SPE-201330-MS

Fruit Extracts as Natural, Green, Non-Toxic Corrosion Inhibitors

Jun Hong Clarence Ng, Tariq Almubarak, and Hisham A. Nasr-El-Din, Texas A&M University

Copyright 2020, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Annual Technical Conference & Exhibition originally scheduled to be held in Denver, Colorado, USA, 5 – 7
October 2020. Due to COVID-19 the physical event was postponed until 26 – 29 October 2020 and was changed to a virtual event. The official proceedings were
published online on 21 October 2020.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
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Abstract
Corrosion inhibitors currently used in the oil and gas industry are associated with environmental concerns
and severe health risks. Recent advancements in corrosion inhibition technology had successfully tackled
environmental concerns, but still faces issues with toxicity and performance at high temperatures. This
work aims to develop environmentally friendly and non-toxic corrosion inhibitors that can overcome these
limitations. Extracts of 14 common fruits were tested as sources of potential corrosion inhibitors.
In order to determine the inhibition effectiveness of the different fruits, N-80 coupons were exposed to
15 wt.% HCl solutions at temperatures between 77-250 °F with 0.2-2 wt.% of dried ground fruit for 6 hours.
In addition, a control solution containing no corrosion inhibitor was used to establish a corrosion rate for a
base case. Upon identifying high performing dried ground fruits, extracts of these fruits were subsequently
tested to save cost by minimizing quantity needed while achieving acceptable performance.
At a concentration of 2 wt.%, fruits 1 and 2 were found to perform the best, exhibiting more than 98%
corrosion inhibition efficiency at 77°F. Fruits 11 and 12 were observed to perform the worst, going so far as
to enhance corrosion on the coupons. At 150°F, the corrosion rate of fruit extract 1 was 0.00436 lb/ft2, while
that of fruit extract 2 was 0.0277 lb/ft2. At 200°F, the addition of a corrosion inhibitor intensifier resulted in
a corrosion rate of 0.00130 lb/ft2 for fruit extract 1 and 0.0173 lb/ft2 for fruit extract 2. At 250°F, a second
corrosion inhibitor intensifier was used. The resulting corrosion rate was 0.0320 lb/ft2 for fruit extract 1 and
0.00963 lb/ft2 for fruit extract 2. These results show that a naturally occurring, green, non-toxic corrosion
inhibitor can be developed from these fruits and can comfortably pass the industry requirement of achieving
corrosion rates below 0.05 lb/ft2 for low carbon steel tubulars.
Corrosion during acid treatments causes destruction to the tubulars and downhole equipment.
Consequently, this leads to an increase in expenditure to maintain well production rates and well integrity.
Therefore, corrosion inhibitors must be included in any acid treatment formulation. The results in this work
share two new naturally occurring, green, non-toxic, high-temperature stable corrosion inhibitors that can
be developed from fruits and can successfully protect the tubular during acid treatments.
2 SPE-201330-MS

