SPE 95004
Tube Pickling Procedures: Case Studies
S.H. Al-Mutairi, SPE, and H.A. Nasr-El-Din, SPE, Saudi Aramco
Copyright 2005, Society of Petroleum Engineers
This paper was prepared for presentation at the SPE European Formation Damage
Conference held in Scheveningen, The Netherlands, 25-27 May 2005.
This paper was selected for presentation by an SPE Program Committee following review of
information contained in a proposal 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
SPE meetings are subject to publication review by Editorial Committees of the Society of
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Abstract
Tubing pickle treatments can eliminate formation damage that
is caused by introducing millscale, pipe dope and other tubular
contaminants into the formation. Two of acid pumping
techniques implemented to perform the pickling treatments are
bullheading and coiled tubing. In the bullheading method, the
acid is pumped down the tubing, then the spent acid is lifted to
the surface using reservoir pressure. Coiled tubing is another
method where the acid is pumped down the coiled tubing, and
flowed up through the tubing/coiled tubing annulus.
This paper examines the advantages and disadvantages of
the two commonly used techniques for tubing pickling:
bullheading and coiled tubing. The efficiency of each method
is analyzed based on extensive analysis of field samples. In
addition, the paper also addresses the effects of acid volume,
concentration, and pumping flowrate on the efficiency of
removing mill scale from the wellbore.
Field data indicated that tubing pickle is a must. Extremely
high levels of total iron (up to 105,000 mg/l) were noted in the
spent acid. The relationship between dissolved iron and acid
concentration profile depended on the mode of acid pumping.
In the case of bullheading, the iron peak coincides with the tail
of the acid peak, whereas it coincided with the leading edge in
the case of coiled tubing.
Introduction
Tubing pickle is the process of removing mill scale, pipe dope,
debris and other contaminants from the well tubulars using
acids and/or other solvents without permitting the entrance of
these fluids into the formation.1-8 The process can be
considered as flow in a tube or annulus with heterogeneous
chemical reactions occurring at the wall of the tube.9,10
From well stimulation point of view, the purpose of the
tubing pickle treatment is to clean the production tubing from
any damaging material prior to conducting the main
stimulation treatment. If not removed or bypassed, these
materials can enter the formation and can cause severe
damage.
There are several methods to perform tubing pickle
treatments, Fig. 1. Application of a certain method depends on
well characteristics and the economics of the job. If the well is
cased and not yet perforated, the treatment can be circulated
through the tubing/casing annulus, circulated through the drill
pipe if available, or using coiled tubing. In the coiled tubing
case the fluids are pumped through the coiled tubing to the
bottom of the tubing then circulated to the surface through the
coiled tubing – tubing annulus. On the other hand, if the well
is perforated the pickling fluids can be bullheaded through the
tubing and the reservoir pressure can be utilized to lift the
spent acid to the surface. However, coiled tubing and
circulation through the annulus can be used in a perforated
well provided that fluids donot enter the formation.
A common practice that is utilized in tubing pickling
treatments is to use hydrochloric acid at concentrations up to
20 wt%.7 The major concern with using higher HCl
concentrations is protecting the integrity of well tubulars. Both
the corrosion inhibitor loading and cost of the job increase
with increasing acid concentration.
The choice of pickling fluids is determined based on the
type of the steel in the well. Low-carbon steels such as L-80
and C-95 can sustain HCl acid with concentrations up to 20
wt% with proper corrosion inhibition. On the other hand,
Super Cr-13 is vulnerable to corrosion in acidic environments
and needs not to be exposed to HCl at all. In such cases, a new
class of nearly neutral and environment friendly chemicals
was introduced.11,12
Several acid additives are included in the treatment
formulation to serve different functions. Corrosion inhibitors
and corrosion inhibitor intensifiers are used to protect the base
metal. In addition, water-wetting agents are used to enhance
acid scale contact. A slug that contained an organic solvent is
used ahead of the acid to remove pipe dope and other oily
materials.7 A gel spacer is used to separate the different fluid
