SPE 81138
Improving Wellbore And Formation Cleaning Efficiencies With Environmental Solvents
And Pickling Solutions
James Curtis, SPE, and Leonard Kalfayan, SPE, BJ Services Company
Copyright 2003, Society of Petroleum Engineers Inc.
This paper was prepared for presentation at the SPE Latin American and Caribbean Petroleum
Engineering Conference held in Port-of-Spain, Trinidad, West Indies, 2730 April 2003.
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, as
presented, have not been reviewed by the Society of Petroleum Engineers and are subject to
correction by the author(s). The material, as presented, does not necessarily reflect any
position of the Society of Petroleum Engineers, its officers, or members. Papers presented at
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Abstract
The purpose of a chemical stimulation treatment, be it based
on acid, solvent, or other systems, is to remove formation
damage and increase productivity/injectivity, by restoring or
improving the reservoir permeability in the near-wellbore
region. A fundamental preliminary step in most successful
matrix stimulations is a tubing cleanout commonly referred to
as a pickling treatment. A tubing pickle is often necessary to
remove mill scale, rust and other iron deposits from the
tubular walls, in order to prevent their injection into the
reservoir with detrimental effects to permeability. The
pickling treatment also prevents the spending of the
subsequent chemical treatment; the creation and injection of
damaging precipitates; and the formation of iron-induced
sludge in the reservoir. Common pickling solutions include
corrosive hydrochloric or acetic acid. Additionally, the
pickling solution often contains a hazardous organic solvent
and surfactants to remove asphaltene or wax deposits and
damaging pipe dope residues.
Such hazardous pickling solution is reversed out of the
tubing and recovered at surface where it must be neutralized,
treated and properly disposed of. The surface handling of the
recovered pickling solution poses significant safety and
environmental hazards, due to its acidity and toxicity. A very
common hazard is the release of deadly hydrogen sulfide gas
in the return tank due to the reaction of the acid with iron
sulfide scale deposits in the tubing.
This paper discusses the use of a neutral pickling solution,
containing environmentally favorable derusting oxidizers,
surfactants and solvent solutions/dispersions, which also
prevent the liberation of hydrogen sulfide gas. This paper also
presents an analysis of the chemical mechanisms of this
solution, some treatment design guidelines, and its technical,
safety, environmental and economic benefits, compared to
conventional pickling solutions. An environmentally-
favorable solvent replacement for the conventional aromatic
solvent will also be discussed. Successful case histories in a
variety of environmental pickling and other applications will
be reviewed.
Purpose of Pickling Treatments
The use of pickling treatments has been well documented.
The many purposes and benefits of tubing pickles include iron
control, scale removal, sludge prevention, removal of
damaging pipe dope, asphaltene or paraffin deposits,
elimination of spent acid being injected into formation,
prevention of sulfur-species deposition, improvement in
stimulation treatment results, and reduction of overall
treatment cost.1 25
Surface tanks, treating lines, wellbore tubulars and coiled
tubing must be properly cleaned of damaging solids, carbonate
scales and other deposits prior to injecting acid into
formation.3,11 Circulation of pickling acids and solvents
through tubing removes these deposits, allowing them to be
reversed back to surface instead of being injected into the
formation. This is particularly important for gravel packed or
frac packed completions, which are sensitive to particulate
invasion and plugging by pipe dope.
Iron Control
Iron control is arguably the most important function of a
pickling treatment. Ferric iron is generally considered the
most problematic form. There is potential for creating
formation damage in any acid treatment due to the
precipitation of gelatinous ferric hydroxide, as the pH of the
spent acid rises above about 2.2.15,18,26 Ferrous hydroxide has
been reported to precipitate only above pH 7, so it is not
generally considered problematic.15 However, it has been
reported that ferrous hydroxide could precipitate from spent
acid/formation water mixtures at pH as low as 5 6.12
In sour wells, the reaction of mineral acid with the iron
sulfide scale present in tubulars will produce poisonous
hydrogen sulfide gas and ferrous iron. As the acid spends to a
pH above 1.9, the H2S subsequently reacts with the ferrous
iron to precipitate damaging elemental sulfur and iron
sulfide.9,20,21,25
Another significant challenge in acid stimulation is the
inducement of damaging asphaltic sludges by the
incompatibility of spent acid and certain formation crudes,
which can be exacerbated by the presence of ferric
iron.7,8,13,27,28 Both ferric and ferrous iron promote sludging,
2 IMPROVING WELLBORE AND FORMATION CLEANING EFFICIENCIES WITH ENVIRONMENTAL SOLVENTS AND PICKLING SOLUTIONS
but ferric iron is observed to cause a more severe sludging
tendency. Therefore, a key aspect of prevention of acid-
induced sludges is to focus on managing the ferric iron content
in the acid.
Numerous studies and field observations have identified
wellbore tubulars as the main source of ferric and ferrous
iron.2,3,617,1922,2425 There are three measures that can be
taken to manage this iron:
1) Perform tubing pickling procedures to eliminate or
reduce iron contamination in subsequent acid stages.
2) Adjust the acid type for example, replace the
hydrochloric acid with acetic acid or HV acid,29
which are less prone to sludging and have more
efficient iron chelating abilities.
