Professional Documents
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in Sulfuric Acid
J. Liu1 and C. Vipulanandan, M.ASCE2
Abstract: Epoxy-based coatings are used in the rehabilitation and protection against acid attack in industrial and wastewater facilities
made of concrete and clay bricks. In this study, the performance of two epoxy-based coatings on sewer grade clay bricks was evaluated
using a combination of bonding strength and acid resistant tests over a period of three years. The test results showed that the bonding
strength of the epoxy coatings depended on the dry and wet surface conditions of the clay brick at the time of coating. The bonding
strength varied from 0.2 MPa to 3 MPa. The coating films effectively reduced the liquid uptake of the coated clay bricks and pinholes
influenced the weight gain of the coated clay bricks. There was no direct relationship between bonding strength and acid resistant 共weight
gain兲 of the tested coatings. A film model was developed to predict the weight change in coated clay bricks. The mass transfer coefficients
of the coatings varied from 0.8⫻10⫺12 to 7.8⫻10⫺12 m2 /s and 1.7⫻10⫺12 to 6.6⫻10⫺12 m2 /s in deionized water and 3% sulfuric acid,
respectively.
DOI: 10.1061/共ASCE兲0899-1561共2004兲16:4共349兲
CE Database subject headings: Epoxy coatings; Clays; Bricks; Bonding strength; Acids; Models; Verification.
Introduction 1999兲. The surface moisture will depend on the porosity of the
substrates and hydrostatic pressure due to the groundwater table.
Clay bricks along with cement concrete have been widely used in Coatings can debond and blister if the hydrostatic pressure ex-
the construction of industrial and municipal wastewater facilities. ceeds the tensile adhesion of the coating material. Bonding be-
Many municipalities are discovering that cement concrete and tween the clay brick surface and the coating material is another
other cement-based materials in the wastewater collection and important factor that must be evaluated to determine the long-
treatment facilities are subjected to microbial-induced deteriora- term performance of the coating.
tion and the cementitious materials are degrading rapidly 共Sand Since several factors in the field can affect the performance of
et al. 1994; Soebbing et al. 1996兲. In most cases, the pH on the a coating, it is important to identify the factors through controlled
surface of sewer pipes and manholes is less than 1 共in the worst experiments where important variables are studied one at a time
case, the pH is 0.5兲 共Islander et al. 1991兲; hence, it is important to to evaluate coating materials used for rehabilitating and protect-
determine how to control this deterioration and extend the life of ing industrial and municipal wastewater facilities.
the facilities. Coating is one method currently being adopted to
control the degradation of wastewater facilities; however, the ef-
fectiveness of this method for rehabilitating sewer pipes and treat- Objectives
ment facilities is still in question 共Vipulanandan et al. 1996兲. Al-
though clay bricks are generally nonreactive material, they are The overall objective is to investigate the long-term performance
bonded together with cement mortar, and hence, it is important to of epoxy coated sewer clay bricks. Specific objectives are to: 共1兲
coat the mortar and clay bricks together to protect wastewater Determine the effect of initial moisture 共in the brick兲 on the bond-
systems. ing strength; 共2兲 determine the behavior of coated bricks with and
Wastewater and industrial facilities are generally wet and without pinholes in water and 3% sulfuric acid; 共3兲 determine the
hence the application of coating materials onto porous surfaces is correlation between bonding strength and chemical resistance;
considered a challenge and must be evaluated 共Steele and Steele and 共4兲 model the behavior of liquid uptake by coated clay bricks.
1
Post Doctoral Fellow, Center for Innovative Grouting Material and
Technology 共CIGMAT兲, Dept. of Civil and Environmental Engineering, Testing Program
Univ. of Houston, Houston, TX 77204-4003.
