SPE-174277-MS

Prevention of Calcium Carbonate Precipitation during Water Injection into

High-Pressure High-Temperature Wells
Azizollah Khormali, Dmitry G. Petrakov, and Abdul-Latif Benson Lamidi, National Mineral Resources University
(University of Mines); Reza Rastegar, Trican Completion Solutions USA

Copyright 2015, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE European Formation Damage Conference and Exhibition held in Budapest, Hungary, 35 June 2015.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
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Abstract
Complex technical problems, including salt precipitation, can occur during the entire period of the
operation and production of the oil from reservoirs in high-pressure/high-temperature (HPHT) condition.
Inorganic salts deposition occurs during the mixtures of different waters, which are incompatible with
each other. These combinations of waters mostly can be done during waterflooding into the reservoirs to
pressure maintenance. For the effective development of oil reservoirs, which are associated with the
deposition of inorganic salts in HPHT, the selection of inhibitors is required to prevent scaling accounts
for the characteristics of the reservoirs. Effectiveness of the scale inhibitors concentration for specific well
conditions is verified by laboratory tests, considering total dissolved salts and hydrochemical conditions
of the formation. The amount of calcium carbonate (CaCO3)) precipitation in synthetic formation water
was investigated in mixing with the injected water in the range of 100-200C for temperature and 40-70
MPa for pressure. Also, calcium carbonate precipitation was considered in a well at 200C and 70 MPa
in a simulation model with an electrical submersible pump (ESP). The results of the experiments showed
that the possibility of calcium carbonate deposition was increased by growing the amount of the formation
water and temperature. Increasing the pressure had reverse effect on scale formation. In this investigation,
a new inhibitory chemical composition was developed. This scale inhibitor is based on the aqueous
solutions of different acids and isopropyl alcohol. The inhibitor was considered for compatibility with
formation water and core samples; and it was compatible with them at reservoir condition. The new scale
inhibitor had a greater inhibition efficiency and low permeability damage in comparison with the tested
inhibitors. The used materials were effective for scale prevention at high-level. The synergistic inhibitory
effect has been considered for mixtures of inhibitors.
Introduction
Formation and deposition of inorganic salts in the oil producing reservoirs and underground equipment are
recognized as a major operational problem during oil production from wells. Scaling is the primary cause
of formation damage in the injection and production wells (Moghadasi et al. 2003a). Scaling can be
developed in the formation pores in the near wellbore region to reduce porosity and permeability.
Production rate and equipment life are reduced by deposition of the salts. There are different reasons of
2 SPE-174277-MS