3) Use elaborate iron control packages in the acid,
including sequestrants, chelating agents, and
reducing agents (that reduce ferric iron to the less-
problematic ferrous form).
Tubing pickling treatments offer the most cost-effective
method to manage iron. Iron control packages can be
incorporated in acidizing fluid formulations to control as much
as 40,000 ppm dissolved iron, however the cost increases
significantly with iron content (Figure 1). By performing a
tubing pickle, the iron concentration in the subsequent acid
fluid can be reduced to an economically manageable level
(Figure 2).14,19 In this way, the overall treatment cost can be
significantly reduced, and equally important, an improved
stimulation result can be achieved.
Acid Cost, per gallon
0 5,000 10,000
Ferric Iron Control, ppm
Figure 1 Cost of acidizing iron-control packages
The leading edge of acid treatments performed through
uncleaned tubing can result in iron concentrations in excess
of the capacity of even the most efficient iron control
packages. In the field, iron concentrations in spent acid
returns between 40,000 130,000 ppm have routinely been
reported.6,8,9,11,12,16,17,1921,30 The following hypothetical
calculations demonstrate how this can occur.
1) Workstrings. The amount of rust (ferric oxide)
accumulated inside 10,000 ft of untreated 2-7/8
tubing stored on surface racks for two or three
weeks can completely spend 100 gals of 15% HCl
acid. The leading edge of the acid would contain
approximately 86,000 ppm of ferric iron.
2) Old Production Tubing. A 1/64 deposit of iron
sulfide scale inside 10,000 ft of 2-7/8 tubing can
completely spend 1,490 gals of 15% HCl. The
SPE 81138
leading edge of the acid would contain
approximately 130,000 ppm of dissolved iron. As
the treatment acid spends to a pH above 1.9, the
excess iron will reprecipitate as 600 900 lbs of
iron sulfide per 1,000 gals of acid.
3) New Tubing. New tubing is often erroneously
considered to be clean. However, new tubing
contains a residue of mill scale, or magnetite (a form
of ferric/ferrous oxide), which is readily soluble in
acid. The mill scale contained inside 10,000 ft of
new 2-7/8 tubing will completely spend 690 gals of
15% HCl acid. The leading edge of the acid would
contain approximately 57,000 ppm of ferric iron and
29,000 ppm of ferrous iron. The excess ferric iron
will precipitate as ferric hydroxide gel in sweet
formations and cause approximately 100 150 lbs
of elemental sulfur per 1,000 gals of acid to
precipitate in sour formations.
The above calculations also demonstrate an additional
benefit of pickling treatments: the leading edge of the acid to
be injected into formation does not arrive on bottom already
spent. Without a tubing pickle, the acid fluids in formation
will be of lower strength than that designed and pumped at
surface. With the additional benefit of preventing damaging
precipitates and asphaltic sludges, tubing pickling treatments
have been observed to significantly improve acid stimulation
treatment effectiveness, as documented in numerous studies
and field results.6,8,20,21
Tubing Pickle Was Performed
Tubing Pickle Was Not Performed
15,000 20,000
Figure 2 Reduced iron content in main treatment acid
due to a prior tubing pickling treatment, from Suzuki.19
Acid Insoluble Deposits
Often the acid soluble scale, rust or mill scale is coated or
impregnated with hydrocarbon such as paraffin, asphaltene,
condensate and other oily deposits. Even injector wells can
suffer from deposition of suspended oil or compressor
lubricants that can cover the acid soluble deposits and act as a
SPE 81138 J. CURTIS AND L .KALFAYAN
diffusion barrier.23 In sour gas wells, the iron sulfide scale is
often oil-wet and may contain significant quantities of oil or
condensate residues.25
In many wells, there is a high probability of encountering
residues of thread sealant compound, also known as pipe dope,
on the inside of the tubing. Most thread compounds are
composed of a petroleum lubrication grease containing up to
60 wt% heavy metals, such as lead, copper, and zinc. Pipe
dope protects the thread from metal-to-metal contact and from
galling. It also improves the sealing performance of the
thread.31 Unfortunately, pipe dope also does an excellent job
in sealing (plugging) formations, perforations and gravel pack
completions, despite the continued efforts of completions
engineers to enforce best practices for pipe dope application at
the rig site.3,11,12 Mechanized dope applicators, as depicted in
Figure 3, have not found widespread application in the
industry, despite the multitude of evidence of the formation
damage and productivity impairment caused by over-zealous
thread sealant application.
Figure 3 Precise, uniform, mechanized pipe dope
applicator (photo courtesy BJ Tubular Services)
Cleaning of the aforementioned hydrocarbon deposits and
pipe dope residues with aromatic solvents, such as xylene and
toluene, or stable dispersions of the same in aqueous acid,
have been commonplace for decades.15 A simultaneous
cleanout can be achieved with a stable dispersion, as the
aromatic solvent external phase disperses or dissolves the
organic component of the tubing deposits, allowing the acid
internal phase to react with the scale, rust, or mill scale
compounds. Again, the solvent wash component of the tubing
pickle is a critical treatment step in a successful gravel pack or
frac pack completion, to prevent pipe dope plugging.
