. In this
work, water sample was delivered from Egyptian oil field and adjusted at pH 6 to simulate scale formation
then two commercial scale inhibitors (ESI1 and ESI2) were evaluated via compatibility test and dynamic
scale loop. The two scale inhibitors ESI1 and ESI2 achieve a good results toward compatibility test at both
25oC and 90oC temperature. Accordingly, the evaluation criteria were carried out using dynamic scale loop
(the tube blocking test). It is found that the minimum inhibitor concentration (MIC) of scale inhibitor ESI1
was successfully verify at 150 ppm with a fail concentrations at 125 ppm according to evaluation criteria.
While, the minimum inhibitor concentrations (MIC) of scale inhibitor ESI2 was between 2% and 3% that
considered too high for application of this product in the field for given conditions. Finally, only inhibitor
ESI1 was passed all evaluation criteria with 150 ppm MIC.

Key words: Water compatibility, Jar test, Scale inhibitor, Injection pipeline, Calcium carbonate, Barium
sulfate, Minimum inhibitor concentration (MIC), Dynamic scale loop and Scaleval.

INTRODUCTION

Scale can be defined as the undesirable deposition of a solid layer of mineral salts1.
Precipitation of inorganic scale in producing wells is commonly known as oil field scale2.
The most popular types of mineral scales in the petroleum industry are calcium, strontium
________________________________________
*
Author for correspondence; E-mail: [email protected]; Ph.: +(202) 22747847, Fax: +(202)
22747433
Int. J. Chem. Sci.: 14(1), 2016 17

and barium carbonates, and sulfates, whereas calcium carbonate scale considered one of the
most extensive in the pipeline3.

Inorganic scales formation taking place in the petroleum and gas industry is a
noteworthy operational (harmful and expensive) problem that effects adversely in the
production stride of the oil industry4-8. The widely severe problems caused by scale
precipitation are many: reduce the production of oil and gas, formation damage, plugging the
oil-producing formation matrix, blockages in perforations or gravel packs, restricted/blocked
flow lines, safety valves and block failure, pump wear, and corrosion underneath deposits9-18.

The most common solutions to reduce and preventing scales deposition is the use of
scale inhibitors. The commonly inhibitors in the oil industry are phosphates and
polyphosphates, phosphate esters, organic phosphonates, polyacrylates, and various other
polymers and copolymers of phosphonates, carboxylates, and sulfonates1. In recent trend,
loaded ionic liquid (IL) plays an important role in oil field application19-21.

The differential dynamic scale loop (DSL) is a tube blocking system to examine the
precipitation and deposition of scale and other salt crystals in pipe work systems like oil or
water pipelines. The scaleval instrument is used to evaluate the scale precipitation and
deposition under pipeline and reservoir conditions. The apparatus determine the efficiency
of chemical inhibitors against inorganic mineral scales formed through the minimum
inhibitor concentration (MIC), hence the MIC is necessary to perform comparative purpose
for different scale inhibitors. The DSL technique used the tube blocking test as an industry
standard to determine the MIC in dynamic reservoir conditions. Inhibitor efficiency can be
calculated as the ratio between the time needed to tube blocking in the presence of inhibitor
divided by the time needed to tube blocking in absence of inhibitor.

Production engineers are responsible for the design, operation and efficiency of
water handling systems in which thermal, pressure or chemical changes lead to scale
deposition. The differential scale loop provides an accurate, reproducible and fast method
for selecting and quantifying the most effective means of controlling scale deposition under
dynamic pipeline conditions. The instrument is suitable to simulate process or reservoir
temperatures of up to 250°C and pressures of up to 14,500 psi. The system is much
recommended where effects of pressure on scaling tendency are to be studied, and especially
for examining the deposition of anhydride under dynamic conditions.

There is a lack of literature concerning the dynamic study of scaling in pipeline

stimulate to the oilfield that established as a novel method for the determination of the
18 M. Ramzi et al.: Evaluation of Scale Inhibitors….

minimum inhibitor concentration (MIC), necessary to prevent scale formation. This paper
describes incipient technique to the laboratory evaluation of scale inhibitors performance to
prevent scale deposition. Therefore, the performance of two inhibitors to prevent calcite and
barite scale is evaluated experimentally utilizing compatibility test. The compatibility tests
are utilized in order to monitor calcite and barite scale formation in the absence and presence
of scale inhibitors.

