OTC-29445-MS

Mechanical Properties of Cementitious and Non-Cementitious System After

Ageing Tests for Well Abandonment Cementing Operations

Ingrid Ezechiello da Silva, PETROBRAS; Vivian Karla Castelo Branco Louback Machado Balthar and Romildo
Dias Toledo Filho, COPPE/UFRJ; Gabriella de Medeiros de Sá Cavalcante and Robert Lucian de Lima dos Santos,
PETROBRAS

Copyright 2019, Offshore Technology Conference

This paper was prepared for presentation at the Offshore Technology Conference held in Houston, Texas, USA, 6 – 9 May 2019.

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Abstract
The plug and Abandonment (P&A) are the final stage of the life cycle of an oil well. This implies that
the plugging material must withstand the chemicals, temperature and well pressure to ensure its long-
term integrity. Portland cement is the most used material as a safety barrier in P&A operations. However,
the extreme conditions of the well have challenged the mechanical properties of Portland Cement. In this
context, the present work aims to identify the adequate systems as permanent plugging material and to
characterize them with a qualification process based on international references and experimental validation.
Hence, four systems were tested for plug cementing operation with composition variations under pre-
defined ageing conditions. Class G Portland cement slurry was used as reference to allow comparison of
mechanical properties (compressive strength and tensile strength) between flexible cement paste, a system
containing a mixture of Class G Portland Cement with epoxy resin and finally a system with epoxy resin
only. Samples containing Class G Portland Cement were cured for 14 days under well bottom conditions
(3000 psi and temperature of 174 degrees Fahrenheit) and cured for 14 days at well temperature (using a
thermal bath). Samples containing resin were cured for 14 days under well bottom conditions (3000 psi and
temperature of 150 degrees Fahrenheit) and cured for 14 days at well temperature (using a thermal bath).
Finally, the samples were aged for 60 days in a thermal bath at well temperature and exposed to the
brine which is the completion fluid composition which will be above and below in contact with the well
barrier in a P & A operation. The results of the compressive strength tests of the samples aged in brine
showed tha in some systems tested the reduction of the modulus of elasticity occurred, however, it was also
observed the increase of the modulus of elasticity in another system. The same was true of the results of
tensile strength tests of aged samples, the increase of rupture loading in some systems and reduction in the
other ones were observed.
The mechanical tests of the samples before and after ageing were performed to define the best system to
be used in a well abandonment operation aiming for long-term integrity.
2 OTC-29445-MS

Introduction
The life cycle of an oil and gas well comprises the stages of construction, production and abandonment.
Reducing well productivity can make production maintenance costs unviable. Even after the production
recovery operations, the well no longer has productivity that justifies its operation making it necessary to
abandon it, in this case permanent. The objective of the well abandonment operation is to ensure the isolation
of the intervals that present current and future flow potential (ANP, 2016).
Well abandonment campaigns are growing around the world. The plug and abandonment (P&A)
operations aim to restore insulation between the different permeable zones, preventing the migration of
fluids between the formations, either by the well or the annular casing-formation, and the migration of fluids
to the surface or to the bottom of the well and in this way, ensure the integrity of the well in the long term.
The Brazilian oil regulator, ANP, has defined in the regulation of the Well Integrity Management System
(SGIP), the concept of the independent safety barrier envelops (SBE). The SBE is a set of one or more well
barriers with the aim of preventing unintentional flow of fluids from the formation to the environment and
the flow between different intervals in the well, considering all possible paths (ANP). The permanent SBE
has as its philosophy the restoration of the original seal provided by the sealant formations. At the base of
the permanent SBE there should be a competent, impermeable and without potencional flow formation that
avoids the migration of fluids. It shall be ensured that the cemented annular tubing of the metal pipes and
the cement plug inside the tubing with the smaller diameter or the open hole act to prevent undesired influx
(IBP, 2017). Cement paste or other material with similar performance should be used as barrier element
in operations of P&A.
The quality and performance of a Plug and Abandonment operation depends directly on the type of
plugging material and plug placement technique. Barriers may be categorized as cementitious or mechanical
barriers. It should be noted that mechanical barriers are used as temporary P & A barriers and are not allowed
as permanent barriers (Khalifeh et al., 2013).
Cement or blends plugs used in well abandonment operations must have physical, chemical and
mechanical properties capable to ensure sealing and integrity of the well during the time the well will be
suspended or during its life cycle even after abandonment. In this way, the pastes used in these operations
should be designed in order to avoid fluid migration and retraction of the slurry, which may form microanils/
cracks, and ensure a good adhesion between the casing / formation. Pastes formulated with class G Portland
cement are the most used system in plugging operations. However, these slurries must endure the mechanical
stresses of the well and resist the CO2/H2S, when applied. Portland cement pastes, are not always able to
maintain these characteristics at well temperature and pressure conditions over their lifetime.
Another challenge encountered in some P&A operations is the difficulty of removing the production/
injection tubing to execute plugging operations due to the age of the wells being abandoned. In this scenario,
through-tubing (TT) abandonment is one of the solutions found by the industry to deal with this issue.
This solution in which part or all of the tubing remains in the well and the SBE are constituted with the
placement of the permanent SBE well barriers elements in the annulus between the tubing and the casing
the as well as inside the column, where cement is found in the annulus between the casing and the sealant
formation and, if applicable, also between casings (IBP, 2017).
Through-tubing tecnique is generally accomplished by means of a coiled tubing, which is lowered
through the inside of the production column, whereby the plugging material is displaced to the desired depth.
In figure 1 is shown an example of a TT operation in which was estabilished two safety barrier envelop
(primary and secondary).
OTC-29445-MS 3