stages of the treatment. It also works as displacement fluid and
can be used a head of the pickling fluids in the case of
perforated wells. Hydrogen sulfide scavenger and iron control
agents are included only if the well is perforated. Tables 1
and 2 give acid formulation used to pickle well tubulars by
bullheading and coiled tubing methods, respectively. More
details on the acid formulation were given by Nasr-El-Din et
al.7
Recently, Al-Mutairi et al. describe acid pickling
treatments using bullheading and coiled tubing.10,13 The
objective of the present paper is to compare these two methods
2 SPE 95004
of conducting pickling treatments. A second objective is to
determine which method is the most effective.
Description of Pickling Methods
For cased and unperforated wells, the pickling treatments can
be circulated through the tubing/casing annulus or circulated
through the drill pipe if available. The other two methods of
performing tubing pickle treatments are bullheading and using
coiled tubing. Below is a brief description for each method.
Bullheading Method
Bullheading the acid is considered the economical choice
when compared with using coiled tubing. In the bullheading
case, the reservoir pressure is utilized to lift the spent acid
during the flowback stage. It requires the well to be
perforated. The pickling fluids are bullheaded through the
tubing and the fluids that originally were in the well before the
pickling are displaced inside the reservoir. Then, pumping is
stopped and then the well is open to flow. The path for the
pickling fluids during pumping and flowback is the same. In
this way, the acid contacts the tubing two times.
Some technical difficulties are associated with using this
method. First, the job should be designed so that pumping is
stopped when the acid is at a save distance above the
perforations. Usually, acid pumping is stopped when it is
nearly 50 ft above the upper set of the perforations. Entrance
of pickling fluids into the formation will cause severe
formation damage. Second, operators have to deal with high
formation pressures that have direct communication with the
wellbore. Third, a gel spacer should be used to separate the
produced gases and spent acid. Fourth, wells with high H2S
content can cause serious problems for both the operation and
the workers. H2S scavengers must be considered in designing
the recipe of the pickling fluids. Finally, this method requires
sufficient reservoir pressure to lift the spent acid to the
surface.
Coiled Tubing Method
Coiled tubing is the costly option of conducting pickling
treatments. The first step is to run the coiled tubing in the hole
until it is a few feet off the bottom of the well. The pickling
fluids, then, are pumped down through the coiled tubing and
circulated up to the surface through the coiled tubing – tubing
annulus.
Several shortcomings are encountered with using the
coiled tubing method. First, coiled tubing has a smaller
diameter which will limit the acid pumping rate. Second, the
tight clearance between well tubulars (tubing or liner) and the
coiled tubing can limit flowrate and restrict transportation of
the acid that is loaded with reaction products. Third, the acid
contacts the outer surface of the coiled tubing when the acid
flows out of the well. This additional surface area consumes a
certain amount of acid that should be accounted for.
Unfortunately, there is no accurate method to estimate this
requirement. Fourth, when using coiled tubing for pickling a
perforated well there must be no communication between the
formation and the wellbore.
One main difference between bullheading and using the
coiled tubing method is that acid contacts the tubing and the
liner two times in the bullheading case; whereas it contacts the
tubing and the liner only once in the coiled tubing case. The
effect of the method on the contact time is discussed later in
the paper.
Flowback Profiles – Case Studies
Bullheading Method
The first case involved well A, a cased and perforated well
that has been pickled by bullheading 4,520 gals of nearly 15
wt% HCl, Table 3. The well is completed with 12,217 ft of
4.5-inch diameter C-95 tubing, and 571 ft of 7-inch diameter
L-80 liner. When the acid is bullheaded, the leading edge of
the acid (acid front) contacts the tubing first. Therefore, mill
scale is removed during the reaction with the early flow of
acid. The live acid that comes later is in excess and does not
find a scale to react with until the acid advances to unreacted
scale down the tubing. The live acid is inhibited with
corrosion inhibitors, which prevent or at least reduce the
dissolution of well tubulars. Thus, in its way up the inhibited
