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Halite Scale Formation Mechanisms, Removal and Control A Global
Halite Scale Formation Mechanisms, Removal and Control A Global
This paper was prepared for presentation at the SPE International Symposium on Oilfield Chemistry held in The Woodlands, Texas, USA, 8–10 April 2013.
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 of the paper have not been
reviewed by the Society of Petroleum Engineers and are subject to correction by the author(s). The material does not necessarily reflect any position of the Society of Petroleum Engineers, its
officers, or members. Electronic reproduction, distribution, or storage of any part of this paper without the written consent of the Society of Petroleum Engineers is prohibited. Permission to
reproduce in print is restricted to an abstract of not more than 300 words; illustrations may not be copied. The abstract must contain conspicuous acknowledgment of SPE copyright.
Abstract
Halite scale has long been a challenge in the oil and gas industry. In recent years there has been a marked increase in the
occurrence of this scale type due to the increased development of hotter and deeper gas and gas condensate fields. As the
formation of this scale is commonly in the downhole production tubing, it is a challenge to identify and mitigate, so a non-
conventional approach has to be taken for removal and control. Furthermore, it is very difficult to replicate the formation of
this scale in the laboratory with complex and specific equipment being utilized to replicate field observations.
This paper provides a review of several examples of halite scale formation in the field, detailing the mechanism of deposition
and the strategies employed to remove and subsequently prevent reoccurrence. Details are also provided for two different
types of laboratory test methods; the first being a simple static test method designed to quickly screen the extent of halite
challenge and the suitability of a range of inhibitors. The second laboratory method concerns a novel, dynamic method whose
primary aim is to accurately measure and predict the severity of scaling in the field, and then go on to determine the
minimum effective dose of inhibitor required to prevent build-up.
The different types of halite inhibitor chemistries are evaluated, including the use of wash water and where this is used in
combination with organo-ferrous compounds, as well as more novel polymeric compounds. The paper concludes by
providing an insight into the economics of the different types of treatment, namely the use of wash water versus the use of
chemical inhibitors and combinations of these two techniques.
Introduction
Halite (NaCl) has been considered as a non-conventional scale but with the recent upsurge in deep-water, high pressure, high
temperature, gas condensate fields there has been more coverage of this type of scale in the literature (Kleinitz et al., 2001a;
Kleinitz et al., 2001b; Guan et al., 2008a; Guan et al., 2008b; Chen et al., 2009a; Chen et al., 2009b; Van Dorp et al., 2009;
Djamali et al., 2012; Spicka et al., 2012). Halite precipitation is unsurprisingly more often a challenge in high salinity wells
and can plug downhole production tubulars, topside process equipment, and pumps. Deep, high temperature wells are
particularly susceptible to halite deposition as they can be prone to a greater degree of cooling, one of the major drivers for
deposition. Unlike conventional carbonate and sulfate scales, for halite scale the driving force for precipitation is small yet
the concentration of ions is huge (Smith and Przybylinski, 2006).
The most common method of countering the deposition of halite scale is the injection of fresh or less saline water, via batch
treatments to the affected zones or via continuous injection upstream of the deposition zones. This is a very valid approach
that is both cost effective and efficient. However, this is not always the most practical solution as the large volumes of fresh
water may not be available, nor may it be possible to introduce the water in the required volume to the affected zones. In
these instances, sub-stoichiometric chemical halite inhibitors are a valid alternative.
Much theoretical work has been performed on halite scale precipitation and include mechanistic crystal growth studies (Guan
et al., 2008), modeling studies (Jasinski and Frigo, 1996) and thermodynamic studies (Shipley et al., 2006). A comprehensive
field study (Kleinitz et al., 2001) yielded useful observations on the early detection of halite precipitation on the basis of
2 SPE 164081
simple quotients of ionic ratios: Na/Li, Na/K and Na/(Ca+Cl) were shown to be of particular relevance. Studies on the
influence of hydrate inhibitors, such as methanol and ethylene glycol, on halite deposition is very relevant because it is often
found that halite forms in gas condensate wells that are more prone to hydrate formation, such as, in oil wells.. It has been
found that hydrate inhibitors adversely affect halite scale formation (Kan et al., 2003).