EXPERIMENTAL
Material
Brine water

The water sample used in this study were synthesized to simulate brine water, the
composition of water was given in Table 1.

Table 1: Water composition

Ions Conc. (ppm)

Na 70060
K 2065
Mg 7245
Ca 3300
Sr 16
Ba 13
Cl 131074
SO4 3870
HCO3 12
pH 6

Scale inhibitors

Two coded scale inhibitors (ESI1 and ESI2) were delivered from Egyptian oil field
for laboratory evaluation to meet specific criteria such as pH measurements, thermal stability
at 130oC, compatibility testing with filtered brine water and dynamic “tube blocking” test.
The evaluation criteria were shown in Table 2.
Int. J. Chem. Sci.: 14(1), 2016 19

Table 2: Evaluation criteria

Test Pass Fail

pH for 100% product >5 <5
Thermal stability at 130oC Clear with or without change in Precipitation
the color
Compatibility with water Clear solution for all ranges of Faint Haze, Haze or
concentration (100 ppm, 1%, precipitated solution
5%, 10%, 25%, 50% and 90%)
at both ambient and 90oC
Tube blocking test Resist deposition for a period of < 3 Times of blank
3 times of blank scale-up time scale-up time

pH Measurements

The pH values of two scale inhibitors (ESI1 and ESI2) were measured with pH meter
calibrated with two buffer solutions of pH = 4.0, and 7.0 and the results are tabulated in
Table 3.
Thermal stability

Thermal stability is an important property for high temperature oil well application
of scale inhibitors. Thermal degradation of molecules may severely affect their scale
inhibiting efficiency. The thermal stability of two types scale inhibitors (ESI1 and ESI2) were
tested at 130oC. A quantity of approximately 15 mL of each inhibitor solution under
investigation were placed in transparent bottles and checked for clearance then photographed
before exposing to the thermal test. The solutions of the inhibitors were transferred into a
high pressure high temperature stainless steel vessels and left into the oven at 130oC for
24 hrs. After 24 hrs of incubation, the vessels were removed from the oven and left to cool
for two hrs then the inhibitors solutions were transferred again to transparent bottles and
checked for any change in the shape that could be occurred due to high temperature, and
then the bottles were photographed again after exposed to a high temperature.
Compatibility testing of inhibitors

The compatibility of water with two types scale inhibitors (ESI1 and ESI2) was tested.
Brine water was filtered through 45 micron filter prior to compatibility testing. The
evaluated scale inhibitor were mixed with brine water to cover a whole range of
concentrations (0 ppm, 100 ppm, 1%, 5%, 10%, 25%, 50% and 90%) in a transparent glass
20 M. Ramzi et al.: Evaluation of Scale Inhibitors….

tubes of total volume of 15 mL. All concentration tubes were checked for any sign of
incompatibility (haziness, precipitation …etc.) and photographs were taken for all test tubes
to be an evidence for the test. The tests were carried out at both ambient and 90oC
temperatures. The above steps were repeated with the other evaluated inhibitors.
Dynamic tube blocking test

The main benefit of dynamic tube blocking experiments compared to static one is
the wide range of pressure and temperature in order to simulate real downhole production
conditions. Performance of the scale inhibitors in dynamic flowing conditions was evaluated
with the help of a dynamic tube blocking apparatus. The tests were performed at temperature
of 120oC, pressure of 120 bar = 1740 psi with 2% calcium as cation solution and 3870 ppm
sulfate as anion solution. The two solutions were filtered, adjust at pH 6, preheated through
coils and pumped at combined flow rate of 10 mL/min (5 mL/min for each). The test
inhibitors are compared regarding their ability to prevent scale formation and adherence at
the following application conditions: coil length of 1 m, coil internal diameter (ID) of 0.8.
Scale inhibitors were mixed with anionic fraction at the duplicated recorded dose and the
solutions were injected at 1:1 ratio. Scale inhibitor concentration was increased stepwise
(starting from blank) until injection pressure (DP) remained constant and no blocking of tube
was observed for at least 15 min of flow. The concentration at which no blockage took place
was considered as minimum inhibitor concentration (MIC).