Figure 1—Example of Through-Tubing abandonment well operation (IBP, 2017).

Due to the mentioned arguments and challenges, new materials are being studied to be used for suspension
and abandonment of wells.
The experimental long-term integrity tests were based upon the Guidelines on qualification of materials
for the suspension and abandonment of wells, Oil & Gas UK (2015). The guideline has defined nine types
of materials that can be used in P&A operations as long as they meet the requirements and are validated
according to the ageing tests and acceptance criteria. In this work a comparative study of the mechanical
properties between the conventional paste system, the cement paste mixed with epoxy resin and the epoxy
resin-only type based (type A and type C) was carried out, see table 1. The main objective is to increase the
reliability of the material used in plugging to ensure the sealing and integrity of the well in the long-term.

Table 1—Materials for the suspension and abandonment of wells studied (Oil & Gas UK, 2015).

Type Material Examples

A Cements / ceramics (setting) Portland API class cement, Pozmix, slag, phosphate cements, hardening ceramics,
geopolymers

C Thermosetting polymers and composites Resins, epoxy, polyester, vinylesters, including fibre reinforcements

In TT operation the cement paste is displaced in the anular and inside of the tubing/casing using the
coiled tubing. Because coiled tubing has a much smaller internal diameter than casing and work string,
selection of the plugging material and the design of the paste requires greater attention when compared
to conventional operation such as low viscosity, stability and higher thickening time values higher values.
Nowadays, class G Portland cement paste is the most used system in conventional abandonment operations.
Due to the peculiarities of a cementing operation with coiled tube, new additives and plugging materials are
being studied to improve the properties of Portland cement paste or for replacement.
The main problem related to cementing operations using coiled tubing are the possibility of premature
setting of the slurry. Slurry design should ensure that thickening time is sufficient to circulate the entire
slurry volume and withdraw the tubing/casing from the well.
In this context, the present work aims to evaluate four systems used by Petrobras as permanent plugging
material at Brazilian wells. Mechanical properties through uniaxial compression test (unconfined test) and
splitting tensile strength test (Brazilian test) were evaluated after autoclave cure, thermal cure and thermal
cure/thermal ageing.
4 OTC-29445-MS