Two of the best described inhibitors in the literature are nitrilotriacetamide (NTAA) and potassium ferricyanide. NTAA has
successfully inhibited halite formation but requires 250 to 500 mg/L to do so. While the molecule is expensive to
manufacture, it is high temperature stable and has a relatively favorable biodegradation profile (Ralston and Persinski, 1968;
Guan et al., 2008). Potassium ferricyanide has been shown to inhibit halite but is poisoned by ferrous ions and can cause
secondary deposition of insoluble reaction products and therefore, requires to be formulated with a suitable chelating agent
such as citric acid or nitrotriacetic acid (Glasner and Zidon, 1974; Place and Smith, 1984; Zaid, 1995).
An excellent field study is given on the performance of potassium ferricyanide (Frigo et al., 2000). Interestingly, in this
study, the performance in the field was lower than that in the laboratory where close to 100% inhibition performance was
achieved. It was postulated that this was due to incompatibility with the high levels of iron present in the produced water, or
due to excessive liquid phase evaporation. During the 3 month long field trial, halite precipitation was not completely
suppressed but increases in performance of equipment were observed that would have otherwise quickly failed.
Kleinitz et al. (2001) discussed observations where tubing linings have been used that release lead and cadmium to inhibit
halite deposition. This study also focuses on removal methods and goes into some detail on the relative dissolution rates of
pure water, 2% KCl solution, and 2% KCl with 3% of butyl glycol solution. The 2% KCl is used to prevent damage to clay
minerals in the reservoir and the 3% butyl glycol was used to decrease the interfacial tension to facilitate back flow of the
treatment slug.
It has been postulated in the literature that the most likely mechanism for the most effective prevention of halite is nucleation
inhibition; although, work performed showed significant crystal morphology modification showing that, in fact, inhibitors
can also work via crystal growth inhibition (Guan et al., 2008). This work also states that the current (2008) commercially
available halite inhibitors were only effective at concentrations >250 mg/L. Three new compounds were studied (two
inorganic and one organic nitrogen-based product) and benchmarked against NTAA and potassium ferricyanide. All products
tested resulted in changes to the halite crystal morphology, changing the normally cubic crystals to varieties of shapes and
much smaller crystals. The new chemistries showed improved static inhibition efficiency against NTAA and potassium
ferricyanide. A dispersive mechanism has also been proposed for halite inhibitors where a reduction in the agglomeration and
settling of suspended particles occurs (Chen et al., 2009).
The influence of calcium, magnesium and zinc ions on the efficacy of inorganic and organic halite inhibitors was studied by
Smith and Przybylinski (2006). It was found that calcium ion enhanced the activity of inorganic inhibitor and decreased the
efficacy of the organic inhibitor. Magnesium had negligible effect on either inhibitor and zinc had a significant inhibitory
influence of its own. This influence however, was cancelled by the presence of the organic and especially by the inorganic
inhibitor. No detail is given on the exact chemical nature of the inhibitor chemistries in this work other than they are
formulated products.
A multifunctional polymeric inhibitor has been reported in the literature that is effective against carbonate and sulfate scales
as well as halite (Spicka et al., 2012). No details are given on the chemistry itself , but ample detail is given on the testing
methods employed and the work concludes by stating that a combined fresh water/halite inhibitor approach is a viable option
to help reduce the costs associated with a purely fresh water strategy.
happens in the field; whereby, hot saturated fluids cool to a certain temperature and precipitate halite as a result. There are
two broad types of test that can do this simulation and they can be distinguished into two categories: static and dynamic.
Other researchers have achieved supersaturation by evaporating water from the saturated solutions of NaCl (Glassner and
Zidon, 1974). While this does mimic more closely what actually occurs in the field, when compared to the cooling method
described above, the degree of supersaturation that can practictably be achieved is very limited. In order to achieve higher
levels of supersaturation, an alternative method has been developed and employed by several researchers (e.g. Frigo et al.,
2000; Smith and Przybylinski, 2006). The principal of these techniques is mixing of incompatible brines - one containing a
saturated solution of NaCl and the other containing CaCl2 plus NaCl. This enables relatively large supersaturation to be
achieved almost instantaneously as well as isothermally upon mixing. The degree of supersaturation can be modified to
mimic exactly what is present in the field (e.g. Frigo et al., 2000). Further work to that of Frigo et al. (2000) has found that
mixing a nearly supersaturated solution of NaCl with smaller amounts of nearly supersaturated LiCl, CaCl2, sodium
thiocyanate, MgCl2 will result in a supersaturated halite solution (Smith and Przybylinski, 2006). Furthermore, a
concentration sodium hydroxide solution will also precipitate halite from a saturated or nearly saturated solution of NaCl, but
can result in an undesirably high and unrepresentative pH.