Typical Field Procedures
Pickling treatment procedures vary from company to
company, and even within companies. Some common
considerations and contradictory advice found in the literature
are reproduced below:
A pickling treatment of both tubing and annulus is
more effective than tubing only. If possible, the
pickling procedure should be done before the well
is perforated (to maximize contact time).6
Use 50 - 100 gals of solvent per 1,000 ft of tubing
(or 250 gals total) to facilitate removal of organic
materials, oily films or pipe dope. A common
alternative is to use a stable dispersion of solvent
in acid for simultaneous treatment.1,32
3
Use 100 gals of 10% or 15% HCl acid per 1,000 ft
of tubing. If the casing is also to be pickled, the
volume to use may need to be adjusted depending
on the extent of the iron scale present.32
Acid exposed to both the inside and outside of the
tubing, and also the inside of the casing, will
contact approximately four times the surface area
of the tubing alone. Acid pickle volumes should
be adjusted accordingly.17
Dilute or weak acids should be favoured.7
Use high concentration acid and circulate at the
highest possible rate.9
Perform pickling treatment such that at least 15
minutes of contact time is achieved.7
Circulate acid down tubing at 0.5 2.5 bpm.14,32
Reverse circulate out at 4 5 bpm.32
It is important to increase the residence time for
the acid to dissolve more corrosion products.23
Iron control chemicals are not required in the
pickle acid.24 However, if the potential exists that
the pickle acid could be lost to formation, then full
additives, including iron control should be
included.32
A sulfide scavenger should be added to pickle
acids in areas known to contain iron sulfide
corrosion.20,21,24
If the reservoir pressure is too low for circulation
or circulation is not otherwise possible, foam or
atomize the acid and displacement fluid.7
(Authors note: Alternatively, if available, activate
the gas lift system to flow back the pickle acid.)
Coiled tubing may reduce the amount of pickling
acid required 7 (Authors note: However, the both
the interior and exterior of the coiled tubing should
be pickled).
The returned pickle acid should be neutralized with
sodium bicarbonate or sodium hydroxide and
disposed of according to environmental
regulations.32
Challenges With Conventional Pickling Treatments
Some of the principal challenges involved with performing
acid pickling treatments, are the extreme safety and
environmental hazards posed by flowing live acid to the return
tank. Not only is the returned fluid extremely corrosive, but it
is also toxic and hazardous to the environment. The most toxic
components of pickling fluids may include the acid itself
(hydrochloric, acetic or formic), corrosion inhibitors (which
may contain thiourea, propargyl alcohol, methanol, acetylenic
alcohol, etc.), iron control agents (which may contain
nitrilotriacetic acid, thioglycol, cupric chloride, etc.), sulfide
scavengers (which may contain aldehyde, naphthalene, xylene,
methanol, ethylbenzene, etc.) and aromatic solvents such as
xylene, ethylbenzene or toluene.
In sour wells, the reaction of mineral acid and iron sulfide
scale will liberate deadly hydrogen sulfide gas. Even when
sulfide scavengers are used in the pickle acid, appropriate
safety precautions must be taken to ensure that toxic H2S gas
is not released into the atmosphere at the return tank and self-
4 IMPROVING WELLBORE AND FORMATION CLEANING EFFICIENCIES WITH ENVIRONMENTAL SOLVENTS AND PICKLING SOLUTIONS
contained breathing apparatus is available for properly-trained
personnel.33
Severe emulsion upsets can occur in surface treating
facilities when returned acids are flowed to the plant.3437 As
the returned acid commingles with other produced fluids and
the pH begins to increase, emulsions begin to form and fine
solids can precipitate which act to stabilize the emulsions.
These emulsions can be hard to break. In some cases, the
degree of emulsion decreases upon neutralization of the acid;
however, in others the tendency actually develops upon
neutralization.37
Alternatives to Acid Pickling
In wells with crude oils that are extremely sensitive to acid-
induced sludging, hydraulic fracture stimulation with proppant
may be a viable alternative to matrix or acid fracturing
stimulation.7 Such a procedure might preclude the need for an
acid pickling step.
Recent improvements in erosion-resistant internally
coated completion workstring technology provided technical
and economic success for a frac pack campaign in the Gulf of
Mexico. The coating eliminated the need for acid pickle
treatments prior to the frac packs, due to the minimization of
internal pipe rust. Savings were achieved by eliminating the
cost to purchase, transport and dispose of pickle acid. This
was in addition to the elimination of safety, environmental and
liability risks associated with handling and disposing of the
returned pickle acid.38 This method does not specifically
address the issue of pipe dope residues.
Highly sequestered rust removal solutions were
envisioned by Delorey and Taylor7 in cases where the pickle
acid cannot be reverse circulated back to surface. The
sequestered solution would be allowed to feed into the
formation, but would not cause iron precipitation problems.
This provides a convenient introduction for the novel neutral
pH pickling solution presented in this paper.