RESULTS AND DISCUSSION

pH Measurement

The pH measurement of scale inhibitors ESI1 and ESI2 are 5.2 and 6, respectively as
shown in Table 3, the pass criteria should be greater than 5 this means that the two inhibitors
pass in this test.

Table 3: pH values of evaluated inhibitors

Inhibitor code pH Value Pass criteria (> 5)

ESI1 5.2 Pass
ESI2 6.0 Pass

Thermal stability

The result of the thermal stability test of the two scale inhibitors before and after
exposing to 130oC indicated that the two inhibitors ESI1 and ESI2 were not precipitated so
Int. J. Chem. Sci.: 14(1), 2016 21

their succeed to pass thermal stability test. The visual observation are presented in Fig. 1,
and exhibited that at ambient temperature a clear pale yellow liquidfor inhibitor ESI1 and
clear very pale yellow liquid, for inhibitor ESI2, but after exposing to 130oC a clear dark
amber liquid for both inhibitors were display. It's observed that there was no precipitation
for inhibitors at all tempratures.

Fig. 1: Visual observation of inhibitors ESI1 and ESI2 before and after thermal
stability test

Compatibility test with brine water

The result of the compatibility test of the two scale inhibitors with brine water at
both ambient and 90oC were tabulated in Tables 4-5. The recorded results were taken
immediately and after 24 hrs at 25oC, also taken after 15 min at 90oC. The obtained results
indicated that there no any precipitation took place at any scale inhibitors concentrations and
temperatures. It was observed a very clear solution for eight photographs appear at the left
hand side taken immediately at 25oC temperature for scale inhibitor ESI1 Fig. 2(a) and that
the clarity not changed after 24 hrs at the same temperature Fig. 2(b), worthy, the clarity still
not changed even after 15 min at 90oC Fig. 2(c). The same phenomenon observed with scale
inhibitor ESI2 Fig. 3(a-c).

Table 4: Compatibility test of scale inhibitor (ESI1) with filtered brine water
25oC 90oC
No. Inhibitor conc.
Immediately After 24 hrs. After 15 min
1 0 ppm (Blank) C C C
2 100 ppm C C C

Cont…
22 M. Ramzi et al.: Evaluation of Scale Inhibitors….

25oC 90oC
No. Inhibitor conc.
Immediately After 24 hrs. After 15 min
3 1% C C C
4 5% C C C
5 10% C C C
6 25% C C C
7 50% C C C
8 90% C C C
C = Clear, FH = Faint Haze, H = Haze, PPT = Precipitate

Table 5: Compatibility test of scale inhibitor (ESI2) with filtered brine water
25oC 90oC
No. Inhibitor conc.
Immediately After 24 hrs After 15 min
1 0 ppm (Blank) C C C
2 100 ppm C C C
3 1% C C C
4 5% C C C
5 10% C C C
6 25% C C C
7 50% C C C
8 90% C C C

(a) Immediately at 25oC temperature (b) After 24 hrs at 25oC temperature

Int. J. Chem. Sci.: 14(1), 2016 23

(c) After 15 min at 90oC

Fig. 2: Compatibility test of scale inhibitor (ESI1) with filtered brine water

(a) Immediately at ambient temperature (b) After 24 hrs at ambient temperature

(c) After 15 min. at 90oC

Fig. 3: Compatibility test of scale inhibitor (ESI2) with filtered brine water
24 M. Ramzi et al.: Evaluation of Scale Inhibitors….

Dynamic tube blocking tests

A series of dynamic tube blocking tests have at 120°C and 1740 psi to assess the
performance of scale inhibitors coded ESI1 and ESI2 in preventing scale precipitation of
brine water. The result of blank test (without scale inhibitor) represented in Fig. 4. Fig. 4
represent differential pressure versus time plot for blank test (without scale inhibitor) shows
that, the average blank time was determined to be approximately 5 min and so the scale
inhibitor must resist scale deposition (determined to be a rise in DP of 1psi) for a period of
14 min (3 times the blank scale-up time) according to evaluation criteria.