One particular study (Chen et al., 2009) compared directly the use of dynamic tests (see below) to the static cooling method
and found large discrepencies between the two methods. It was concluded that dynamic halite tests were more representative
of halite formation in the field and showed good reproducibility.
It is also possible to observe the in situ crystal morphology in aqueous solution under the microscope. This enables
determination of how inhibitors affect the size, shape, growth patterns and number of crystals forming in an inhibited and
non-inhibited environment (e.g. Guan et al., 2008).
Other variations on the dynamic technique described above are possible, taking into consideration some of the methods used
in more advanced static testing. These techniques have not been described in the literature but involve pumping two or three
brines in a dynamic scale loop. The first contains a nearly saturated NaCl solution and the second a CaCl2, LiCl2 or MgCl2
brine. The optional third brine can contain nearly saturated NaCl solution of the same ionic strength as the first brine and be
dosed with scale inhibitor. The ratio of the brines can be varied so that the scale inhibitor is stepwise reduced in order to
determine the minimum effective dose required to inhibit scale formation in the loop.
Case History
Background
This case history concerns an onshore well that produced from an extreme high pressure (18,500 psi / 1275.5 bar) and high
temperature (290°F / 143.5°C) reservoir. During the initial well test, a significant water cut was recorded and the salinity was
very high and halite deposition occurred both on the surface and downhole ,fouling the well test equipment. The well test
yielded approximate flow rates of 1,000 bbl.day-1 of ~50°API condensate, 3,000 bbl.day-1 produced water, and 5 MMscf.day-
1
of gas (~1% CO2 and 1,000 ppm H2S). The produced water composition has been summarized in Table 1. Stable flow could
4 SPE 164081
not be achieved during the well test due to halite deposition and the test was abandoned ahead of plan. It was planned to re-
enter the well after a suitable halite mitigation strategy was developed and could be employed during the planned Extended
Well Test (EWT). This would enable a more representative flow rate well test and gather representative reservoir data in
order to enable evaluation of the commercial potential of the field. Halite inhibition was regarded as the key critieria for
success and an extensive chemical screening process was undertaken in order to provide a ‘best-in-class’ solution for this
well. The halite inhibitor injection point was marginally above the packer via a chemical injection line capable of injecting a
maximum flow rate of between 40 and 60 bbl.hour-1.
There were four methods identified for mitigating deposition of halite in the producing wells and associated surface process:
Water shut off application
Control the system pressure and temperature to keep the fluids undersaturated with respect to halite
Injection of wash water to keep the fluids undersaturated with respect to halite scale
Injection of halite scale inhbitors.
It was identified that the location of halite deposition and amount of scale formation was influenced by the water/gas ratio
and the drawdown on the well. There was not enough confidence in water shut off being a viable long term solution for
controlling halite scale formation and very high localized drawdown occurred in certain producing intervals of the reservoir.
The modeling of halite scale formation showed that injection of enough wash water would prevent supersaturation of halite
and remove the deposition potential. However, it was not believed to be operationally sustainable to continuously deliver the
large amounts of water and, therefore, halite inhibitors were identified to be the most viable option for ensuring flow
assurance in this well. What was clearly identified were producing conditions where the drawdown was such that halite
deposition potential existed upstream (below) of the point of halite scale inhibitor / wash water injection; operational limits
were set to avoid these producing scenarios.
Due to the extensive nature of the testing, not all procedures and test data has been included here. Focus has been given to the
previous application history modeling of halite formation and performance testing.
The second application example is from a gas compression plant in East Texas. Product A was used as a halite inhibitor
injected continuously into the producing flow-line. The performance of Product A was monitored by visual inspection of
flow-line valves. The application of Product A was successful and no halite deposition was reported.
hydrocarbons and gaseous phases. Most importantly it can include a halite solubility evaluation and model in situ evaporation
which is key to many halite deposition scenarios.
