Corrosion Engineering (Practical)

Name: Farwa Naeem Roll No: 16MME-S2-317

Semester: 6th Session: 2016-20

Date of Submission: 12/11/2019

Experiment No. 1
Calculate the weight loss of Aluminum in a 0.5 M Sodium Sulphate solution as per NACE-
TM-0169/ASTM G31

Lab Instructor Signature: ________________

Grade/Marks: _______________
Figure 1-Aluminum sample in an unclean condition

Figure 2- Aluminum sample in a clean condition

Figure 3- Measuring weight of the cleaned sample

Experimental Title
Calculate the weight loss of Aluminum in a 0.5 M Sodium Sulphate solution as per NACE-
TM-0169/ASTM G31

Objective
Objective of this experiment is to find out the Weight loss rate/ Degradation rate (decrease in
the metal weight with time in a specific electrolyte) of the aluminum sample in a 0.5 M
sodium sulphate and also observe the change in physical & chemical parameters due to metal
and electrolyte interact with the passage of specific time interval.

Principle
Dissolution takes place as metal atoms are ionized and pass into solution, leaving their
electrons within the original metal surface. Whereas free electrons within the metal are taken
up by chemical species such as O2 and H2O in reduction reactions.
Other parameters like Conductivity & Temperature increase with increase in ion formation.
pH decreases with increasing temperature i.e. acidic.

Background
When metal/ alloy is dipped in an electrolyte, corrosion takes place by;
1. Chemical reaction
2. Electrochemical reaction
3. Physical reaction (Mechanical Reaction)
Components of corrosion process includes;
1. Anode
2. Cathode
3. Electrolyte
4. Metallic path
If any of the component is missing, corrosion will not occur.
Parameters like pH, temperature and conductivity will help determining ions presence in
solution. As ion formation is directly related to corrosion process.
Standard for experiment

 NACE-TM0169-2000
 ASTM G31
Figure 4- Measuring Conductivity and temperature on pH/mV/EC/TDS & Temperature
Meter AD8000, Adwa instrument, Hungry

Figure 5- Measuring pH using pH meter

Figure 6- Al sample immersed in Electrolyte

Apparatus
 1. Drill Press
2. Vernier caliper
3. Emery paper (P120, P250, P320)
4. pH meter
5. Thermometer
6. Conductivity meter
Materials
1. Aluminum metal sample
2. Sodium sulphate
3. Water
Procedure
1. Took the photograph of the aluminum sample in an unclean condition with the white
background as shown in the figure 1.
2. A hole was made on the top of the aluminum sample by using a drill machine (Drill Press,
ZJ4110, Capital Company, Pakistan). (hanging purpose).
3. Calculated the diameter of the drill bit by using Vernier caliper. That also tell the hole
size.
Diameter of Drill bit = 0.383 cm
Radius of Holes = 0.192 cm
4. Grinded the sample with the help of emery paper (P120, P250, P320) to remove
impurities from the surface of the metal and to expose is completely to electrolyte.
5. Again, took the photograph of the sample in a clean condition with the white background
as shown in figure 2.
6. Measured the weight (Figure 3) and dimensions (Length, Width and Thickness) of the
sample after cleaning, to calculate the surface area of the sample by using the following
formula.
Surface Area = 2[( L ×W )+(T ×W )+( L×T )−π r 2 ]
7. Prepared a solution of 0.5 M sodium sulphate (electrolyte).
8. Measured its conductivity, temperature with the help of coordinate measuring machine
(pH/mV/EC/TDS & Temperature Meter AD8000, Adwa instrument, Hungry) see figure
4, pH and color of solution (Figure 5). Immersed the aluminum sample in 0.5 M sodium
sulphate solution for one week (7 days) to undergo corrosion (Figure 6).
9. After one week took out the sample. Took photograph with white background.
10. Again, measured its conductivity, temperature with the help of coordinate measuring
machine, pH and color of solution.
11. Cleaned sample by cleaning solution.
12. Measured weight and dimensions.
 Results & calculations
Specimen: Aluminum metal Cleaning Solution: _____________
Solution: 0.5 M Na2SO4