Experimental
In this work were studied four paste systems, divided into two groups. The first one was focused at TT
operation (using coiled tubing) and the second one at conventional operation.
For plugging operation with coiled tubing, this study compared the system currently used as permanent
well barrier, Class G Portland Cement (Conventional Paste, P1), with flexible and expanding cement system
(Flexible-Expandable Paste, P2).
The Class G Portland cement paste is the system required in most cases of plugging wells operations
because it is similar to the caprock properties that it is replacing. However, there are situations that it may be
not appropriate (Oil & Gas UK, 2015). For Flexible-Expandable Paste, were used a proprietary blend that it
is a mixture of Class G Portland Cement, diferent size granulars materials and a flexible material. According
to Wu et al. (2014), the flexible material in the cement blend will increase the flexibility of the set cement. In
addition, the expansion material exhibits the best property characteristics with respect to expansion against
the hard formation and decreases the risk of creating microannulus.
For conventional plugging operations were studied two paste systems that could replace class G Portland
cement, defined as: Mixture of Class G Portland Cement and epoxy resin (Cement-Resin Paste, P3) and
Epoxy Resin (P4).
Resin is chemical inert and resistant to acid and hydrocarbons. Its mechanical properties (compressive
and tensile strength) have higher performance in comparison to base cement. The addition of resin in cement
slurry could improve the mechanical properties of base cement slurry.
The resin could be applied as a secondary well barrier in plugging operations meanwhile the moisture of
cement and resin as the primary barrier. It is importante to consider that resin-based paste could be also used
at remediation and squeeze operations. The most advantage of this class of material is that it is solid particle
free. For this work purposes, the cement paste was designed to achieve the properties shown in tables 2 e 3.

Table 2—Properties of the pastes studied for the abandonment operations with coiled tubing.

Property Acceptance Criteria

Gravity Density 15,8 ppg

Free Fluid Zero

Fluid Loss <120 mL

Sedimentation Δρ ≤ 0,5 ppg and lowering of the top of the test specimen <5 mm

Reology (BHCT=153°F) VP<80Cp, LE<15lbf/100ft2

Table 3—Properties of the pastes studied for conventional abandonment operations.

Property Acceptance Criteria

Density 15,8 ppg

Free Fluid Zero

>80mL
Fluid Loss
<120 mL

Sedimentation Δρ ≤ 0,5 ppg and lowering of the top of the test specimen <5 mm

Reology (BHCT=120°F) 100<L300<120 (BHCT)

BHCT = Bottom-hole Circulation Temperature

In material qualification for well plugging operations, the UK Guideline (Oil & Gas UK, 2015) establishes
a series of experimental tests that should be executed before and after the ageing process. In this work will
be presented the mechanical test results for the four paste systems.
OTC-29445-MS 5

The compression mechanical strength tests allow the identification of tensile and strain relationship after
the ageing process. This will lead to rupture limits results and elasticity modulus information.
It is desirable that cement plugs used as well barrier operations works in its mechanical elastic region.
To determine the indirect tensile strength of the specimens, the Brazilian test of diametrical compression
(Splitting Tensile Strength of cylindrical specimens) was carried out.
Because it is a wellbore operation, the material used for plugging must have low permeability so, that
there is no migration of undesirable gases into the environment. Furthermore, chemical reactions may occur
between well fluids and the material used in the plugging which may compromise the integrity of the plug.
In these chemical reactions can occur loss or increase of mass, for this reason the measurement of the dry
mass before and after the ageing must be performed.
Table 4 presents the summary of the tests performed on the 4 slurries systems before and after ageing
in brine.

Table 4—Summary of the tests performed.

Property Test Acceptance Criteria (*)

Before Ageing After Ageing

UCS ASTM C39/C39M (2018) >1.4 MPa (200 psi) >1.4 MPa (200 psi)
ABNT NBR 5739 (2018)
ASTM C496 (2017)

Indirect tensile strength ABNT NBR 7222 (2011) >1.0 MPa (145 psi) >1.0 MPa (145 psi)
(Brazilian test)

(*)Guideline on Qualification of Materials for the suspension and abandonment of wells (Oil & Gas UK, 2015).

Preparation of Pastes for Specimens Molding

API RP 10B-2 (2013) and Petrobras Laboratory Tests Procedures (Procelab, 2014) were used to prepare
and testing the slurries except for preparation of resin system. According to API RP 10B-2 (2013), for
unconvencional paste formulations, others methods of paste prepare should be undertaken since the service
provider and the user had agreed the method. The preparation of the resin system to carry out the laboratory
tests followed an internal procedure of the service company due to its specificities. In this way, the
components of the system, all liquids, were mixed in a becker, once there is no need to use the blender
(see figure 2).

Figure 2—Prepare of resin slurry in a glass vessel.