Initial modeling used produced water only to generate a relationship between temperature and pressure and the halite
deposition envelope. This then was made more representative by including a gas phase, and then finally adding in a
condensate phase. It was observed that there were significant differences between these models with the three phase model
having a lower temperature of deposition (more stable with respect to halite scale). It was also noted that a large difference in
scaling tendency from the same produced water composition was possible dependent upon the produced fluid and gas rates.
As there was a degree of uncertainty in these rates, a worst case position was taken and it was observed that given the
pressure drop from reservoir to surface was so high, there could effectively be no corresponding temperature drop; otherwise,
halite scale was predicted to form downhole. The produced fluids will experience pressure and temperature drops on transit
from reservoir to surface and significant halite scale was predicted to form downhole.
Exactly where in the well halite scale was predicted to form was difficult to model because it was found to be determined by:
Accurate characterization of halite precipitation requires a thorough understanding of the above parameters. It was possible to
correlate process modeling with halite modeling to determine the likely operating conditions in the well, given the various
possible production rates, i.e. different drawdowns and water to gas ratios. From this data it was possible to simulate where
the most likely locations of halite scale deposition would be. In all cases it was observed that halite precipitation would occur
downhole and would be confined to the upper tubing (above the test packer) when increased drawdown was applied.
The significance of this observation was that water shut off was no longer considered a viable approach for this well because
halite scale formation could move further downhole if the water rates decreased drastically and then be upstream of the halite
inhibitor or wash water injection point.
Performance Testing
A combination of static and dynamic testing was performed to evaluate suitable chemistries for application during the EWT.
Several different formulated products were tested including:
NTAA
Potassium ferricyanide
Product A - Alkyl naphthalene sulfonate
Product B - Acrylic copolymer 1
Product C - Acrylic copolymer 2
Product D - Sulfonated polycarboxylate
Product F - Polyacrylic acid homopolymer
Static testing was performed in accordance with the more advanced methodology described above that achieves
supersaturation by mixing brines together. The ionic composition of the supersaturated brine was split between two
brines,with all the NaCl in one brine (close to supersaturation) and the other ions (such as CaCl2 etc. in the second brine).
This procedure was designed to determine the efficiency of a product at inhibiting the formation of halite crystals under static
field conditions. These static tests gave an assessment of the ability of each product to inhibit both crystal growth and
nucleation and allow direct comparison of performance.
The synthetic brines were prepared by adding approximately 75% of the required salts and heating to 75°C for one hour. The
remaining salt was then added and the brine kept at temperature (although these brines should not be supersaturated, this
precaution was taken in order to completely avoid any seeding of salt crystals). The required amount of scale inihibitor was
injected neat into the NaCl only brine. The required amount of the counter ion brine was added and mixed well at
temperature. The tests were left to cool to 25°C and observed for 4 hours. Two blank samples containing just the test brines
and no inhibitor were included as a reference in every set of tests. The crystal amounts were determined through filtration and
drying and ranked against one another and an estimation of crystal size was made with respect to the blank tests.
6 SPE 164081
The results of static halite testing have been presented in Table 2 and a product ranking in Table 3. Product A provided
effective inhibition of halite formation at applied doses of 50 ppm and above with complete inhibition at 100 ppm. An
applied dose of 500 ppm, Product B provided inhibition of halite formation in the static test. The inhibitors, Product D,
NTAA, Product F, and potassium ferricyanide provided limited inhibition of halite and showed crystal modification
properties. They reduced the size of the formed crystals and at very high applied dose rates yielded approximately 50%
inhibition. Photographs of Product A performance have been placed into Figure 1 as an example of the test outputs.
Both cystal growth and nucleation inhibition functions were observed in tests with the majority of the candidate products.
Product A had a distinct chemistry to the other products evaluated and the excellent halite inhibition performance it
demonstrated suggested that it had a different mechanism of halite inhibition.
Dynamic testing was performed on Product A only in order to determine a more accurate MIC. The test method utilized three
pumps to introduce the following brines:
This kept continuity with the supersaturation methodology used for static evaluation. The brines were identical to that used
in static testing and were maintained at 75°C prior to introduction into the rig. The temperature of the oven was maintained at
25°C to provide the same cooling experienced by the static tests (albeit for a much shorter exposure time and more severe
than will be the case in the field). The pump rate was 3 mL.min-1 and the method basically adapted an industry standard
dynamic scale loop test, used for conventional scale inhibitor evaluation, with some minor modifications.