Table 1- Corrosion rate measurement of Al by Weight Loss method

Sr Time Thickness Length Widt Surface Densit Initial Final Weight Corrosion
. (hours) (cm) (cm) h Area y weigh Weight Loss rate
No (cm) (cm2) (g.cm-3) t (g) (mg)
(g)
(gmd (mpy)
)
1. 0 0.262 4.987 3.760 19.052 2.75 12.89

pH of electrolyte = 6
Conductivity of electrolyte = 63.3 mS
Temperature = 29.6 ℃
Color of electrolyte = colorless

After 1 week
Figure 5: Photograph of 0.5 M sodium sulphate solution in which aluminum sample is
immersed (after 1 week)

Figure 6: Photograph of Aluminum sample before cleaning (after 1 week)

Figure 7: Shows pH of the electrolyte

Procedure
1. Photograph of 0.5 M sodium sulphate solution in which aluminum sample was
immersed, was taken, as shown in figure 1.
2. Again, photograph of aluminum sample when taken out of 0.5 M sodium sulphate
solution, was taken as shown in figure 2.
3. The pH, Conductivity, Temperature and color of 0.5 M sodium sulphate solution was
noted as shown in figure 3 & 4.
4. Aluminum sample was cleaned with 70% nitric acid (HNO3) for 2-3 min. followed by
light scrub using cotton at room temperature.
5. Sample was dried using dryer (Dryer, JB-4, Conversion). Photograph of aluminum
sample was taken as shown in figure 5.
6. Weight and dimensions (Length, width & thickness) of aluminum sample was
measured to calculate surface area and corrosion rate.
7. Again, aluminum sample was immersed in 0.5 M sodium sulphate for further
observations. (figure 6)
Figure 8: Shows Conductivity & Temperature measurement of electrolyte

Figure 9: Photograph of Aluminum sample after cleaning (after 1 week)

Figure 6: Shows Al sample immersed again

Discussion
Coupons method of corrosion testing is the most common of all corrosion rate measurements.
A clean coupon of material of interest is measured, weighted, exposed to a corrodent for a
known period, removed, cleaned and reweighed. The rate of metal loss due to corrosion is
calculated then.
We were provided with an aluminum sample (as coupon) to calculate weight loss /
degradation rate i.e. changes in sample with change in environment. It’s a time dependent
process. Corrosion based upon three reactions
1. Chemical reaction
2. Electrochemical reaction
3. Physical reaction.
And have four components
1. Anode
2. Cathode
3. Electrolyte
4. Metallic path
But aluminum hardly found any of above component. Hence the corrosion observed in
sample was too low to neglect. None of above reaction take place. Reason behind this is
corrosion resistant property of Al plus some structure hardening of the sample as the sample
was cold worked (hammered at room temperature) in order to remove its curve and prepare it
for grinding etc.
Although conductivity and temperature of 0.5 M Na 2SO4 electrolyte changed a bit in this time
duration. Electrolyte is a solution conduct electricity by either anions or cations. So,
conductivity increase, as number of ions increase. Meanwhile as temperature increase, ions
solubility in solution also increase. Present case is contrary, as very small number of ions
precipitate out. This factor cause decrease in conductivity and temperature.
 Results & Calculation
Specimen: Aluminum metal Cleaning Solution: 70 % HNO3
Solution: 0.5 M Na2SO4

Table 2: Corrosion rate measurement of Al by Weight Loss method

Sr. Time Thickness Length Width Surface Density Initial Final Weight Corrosion
No (days) (cm) (cm) (cm) Area (g/cm3) weight Weight Loss rate
2
(cm ) (g) (g) (mg)
(gmd) (mpy)
1. 0 0.262 4.987 3.760 41.852 2.75 12.89 -- -- -- --
2. 7 0.26 4.993 3.792 42.202 2.75 12.89 12.89 0 0 0