Rust Conversion and Phosphate Coating
Phosphating is the process for the production of a phosphate
coating on steel articles by immersion in an aqueous solution
of metal ions and phosphate. The metal surface is converted
to an insoluble crystalline phosphate protective coating that
can be utilized to prevent corrosion, to serve as a base for
paint, to resist wear and to facilitate the deep drawing of
metals.39
A wide variety of water or solvent-based conversion
coatings, also known as rust converters, are commercially
available. These products react directly with rusted surfaces
to form inert organometallic complexes. They can generally
be classified as products that impregnate rust, convert rust to
magnetite, inactivate soluble salts or convert iron oxides to
other products.40,41 They are generally applied by brushing,
spraying or prolonged immersion.
Steel surfaces treated with phosphate coatings generally
take on a silvery or gun-metal appearance, as commonly seen
on rifles, shotguns, revolvers, buttons, screws, pen points,
buckles, pins, saw teeth, bicycle chain links and typewriter
parts. Commercial, multi-step processes that fall into this
general category include Parkerizing, Bonderizing, and
Coslettizing.39
SPE 81138
Novel Pickling Solution Development
A novel, near-neutral pH derusting, passivating and pickling
solution (hereafter referred to as neutral deruster) was
developed, based on iron phosphate coating technology, to
address the challenges associated with acid pickling. The
neutral deruster offers advantages in terms of safety and
simplicity of operations, when compared to acid pickling
fluids. The deruster solution has a mild pH and thus requires
minimal safety handling and disposal precautions, and is less
likely to cause process facility upsets.
The neutral deruster is an environmentally favorable
formulation capable of deoxidizing a wide variety of metals
through its chelating action. It contains a phosphonate source
in acidic form, buffering agents, and a catalyst to speed up the
reaction at low temperature. The novelty of this system is that
passivation is accomplished in a single step, compared to the 3
to 5-step commercial processes.
Although the process is based on iron phosphating, the
solution itself does not contain any iron. The iron source is
provided by the tubular substrate. In addition to maintaining a
mild pH, the buffers also act to transform the excess iron into
microscopic iron carbonate, which is easily maintained in
suspension due to its small size (the particles typically pass
through a 2.5 micron filter paper). As the neutral deruster
solution de-oxidizes and passivates the metal surface, the fluid
takes on a black appearance, due to the suspended iron
carbonate particles.
The neutral deruster reacts with rust, mill scale and the
steel substrate itself, producing a protective phosphate film
that coats the metal and helps to provide longer-term corrosion
protection through a passivity mechanism. This corrosion
protection will last for several days or weeks. Depending on
treatment variables, a gunmetal silvery or dark gray surface
surface is formed.
The derusting concentrate is supplied as a liquid additive
and is diluted to a concentration of 6 12% by volume. At
these concentrations, there is no need to add additional
surfactants or clay control additives. Solvents and/or non-
emulsifiers may be required, depending on the type of crude
oil to be encountered.
The phosphonic acid component is also a competent
calcium-sequestering agent in the presence of iron, removing
scales and other carbonates particles. In wellbores that
contain carbonate scales, the neutral deruster yields a similar
performance to ethylenediamine tetraacetic acid (EDTA) and
nitrilotriacetic acid (NTA).
The speed of reaction and the quantity of iron that can be
sequestered are dependent on the deruster concentration and
temperature. Most formulations are stable with up to
12,000 ppm of ferric iron in solution.
At ambient temperature, the neutral deruster quickly
removes rust from metals through chemical action and by
loosening deposits that slough off the surface. Laboratory
testing has suggested that by attacking the rust at the substrate
interface, it is generally possible to remove all of the deposit
through a combination of chemical dissolution and sloughing.
Sloughing occurs when the underlying rust is dissolved,
allowing surface flakes to detach without complete
dissolution.
SPE 81138 J. CURTIS AND L .KALFAYAN
Iron sulfides are not chemically reactive with the neutral
deruster. Consequently, there will be no H2S evolution, in
contrast with conventional acid pickling treatments an
important safety advantage. However, the iron sulfide
deposit can still be effectively removed by the sloughing
mechanism, taking advantage of the layered structure of
typical iron sulfide scales, as described in more detail below.
Several investigators have studied the composition and
physical characteristics of iron sulfide scales. For gas wells,
the scale is often loose and porous, while in water wells the
scale may be more dense and adherent to the tubing wall.42
Iron sulfide scale is heterogeneous, commonly containing iron
carbonate, iron oxides, and mixed iron sulfide mineral forms
(troilite, mackinawite, pyrrhotite and pyrite listed in order
of acid solubility). 20,21,22,25,43 In one study, the layer next to the
flow stream was found to be iron sulfide and the layer closest
to the pipe wall was iron chloride.22 This layered structure
allows the neutral deruster to loosen the iron sulfide deposit at
the substrate, permitting it to be removed from the tubing by
sloughing and mechanical agitation from fluid flow.
Alternative Solvents
Governmental regulations regarding the usage, disposal
and volatile-emission limits of aromatic solvents, such as
xylene and toluene, are becoming increasingly restrictive. The
flammability, acute toxicity and environmental contamination
concerns have made their use less attractive.44
In many countries in Central and South America,
regulations exist to monitor, control and restrict the
production, manufacture, preparation, transformation, storage,
importation, exportation, marketing, transportation or other
types of transactions involving certain chemical substances
that are also used in the illicit production, manufacture,
preparation, or extraction of narcotic drugs and psychotropic
substances.45 Both xylene and toluene are typically on this list
of controlled substances, greatly complicating their usage in
oilfield applications in these countries.