2
Chairman, Professor, and Director of the Center for Innovative
Grouting Material and Technology 共CIGMAT兲, Dept. of Civil and Envi- Clay Brick Properties
ronmental Engineering, Univ. of Houston, Houston, TX 77204-4003. The average compressive strength of the dry clay brick was 36.9
Note. Associate Editor: Jason Weiss. Discussion open until January 1, MPa 共5,355 psi兲 which meets the requirements in ASTM C 32
2005. Separate discussions must be submitted for individual papers. To
共ASTM 1999兲 for sewer brick 关minimum compressive strength 34
extend the closing date by one month, a written request must be filed with
the ASCE Managing Editor. The manuscript for this paper was submitted MPa 共5000 psi兲兴. The average compressive strength of the satu-
for review and possible publication on September 4, 2002; approved on rated clay bricks was 29 MPa 共4,200 psi兲. The average pulse
September 23, 2003. This paper is part of the Journal of Materials in velocity of the clay brick was 2552⫾100 m/s 关共8,372 ft/s兲 共based
Civil Engineering, Vol. 16, No. 4, August 1, 2004. ©ASCE, ISSN 0899- on 25 specimens兲兴. The average unit weight of clay brick speci-
1561/2004/4-349–355/$18.00. mens varied between 19.0 kN/m3 共120 pcf兲 and 22.1 kN/m3 共138
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Table 1. Properties of Epoxy Coating Materials
Pulse Hardnessb
Coating Densitya velocitya Thicknessb Application
material 共kg/m3兲 共m/s兲 Barcol Shore 共mm兲 condition
Epoxy-1 1,680 2,829 35– 42 67–72 3.2 Dry and wet surfaces
Epoxy-2 1,530 2,730 36 – 40 71–75 1.5 Dry and wet surfaces
Remarks Difference was 10% Difference was 3% Similar hardness Different coating Physical properties
thickness of the coatings
varied by no more
than 10%
a
Bulk coating material properties.
b
Coating film properties.
pcf兲. The average flexural strength was 7.0 MPa 共1,000 psi兲. The CIGMAT „2000b… CT-3 共Modified ASTM C 321兲. In this test,
average direct tensile strength of clay brick was 2.3 MPa 共340 the coating was sandwiched between a pair of clay bricks and
psi兲 关varied from 1.4 共210 psi兲 to 3.2 MPa 共468 psi兲兴. The water then tested for bonding strength 关Fig. 1共b兲兴.
absorption of the sewer clay brick was 17% after 24 h in deion-
ized 共DI兲 water.
Chemical Resistance
In order to study the chemical resistance of the coated clay bricks,
Coating Properties
CIGMAT CT-1 共CIGMAT Standard 共1999兲, modified ASTM G
Two different epoxy coatings were selected for testing. The bulk 20兲 was used. The coated specimens were immersed in a selected
material properties of the two coatings were determined using 38 test reagent to half the specimen height in a closed bottle so that
mm diameter⫻76 mm height cylindrical specimens and the re- the specimens were exposed to the liquid phase and vapor phase
sults are summarized in Table 1. Since there are no standard tests 共Fig. 2兲. In this test, 51 mm 共2-in.兲⫻76 mm 共3-in.兲⫻152 mm
to evaluate the performance of coated clay brick, ASTM tests 共6-in.兲 clay brick prism specimens were used. Dry and wet speci-
were modified and used in this investigation. mens were coated on all sides and tested. For the test, two pin-
holes were drilled into the coated specimen approximately 15 mm
deep to represent defects in the coating. In order to determine the
Bonding Strength
effect of pinhole size, diameters of 3 mm, 6 mm, and 13 mm were
Bonding strength between sewer clay bricks and coating materials selected for testing. The test reagents selected for this study were:
was determined over a period of three years. The clay bricks 共dry 共1兲 DI 共pH⫽5 to 6兲, and 共2兲 3% sulfuric acid solution 共pH⫽0.45;
and wet兲 were coated by respective manufacturers and the coated representing the worst reported condition in municipal wastewater
specimens were cured under water up to the time of testing. The systems兲. In this test, the changes in 共1兲 the weight of specimen
dry clay bricks were kept at the room environment 共temperature and 共2兲 the appearance of specimen were monitored at regular
23°C⫾2 and humidity 55%⫾5兲 while the wet clay bricks were intervals. A total of 32 coated specimens 共16 dry and 16 wet兲 were
submerged in water for 7 days before coating. Two different tested for each coating material. Control tests were performed
bonding tests: the Center for Innovative Grouting Materials and with no pinholes.
Technology 共CIGMAT兲 CT-2 关CIGMAT Standard 共2000a兲, modi-
fied ASTM D 4541兴 and CIGMAT CT-3 关CIGMAT Standard
共2000b兲, modified ASTM C 321兴 were used to determine the Results and Discussion
bonding strengths of coatings to clay bricks.