scale in various fields because of the complicated conditions for the formation of salts. Water is the
paramount importance of scaling because the precipitation of salts occurs only when the water is produced
and combined with other incompatible waters. In most cases, scaling is found in the oil field by
precipitation from water, which comes naturally in the reservoirs or as a result of establishment of
formation water supersaturation with salt-forming components when two incompatible waters are satisfied
in the formation. Whenever the water is produced from the wells or the injected water is used for oil
recovery during waterflooding, there is the possibility of formation of inorganic salts (Moghadasi et al.
2003b).
Seawater is sometimes used as the injected water and has a tendency to become rich by ions, which
are byproducts of water evaporation. The injected water into reservoir forms a specific chemical
composition through the exchange with reservoir rocks and fluids. Produced water is also injected into the
reservoir to improve oil recovery in the waterflooding process, in connection with this; low quality of the
injected water will lead to the formation of salts, which can reduce oil production rate. Water usually
comprises a plurality of divalent cations of calcium and magnesium in carbonate and sandstone reservoirs
(Kohler et al. 2001). The exact composition of water is a complex dependence on mineral diagenesis and
other changes occurring in the flow of reservoir fluids and their mixing. The various processes of oil
production inevitably lead to the changes in the equilibrium conditions of calcium carbonate ions whereby
the salt is deposited. If these changes allow fluid components to be above the limit of mineral solubility,
the automatic carbonate formation occurs resulting from changes in temperature and pressure, and it leads
to halide of crystallization and precipitation (Daniels et al. 2014; Kan and Tomson 2010).
Calcium carbonate precipitation is one of the most widely distributed of scales in the reservoir and
downhole equipment under certain conditions. The main factor contributing to the deposition of calcium
carbonate is a partial transformation of calcium bicarbonate that occurs during heating, especially at high
temperatures (Smith et al. 2003). The solubility of calcium carbonate is largely dependent on the content
of carbon dioxide in water, which is in certain quantitative proportions with bicarbonate (HCO3-), and
carbonate (CO32-) ions in dynamic equilibrium. The content of carbon dioxide in the highly mineralized
water is difficult to determine. However, the quantitative relation among CO2, HCO3- and CO32-
(carbonate equilibrium) can be determined by the concentration of hydrogen ions (Chen et al. 2010).
Prediction of the formation possibility of calcium carbonate during the oil production from the reservoir
with waterflooding is based on the consideration of processes that contribute to the formation of the
precipitated solid from aqueous solutions as follows: mixing of incompatible waters, which are moved by
the oil; decomposition of calcium bicarbonate as the result of changes in physical and chemical
conditions; solubility reduction of calcium carbonate in water.
The most appropriate method to prevent deposition of inorganic salts is the use of chemical reagents
- scale inhibitors. They are periodically injected into the reservoir or pumped into the annular space of
production wells using chemical dosing units (electric pump) (Levanyuk et al. 2012). Inhibitors that the
so-called threshold effects cover microcrystalline nucleus of formed deposits, slow down their growth and
keep in suspension. Selecting the scale inhibitor for oilfield in which operation of equipment is
complicated by the presence of scaling, is based on the chemical composition of the precipitated salt and
technological properties of the reagent, including the inhibitory activity, the state of aggregation,
compatibility with formation water, corrosivity, lack of effect on the preparation of oil and thermal
stability (Tomson et al. 2003). A disadvantage of scale inhibitors in liquid form is a fast removal of large
quantities of the reagent in the initial period after starting the production in the well.
Oil production from deep wells, in which there are serious technical difficulties, which are associated
with the development and exploitation activity through unequal fracture rocks on the bottomhole and
geological heterogeneities, is a sufficiently complicated process (Ramstad et al. 2005). As far as the
solubility of calcium carbonate decreases with increasing temperature, if the oil is produced using ESP in
HPHT wells in which there is a probability of calcium carbonate formation, the ESP will be indispensable
SPE-174277-MS 3

failed caused by the deposition (Poynton et al. 2008). Therefore, the study of the prevention of calcium
carbonate deposition in HPHT wells is the actual problem. Then, the objectives of this study are the
experimental investigation of calcium carbonate deposition during mixing the injected and formation
waters in HPHT oil wells and its scale inhibition.