Introduction
Hydrochloric acid is commonly used for inorganic scale removal, matrix acidizing, acid fracturing, and
many other forms of stimulation treatments (Chang et al. 2008; Rafie et al. 2014; Almubarak et al. 2015).
However, HCl is a strong acid that can cause severe corrosion of well tubulars and equipment downhole,
especially at high temperatures (Buijse et al. 2004; Mahmoud et al. 2010; Almubarak et al. 2017). Corrosion
costs are estimated at around 1.372 billion USD per year, according to a recent NACE survey.
There are several techniques that can be utilized to lower corrosion damage during stimulation treatments.
The simplest method is to add corrosion inhibitors to the pumped acids. These corrosion inhibitor molecules
will stick to metal surfaces creating water-repelling barriers that will reduce the reaction between HCl and
the well tubular or downhole equipment. This technique has proven to be successful throughout the years,
and the addition of corrosion inhibitors became a necessity in any acid treatment (Smith et al. 1978; Crowe
and Minor 1985; Frenier et al. 1988).
At temperatures above 200°F, strong acids such as HCl become extremely aggressive, and having a
corrosion inhibitor by itself is no longer able to protect the tubulars (Brezinski 1999). At these elevated
temperatures, corrosion inhibitor intensifiers such as potassium iodide (KI) and formic acid are required
(Al-Katheeri et al. 2002; Cassidy et al. 2007; Khadom et al. 2018). Even with the combination of corrosion
inhibitors and corrosion inhibitor intensifier many pumped formulas are unable to provide satisfactory
corrosion rates or are banned due to environmental regulations (Marques and Mainier 1994; Al-Taq et
al. 2012). The next phase of development targeted lowering and controlling the reaction rate of HCl at
these high-temperature conditions. That was done through a variety of techniques such as emulsifying it
in diesel or increasing its viscosity by the addition of polymers (Norman and Conway 1983; Navarrete
et al. 2000; Pandya and Wadekar 2013; Zakaria and Nasr-El-Din 2016). However, that required a list of
additional additives that raised several incompatibility issues with the corrosion inhibitors (Hill and Jones
2003; Cassidy et al. 2012; Sabhapondit et al. 2012; Syafii et al. 2016). Some of the more innovative and
promising techniques to lower corrosion rates include downhole generation of HCl, completely avoiding
tubular and equipment damage throughout the pumping operation while maintaining the high strength and
reaction rates of HCl towards the formation (Sokhanvarian et al. 2017). In any case, even with all these
technological advancements, corrosion inhibitors are still essential and required to keep the operators at
ease knowing that precautions have been taken to protect downhole equipment during these acid treatments.
Metals used in the oil industry can generally be divided into 2 categories: low-carbon steel and corrosion
resistant alloys (CRAs). Low-carbon steels such as C-95, N-80, and P-110 are iron-based metals alloyed
with carbon and low manganese content. These steels are relatively cheap and are thus a popular choice
for casing and tubing material. CRAs refer to metals such as stainless steel and other non-iron based alloys
such as Hastelloy or Incoloy. These metals usually contain chrome, nickel, and molybdenum to enhance
their corrosion resistance. Due to its widespread usage in the oil and gas industry, N-80 was chosen as the
sample material for these tests (Finsgar and Jackson 2014).
There are eight main types of corrosion (Fontana and Greene 1967): uniform corrosion, galvanic
corrosion, crevice corrosion, pitting, intergranular corrosion, selective leaching, erosion, and stress-
corrosion cracking. Each of these corrosion types involves a unique mechanism, and thus require a different
method of protection. In the petroleum industry, the use of strong acids such as HCl, organic acids such as
formic acid, and the presence of chloride ions causes uniform corrosion, crevice corrosion, and pitting to
be the most prevalent forms of corrosion present (Finsgar and Jackson 2014). Under specific conditions,
other forms of corrosion have also been observed in the oil field, such as stress-corrosion cracking in the
presence of hydrogen sulfide (H2S).
Corrosion inhibitors operate by adsorbing to the surface of the metal to create a protective layer that
reduces contact between the metal surface and the corrosive substance which inhibits the cathodic/anodic
reactions, or by poisoning the production of H2 (Rostami and Nasr-El-Din 2009). According to Finsgar
SPE-201330-MS 3

and Jackson (2014), many different types of chemical structures are used, such as acetylenic alcohols,
imidazolines, and quinolone derivatives. Generally speaking, the most common types of corrosion inhibitors
used in the oil and gas industry are typically quaternary amines or sulfur-containing compounds (Son 2007;
Ng et al. 2018). Although commonly used corrosion inhibitors are effective, they are usually harmful to
the environment as well as to human health (Rani and Basu 2012; Chigondo and Chigondo 2016). These
mentioned compounds contain sulfur, nitrogen, and oxygen atoms as they help the molecule better adsorb
to the surface of the metal. Since many naturally occurring chemicals also contain these groups, it is no
wonder they would also possess corrosion-inhibiting properties.
Many authors have examined plant extracts and products, especially fruits and their juices, as corrosion
inhibitors. Yaro et al. (2011) tested peach juice as a corrosion inhibitor for mild steel in 3.6 wt% HCl between
86°F and 140°F. They found that the peach juice showed a corrosion rate of 0.00094 lb/ft2 per hour. Sedik et
al. (2020) examined the effect of dardagan fruit extract with 3.6 wt% HCl as a corrosion inhibitor for mild
steel at 77°F and observed a 92% corrosion inhibition efficiency over 1 hour of testing. da Rocha (2010)
tested aqueous extracts of mango, orange, passion fruit, and cashew peels as corrosion inhibitors on mild
steel in 3.6 wt% HCl at 77°F for up to 24h. They observed a range of inhibition efficiencies of 67% to 86%
over 1h and 93% to 96% over 24h. Zhao et al. (2019) used bitter gourd in 3.6 wt% HCl to determine its
effectiveness as a corrosion inhibitor on mild steel at 77°F and observed inhibition efficiencies between 55%
and 96%. Umoren et al. (2015) tested red apple juice as a corrosion inhibitor for mild steel at temperatures
between 86°F and 140°F in 1.8 wt% HCl and found inhibition efficiencies of up to 90%. However, these
corrosion inhibitors derived from natural products have not been tested at temperatures above 150°F and
higher acid concentrations.
Corrosion inhibitors are additives that must be included in acidizing treatments in order to minimize
damage to the tubulars and other downhole equipment. However, these inhibitors are also typically
environmentally damaging and harmful to human health (Singh and Bockris 1996). Therefore, this paper
seeks to examine the corrosion inhibiting properties of several edible fruit extracts at downhole conditions
with high concentrations of HCl. The objective of this paper is to present an alternative variety of corrosion
inhibitors that are environmentally friendly and non-toxic.