CIGMAT „2000a… CT-2 共Modified ASTM D 4541兲.In this
Bonding Strength
test, 51 mm 共2-in.兲 diameter circular area was used for testing
关Fig. 1共a兲兴. Coated clay bricks were cored using a diamond core The failure types were characterized as follows: 共1兲 Substrate
drill to a predetermined depth to isolate the coating. A metal fix- failure—Type-1, 共2兲 coating failure—Type-2, 共3兲 bonding
ture was then glued to the isolated coating section using a rapid failure—Type-3, and 共4兲 bonding and substrate failure—Type-4.
setting epoxy.
Fig. 1. Bonding test setup: 共a兲 CIGMAT CT-2 test and 共b兲 CIGMAT Fig. 2. Chemical tests on coated clay brick with pinholes-CIGMAT
CT-3 test CT-1 test
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Type-1 is the most preferred, where the substrate fails indicating
that the bonding strength is higher than the tensile strength of the
clay bricks. The failure types observed in the tests are shown in
Fig. 3. The variations of bonding strength with time for both
coatings are shown in Figs. 4 and 5 using CIGMAT CT-2 and
CT-3 tests, respectively.
Based on the CIGMAT CT-2 tests 关Figs. 4共a and b兲兴, Epoxy-1
initially had a very high bonding strength with the dry clay brick
surface and the failure was Type-1 where the clay bricks failed.
After a longer period of immersion, the bonding strength of
Epoxy-1 on the surface of dry clay bricks decreased and the fail-
ure type also changed from Type-1 to Type-3 共bonding failure兲.
Epoxy-1 had a lower bonding strength with wet clay bricks ini-
tially and the failure type was Type-3 关Fig. 3共c兲兴. Epoxy-1 gradu-
ally developed the bonding strength and the failure types changed
from Type-3 to Type-1 and Type-2. The results indicate that the
surface moisture conditions affected the performance of the
Epoxy-1 coating. Epoxy-2 had a good bonding strength to both
dry and wet clay brick surfaces during the testing period. The
bonding strengths of Epoxy-2 to dry and wen clay bricks were all
above the 1.4 MPa 关200 psi, which was recommended by Liu and
Vipulanandan 共1999兲兴 as the minimum required bonding strength
of coating with concrete and the failure type was Type-1.
Based on CIGMAT CT-3 tests 关Figs. 5共a and b兲兴, Epoxy-1 had
mixed results with both dry and wet clay brick surfaces; failure
Types-1, 2, and 3 were observed. Epoxy-2 had very consistent test
results and the bonding strengths of Epoxy-2 to clay bricks deter-
mined using the CIGMAT CT-3 test were comparable to the
bonding strength determined using the CIGMAT CT-2 test.
From the bonding test results, failure Types-1, 2, and 3 were
observed with Epoxy-1 coated clay bricks. The results indicate
that the bonding strength of Epoxy-1 to clay bricks was sensitive
to the surface moisture conditions of the clay bricks. On the other
hand, the bonding strength of Epoxy-2 coating to clay bricks was
not influenced by the initial dry/wet nature of the clay bricks. All
failures were Type-1 关Fig. 3共a兲兴 for Epoxy-2 coated clay bricks in
the CIGMAT CT-2 and the CIGMAT CT-3 tests.
Chemical Resistance
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Fig. 4. Bonding test results from CIGMAT CT-2 tests: 共a兲 dry coated Fig. 5. Bonding test results from CIGMAT CT-3 tests: 共a兲 dry coated
clay brick and 共b兲 wet coated clay brick clay brick and 共b兲 wet coated clay brick
wet clay bricks had a 6.8% weight increase during the same pe-
riod. The results indicate that the surface conditions affected the
chemical resistance 共uptake of acid兲 of Epoxy-2 coating when
immersed in 3% sulfuric acid solutions.
The effects of pinholes on the weight increase of Epoxy-2
coated clay bricks are shown in Fig. 8, where specimens with
pinholes showed faster and greater weight gain as compared to
specimens without pinholes. For the range of pinhole sizes tested,
its effect on the rate and total weight gain are inconclusive.