For the preparation of the cement paste mixed with resin the following procedure was performed. The
cement paste was prepared according to API RP 10B-2 (2013) orientation using the blender. At the end of
the mixing, the equivalent of 20% of the slurry volume was removed and the equivalent volume of resin
added. This blend was homogenized in the blender for about 1 minute.
6 OTC-29445-MS

The systems studied to perform operation with coiled tubing were prepared according to API RP 10B-2
(2013). All systems were mixed with 44% BWOC water and had a density of 15.8 ppg.
The slurry formulation for each System is shown in table 5. For the well abandon scenario, it is necessary
that the slurries contain specific additives to improve the performance of the paste in its fluid state and after
its hardening.

Table 5—Systems Design.

System Design

Conventional Paste (P1) Class G Portland Cement

Antifoamer
Dispersant
Control Agent
Retarder
Viscosifier

Flexible and Expadable Paste (P2) Blend (Class G Portland Cement +

flexible material)
Antifoamer
Dispersant
Retarder
Viscosifier
Control Agent
Latex
Expanding
Additive

Cement-Resin Paste (+ 20% resin Resin Epoxy

epoxy) (P3) Class G Cement Portland
Antifoamer
Control Agent
Retarder
Viscosifier

Epoxy Resin (P4) Epoxy Resin

Hardener
Accelerator

For mechanical tests, 18 cylindrical specimens (2" x 6") were molded for each system. Six specimens
were cured for 14 days in a pressurized consistometer (non-aged) according to the ramps obtained from
computational simulations for operation and the other 12 specimens were cured for 14 days at thermal bath
at bottom-hole static temperature (BHST). Of these 12 specimens, six were only cured (non-aged) and the
other six were cured and aged for 60 days immersed in brine. After the curing time, the specimens were then
demoulded, faced and cut to the appropriate sizes for the tensile and compressive strength tests. Cylindrical
specimens intended for the compressive strength tests measure 2" x 4" while the specimens for the tensile
strength tests measure 2" x 1". Mechanical tests were carried out on non-aged test specimens. The remainder
of the specimens were immersed in brine and placed in a thermal bath for the ageing of 60 days. The ageing
process was performed according to some recommendations of the UK Guideline (Oil & Gas UK, 2015).
For the conventional operations the temperature ramps were obtained from computational simulations. For
the coiled tubing operations, the temperature ramps were obtained from measurements of temperature in
situ (telemetry).

Ageing Process of Specimens

According to the UK, an individual autoclave should be used to measure the ageing behavior of each system
studied, with three duplicate samples for each measurement. However, the samples were initially aged in
thermal bath at the static temperature of the well (BHST). The purpose of the complete ongoing study is to
compare the ageing of the samples in a thermal bath with the samples in autoclaves simulating the pressure
and temperature conditions of the well at the ages of 30 days, 60 days and 90 days. In this work, will be
OTC-29445-MS 7

presented the results of the ageing of the brine immersed samples for 60 days. In this work, the fluid used
for the ageing process was a NaCl brine having a density of 9.6 lb / gal. The composition of the NaCl brine
used in the ageing process of the samples is shown in table 6.

Table 6—Chemical composition of Brine.

Constituent Concentration

Water -

KCl 3.5 lb/bbl

NaCl 49.0 lb/bbl

NaHSO3 @ 40% 0.045% v/v

C5H8O2 @ 40% 0.053

Surfactant 0.20

NaOH @ 25% pH 8 – 9

The specimens were placed in a glass vessel containing the brine. The volume ratio of brine to sample
volume was 2: 1. The glass vessels were immersed in a thermal bath for 60 days at the BHST temperature.
After the ageing time, the samples were sent to the mechanical tests. The table 7 summarizes the ageing
conditions for each system studied.

Table 7—Test conditions for ageing tests.

System Specimens Name Cure Press. (psi) Cure Temp. Ageing(1)

(°F/°C) Temp. (°F/°C)

P1 P11 3000 174/79 Non-ageing

P12 Patm 174/79 Non-ageing

P13 Patm 174/79 174/79

P2 P21 3000 174/79 Non-ageing

P22 Patm 174/79 Non-ageing

P23 Patm 174/79 174/79

P3 P31 3900 150/66 Non-ageing

P32 Patm 150/66 Non-ageing

P33 Patm 150/66 150/66

P4 P41 3900 150/66 Non-ageing

P42 Patm 150/66 Non-ageing

P43 Patm 150/66 150/66

(1)The ageing process were performed at atmospheric pressure.