It is evident that the replacement of aromatic solvents in
the oilfield is both logistically and operationally efficient as
well as socially and environmentally responsible.
Alternative solvents that have been investigated include
aromatic distillates, Stoddard solvent (dry cleaning solution),
natural extracts, hydrolysable aprotic halogenated organic
solvents, thiocarbamates, aliphatic and cyclic amines, non-
aromatic and aromatic napthas, proprietary non-aromatic
alkenes, and esthers.46,47 Some promising results were
obtained, however none of these alternatives has found
widespread use.
Terpenes are defined as a group of unsaturated aliphatic
cyclic hydrocarbons that, unlike petroleum distillates, are a
renewable resource derived from plant products such as
orange peels and the resinous sap of pine trees. They are
widespread in nature, found mainly in coniferous plants as
constituents of essential oils. Terpenes are composed of
isoprene units, usually having 5n carbon atoms and the
molecular formula (C5H8)n, where n is the number of isoprene
units.
Common terpenes include d-limonene (orange oil), alpha
and beta pinene (Pine Sol), turpentine, carotene, camphor
oil, citronella, nepetalactone (catnip) and menthol (from
5
peppermint oil). They have been used by many industries in
several applications, including fragrances, flavors, food
additives, toothpaste, insecticides and, in the last few years
due to the banning of new production of chlorofluorocarbons
(CFCs) and trichloroethane as powerful cleaning and solvent
solutions.48
Terpenes have high solvency, compared to aromatic and
chlorinated solvents, however they are rapidly biodegradable,
less toxic and less flammable.44,48,49 When used, either alone
or in combination with other solvents and surfactants, terpenes
are excellent substitutes for the aromatics in a wide variety of
oilfield applications, including tubing pickling.50
By combining selected terpenes with an appropriate
surfactant package, an environmentally favorable dispersion
can be prepared in the neutral deruster pickling solution
(hereafter referred to as neutral terpene deruster). This
neutral terpene deruster solution therefore serves to
simultaneously remove iron scale, rust, mill scale, organic
hydrocarbon deposits and pipe dope in a single operation.
Laboratory Evaluations
The objectives of the laboratory testing were to:
1) Evaluate the rust removal performance on coil
tubing pipe coupons, comparing 15% HCl acid and
the neutral deruster pickling solution.
2) Evaluate the use of the neutral deruster for
preventing rust from reforming on tubing after its
initial removal.
3) Evaluate the efficiency of the neutral terpene
deruster and also of HCl acid containing the
terpene/surfactant package for simultaneously de-
rusting and cleaning rusty metal coupons covered
with pipe dope.
Evaluation of Rust Removal Performance
Heavily rusted pieces of coiled tubing were utilized in the de-
rusting tests. The weights and dimensions of each coiled
tubing coupon were measured before testing. Pictures were
also taken of the original rusted coupons and tested fluids for a
before/after comparison.
The test solutions (400 ml) were heated to 140 F on a hot
plate and were stirred with a magnetic stir bar on equal stirring
speeds for the de-rusting tests. After the test solutions came to
temperature, each corresponding coupon was suspended in the
solution by Teflon lines from a glass rod resting on top of the
solution glass jar. The coiled tubing coupons were allowed to
react in the solutions for one hour at 140 F with constant
stirring. After the one-hour reaction time, the coupons were
removed from the test solutions, dipped in distilled water, and
allowed to air dry. The coupons were then weighed and the
physical characteristics were recorded.
Initial and final pH values were measured with a digital
pH probe. Total suspended solids (T.S.S.) tests were
conducted by filtering a homogenous 100 ml sample of the
pickling solution through a pre-weighed 2.5 micron filter
paper, drying the collected solids, determining the solids
weight, and calculating the T.S.S. content. The initial and the
final weights of the coiled tubing coupons were used to
determine the percent weight loss of each coupon. Filtered
6 IMPROVING WELLBORE AND FORMATION CLEANING EFFICIENCIES WITH ENVIRONMENTAL SOLVENTS AND PICKLING SOLUTIONS SPE 81138

and unfiltered samples of the pickling solutions were analyzed

by the direct current plasma technique to determine the total
iron content and total soluble iron concentrations.
These measurements are indicative of each pickling
fluids iron removal efficiency and de-rusting capabilities, as
shown in Table 1 and Figures 4 6. The neutral deruster
solutions showed equal or better iron removal efficiency
compared to HCl acid, and caused less weight loss.
HCl Before HCl After Deruster Before Deruster After

Figure 6 Comparison of HCl and neutral deruster

Coupon Total Iron
Pickling % Weight Initial / Final T.S.S. Unfiltered / Filtered solutions before and after pickling. (Note the black color
Fluid* Loss pH (mg/l) (mg/l) of deruster due to suspended microscopic iron carbonate
A 2.43 % -0.44 / -0.45 91 2,796 / 2,359 particles).