Initial readings of electrolyte Readings of electrolyte After 1 week

pH of electrolyte = 6 pH of electrolyte = 6
Conductivity of electrolyte = 63.3 mS Conductivity of electrolyte = 62.2 mS
Temperature = 29.6 ℃ Temperature = 24.8 ℃
Color of electrolyte = colorless Color of electrolyte = colorless

After 2 week

After 3 week
Figure 10: Photograph of 0.5 M sodium sulphate solution in which aluminum sample is
immersed (after 21 days)

Figure 11: Photograph of Aluminum sample before cleaning (after 21 days)

Figure 12: Shows pH of the electrolyte after 21 days

Procedure
1. After 21 days, Photograph of 0.5 M sodium sulphate solution in which aluminum
sample was immersed, was taken, as shown in figure 1.
2. Again, photograph of aluminum sample when taken out of 0.5 M sodium sulphate
solution, was taken as shown in figure 2.
3. The pH, Conductivity, Temperature and color of 0.5 M sodium sulphate solution was
observed & noted as shown in figure 3 & 4.
4. Aluminum sample was cleaned with 70% nitric acid (HNO3) for 2-3 min. followed by
light scrub using cotton at room temperature.
5. Sample was dried using dryer (Dryer, JB-4, Conversion). Photograph of aluminum
sample was taken as shown in figure 5.
6. Weight and dimensions (Length, width & thickness) of aluminum sample was
measured to calculate surface area and corrosion rate.
7. Again, aluminum sample was immersed in 0.5 M sodium sulphate for further
observations. (figure 6)
Figure 13: Shows Conductivity & Temperature measurement of electrolyte after 21 days

Figure 14: Photograph of Aluminum sample after cleaning (after 21 days)

Figure 6: Shows Al sample immersed again

Discussion
After 21 days, again little ions deposition over the surface of Al sample immersed in 0.5 M
Na2SO4 solution is observed, visible in the form of white matter (aluminum oxide), see figure
6. Including, our sample contain a crack, which was not quite visible early but propagates
deeper with the passage of time and became visible. This is because of the reason that
electrolyte being little acidic, etched the sample and reveal the structure. But still this has no
effect on weight and surface area of overall Al sample. Variation in thickness, length & width
(From table 1) is just a human error. Therefore, we can call it just surface imperfections, not
corrosion.
Conductivity and temperature of 0.5 M Na2SO4 electrolyte changed a bit in this time duration.
Conductivity decreases indicating ions precipitation and settling at the bottom of flask and on
the surface of Al sample. Decrease in temperature of 0.5 M Na 2SO4 electrolyte indicate the
same factor i.e. decrease in solubility of ions in solution.
 Figure 15: Precepted ions visible on surface.

Results & Calculation

Specimen: Aluminum metal Cleaning Solution: 70 % HNO3
Solution: 0.5 M Na2SO4 Radius of Holes: 0.192 cm

Table 3: Corrosion rate measurement of Al by Weight Loss method

Sr. Time Thickness Length Width Surface Density Initial Final Weight Corrosion
No (days) (cm) (cm) (cm) Area (g/cm3) weight Weight Loss rate
(cm2) (g) (g) (mg)
(gmd) (mpy)
1. 0 0.262 4.987 3.760 41.852 2.75 12.89 -- -- -- --
2. 7 0.26 4.993 3.792 42.202 2.75 12.89 12.89 0 0 0
3. 14 0.259 4.988 3.791 42.134 2.75 12.89 12.89 0 0 0
4. 21 0.257 4.987 3.785 42.03 2.75 12.89 12.89 0 0 0

Surface Area = 2[( L ×W )+(T ×W )+( L×T )−π r 2 ]

Initial readings of electrolyte Readings of electrolyte After 21 days

pH of electrolyte = 6 pH of electrolyte = 6
Conductivity of electrolyte = 63.3 mS Conductivity of electrolyte = 61.1 mS
Temperature = 29.6 ℃ Temperature = 23.0 ℃
Color of electrolyte = colorless Color of electrolyte = colorless