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Fig. 7. Weight changes of coated clay bricks for various solutions:
共a兲 deionized water 共DI兲 and 共b兲 3% sulfuric acid Fig. 8. Weight changes for coated clay bricks with pinholes in 3%
sulfuric acid: 共a兲 dry coated clay brick and 共b兲 wet coated clay brick
S iCT ⫺S 0
CT
⫽
x
ᐉ
(1) W 共 t 兲 ⫽A 冕
0
t
Fdt⫽
AgD CT S CT
ᐉ
0
冕 t
0
e ⫺
CT
t
dt (4)
冉 冊
constant.
dS Eq. 共5兲 is the model to predict the weight change in coated
F⫽⫺D CT (2)
dx clay bricks after different periods of immersion. If the initial
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Table 2. Material Parameters in Deionized 共DI兲 Water and 3%
Sulfuric Acid
Mass transfer
coefficient, D CT Material parameter
(⫻10⫺12 m2 /s)  CT (⫻10⫺8 l/s)
Coating Surface 3% sulfuric 3% sulfuric
material condition DI water acid DI water acid
Epoxy-1 Dry 7.80 5.49 2.88 2.00
Wet 1.42 6.61 0.69 2.94
Epoxy-2 Dry 2.03 1.67 1.92 1.74
Wet 0.80 6.64 1.84 3.95
Remarks Dry and wet Dry⬎wet Wet⬎dry Dry⬎wet Wet⬎dry
condition
AgS CT
0 D CT CT
⌬W%⫽ CT ᐉ
共 1⫺e ⫺ t 兲 ⫻100 (7)
W 0
The ultimate saturation for bulk coating material (S CT 0 ) was
obtained from immersion tests on pure coating materials. For the
epoxy coatings tested, the average values of S CT0 were 11 kg/m
3
3
and 13 kg/m in DI water and 3% sulfuric acid, respectively. By
using Eq. 共7兲 to predict the weight change of the coated clay
brick, the mass transfer coefficient, D CT and the material param-
eter  CT of coatings under different testing conditions were ob-
tained. The lower the values of D CT and  CT , the better the coat-
ing in protecting the clay bricks from weight gain.
The values of the mass transfer coefficient, D CT and the coat-
ing material parameter  CT are summarized in Table 2 for the two
epoxy coatings. The model predictions are compared to the ex-
perimental data in Figs. 11共a and b兲. The model predictions
agreed with the experiment results. From Table 2, the mass trans-
fer coefficients (D CT ) of the epoxy coatings on the dry surface
conditions were higher than on the wet surface condition in DI
water. On the other hand, the mass transfer coefficients (D CT ) of
Fig. 9. Relationship between the bonding strength and the chemical the epoxies on the dry surface conditions were lower than on the
resistance of the epoxy coatings: 共a兲 deionized water 共DI兲 and 共b兲 3% wet surface conditions in 3% sulfuric acid. The results indicate
sulfuric acid that the mass transfer coefficients (D CT ) not only depend on the
coating material and the type of solution but also depend on the
surface conditions at the time of application. The material param-
weight of the specimen was W 0 , the percentage weight change eter  CT was higher for dry conditions as compared to wet con-
(⌬W) of the tested specimen can be represented as ditions in DI water and the trend was reversed in 3% sulfuric acid
solution. The parameter  CT varied between 0.7 to 3.95
W共 t 兲 ⫻10⫺8 l/s. The parameters D CT and  CT for Epoxy-1 were higher
⌬W%⫽ ⫻100 (6)
W0 than the Epoxy-2 in the dry conditions and the results were re-
where W 0 ⫽initial weight of the specimen 共kN兲. versed in the wet conditions. The results indicate that Epoxy-2
Eq. 共6兲 can be rewritten as was better than Epoxy-1 in the dry conditions while Epoxy-1 was
better than Epoxy-2 in the wet conditions.
Conclusions
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gain of the coated clay bricks; hence in evaluating coating
materials, both the bonding strength and the chemical resis-
tance of coated clay bricks must be studied.
4. The predictions of weight change in coated clay bricks using
the film model were in agreement with the experimental
data. The mass transfer coefficient and the coating parameter
for coating materials have been determined. These param-
eters can be used to compare the performance of coatings.
Acknowledgments
This project was supported by the CIGMAT under grants from the
City of Houston, National Science Foundation 共Nos. CMS-
9526094 and CMS-9634685兲, and various industries.
References
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