B 1.55 % 6.06 / 6.91 69 1,995 / 1,832
C 2.24 % 6.02 / 6.46 97 3,088 / 3,017 Evaluation of Rust Prevention
D 2.07 % 6.03 / 6.31 83 2,897 / 2,657 Laboratory evaluations were performed on coupons from a
*A: 15 wt% HCl acid + 2 gpt nonionic surfactant + 1 gpt corrosion inhibitor high pressure workstring, used exclusively for hydraulic
B: 5 vol% neutral deruster in fresh water
C: 12 vol% neutral deruster in fresh water fracture treatments in Colombia, to determine the
D: 12 vol% neutral deruster in fresh water + 1 gpt corrosion inhibitor effectiveness of the protective phosphate coating in preventing
rust from reforming on the surface of the tubing. Eight
Table 1 Comparison of HCl acid and neutral deruster coupons from the 4-1/2 Q125 grade tubing were analyzed as
iron removal and derusting efficiency follows:
Two coupons were left exposed to atmospheric
storage conditions, without receiving any treatment.
The remaining six coupons were soaked in a 2 wt%
KCl brine (with 2 gpt nonionic non-emulsifier and
2 gpt nonionic low-tension surfactant) for two hours
at 180 F to simulate wellbore conditions during a
workover. Two of these brine-soaked coupons were
then left exposed to atmospheric storage conditions
without receiving additional treatment.
Two of the brine-soaked coupons were subsequently
Before After immersed in a 7.5 wt% HCl pickling solution for
30 minutes at 180 F, while manually agitating the
Figure 4 Coiled tubing coupon pickled with 15 wt% container for 30-second intervals every 10 minutes.
HCl acid + 2 gpt nonionic surfactant + 1 gpt corrosion These coupons were subsequently left exposed to
inhibitor atmospheric storage conditions, without receiving
any additional treatment.
The remaining two brine-soaked coupons were
subsequently immersed in a 6 vol% neutral deruster
pickling solution for 30 minutes at 180 F, while
manually agitating the container for 30-second
intervals every 10 minutes. These coupons were
subsequently left exposed to atmospheric storage
conditions, without receiving any additional
treatment.

Before After In each case, photographs were taken of the coupons to

Figure 5 - Coiled tubing coupon pickled with 12 vol%
neutral deruster in fresh water. (Note silvery finish from
phosphate coating).
compare before/after conditions. The results indicated that
after as little as one week, the only coupons that did not
experience any renewed rusting were the two samples treated
with the neutral deruster, as shown in Figures 7 9.
Based on these results, it is planned to clean and protect
this workstring from corrosion damage, by circulating and
soaking the neutral deruster solution before pulling the tubing
out of well and storing it at surface between subsequent
hydraulic fracture treatments.
SPE 81138 J. CURTIS AND L .KALFAYAN 7

After the coupons were dry, the coupons were weighed

2 wt% 2 wt% KCl 2 wt% KCl and the physical characteristics were recorded. The initial and
KCl only followed by followed by 6 vol% final weights of the L80 coupons were utilized to determine
7.5 wt% HCl neutral deruster the percent weight loss of the coupons. Visual observations
No Treatment were noted, and photos of the coupons were also taken. This
data indicates the pipe dope cleaning and rust removal
efficiency.
The results, as shown in Table 2 and Figures 10 and 11,
clearly indicate that effective pipe dope cleaning cannot be
obtained by either HCl acid or the neutral deruster in the
absence of a solvent phase. Furthermore, the rust removal
Figure 7 Q125 coupons immediately after soaking in efficiency is severely diminished in the absence of solvent
brine and pickling solutions. Although difficult to because the metal surface is left oil-wet (coated with dope).
distinguish in this photo, the coupon pickled with neutral The addition of the terpene/surfactant package to HCl acid
deruster took on a silvery-black appearance, due to the improved its cleaning efficiency significantly, but rust was
protective phosphate coating. still observed in two cases, and an oil-wet surface was
maintained in the third case.
In all cases, the neutral terpene deruster yielded perfect
cleaning of pipe dope and complete rust removal, leaving the
metal in a (desirable) water-wet condition.

Pipe Dope
Pickling Pipe Removed Visual
Fluid* Dope** (% by wt.) Observations
F1 D1 98.3 Pipe dope and rust present.
F1 D2 87.6 Oil wet surface with pipe dope present.
F1 D3 88.0 Rust and pipe dope still present.
F2 D1 99.7 Oil wet surface with pipe dope present.
F2 D2 100 No pipe dope but rust remains on surface.
Figure 8 Q125 coupons after 7 days storage in F2 D3 100 No pipe dope but rust remains on surface.

atmospheric conditions. All coupons show renewed F3 D1 96.5 Oil wet surface with pipe dope and rust.
F3 D2 no data Rust and pipe dope still present.
rusting, except those treated with the neutral deruster. F3 D3 43.1 Oil wet surface with pipe dope present.
F4 D1 100 Water wet surface. No pipe dope or rust.
F4 D2 100 Water wet surface. No pipe dope or rust.
F4 D3 100 Water wet surface. No pipe dope or rust.