acid has very negligible reaction with the base metal. Because
the acid returns through the same bath during well flowback,
the tail of the acid (i.e., last acid pumped) is produced first.
Figure 2 shows the pH, Cl and Ca concentrations as a
function of flowback time. The pH was nearly zero during the
production of live acid. The chloride ion concentration was
low initially, then increased during the production of the acid.
The chloride ion decreased towards the end of the acid slug,
then increased again upon the production of the kill fluid. It
should be mentioned that the kill fluid that was originally in
the wellbore was squeezed into the formation during pumping
the acid slug. The concentration of calcium ion also increased
upon the production of kill fluid (78 pcf calcium chloride
brine) from the formation.
Figure 3 shows that reaction products (total iron) existed
in the late stages of well flowback. The data show that the
total iron was concentrated in the front of the acid.
Accumulation of iron in the acid front produced an iron peak
of about 3,500 mg/l. Iron concentration decreased to low
values of around 300 mg/l at the acid tail and below detection
limit after the acid slug. In an effective pickling treatment,
iron concentration should be below the detection limit before
the whole acid slug exit from the well. In the case of well A, it
took 6 minutes for the acid slug to exits the tubing. This is
relatively a short time for the mill scale to dissolve completely
by the acid. The long tailing of the iron concentration curve
might have been caused by dispersion of spent acid slug. The
effect of dispersion is expected to be significant because of the
gas produced during lifting the acid by reservoir fluids.
Because the chloride ion is not consumed in the reaction, it
can be used as a tracer. Therefore, the region between the live
acid curve and chloride ion curve corresponds to the acid
consumed by the reaction with the mill scale, Fig. 4.
Figure 4 shows that only a fraction of the acid was
consumed by mill scale. Obviously, the amount of acid
pumped in this case is more than that needed to dissolve mill
scale. There is a need to optimize the treatment and reduce the
amount of acid.
The results shown in Figs. 3 and 4 suggest that only the
front of the live acid is reacting with mill scale. Hence, if the
whole slug of live acid is reacting at the same time, then high
iron concentrations would appear during the whole time
SPE 95004
interval where the spent acid is produced. It is important to
note that the amount of mill scale for given tubing is limited.
The pH was nearly zero during the production of live acid,
Fig. 2. It reaches nearly 4 at the end of sampling period. It is
most likely that iron would not precipitate under these
conditions. It is well known that Fe(II) will precipitate at pH
values greater than 6, whereas Fe(III) will precipitate in sweet
environments at pH values greater than 1-2.14
It should be mentioned that a suitable H2S scavenger was
added to the acid formulation to minimize the impact of the
gas penetrating from the formation to the wellbore.15
The tubing used in well A is made of low carbon steel. If
the acid reacts with the base metal, then it is expected to
observe manganese in the flow back samples. Figure 5 and
Table 4 show the manganese concentration along with the
iron concentration as a function of flowback time. Manganese
was detected in the flow back samples, albeit at much lower
concentrations. The variation of Mn concentration with time
was very similar to that of total iron. This trend indicates that
the acid did react with the tubing. To examine acid reaction
with the tubing the total amount of iron dissolved by the acid
was determined by calculating the area under the iron
concentration curve, Fig. 3. The amount of iron was found to
be 62.65 kg and that of the manganese was 2.09 kg. This
means that the corrosion rate in this case was 0.0051 lb/in.2,
which is significantly less than the allowable corrosion rate of
0.05 lb/in.2,16
The amount of dissolved iron can be also used to
determine the thickness of mill scale layer. If the thickness of
the scale was assumed to be independent of length, then the
average scale thickness is 0.000546 inch, Table 3.
Table 5 gives scale thickness in several wells. It also gives
the maximum iron concentration that was obtained during
pickling treatments conducted by bullheading and coiled
tubing. In general, high iron concentrations were observed.
Invasion of this iron to the formation might cause severe
formation damage. Therefore, every effort should be made to