The results showed that 100 ppm of Product A prevented scale deposition in the coil and that a blank test gave a blocking
time of under 1 hour. This was considered to be a worst case scaling environment, driven by the severe cooling by operating
the oven at 25°C. The challenge in the laboratory testing was to keep the conditions as close to reality as possible while at the
same time ensuring conditions were harsh enough to induce scale formation in the test in a reasonable amount of time. At
oven temperatures higher than 25°C the scale formation occurred in the capilliary at times >6 hours and would not be
practicable for evaluation.
The volume of required wash water alone was not economic. There was no suitable nearby aquifer, nor any pipeline to import
water, therefore it would have to be trucked to the location for injection as diluent. This was very expensive when compared
to the reduction possible using scale inhibitor in fresh water as a carrier solvent. Product A was applied as a 10,000 ppm
concentrate in diluent water (due to the sizing of the injection system). This resulted in injection of 75 bbl.day-1 of injection
water dosed itself with 10,000 ppm of Product A. This represents injection of 250 ppm of neat Product A. While this is
greater than determined in the laboratory testing, due to the previous experiences of halite scale in this well a risk averse
approach was taken and overinjection acknowledged.
The well was brought online and injection of the halite inhibitor successfully kept the production tubing clean during the
EWT, which was able to get long, multi-choke setting and rate well test data. The cleanliness of the tubing was determined
from the stable flow rates of produced water, condensate and gas. Ultimately the data showed different results to those
initially gathered from the abandoned well test and the operator was able to successfully determine the future viability of this
asset.
Conclusions
A review of the literature yielded several different testing methods that have been previously used to evaluate halite
inhibitors. The most developed methods were used in this study to evaluate the suitability of candidate products for a field
EWT.
Product A (an alkyl naphthalene sulfonate) performed the best in both static and dynamic tests, compared to the previously
reported NTAA and potassium ferricyanide, as well as other industry available inhibitor chemistries.
Field application was successful in inhibiting the formation of halite scale despite the severe amounts predicted downhole,
mainly driven by the high gas rate, assumed dry gas production and rapid depressurization and temperature losses after the
fluids leave the reservoir.
Injection of the halite inhibitor saved significant potential cost from application of wash water alone, due to the remote nature
of the well. The successful treatment strategy allowed an accurate multi-rate well test which, in turn, provided the data
SPE 164081 7
necessary for the further economic evaluation and commercial decision making for the development of this marginal field.
Acknowledgments
The authors would like to thank the Society of Petroleum Engineers for the opportunity to present this work and to Clariant
Oil Services for allowing it to be published.
References
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8 SPE 164081
Sodium 89,000
Potassium 24,000
Magnesium 25,000
Calcium 45,000
Strontium 2,680
Barium 58
Iron 600
Bicarbonate 375
Sulfate 150
Chloride 259,000
pH 3.2
TDS 445,863
SG 1.312 g.cm-1
Large Crystals Large Crystals Large Crystals Large Crystals Hazy but no
Product B (0%) (0%) (0%) (92%) crystals
(100%)
Large Crystals Hazy but no Hazy but no Hazy but no Hazy but no
Product A (87%) crystals crystals crystals crystals
(100%) (100%) (100%) (100%)
Large Crystals Large Crystals Large Crystals Large Crystals Large Crystals
Product C
(0%) (0%) (0%) (00%) (22%)
Large Crystals Large Crystals Large Crystals Large Crystals Large Crystals
Product F
(0%) (0%) (0%) (0%) (42%)
Large Crystals Large Crystals Tiny Crystals Tiny Crystals Tiny Crystals
Product D
(0%) (0%) (0%) (23%) (40%)
Large Crystals Large Crystals Tiny Crystals Tiny Crystals Tiny Crystals
NTAA
(0%) (0%) (0%) (0%) (46%)
Large Crystals Large Crystals Large Crystals Large Crystals Large Crystals
Potassium Ferricyanide
(0%) (0%) (21%) (22%) (54%)
Large Crystals (0%)
BLANK
Large Crystals (0%)
BLANK
Product Rank
Product A 1
Product B 2
Product D =3
NTAA =3
Product F =3
Potassium Ferricyanide =3
SPE 164081 9
Dose Observation
Blank 1
50 ppm
100
ppm
200
ppm
500
ppm
1,000
ppm