Experimental Methods
Materials
A group of 14 different edible fruits was selected from the shelves of local grocery shops. These fruits were
dried and ground into a powder using a spice blender. Extracts of the fruit were obtained from a chemical
company at a purity of more than 95%. A concentration of 36.4 wt% HCl was diluted using tap water to
create the 15 wt% acid solution for the tests.

Coupon Preparation
N-80 coupons with a surface area of 3.62 in2, and 2 centered holes of 0.15 in diameter were prepared
according to ASTM G31. A single coupon was used per corrosion test. They were washed with DI water
followed by acetone and allowed to air dry. The coupons were polished by the manufacturer with a 600
grit finish; therefore, no further polishing was required. After drying, the coupons were weighed on a scale
with 1 mg accuracy.

Equipment
Corrosion tests were carried out in a Series 4523 1 liter Hastelloy B benchtop reactor with a maximum
temperature and pressure rating of 662°F and 1,800 psi. The set-up is shown in Fig. 1. The prepared coupons
were mounted on the coupon holder using PEEK screws and washers to prevent galvanic corrosion for
autoclave tests. The coupon and solution were placed into the reactor autoclave, which is sealed by 2 C-
4 SPE-201330-MS

clamps. N2 gas is supplied to the reactor from a tank connected to the reactor using a series of rubber hoses
and check valves. Gas from the reactor was released into a scrubber containing 400 ml DI water to remove
any harmful vapors before releasing it into a fumehood. For room-temperature tests (77°F), the coupon was
suspended in a 150 mL beaker containing the HCl solution. Teflon tape was passed through the holes on the
top of the coupon, and the ends tied around a beaker cover. This would allow the coupon to be suspended
in the acidic solution.

Figure 1—Corrosion reactor set-up used.

Corrosion Tests
700g of 15 wt% HCl solution was prepared using 36.4 wt% HCl stock solution diluted with tap water (<500
ppm) for tests in the autoclave above. For room-temperature tests, 140g of 15 wt.% HCl solutions were
prepared. Ground dried fruits were used for the room temperature tests, while fruit extracts were used for
higher temperature tests. In both cases, 2 wt.% of fruit extract was added to each test. All tests were carried
out over a duration of 6 hours. A control test was also carried out to present a baseline corrosion rate in
the absence of a corrosion inhibitor. When using the autoclave, the pressure was kept at 400 psi to prevent
excessive evaporation of the acid solution. N2 gas was also passed through the solution for about 10 minutes
before the start of the test in order to deaerate the solution. This was done to avoid the effects of O2 on the
test. Nitrogen gas was used because it is inert. Dimensions and weight of the coupon were taken before and
after each test to determine the corrosion rate using the weight loss method according to Eq.1:

(1)

Results and Discussion

The room temperature tests were conducted prior to the high-temperature ones in order to determine the
performance of each corrosion inhibitor. A list of the 14 different fruit results is shown in the table below,
along with the base case for the room temperature tests.
SPE-201330-MS 5

As can be seen from Table 1, the fruits tested displayed a range of inhibition efficiencies with some, such
as fruits 11 and 12, even having higher corrosion rates than the base. Considering only those with positive
effects, fruits 1 and 2 performed the best, providing more than 90% inhibition efficiency and fruit 8 was
the worst performer, at only 11.8% at room temperature. From this experiment, best-performing fruits were
evaluated at higher temperatures using the autoclave.

Table 1—Corrosion rate for the 14 fruits at 77°F in 15 wt.% HCl at 2 wt.% concentration each on N-80.

Inhibition
Fruit Corrosion Rate (lb/ft2)
Efficiency (%)

Base 0.0142 -
1 0.00025 98.2
2 0.00009 99.4
3 0.0035 75.4
4 0.00614 56.8
5 0.00382 73.1
6 0.00365 74.3
7 0.00617 56.5
8 0.01252 11.8
9 0.00541 61.9
10 0.00644 54.6
11 0.01522 -7.2
12 0.01944 -36.9
13 0.00718 49.4
14 0.00617 56.5

The next set of corrosion tests were conducted at 150°F with fruit 1 and 2 since they performed best. For
the subsequent experiments, extracts of the fruits were used. The results for the tests are shown in Table
2 below.

Table 2—Corrosion rate for the fruit extracts 1 and 2 at 150°F in 15 wt.% HCl at 2 wt.% each on N-80.