remove iron and other contaminants from the wellbore area.
It is important to note that the scale thickness given in
Table 5 is based on the following assumptions: (1) the scale is
pure magnetite, and (2) it is uniformly distributed over the
total inside surface area of the tubing and liner contacted by
the acid.
Coiled Tubing Method
Well B is a cased and unperforated well that was pickled with
3,000 gals of 15 wt% HCl. The well is completed with 11,387
ft of 5.5-inch diameter C-95 tubing, and 2,013 ft of 4.5-inch
diameter C-95 liner, Table 3. Similar to the bullheading case,
when the acid is pumped through the coiled tubing, the leading
edge of the acid (acid front) contacts the tubing first. Mill
scale is removed during acid reaction with the early flow of
acid. The live acid that comes later is in excess and does not
find a scale to react with until the acid advances to unreacted
scale in the tubing. The live acid is inhibited with corrosion
inhibitors, which reduce acid reaction with well tubulars.
Thus, in its way up the inhibited acid has very negligible
reaction with the base metal. Because the acid continues
through the tubing/coiled tubing annulus during well
3
flowback, the leading edge of the acid (i.e., first acid pumped)
will appear first in the well flow back samples.
Figures 6 to 8 show the pH, Cl, Ca, HCl, total iron and
manganese in the flow back samples. In general, the trends
noted with the concentration of these species were similar to
those noted in the case of bullheading. However, the timing of
various peaks was different. Some of the major differences in
the peaks are as follows. First, the time at which the acid slug
appears at the well head was much longer than that noted in
the bullheading case. Also, the time needed for the acid slug to
exit from the well was much longer for the case of coiled
tubing. These trends reflect the low pumping rate that was
used in the coiled tubing case, Table 3. Unlike iron results
obtained in the bullheading case, iron peak lagged the acid
slug. This is due to the mode of flow in the case of coiled
tubing where the acid flows thought the coiled tubing, then
through the CT/tubing annulus. The variation in Mn ion
concentration was similar to that noted with the total iron.
The amount of iron that has been removed by the acid was
calculated to be 57.12 kg, and that of the manganese was
0.554 kg. The scale thickness was found to be 0.00041 inch,
Table 3. This means that the corrosion rate in this case was
0.0039 lb/in.2, which is significantly less than the allowable
corrosion rate of 0.05 lb/in.2,16
Acid Volume and Flowrate
It is evident from the flowback results that the volume of acid
used to pickle the tubing was overestimated. However, there
were a few examples of pickle design where the acid volume
was underestimated. Insufficient acid volume created U-
shaped iron profile in the bullheading treatment that was
conducted on well C. Only 1,300 gals of 20 wt% HCl were
used to pickle the tubing of this well.
Figure 9 shows that the pH, Cl and Ca ion concentrations
were similar to those noted with well A. However, two iron
peaks appeared in Fig. 10: a large peak occurred when the
acid contacted the scale for the first time in its way down, and
anther smaller peak occurred when the acid returned back and
contacted some unreacted scale. The acid concentration did
not show the U-shaped profile.
Figures 11 and 12 show that the concentration of
manganese behaved similar to that of iron. The chloride ion
showed a profile similar to that obtained with the acid. The
concentration of Mg and calcium were in general low and
indicate that the acid did not invade the formation.
It is clear from the results obtained with well C that the
amount of acid used was not enough. The reason of
underestimating the volume of the acid is that the amount of
mill scale is not known prior to the pickling treatment. The
common practice is to use a fixed volume of acid per a square
foot of the internal surface area of the tubing.
From the previous discussion, it can be inferred that the
amount of scale should be the major determinant of the acid
volume. Knowing the scale volume, one can calculate the
required amount of acid using reaction stoichiomitry. The
following equation can be used to calculate the minimum
volume of 20 wt% HCl acid (V in gallons) required to remove
magnetite during tubing pickling treatments:9
4 SPE 95004
V = 4.6874 × t s × L × F × [d + t s ]
where,
ts = Thickness of the scale (in.)
L = Length of tubing or liner (ft)
d = Diameter of tubing or liner (in.)
F = Safety factor
Acid pumping rate is another important variable in
designing an effective pickling treatment. However, the