Laboratory test methods and materials

The possibility of selecting the inhibitors is limited because the range of scale inhibitors, which are
produced by the chemical industry, not great. Obviously, it is connected to the complexity and time-
consuming for development and synthesis of new active chemical compounds (Ketrane et al. 2009).
However, creation of multicomponent mixtures of different scale inhibitors with a synergistic inhibitory
effect is more economical and no less effective way as expanding assortment of the scale inhibitors to
improve their quality (Liu et al. 2012). Certain principles of combining inhibitors to obtain a synergistic
effect of the compositions are developed. The effect that is greater than the sum of single actions of the
initial components. The compilation of compositions is the result of empirical selection. One of the
conditions is well known that inhibitors of different chemical nature should be used for obtaining the
synergistic multicomponent compositions.
Calcium carbonate precipitation prediction based on a comparison of the actual value of a parameter
(Eeq), which is characterized by an equilibrium condition between the liquid phase on the one hand, solid
and gaseous phases on the other hand with the calculated value of this parameter upon the saturation of
water with calcium carbonate. Saturation index is accepted for use as an indication of scaling (SIEeq,fac-
Eeq,cal). The water tends to formation of salt precipitation when the actual value of Eeq is greater than the
calculated value. If the saturation index is negative, this water is capable of dissolving calcium carbonate
being aggressive (Mavredaki and Neville 2014). The water is at the equilibrium saturation with calcium
carbonate in case of SI0. Saturation index allows only qualitatively evaluating the ability of water to
precipitate or dissolve salts. Determination of saturation index is carried out through correlation for each
salt and there is the difficulty of measuring the concentration of all ions in HPHT wells (Yuan et al. 1997).
In addition, saturation index only qualitatively indicates the probability of the salt formation, so, in this
paper, instead of getting the saturation index, is measured mass of precipitated calcium carbonate under
HPHT condition (Zhang et al. 2014).
Method of investigation of the scale inhibitors lies in the fact that the process of calcium carbonate
scale formation and precipitation prevention is studied in synthetic formation water with core samples and
controlled for HPHT condition. Scale inhibitor efficiency is determined as the percentage of calcium,
which is retained in solution with the inhibitor from its total content. Experiments are carried out on
simulated water of the chloride-calcium type that is characteristic for formation waters. The solutions of
formation water with the scale inhibitors are thermostated for 24 hours at temperature of 200C. Working
samples contain different amounts of the scale inhibitors. After thermostating and cooling, the precipitated
calcium carbonate is filtered off and the content of calcium carbonate ions is determined in the filtration.
Efficacy of inhibition is calculated using the following equation (Eq. 1):
(1)

where E is the scale inhibitor efficiency, m0 and m are the masses of salt precipitate in the solution with
inhibitor and without inhibitor in gram, respectively.

Results and Discussion

Incompatibility of formation water with injected water can serve as the main cause of supersaturation of
produced water from the oil wells. To quantitatively estimate the influence of mixing of injected and
formation water in the process of formation of calcium carbonate, laboratory experiments were carried out
4 SPE-174277-MS

with the sample, which were placed in a mixture of water and were periodically vigorously stirred with
a magnetic stirrer. It should be added that the mixture of the formation and injected water were
incompatible. The results of the experiments are shown in Table 1. Mixing of the formation chlorine-
calcium water containing calcium ions with sodium carbonate surface water relative leads to satiation of
calcium carbonate. As shown in Table 2, synthetic formation water has different ions. Total dissolved salt
of this water is high (147400 mg/l). The formation water is capable of forming and precipitating of
calcium carbonate in mixing with injected water.

Table 1Effect of chemical incompatibility of injected and formation waters in the scaling process at 200C and 70 MPa
Mass of core sample

No. Volume ratio of formation water to injected water Initial mass of core sample In 24 hours In 48 hours In 5 days

1 1:1 16.3592 16.4195 16.5347 16.7712

2 2:1 16.3592 16.6367 16.9158 17.2617

Table 2Formation water properties at 200C and 70 MPa

Ion content (mg/l)

pH Density(kg/m3) K Ca2 Na Sr2 Mg2 Cl- HCO3- CO32- SO42- Total dissolved salts (g/l)

6.8 1074 1209 23662 39484 759 1826 48273 23758 7462 941 147.4

The dependence of the total amount of precipitation of calcium carbonate on the volume ratio of
formation to injected water has complex nature when mixing the waters. Figures 1 and 2 show that the
dependence of concentration of formed calcium carbonate salt (mass) has a maximum at a ratio of 0.8. The
temperature growth causes the increase in the amount of precipitated calcium carbonate at high pressure
(70 MPa). As shown in Fig. 2, there is no considerable difference of formed salt quantity by changing
pressures at high temperature (200C).