Inhibition
Temperature (°F) Fruit Extracts Corrosion Rate (lb/ft2)
Efficiency (%)

150 Base 0.371 -

150 1 2 0.00436
150 2 2 0.0277

As can be observed from the results, fruit extracts 1 and 2 were both able to provide sufficient corrosion
inhibition to the coupons. The industry standard for allowable corrosion rate for carbon steel is 0.05 lb/
ft2 over 6h (Kalfayan 2008). Despite fruit extract 2 having a higher corrosion rate than fruit extract 1, it is
important to note that both fruit extracts showed good inhibition efficiency of over 90% as compared to the
base case. Furthermore, this shows that even a slight increase in temperature from 77˚F to 150 ˚F can cause
a significant increase in corrosion rate, especially when high concentrations of HCl are used.
Since both fruits showed success at 150˚F, fruit extracts 1 and 2 were tested 200°F. A summary of the
corrosion rates at these conditions can be found in Table 3 below.
6 SPE-201330-MS

Table 3—Corrosion rate for the fruit extracts 1 and 2 at 200°F in 15 wt.% HCl on N-80.

Intensifier Corrosion
Temperature (˚F) Fruit Extracts C.I. Conc. (wt.%)
Conc. (wt.%) Rate (lb/ft2)

200 Base - 1 0.510

200 1 2 1 0.0013
200 2 2 1 0.0173

At 200°F, 1 wt.% of corrosion inhibitor intensifier was added to 2 wt.% of fruit extracts 1 and 2. The
corrosion rate was observed to be 0.0013 lb/ft2 for fruit extract 1 and 0.0173 lb/ft2 for fruit extract 2. At this
temperature, a base case corrosion rate in the absence of any corrosion inhibitor and intensifier could not
be established since the coupon was found to be completely dissolved by the end of the test. Therefore, the
base case was changed to include 1% corrosion inhibitor intensifier only to verify the effectiveness of both
fruit extracts. The result was a significant increase in the corrosion rate to 0.510 lb/ft2. Furthermore, little
damage was observed to the N-80 coupons, as can be seen in Fig. 2.

Figure 2—Before and after images of the coupons for 200°F corrosion test with 15 wt.
% HCl with 1 wt.% intensifier and 2 wt.% (a) fruit extract 1 and (b) fruit extract 2.

Subsequently, both fruit extracts were tested at 250°F where a corrosion rate of 0.0320 lb/ft2 and 0.00963
lb/ft2 were observed for fruit extracts 1 and 2, respectively. Due to the increase in temperature, 1 wt% of a
second corrosion inhibitor intensifier was added to the formula used at 200°F.

Table 4—Corrosion rate for the fruit extract 1 and 2 at 250°F in 15 wt.% HCl on N-80.

Intensifier 1 Intensifier 2
Temperature (˚F) Fruit Extract C.I. Conc. (wt.%) Corrosion Rate (lb/ft2)
Conc. (wt.%) Conc. (wt.%)

250 1 2 1 1 0.0320
250 2 2 1 1 0.00963

Conclusion
From this work, it can be shown that naturally occurring and environmentally friendly corrosion inhibitors
that can be extracted from various edible fruits provide significant corrosion inhibition against 15 wt.% HCl
at a variety of temperatures. More work in this area will include identifying other corrosion inhibitors and
the chemical structures that provide these inhibiting capabilities.
SPE-201330-MS 7

Based on the lab tests, we conclude the following:

1. Fruit extract 1 can protect low carbon steel from corrosion in a solution of 15 wt% HCl resulting in
a corrosion rate of 0.00436 lb/ft2 over 6 hours at 150°F.
2. Fruit extract 2 can protect low carbon steel from corrosion in a solution of 15 wt% HCl resulting in
a corrosion rate of 0.0277 lb/ft2 over 6 hours at 150°F.
3. The corrosion rate of 15 wt% HCl on low carbon steel is significantly higher at 200°F, completely
dissolving the coupon within 6 hours in the absence of corrosion inhibitors.
4. A corrosion inhibitor intensifier can be used in addition to corrosion inhibitors for higher temperature
applications (>200°F) to improve the performance of the corrosion inhibitor. Fruit extracts 1 and 2
had a corrosion rate of 0.00130 lb/ft2and 0.0173 lb/ft2 at 200°F over 6h, respectively.
5. At 250°F, a second corrosion inhibitor intensifier can be added, allowing the corrosion inhibitors to
achieve corrosion rates of 0.0320 lb/ft2 and 0.00963 lb/ft2 for fruit extracts 1 and 2, respectively.

Nomenclature
H2S Hydrogen Sulfide
HCl Hydrochloric Acid
KI Potassium Iodide
PEEK Polyether Ether Ketone
Room temperature 77°F

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