window of flowrates that can be achieved in the field is
narrow and is limited by operational limitations, especially
when using coiled tubing. Some recommendations call for
using high flowrates since the process is mass transfer
controlled. In a mass transfer controlled processes, the high
flowrate would reduce mass transfer effects and allow faster
reactivity. On the other hand, low flowrates increase contact
times and enhance scale removal. Previous studies showed
that flow rates up to 4 bbl/min provided enough contact time
for that specific case.9,10
Contact Time
The pickling process involves reaction of the HCl acid with
various tubular contaminants inside the tubing. Therefore, it is
important to provide enough contact time for the reaction to
take place. In the bullheading case, the acid flows through the
production tubing while it flows through the annulus in the
coiled tubing case. Therefore, in bullheading, the cross
sectional area is larger than that when using the coiled tubing.
Thus, bullheading provides less contact time because area of
flow is larger and length of acid slug is less. On the other
hand, coiled tubing provides more contact time because only
smaller area is available for the flow and the acid slug is long.
Figure 1 shows differing acid slug lengths when using same
volume of acid for both cases.
Contact time can be controlled through either the volume
of the acid or through the pumping flowrate. Larger acid
volumes and less flowrates provide better contact time. It
should be mentioned that in the bullheading case the acid
contacts the tubing twice.
Conclusions
In this work, two methods of performing tubing pickle were
described and compared. The following conclusions can be
drawn from this work:
1. Both bullheading and coiled tubing methods are effective in
removing mill scale provided that the treatment is well
designed.
2. A U-shaped iron profile was noted when the acid volume
was not adequate to remove the mill scale.
3. The timing of iron peaks was found to be a function of acid
pumping mode.
4. The acid pickling treatment removed significant amounts of
mill scale. Therefore, it is strongly recommended to pickle the
well tubulars before acid treatment.
Acknowledgments
The authors wish to acknowledge the Saudi Arabian Oil
Company (Saudi Aramco) for granting permission to present
and publish this paper. Udhailiyah Lab Unit, SALD and the
Chemistry Unit and Advanced Instruments Unit of the R&D
Center, Saudi Aramco were very helpful in their field
monitoring and analysis of the spent acids, respectively.
Members of the Stimulation R&T Team, Saudi Aramco are
acknowledged for processing well flow back samples. All
engineers in Gas Production Engineering Division and local
service companies are acknowledged for many useful
discussions. The authors also would like to thank Dr. A. D.
Hill of Texas A&M University for his helpful discussions.
References
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Details Vital for Minimizing Formation damage,”
paper SPE 5702 presented at the 1976 SPE Symposium
on Formation Damage Control, Lafayette, LA, 29-30
January.
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Planning, Execution and Evaluation of Acid
Treatments in Sandstone Formations,” paper SPE
11931 presented at the 1983 Annual Technical
Conference and Exhibition held in San Francisco, CA,
5-8 October.
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1984) 2055.
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Indicate Tubing is Main Source of Iron Precipitation
in the Wellbore,” OGJ (Sept. 3, 1984) 87.
6. Gougler, P.D., Jr., Hendrick, J.E. and Coulter, A.W.:
“Field Investigation Identifies Source and Magnitude
of Iron Problems,” paper SPE 13812 presented at the
1985 SPE Production Operations Symposium,
Oklahoma City, OK, 10-12 March.
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Driweesh, S.M.: “Lessons Learned from Acid Pickle
Treatments of Deep/Sour Gas Wells,” paper SPE
73706 presented at the 2002 International
Symposium and Exhibition on Formation Damage
Control, Lafayette, LA, 20 – 21 Feb.
8. Loewen, K., Chan, K.S., Fraser, M., Leuty, B.: “A
Well Stimulation Acid Tube Clean Methodology,”
paper CIM/SPE 90-47 presented at the 1990
Petroleum Society of CIM/SPE International
Technical Meeting, Calgary, AB, June 10 – 13.
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Conjunction With Matrix Acidizing Treatments,”
M.Sc. Thesis, University of Texas at Austin, August,
2004.
10. Al-Mutairi, S.H., Hill, A.D. and Nasr-El-Din, H.A.:
“Modeling of Tubing Pickling in Conjunction with
Acidizing Treatments,” paper SPE 93291 presented
SPE 95004 5