Figure 1Calcium carbonate precipitation for different temperatures at 70 MPa

SPE-174277-MS 5

Figure 2Calcium carbonate precipitation for different pressures at 200C

Simulation of changes in the salt saturation of formation water allows predicting the potential of the
salt deposition, the intensity of scaling in the reservoir, well and ESP. The developed software tools that
are based on the algorithms of Oddo and Tomson (1994) have been used for simulation of quantity of the
calcium carbonate precipitation in the well with ESP to a depth of 3700 m (Ragulin et al. 2006). In the
simulated condition, the pump was at 200C and 70 MPa. As shown in Fig. 3, the largest amount of
calcium carbonate was precipitated in place of ESP because of pressure and temperature condition. The
simulation results illustrated dependency of the amount of the formed calcium carbonate on the well
depth, which are the basis for identifying areas of salt deposition and are required information for the
development to prevent salt precipitation. Figure 3 shows that above the ESP, with increasing depth of the
wells, the probability of calcium carbonate formation normally grows in two different slopes until ESP.
But, the amount of precipitation has very sharply increased in the depth in which ESP is located. The
reason for this change in precipitation of calcium carbonate is the growth of the temperature (high
temperature condition).
6 SPE-174277-MS

Figure 3Salt deposition in the oil well with ESP production

The most important in the development of inhibitory protection technologies is the selection of an
effective inhibitor of scaling with respect to the specific parameters of exploitation of the wells and the
chemical composition of produced water. Figure 4 shows the inhibitors of prevention of the calcium
carbonate deposition under HPHT condition. Inhibitor No. 4 is a new scale composition of calcium
carbonate with defined concentration of the contents. Table 3 illustrates the results of the research the
effectiveness of various inhibitors. The inhibitor No. 4 has the highest efficiency for the prevention of
calcium carbonate in the bottomhole formation zone (core samples at HPHT condition) and production
equipment. This inhibitor shows a high anti-scaling activity in the heat exchange system of thermochemi-
cal dehydration and oil desalting. The scaling prevention treatment by inhibitor No. 4 is exposed to the
crystallization of calcium carbonate. The stabilizing effect by polyphosphates is reduced to the violation
of the crystallization process resulting binding complex of salts rigidity and surface blocking of arising
crystallization centers.
SPE-174277-MS 7

Figure 4 The used scale inhibitors for experiments at HPHT condition

Table 3Efficiency of the scale inhibitors at 200C and 70 MPa

Protection at concentration of mg/l (%)

No. Scale inhibitor composition 10 20 50 70 100

1 nitrilotrimethylphosphonic acid 43 55 61 68 72
2 aqueous solution of acrylic 38 47 59 75 77
3 based on phosphorus 35 45 61 67 73
4 oxiethilidendiphosphone acid 4%, ammonium chloride5%, 51 77 81 87 90
polyethylene polyamine-N-methylphosphonic acid 6%,
hydrochloric acid 12%, isopropyl alcohol 3%, water
remaining (new inhibitor)

The results of research on the effectiveness of mixtures of scale inhibitors, based on the new scale
inhibitor (No. 4), are presented in Table 4. The table shows the optimum composition and concentration
and the synergistic effect of the mixtures at the given concentrations and compositions. The presented
results allow selecting the mixtures and their working concentration for the most effective application. The
effectiveness of compounds, which are given in Table 4, is greater than the effectiveness of the most
efficient scale inhibitor No. 4. As shown in the table, it follows that the mixture of inhibitors No. 3 and
No. 4 at a ratio of 35:65 in comparison with other compounds has the maximum synergistic effect and
maximal efficiency at appropriate concentrations. Therefore, certain parameters that are relevant for
practical use of the inhibitors can be determined in this mixture.
8 SPE-174277-MS

Table 4 The optimum composition and concentration mixtures scale inhibitors at 200C and 70 MPa
Mass content of the
Mixture of the scale inhibitor No. 4 in Concentration of mixture Synergistic inhibitory Effectiveness of the
inhibitors mixture (%) (mg/l) effect mixture (%)