45

Blank‐1 Blank‐2
40

Press = 1740 psi
35
Temp. = 120C

30

25
dp, psi

20

15

10

0
0.000 1.000 2.000 3.000 4.000 5.000 6.000 7.000
‐5
Time, min.

Fig. 4: Differential pressure versus time plot for blank test (without scale inhibitor)

Fig. 5 show the differential pressure versus time plot during application of inhibitor
(ESI1). This figure shows the MIC (Minimum inhibitor concentration) for inhibitor (ESI1)
can be regarded as 150 ppm or a little bit lower with a fail concentrations of 125 ppm
according to evaluation criteria. The concentration of 150 ppm of inhibitor (ESI1) can resist
brine water scale deposition for a period of more than 30 min, which is more than 6 times of
the blank scale-up time (Pass Criteria), while the concentration of 125 ppm can resist the
brine water scale deposition for a period of only 12 min, which is a little bit less than 3 times
of blank scale-up time (Pass Criteria) these results tabulated in Table 6. While in case of
scale inhibitor (ESI2) the MIC was between 3% - 2%, with a fail concentration below 2%,
which is too high for application of this product in the field for given conditions. There is no
need to carry out more test to tune the MIC because it will be too high for application of this
product in the field for given conditions. These data tabulated in Table 7 and represented in
Fig. 6.
Int. J. Chem. Sci.: 14(1), 2016 25

Table 6: Tested inhibitor concentration (ESI1) against pass criteria

Tested inhibitor conc. Pass criteria 3 time blank scale-up time

Time (min)
(ppm) (~14 min)
0 ppm (Blank 1) 4.9
0 ppm (Blank 1) 4.5
1000 ppm > 30 Pass
500 ppm > 30 Pass
350 ppm > 30 Pass
300 ppm > 30 Pass
200 ppm > 30 Pass
150 ppm > 30 Pass
125 ppm ~ 12 Fail
100 ppm ~6 Fail

Table 7: Tested inhibitor (ESI2) concentration against pass criteria

Tested inhibitor conc. Pass criteria 3 time blank scale-up time

Time (min)
(ppm) (~14 min.)
0 ppm (Blank 1) 4.9
0 ppm (Blank 1) 4.5
10% > 30 Pass
5% > 30 Pass
3% > 30 Pass
2% ~ 13 Fail
1.50% ~ 8.8 Fail
1% ~ 5.8 Fail
200 ppm ~5 Fail
26 M. Ramzi et al.: Evaluation of Scale Inhibitors….

45
Inhibitor E Blank‐1
40 Blank‐2
1000 ppm
35 500 ppm
350 ppm
300 ppm
30
200 ppm
150 ppm
25 125 ppm
100 ppm

dp, psi
20
Press.  = 1740
Temp. = 120oC
15

10

0
0.000 5.000 10.000 15.000 20.000 25.000 30.000 35.000
‐5
Time, min.

Fig. 5: Differential pressure versus time plot during application of inhibitor (ESI1)

45
Inhibitor F Blank‐1
40 Blank‐2
10%
35 5%
3%
30 2%
1.50%
25 1%
200 ppm
dp, psi

20
Press.  = 1740
Temp. = 120oC
15

10

0
0.000 5.000 10.000 15.000 20.000 25.000 30.000 35.000
‐5
Time, min.

Fig. 6: Differential pressure versus time plot during application of inhibitor (ESI2)

CONCLUSION

All evaluated inhibitors were passed the pH criteria. Scale inhibitors ESI1 and ESI2
were compatible with brine water at both ambient and 90oC temperature. Accordingly, they
met the second step form the evaluation criteria and transferred to the final step of the
evaluation criteria (the tube blocking test). The minimum inhibitor concentration (MIC) for
inhibitor (ESI1) can be regarded as 150 ppm or a little bit lower with a fail concentrations of
125 ppm according to evaluation criteria. The minimum inhibitor concentration (MIC) for
inhibitor (ESI2) was between 2% and 3%, which is too high for application of this product in
the field for given conditions. Generally, only inhibitor ESI1 was passed all evaluation
criteria with 150 ppm MIC.
Int. J. Chem. Sci.: 14(1), 2016 27

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Accepted : 23.12.2015

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