Experiment no -1

Corrosion of Mild Steel

1.1 Objective
The objective of this experiment is to study the effect of the concentration of H 2SO4, exposure
time and temperature on the corrosion rate of mild steel.
1.2 Introduction
The impact of corrosion is pervasive in daily life, triggering accidents in industries, on highways,
and at homes. Financially, it incurs a hefty 4-5% loss of industrialized nations' GDP yearly.
Gaining insights from electrochemistry, materials science, and corrosion could potentially avert
25% of this expense, emphasizing its crucial relevance. Corrosion is a significant concern in
industries where metals are exposed to aggressive environments. Mild steel, commonly used for
its favorable mechanical properties, is susceptible to corrosion under certain conditions and cost.
Mild steel is used as a structural member in bridges, buildings etc. It is widely used for the
construction of storage tanks, ships etc. It is readily available, easy to produce with outstanding
ductility and toughness. Its high machinability and weldability aids into its application in almost
all engineering fields. The exposure of mild steel leads to acidic medium leads to corrosion
hence Corrosion is responsible for failure of material. Understanding the effects of different
H2SO4 concentrations, exposure time and at different temperatures on the corrosion resistance of
mild steel is crucial for material selection and corrosion control in relevant applications. Mild
steel is one of the major construction materials. It is excessively used in oil and chemical
industries for handling acid and salt solutions.
2.0 Theory
Anodes and Cathodes:
When mild steel (which is primarily composed of iron) is immersed in sulfuric acid (H 2SO4), it
undergoes both anodic and cathodic reactions. These reactions are part of the overall process
known as corrosion. Corrosion involves the degradation of metals due to electrochemical
reactions with their environment. The electrochemical reactions in these cells can be divided into
two reactions:
1. Anodic reactions
2. Cathodic reactions
Anodic Reaction:
At the anode, iron in the mild steel undergoes oxidation, releasing electrons and forming iron
ions. In the case of sulfuric acid, the anodic reaction can be represented as follows:
2 Fe(s) → 2 Fe²⁺(aq) + 4 e⁻
This reaction involves the conversion of solid iron (Fe) into iron ions (Fe² ⁺) by losing electrons
(e⁻). These electrons are released into the metal and can flow through it as an electric current.
Cathodic Reaction:
At the cathode, the reduction of hydrogen ions (H⁺) from sulfuric acid occurs. This reduction
involves the gain of electrons and the formation of hydrogen gas. The cathodic reaction can be
represented as follows:
2 H⁺(aq) + 2 e⁻ → H2(g)
In this reaction, hydrogen ions (H⁺) from the sulfuric acid accept electrons (e⁻) at the cathode
and are reduced to form hydrogen gas (H2).
Overall Corrosion Reaction:
The overall corrosion reaction involving both the anodic and cathodic reactions can be
represented as follows:
2 Fe(s) + 2 H⁺(aq) → 2 Fe²⁺(aq) + H2(g)
In this reaction, iron (Fe) reacts with hydrogen ions (H⁺) from sulfuric acid to form iron ions
(Fe²⁺) and release hydrogen gas (H2).
In most cases, aside from contamination problems, the primary concern where corrosion is
present, is the life (usually in years) of metals in question.
The corrosion rate is expressed as Mil’s penetration per year (mpy) and determined in the given
formula.
534 Δw
Therefore, the corrosion rate is:
DAT
where, ∆W = weight loss (gms)
D = density of the specimen, (g/cm3)
A = Surface area of specimen, (sq. in)
T = exposure time, (hr.).
The corrosion rates of resistant materials generally range between 1 and 200 mpy. The relative corrosion
resistance of a material can be evaluated using the following criteria:

Relative Corrosion Resistance mpy

outstanding <1
excellent 1-5
good 5-20
Fair 20-50
Poor 50-200
unacceptable >200
 Figure mechanisms of corrosion reaction at the interface
Sir, please check suitable figure location
2.1 Experimental Design:
The effect of the concentration of H 2SO4exposure time and environmental temperature may
affect the corrosion rate. Therefore, to optimize the minimum corrosion rate, design of
experiment (DOE), modelling and simulations are required. Therefore, in this investigation, Box-
Behnken Design of response surface methodology has been adopted. The steps to design the
experiment is described below.
Step-1 Choose the factors (variables) that affect the process or output

Step-2 Select the levels for each factor based on experimentation.