InhibitorsNo. 1 and No. 4 50 5 1.92 66

10 1.78 84
20 1.31 86
60 1.24 92
65 5 1.89 72
10 1.62 78
20 1.27 88
60 1.19 92
85 5 1.81 78
10 1.63 81
20 1.22 90
60 1.14 92
InhibitorsNo. 2 and No. 4 50 5 1.84 61
10 1.77 79
20 1.38 86
60 1.20 91
65 5 1.87 70
10 1.69 79
20 1.32 88
60 1.16 91
85 5 1.88 80
10 1.74 85
20 1.23 89
60 1.13 92
InhibitorsNo. 3 and No. 4 50 5 1.94 62
10 1.89 81
20 1.47 90
60 1.24 92
65 5 2.37 87
10 1.93 88
20 1.38 91
60 1.20 92
85 5 1.98 84
10 1.79 87
20 1.25 90
60 1.16 94

One of the most important indicators in selecting scale inhibitors, as well as all other reagents, is the
ratio of the efficiency to specific consumption of the inhibitor at HPHT condition. Figure 5 illustrates that
four of the investigated mixture compositions of the scale inhibitors (No. 3 and No. 4) with a mass content
of the inhibitor No. 4, which equals to 0.25, 0.45, 0.60 and 0.70, reach a predetermined inhibition
efficiency of 75%. Wherein, the composition of the mixtures of the scale inhibitors with a mass content
of 0.40 for the inhibitor No. 4 reaches the mentioned effectiveness (75%) with minimum specific
consumption at 8 mg/l. Three mixture compositions of scale inhibitors No. 3 and No. 4 reach efficiency
of 80%, and the composition with a mass content of 0.45 of the inhibitor No. 4 provides this efficiency
in the low specific concentration of 15 mg/l. Also, three compositions of the scale inhibitors mass
containing the inhibitor No. 4, 0.25, 0.45 and 0.6 have an efficiency of 90%, but the third composition has
the lowest consumption rate (41 mg/l). From the above described results, it can be concluded that the use
of the multi-component mixtures of the inhibitors No. 3 and No. 4 is more effective depending on the
concentration of the mixtures.
SPE-174277-MS 9

Figure 5The dependence of the minimum concentration of mixtures of the scale inhibitors No.3 and No.4 on the mass content of the
inhibitor No. 4 at 200C and 70 MPa

Permeability reduction of the used scale inhibitors was tested at HPHT condition and the result of the
experiment is shown in Fig. 6 and 7. In the performed experiment, formation water in mixing ratio of
80:20 to injected water has been injected into core sample. Besides the waters, the scale inhibitors were
injected. As shown in Fig. 6, the biggest permeability damage occurs by use of the scale inhibitor No. 3.
The lowest damage occurs by use of the new developed scale inhibitor (No. 4). Figure 7 shows that using
a scale inhibitor in mixtures the permeability declines more slowly in comparison with changes in
permeability of core in Fig. 6. In this case, inhibitors were mixed with a ratio of 60:40 (inhibitor No. 4
to others). The figure illustrates that the lowest permeability reduction occurs for mixture of scale
inhibitors No. 3 and No. 4.

Figure 6 Changes in permeability of core sample by injection of scale inhibitors at dosing rate of 50 mg/l at 200C and 70 MPa
10 SPE-174277-MS

Figure 7Changes in permeability of core sample by injection of mixture of scale inhibitors at dosing rate of 50 mg/l at 200C and 70
MPa

Conclusions
From the experimental investigation of this work the following conclusions can be drawn:
i. Amount of calcium carbonate formation and precipitation increases in wells at HPHT condition
with mixing injected and formation waters. Deposition of the salt in production wells with ESP
rapidly rises because of the high temperature of the engine of the pump.
ii. The new inhibitor is compatible with formation water without the formation of any suspension,
does not have aggressive properties and the accuracy of dosing cannot make high demands.
iii. The result of the experiments can be applied for effective protection of the oil reservoir and
production equipment with minima formation damage in HPHT oil wells. Synergistic effect
reached to 2.37 in low dosing rate of scale inhibitor for the mixture of the new inhibitor with
inhibitor, which is based on the phosphorus. Using the mixture of the new developed inhibitor with
phosphorus is 30 percent more effective in comparison with the single inhibitor of phosphorus for
prevention of calcium carbonate formation at HPHT condition of oil wells.

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