at the 2005 International Symposium on Oilfield

Chemistry, Houston, TX, Feb. 2 – 4.
11. Curtis, J. and Kalfayan, L.: “Improving Wellbore and Table 3. Design and Result Data for Wells A & B.
Formation Cleaning Efficiencies with Environmental
Solvents and Pickling Solutions,” paper 81138 Variable Well # A Well # B
presented at the 2003 SPE Latin America and Pickling Method Bullheading Coiled Tubing
Caribbean Petroleum Eng. Conference held in Port- Acid Concentration, wt% HCl 15 15
of-Spain, Trinidad, West Indies, 27-30 April.
Volume of Acid, gallons 4,520 3,000
12. Berry, S.L., Boles, J.L., Lullo, G.: “Evaluation of a
Safe, Slightly Acidic Tubing Clean-out Fluid,” paper Tubing Type C-95 C-95
SPE 84126 presented at the 2003 Annual SPE Tubing ID, inch 3.92 4.778
Conference and Exhibition held in Denver, CO, 5-8 Tubing Length, ft 12,217 11,387
October. Tubing Surface Area, m2 2329.6 2646.6
13. Al-Mutairi, S.H., Hill, A.D. and Nasr-El-Din, H.A.: Liner Type L-80 C-95
“Pickling Well Tubulars Using Coiled Tubing: Liner ID, inch 6.004 3.92
Mathematical Modeling and Field Application,” Liner Length, ft 571 2,013
paper SPE 94124 presented at the 2005 SPE/ICoTA
Liner Surface Area, m2 166.8 383.8
Coiled Tubing Conference and Exhibition held in
The Woodlands, TX, 12 – 13 April. Flowrate, bbl/min 15.4 0.850
14. Taylor, K.C., Nasr-El-Din H.A. and Al-Alawi, M.: L/min 2448 135
“Systematic Study of Iron Control Chemicals Used Total surface area, m2 2496 3030
During Well Stimulation,” SPEJ 4 (1999) 19-24. ft2 26871 32619
15. Nasr-El-Din, H.A., Al-Humaidan, A., Fadel, B., Thickness, inch 0.000546 0.00041
Frenier, W., Hill, D.: “Investigation of Sulfide Volume/Surface Area, gal/ft2 0.17 0.09
Scavengers in Well Acidizing Fluids.” SPEPF 17
(2002) 229-35.
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Sour Environments: How Do We Avoid Coiled
Tubing Failures,” paper SPE 87622 presented at the
Time Fe Mn HCl
2004 SPE Corrosion Conference held in Aberdeen,
min mg/l mg/l wt%
Scotland, 28 May.
0 22 0 0
Table 1. Acid Formula for Pickling Well # A (Bullheading). 5 34 0 0
6 364 3 0.91
Concentration, 7 749 5 16.3
Material
gpt
8 657 5 16.91
31 % HCl 474
9 688 5 16.8
Live water 480
10 1017 7 16.8
Corrosion Inhibitor 20
11 3463 19 0.18
Inhibitor Intensifier 12
12 233 1 0
Friction Reducer 2
13 44 0 0
Surfactant 2
H2S Scavenger 10 16 103 5 0
30 1146 21 0.38
40 278 38 0
Table 2. Acid Formula for Pickling Well # B (Coiled Tubing). 50 136 27 0
Max 3,463 38 16.91
Concentration,
Material Integ. 25,588.5 854.5 -
gpt
31 % HCl 474 Amount 62.65 2.09 Kg
Live water 490 138.12 4.61 lb
Corrosion Inhibitor 20
Inhibitor Intensifier 12
Friction Reducer 2
Surfactant 2
6 SPE 95004

Table 5. Scale Thickness Calculated from Pickling Table 6. Flowback Results for Well # B (Coiled Tubing).
Treatments Time Fe Mn HCl
Max. min mg/l mg/l wt%
Acid Scale
Total HCl 0 29 9 0
Well # Volume Thickness
Fe, wt%
gals in. 2 46 1 0
mg/l
A BH 3,463 4,520 15 0.000546 4 24 1 0
B CT 27,316 3,000 15 0.000410 6 55 13 0
D BH 105,488 4,000 20 0.0089 8 8 20 0
E CT 29,799 5,000 20 0.0004
10 11 27 0
12 4 24 0
14 10 19 0
16 285 19 0
24 327 20 0
26 264 14 0
38 274 14 0
42 252 13 0
44 146 8 0
51 65 8 0
56 34 2 0
66 9 0 0
76 70 9 0
81 20 7 0
86 12 0 0
96 4 2 0
294 24 0 0
298 8 0 0
300 2 0 0
312 5 0 0
314 5 0 0
321 4 0 0
336 80 0 0
342 2105 29 0
346 27316 223 0.49
348 25532 178 10.93
350 13933 121 14.11
352 10341 72 14.57
381 1999 13 14.98
396 1378 9 14.99
411 651 4 1.21
426 318 2 0.29
Max 27316 223 14.99
Integ. 422660 4097.5 -
Amount
57.12 0.554 Kg
125.92 1.22 lb
SPE 95004 7

Flow

Bullheading provides less Coiled tubing provides

contact time because area more contact time because
of flow is larger. only smaller area is
available for the flow.