After 4 week

Figure 16: Photograph of 0.5 M sodium sulphate solution in which aluminum sample is
immersed (after 28 days)
Figure 17: Photograph of Aluminum sample before cleaning (after 28 days)

Figure 18: Shows pH of the electrolyte measured by pH meter, after 28 days

Procedure
1. After 28 days, Photograph of 0.5 M sodium sulphate solution in which aluminum
sample was immersed, was taken, as shown in figure 1.
2. Again, photograph of aluminum sample when taken out of 0.5 M sodium sulphate
solution, was taken as shown in figure 2.
3. The Conductivity & Temperature of 0.5 M sodium sulphate solution was measured
using pH/mV/EC/TDS & Temperature Meter AD8000, Adwa instrument, Hungry as
shown in figure 4. pH by pH meter and color was noted as shown in figure 3.
4. Aluminum sample was cleaned with 70% nitric acid (HNO 3) for 2-3 min., followed
by light scrub using cotton at room temperature. And was rinsed then, by tap water.
5. Sample was dried using dryer (Dryer, JB-4, Conversion). Photograph of dried
aluminum sample was taken as shown in figure 5.
 6. Weight and dimensions (Length, width & thickness) of aluminum sample was
measured using weighing balance and Vernier caliper respectively, to calculate
surface area and corrosion rate.
7. Again, aluminum sample was immersed in 0.5 M sodium sulphate for 7 day for
further observations. (figure 6)

Figure 19: Measuring Conductivity and temperature of electrolyte on pH/mV/EC/TDS &

Temperature Meter AD8000, Adwa instrument, Hungry, after 28 days
Figure 20: Photograph of dried Aluminum sample after cleaning (after 28 days)

Figure 6: Shows Al sample immersed again for next seven days

Discussion
It is a property of aluminum that it has good corrosion resistance. This is due to the formation
of passive thin oxide film on the surface of aluminum. This is the reason that even after 28
days no change in weight and surface area of overall Al sample is observed, little ions
deposition/ oxide layer over the surface of Al sample immersed in 0.5 M Na 2SO4 solution is
observed, visible in the form of white matter, see figure 6. Already present cracks are also in
their place, without any variation. Variation in thickness, length & width (From table 1) is
just a human error.
Conductivity and temperature of 0.5 M Na2SO4 electrolyte changed a bit in this time duration.
Conductivity decreases indicating ions precipitation and settling at the bottom of flask, and
on the surface of Al sample as shown in figure 6. Decrease in temperature of 0.5 M Na 2SO4
electrolyte indicate the same factor i.e. decrease in solubility of ions in solution.
Figure 21: Precepted ions visible on the surface of sample and at the bottom of flask.
 Results & Calculation
Specimen: Aluminum metal Cleaning Solution: 70 % HNO3
Solution: 0.5 M Na2SO4 Radius of Holes: 0.192 cm

Table 4: Corrosion rate measurement of Al by Weight Loss method

Sr. Time Thickness Length Width Surface Density Initial Final Weight Corrosion
No (days) (cm) (cm) (cm) Area (g/cm3) weight Weight Loss rate
(cm2) (g) (g) (mg)
(gmd) (mpy)
1. 0 0.262 4.987 3.760 41.852 2.75 12.89 -- -- -- --
2. 7 0.26 4.993 3.792 42.202 2.75 12.89 12.89 0 0 0
3. 14 0.259 4.988 3.791 42.134 2.75 12.89 12.89 0 0 0
4. 21 0.257 4.987 3.785 42.03 2.75 12.89 12.89 0 0 0
5. 28 0.260 4.994 3.786 42.146 2.75 12.89 12.89 0 0 0

Surface Area = 2[( L ×W )+(T ×W )+( L×T )−π r 2 ]

Initial readings of electrolyte Readings of electrolyte After 28 days

pH of electrolyte = 6 pH of electrolyte = 6
Conductivity of electrolyte = 63.3 mS Conductivity of electrolyte = 58.2 mS
Temperature = 29.6 ℃ Temperature = 22.1 ℃
Color of electrolyte = colorless Color of electrolyte = colorless