Mechanical Testing
For uniaxial compression tests (UCS), the specimens were ruptured in the load cell with a preload of 0.5
MPa (72.5 psi) and rate of loading rate of 3.0 MPa/minute (435 psi/minute). Figure 3 shows the setup of
compression strength test. The elastic modulus was determined according to ASTM C469 (2017).
8 OTC-29445-MS

Figure 3—Compression test of cylindrical specimens.

For the test of diametral compression (Brazilian test), the test specimens were ruptured in load cell with
preload of 0.2 kN and rate of loading of 0.1 kN/s. Figure 4 shows the setup of diametrical compression test.

Figure 4—Diametrical Compression of Cylindrical Test Specimens.

Results and Conclusions

Visual Inspection
Initially the visual inspection of the samples after the ageing was carried out with the aim of detecting
physical changes in the surfaces of the samples. For samples of P1 and P3 pastes no changes in texture and
color of the test specimens were observed after ageing process. For samples of P2 paste, no color changes
were identified, but small cracks in the surface and salt deposition were observed according to figure 5.

Figure 5—(a) P22 Paste Samples after 14 days of thermal bath cure;
(b) P23 Paste Samples after 60 days of ageing exposure to brine.

Samples of the epoxy resin system (P4) showed significant changes in color after the ageing process, as
can be observed in figure 6.
OTC-29445-MS 9

Figure 6—(a) P42 Paste Samples after 14 days of thermal bath cure; (b) P43 Paste Samples after 60 days of ageing.

Mechanical Testing
The mechanical properties evaluated with the repetition of the tests were treated statistically by comparing
the means, with a confidence level of 95%.
Firstly, a comparative analysis of the results of the mechanical tests of the specimens cured for 14 days in
downhole conditions (autoclave) with samples cured in a thermal bath (BHST) was carried out. The results
of the compression test are shown in Table 8.

Table 8—Uniaxial Compression test results (UCS) - Unaged Specimens.

Property P11 P12 P21 P22 P31 P32 P41 P42

U.S. (MPa) 46.5 ± 3.7 40.0 ± 4.0 25.8 ± 1.2 17.5 ± 0.8 39.8 ± 2.7 38.71 ± 1.08 94.9 ± 7.0 97.9 ± 7.5

U.S. (psi) 6748 ± 539 5802 ± 580 3744 ± 173 2538 ± 116 5772 ± 393 5614 ± 157 13759 ± 1019 14205 ± 1083

E (GPa) 11.2 ± 1.0 11.8 ± 0.9 8.8 ± 1.0 6.1 ± 0.4 8.9 ± 0.4 8.4 ± 0.3 3.0 ± 0.4 2.9 ± 0.2

For samples P1 and P4 were not observed significantly changes for Young’s Modulus and Compressive
Strength. For samples P3 was observed a slight reduction for Young’s Modulus, but without significant
changes in Compressive Strength. It can also be observed that there was a reduction in the Young´s Modulus
and Compressive Strength of samples P2.
For the same test conditions, tensile tests were performed (Brazilian test). The results of the Brazilian
test are shown in table 9.

Table 9—Brazilian test results - Unaged Specimens.

Property P11 P12 P21 P22 P31 P32 P41 P42

Load (kN) 8.06 ± 1.26 8.68 ± 0.72 4.27 ± 0.17 3.02 ± 0.30 4.89 ±0.45 5.81 ± 0.58 * *

Tensile Strength (MPa) 4.10 ± 0.63 4.42 ± 0.37 2.17 ± 0.09 1.54 ± 0.15 2.49 ± 0.23 2.96 ± 0.30 * *

Tensile Strength (psi) 595 ± 91 641 ± 53 315 ± 13 223 ± 21 361 ± 34 429 ± 43 * *

(*)The results of the tensile tests (Brazilian test) were not representative.

There was a slight increase in tensile strength for P1 and P3 samples cured at thermal bath. For samples
P2 was observed a significant reduction in tensile strength.
The study proceeded with the ageing of the samples only in thermal bath since the availability of
autoclaves is much smaller than the thermal baths.
After the ageing process, comparative analyzes were performed between the mechanical parameters of
the unaged specimens and the aged specimens. Firstly, a comparison was made between the results of
the compressive strength tests of samples cured in thermal bath (BHST) with samples aged in brine, as
summarized in table 10.
10 OTC-29445-MS

Table 10—Comparison of uniaxial compression test results (UCS) - samples aged in the same test condition.