Figure 1. A Schematic Diagram of Tube Pickling using Bullheading and Coiled Tubing Methods.

6 1000000
pH
Cl
5
Ca
100000

Cl and Ca Concentration, mg/l

4
pH

3 10000

1000

0 100
0 2 4 6 8 10 12 14 16
Flowback Time, min

Figure 2. pH, Ca & Cl concentrations in flowback samples for Well # A (Bullheading)

8 SPE 95004

20 4000
HCl Acid Tail Acid Front
Fe (Total)

16
3000

Total Iron Concentration, mg/l

HCl Concentration, wt%

12

2000

1000
4

0 0
0 2 4 6 8 10 12 14
Flowback Time, min

Figure 3. Fe & HCl concentrations in flowback samples for Well # A (Bullheading)

1.2 4000
Norm. HCl Acid Tail Acid Front
Norm. Cl
1
Fe (Total)
3000

Total Iron Concentration, mg/l

HCl Concentration, wt%

0.8

0.6 2000

0.4

1000

0.2

0 0
0 2 4 6 8 10 12 14
Flow back Tim e, m in

Figure 4. Fe and normalized Cl & HCl concentrations in flowback samples for Well # A (Bullheading).
SPE 95004 9

40 4000

Mn
Fe (Total)

30 3000

Total Iron Concentration, mg/l

Mn Concentration, mg/l

20 2000

10 1000

0 0
0 2 4 6 8 10 12 14
Flowback Time, min

Figure 5. Fe and Mn concentrations in flowback samples for Well # A (Bullheading).

10 10000000

pH
Cl
8 Ca

100000 Ca and Cl Concentrations, mg/l

6
pH

4
1000

0 10
320 340 360 380 400 420 440
Flowback Time, min

Figure 6. pH and Ca & Cl concentrations in flowback samples for Well # B (Coiled Tubing)
10 SPE 95004

20 30000
Acid Front Acid Tail HCl
Total Fe
25000
16

Total Iron Concentration, mg/l

HCl Concentration, wt%

20000
12

15000

8
10000

4
5000

0 0
320 340 360 380 400 420 440
Flowback Time, min

Figure 7. Fe & HCl concentrations in flowback samples for Well # B (Coiled Tubing)

250 30000
Mn
Total Fe
25000
200

Total Iron Concentration, mg/l

Mn Concentration, mg/l

20000
150

15000

100
10000

50
5000

0 0
320 340 360 380 400 420 440
Flowback Time, min

Figure 8. Fe and Mn concentrations in flowback samples for Well # B (Coiled Tubing).

SPE 95004 11

2.5 1000000
pH

Ca and Cl Concentrations, mg/l

Cl
2 100000
Ca

1.5 10000
pH

1 1000

0.5 100

0 10
0 10 20 30 40 50 60
Flowback Time, min

Figure 9. pH and Ca & Cl concentrations in flowback samples for Well # C (Bullheading)

20 2000
HCl

Total Iron Concentration, mg/l

Fe (Total)
16 1600
HCl Concentration, wt %

12 1200

8 800

4 400

0 0
0 10 20 30 40 50 60
Flowback Time, min

Figure 10. Fe & HCl concentrations in flowback samples for Well # C (Bullheading)
12 SPE 95004

8 2000
Mn

Total Iron Concentration, mg/l

Fe (Total)
Mn Concentration, mg/l

6 1500

4 1000

2 500

0 0
0 10 20 30 40 50 60
Flowback Time, min

Figure 11. Fe & Mn concentrations in flowback samples for Well # C (Bullheading).

250000 200
Cl
Mg
200000

Mg Concentration, mg/l
Cl Concentration, mg/l

150

150000
100
100000

50
50000

0 0
0 10 20 30 40 50 60
Flowback Time, min

Figure 12. Cl & Mg concentrations in flowback samples for Well # C (Bullheading).