* F1: 15 wt% HCl acid + 2 gpt nonionic surfactant + 1 gpt corrosion inhibitor
F2: 15 wt% HCl acid + 2 gpt nonionic surfactant + 1 gpt corrosion inhibitor
+ 25 vol% terpene/surfactant package
F3: 12 vol% neutral deruster in fresh water + 1 gpt corrosion inhibitor
F4: 12 vol% neutral deruster in fresh water + 1 gpt corrosion inhibitor
+ 25 vol% terpene/surfactant package

** D1: Bestolife 2000 pipe dope

D2: Bestolife PTC pipe dope
D3: Shell High Pressure Modified Thread pipe dope
Figure 9 Q125 coupons after 30 days storage in
atmospheric conditions. All coupons show significant Table 2 Comparison of pipe dope cleaning and rust
rusting, except those treated with the neutral deruster. removal efficiencies of HCl and neutral deruster with and
Evaluation of Pipe Dope Cleaning Efficiency without terpene/surfactant package.
Three different types of commercially available pipe dope
were analyzed with heavily rusted L80 metal coupons to
compare HCl and the neutral deruster, with and without the
terpene/surfactant package.
The test fluids were heated to 140 F on a hot plate and
stirred with magnetic stir bars at equal stirring rates during the
pipe dope removal tests. After the test solutions came to
temperature, each corresponding coupon was suspended in the
solution by Teflon lines from a glass rod resting on top of the Figure 10 Poor cleaning efficiency of coupons coated
solution glass jar. The L80 coupons were allowed to react in with pipe dope and treated with pickling fluids without
the solutions for one hour at 140 F with constant stirring, any solvent phase.
after which the coupons were removed from the test solutions
and allowed to air dry overnight.
8 IMPROVING WELLBORE AND FORMATION CLEANING EFFICIENCIES WITH ENVIRONMENTAL SOLVENTS AND PICKLING SOLUTIONS
Figure 11 Cleaning efficiency of coupons coated with
pipe dope and treated with pickling fluids containing
terpene solvent. The neutral terpene deruster achieved
100% cleaning efficiency.
Case Histories
The neutral terpene deruster was developed in Brazil and
introduced to the South American market in 2002. A total of
56 pickling treatments with the neutral deruster were
performed in 2002, mostly in Bolivia and Peru, with several
jobs in each of Brazil, Venezuela, Trinidad and Ecuador. To
date in 2003, at the time of writing, 30 additional jobs had
been performed in Bolivia, Brazil, Colombia, Ecuador, Peru
and Trinidad. Most of the tubing pickles were performed prior
to acidizing treatments. A lesser amount was performed prior
to gravel packing operations. One job was performed to
protect a workstring from surface corrosion, as described in
the laboratory section.
Most pickling treatments were performed with the neutral
deruster/terpene combination; however, in some cases only the
neutral deruster was used. The most common concentration
has been 12 vol%, due to low tubing temperatures. Generally,
50 100 gals per 1,000 ft of tubing have been employed.
In order to maximize contact time, the pickling solution
has usually been circulated down the tubing at the slowest
possible rate, typically 0.5 0.75 bpm, and reverse circulated
as slow as practical to complete the job in a reasonable time.
Damaging precipitates and sludges have been prevented in all
cases.
Due to its environmental, legislative and performance
benefits, the neutral terpene deruster has completely replaced
conventional acid pickles in some countries (Bolivia for
example), even prior to acid and gravel pack treatments
performed by other service providers. Some of the more
interesting jobs are highlighted below:
New Tubing Bolivia
As part of the completion procedure of new wells, the operator
was installing new tubing and subsequently performing matrix
acid stimulation treatments. The operator considered a tubing
pickle to be an unnecessary step in the acid treatment. It was
erroneously believed that the new tubing was clean, as it had
recently arrived from the supplier (an opinion that
unfortunately continues to be quite prevalent in the industry).
After much discussion and debate regarding the detrimental
effects of mill scale deposits in the new tubing, the operator
reluctantly agreed to perform a field trial.
A neutral terpene deruster pickling treatment was
performed as part of the next acid job procedure. The pickle
returns were anxiously monitored. Unfortunately, iron content
was not measured however, the returned pickle fluid showed
the characteristic jet-black color, due to the suspended iron
carbonate particles, pipe dope and other tubular residues.
SPE 81138
When the completion engineer observed the dirty
conditions of the returned pickle fluid, he was so convinced
that he immediately implemented mandatory neutral terpene
deruster pickling treatments on all acid and gravel pack
treatments in this area.
Gas Lift Wells Peru
These acid treatments are performed rig-less. Circulation is
not possible. The tubing pickles are performed by displacing
5 bbls of neutral terpene deruster to the gas-lift valve and
allowing it to soak for 30 minutes. The gas lift system is then
activated to recover the pickling fluid to surface. A dummy is
installed, and the acid treatment is performed by bullheading.
Iron Sulfide Scale Bolivia
An operator was performing matrix acid stimulation
treatments with another service provider in gas wells
containing iron sulfide scale deposits in the tubing. The other
service provider was performing tubing pickles with
10 wt% HCl acid. A serious safety hazard occurred during the
reverse circulation of the spent pickle acid to the return tank.