Property P12 P13 P22 P23 P32 P33 P42 P43

U.S. (MPa) 40.0 ± 4.0 40 ± 4.4 17.5 ± 0.8 27.7 ± 1.5 38.7 ± 1.1 38.8 ± 2.2 97.9 ± 7.5 77.9 ± 20.8

U.S. (psi) 5802 ± 580 5802 ± 638 2538 ± 116 4023 ± 223 5614 ± 157 5630 ± 322 14205 ± 1083 11300 ± 3020

E (GPa) 11.8 ± 0.9 11.8 ± 0.2 6.1 ± 0.4 12.0 ± 1.0 8.4 ± 0.3 8.6 ± 0.3 2.9 ± 0.2 2.3 ± 0.8

For samples P1, no significant changes were observed in the Young´s Modulus and Compressive
Strength. However, for samples P2 was observed an expressive increase in the Young´s Modulus and
Compressive Strength. The increase in the values of these parameters can be explained by the filling of
the pores of the specimens by the hydration products during the ageing process. However, for this theory
to be confirmed, it is necessary to compare and analyze the permeability results and the chemical analysis
results of the samples before and after ageing process. For samples P3 was observed a small increase in
the Young´s Modulus but there was no significant change in the values of compressive strength. For the
P4 samples, a reduction in the values of compressive strength was observed. However, statistically we can
not consider that this reduction was significant. On the other hand, the modulus of elasticity resulted in a
significant reduction. The six specimens of sample P43 were aged together in the same thermal bath under
the same conditions. However, after ageing each specimen showed a different coloration, as can be observed
in figure 7.

Figure 7—Different colors of the six specimens of the P43 samples (samples after compression strength test).

The different shades of brown may indicate that the ageing process was different for each sample. The
tensile and strain curves obtained by the compressive strength test presented great dispersion that can be
justified by this heterogeneous ageing process.
For the same test conditions, tensile tests were performed (Brazilian test). The results of the Brazilian
test are shown in table 11.

Table 11—Comparison of results Brazilian test - samples aged in the same test condition.

Property P12 P13 P22 P23 P32 P33 P42 P43

Load (kN) 8.68 ± 0.72 6,34 ±0.04 3.02 ± 0.30 8,05 ± 2.30 5.81 ± 0.58 5,85 ± 0.03 * *

Tensile Strength (MPa) 4.42 ± 0.37 3.23 ± 0.02 1.54 ± 0.15 4.10 ± 1.17 2.96 ± 0.30 2.98 ± 0.02 * *

Tensile Strength (psi) 641 ± 53 468 ± 3 223 ± 21 595 ± 170 429 ± 43 432 ± 2 * *

(*)The results of the tensile tests (Brazilian test) were not representative.

There was a significant reduction in the tensile strength of the P1 samples after the ageing process while
for the P2 samples an expressive increase in the tensile strength was observed. In addition, no significant
changes in tensile strength were observed for P3 samples.
Figure 8 shows some examples of failure modes of the samples tested during this study.
OTC-29445-MS 11

Figure 8—Examples of sample failure modes: (a) Compressive strength test; (b) and tensile tests.

The P4 system, in addition to presenting results of tensile and compression strengths much higher than
those of the conventional paste, its modulus of elasticity is considerably lower. However, the study of ageing
of the system should continue at various ages and temperatures. The results of compression tests after ageing
process showed a large standard deviation.
Therefore, comparing the mechanical results of all systems studied, it can be concluded that the G Class
Portland Cement mixed with 20% epoxy resin, P3, presented good results after the ageing process.
This system has values of mechanical strength similar to the conventional system (P1), however, it has
a lower modulus of elasticity. In this way, the P3 system can be a potencial substitute for the conventional
system for P & A operations.

Acknowledgements
The authors acknowledge PETROBRAS for financing the work through the PETROBRAS Research Center
(CENPES). In the laboratory of the CENPES the samples were cured in the autoclaves. The authors also
acknowledge the Civil Engineering Program of the Federal University of Rio de Janeiro (UFRJ / COPPE)
for funding through the Coordination for Improvement of Higher-Level Personnel in Brazil (CAPES) -
Finance Code 001. At COPPE/UFRJ the samples were aged in thermal bath and the mechanical tests were
carried out.

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