The acid had reacted with iron sulfide deposits, liberating
deadly hydrogen sulfide gas. Measurements taken at the
return tank indicated an atmospheric H2S concentration of
440 ppm, which is considered to be immediately dangerous to
life and health. At concentrations above 300 ppm, the ability
to perceive the rotten egg odor of H2S is lost. A short
exposure of 15 20 minutes and can lead to an inhalation of a
fatal dose or the complete loss of consciousness.51
The neutral terpene deruster pickling fluid was offered to
the other service provider for use in their next job performed
in this field. The pickle was performed successfully and
safely. A maximum atmospheric H2S concentration of only
8 ppm was measured, less than the time weighted average
(TWA) exposure limit defined by OSHA.51 The acid
stimulation was successful.
This operator has now implemented the neutral terpene
deruster pickling fluid as a standard practice, regardless of
which service provider performs the acid stimulation
treatment.
Fishing Operation - Peru
A fish was lost in this well in 1974. It was subsequently
shut in from 1974 until 1994, when the operator tried to
reactivate the well, doing a pressure test. The tool could not
be lowered past 530 ft, where a 2 3/8 tubing fish was
encountered.
The well was left shut in until January 1996, when an
unsuccessful attempt was made to retrieve the fish. The well
could not be activated. In April 1996, a second unsuccessful
fishing attempt was made, this time pumping two 250-gal
batches of 7.5 wt% HCl acid.
In November 1996, a third fishing attempt was made,
pumping 150 gal of 15 wt% HCl acid and recovering 100 ft of
swabbing cable but the top of fish was left at 2,016 ft.
In December 1996, 350 gal of 7.5 wt% HCl acid was
again pumped, but the top of fish was left at 2,135 ft (inside
the slotted liner). An additional attempt was made at that time
to recover the 5 liner using a packer and explosives, without
success.
SPE 81138 J. CURTIS AND L .KALFAYAN
The well was left shut in from March 1997 to January
2002, at which time another fishing job was planned. It was
concluded that the fish could have been stuck due to a
combination of the following factors:
Ferric oxides in previous attempts, saline
formation water and HCl acid were used.
Silts and formation fines the well has a slotted
liner in open hole.
Organic depositions produced oil is 19 API.
Carbonate scales from formation water.
This time, neutral terpene deruster was displaced into the
hole over the fish, and left to soak for 20 days while waiting
for the workover rig to arrive.
The top of fish was found at 2,161 ft. The rig circulated
completion fluid over the fish and recovered a dark black fluid
(reacted neutral terpene deruster) with traces of fines. A dump
bailer run was performed, recovering pieces of rock, rubber
and sand. The top of fish was washed over with a wash shoe
to 2,190 ft, obtaining frac sand, pieces of iron and carbonates.
On the second day, the tubing was cut at 2,180 ft, and 20
ft of 2-3/8 tubing and swabbing cable was recovered. Then
another 16 ft of fish was recovered at the end of the day,
consisting of 8.5 ft of tubing and 7.5 ft of harpoon tool.
On the third day, pieces of iron and cables were recovered
using a magnet. Finally, the top of fish was hooked up and
tensioned to 85,000 lbs. It was decided to simply push it
down, leaving the top of fish at 2,331 ft, below the pay zone at
2,180 2,300 ft. See Figure 12.
Figure 12 Some of the iron junk and debris that was
unstuck by the deoxidizing and cleaning effect of the
neutral terpene deruster.
The neutral terpene deruster was successful in freeing this
fish, while several previous attempts with HCl acid were
unsuccessful. The well was subsequently returned to
production and is under evaluation for possible acid
stimulation.
9
Conclusions
1. Tubing pickling is fundamental to achieving
successful acid stimulation and gravel packing
treatments.
2. The neutral deruster is a more effective, more
economical, safer and environmentally favorable
replacement for acid pickling fluids.
3. A terpene/surfactant package can eliminate the need
for hazardous, toxic aromatic solvents, such as xylene
and toluene.
4. The terpene/surfactant blend is easily dispersible in the
neutral deruster or other aqueous fluids for
simultaneous removal of organic hydrocarbons, pipe
dope, inorganic scale, rust and mill scale.
5. Workstrings can be effectively and economically
protected from surface corrosion during storage by
treating them with the neutral deruster before pulling
out of hole.
6. The neutral terpene deruster can assist in recovering
stuck fish, particularly in old wells.
Acknowledgments
The authors thank BJ Services for permission to publish this
paper. Special thanks go to the laboratory and engineering
staff throughout the Latin America Region for their diligent
effort in the field-implementation of this new technology, to
Sandy Berry and Rubn Castillo for performing much of the
laboratory testing presented here, and to Gino Di Lullo for his
vision, development, technical support and encouragement.
Nomenclature
bpm = pump rate, barrels per minute
gpt = liquid additive concentration, gallons of additive
per 1,000 gallons of solution
OSHA = Occupational Safety and Health Administration,
U.S. Department of Labor
ppm = concentration, parts per million parts
wt% = concentration, percentage by weight of solution
vol% = concentration, percentage by volume of solution
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SI Metric Conversion Factors

API 141.5/(131.5 + API) = g/cm3
bbl % 1.589 874 E 01 = m3
ft % 3.048* E 01 = m
F (F 32)/1.8 = C
gal % 3.785 412 E 03 = m3
inch % 2.54* E + 01 = mm
lbm % 4.535 924 E 01 = kg
* Conversion factor is exact.