Input Level used (-1, 0 and 1)

parameters
Low Middle High
% of H2SO4 5 12.5 20
Temperature 0C 30 40 60
Time 30 45 60

Step-3 Design an experimental matrix using techniques Box-Behnken Design of response

surface methodology using MINITAB

Run Order % of H2SO4 Temperature oC

 1 5 45
2 12.5 36
3 12.5 48.7
4 12.5 36
5 12.5 23.2
6 12.5 36
7 1.9 36
8 12.5 36
9 20 45
10 20 27
11 23.1 36
12 5 27
13 12.5 36

2.2 Data Collection:

 Conduct experiments based on the experimental matrix described in step 2.
 Measure the response variable for each combination of factor levels.
2.3 Optimization:
 Define the objective of optimization, such as minimizing the response.
 Use optimization algorithms of genetic algorithms to find the optimal factor levels that
satisfy the objective.
 Validation of Optimal Conditions
 Conduct experiments at the optimized factor levels to validate the predicted response.
 Compare the actual response with the predicted response from the model
3.0 Experimental Procedure:
3.1 Sample Preparation:
The mild steel specimens were prepared systematically for the experiment. We have taken
rectangular bar of thickness of 5 mm and width 25mm to make the samples. We have cut the
sample with respect to length as per ASTM G31 Standards. They were polished using different
grades of emery paper to achieve a smooth surface which is free from roughness and scale. After
polishing, the specimens were rinsed with deionized water to remove loose particles and
contaminants. Subsequently, an ultrasonic bath was employed, immersing the specimens in a
cleaning solution to further eliminate any remaining impurities. The cleaned specimens were
then dried in a hot air oven at temperatures between 80 and 100 degrees Celsius, ensuring
uniform drying without contact between the specimens. After cooling to room temperature, the
individual weights of the specimens were measured accurately using a precision balance.
Throughout the process, safety measures were followed.

Fig.1 Schematic diagram of the sample

3.2 Experimental Setup:

Set up a series of glass beakers, each containing H2SO4 solutions with different concentrations (5
to 20%). Equip each beaker with a temperature-controlled heating system to maintain the desired
temperature (30 to 80 degrees Celsius).

Figure.2 Experiment setup for (a) High temperature and (b) Room temperature
3.3 Sample Immersion and Exposure:
Immerse multiple mild steel samples in each H2SO4solution in different beakers, ensuring
complete submergence and avoiding contact with the beaker walls. Prepare multiple replicates
for each H2SO4 concentration and temperature combination to ensure statistical significance.
Allow the samples to stay in the H 2SO4solutions for a predetermined duration to ensure sufficient
exposure for corrosion to occur.

Figure.3 Corrosion testing at (a) High temperature and (b) Room temperature

3.4 Corrosion Monitoring:

Regularly inspect the samples visually to observe any visible signs of corrosion. Measure the
corrosion rate using techniques such as weight loss analysis or electrochemical measurements as
per the theory discussed.

Figure 4 corroded sample in H2SO4 medium

4.Result and discussion
 4.1 corrosion rate (CR) vs % of H2SO4 concentration

Figure 5. sample plot of surace and conuter

Explanation of the diagram:

4.2 CR vs Temperature
Figure 6. sample plot of surace and conuter

Explanation of the diagram:

4.3 Weight loss vs Temperature

Figure 7. sample plot of surace and conuter

Explanation of the diagram:
 4.4 Weight loss vs volume % of concentration

Figure 8. sample plot of surace and conuter

Explanation of the diagram:

 4.5 Analysis of variance and model fitting

Source Sum of Squares df Mean Square F-value p-value

Model 2.645E+10 5 5.289E+09 36.40 < 0.0001 significant

A- % H2SO4 2.347E+10 1 2.347E+10 161.50 < 0.0001

B-Temperature 2.494E+09 1 2.494E+09 17.16 0.0043
AB 2.479E+08 1 2.479E+08 1.71 0.2328
A² 9.348E+06 1 9.348E+06 0.0643 0.8071
B² 2.090E+08 1 2.090E+08 1.44 0.2694
Residual 1.017E+09 7 1.453E+08
Lack of Fit 1.017E+09 3 3.391E+08 1.480E+05 < 0.0001 significant
Pure Error 9165.65 4 2291.41
Cor Total 2.746E+10 12

Explanation of the table:

Corrosion Rate = -21187.756+11935.693 H2SO4-1453.089T-116.628 H2SO4*T-20.608 H2SO42 +

67.675T2 1

Explanation of Equation
4.7 Model Prediction for minimum corrosion rate

Optimal HNO3 Tempeart

High 23.1066 48.5208
D: 1.000
Cur [1.8934] [24.4792]
Predict Low 1.8934 24.4792

Corrosio
Minimum
y = 3692.8544
d = 1.0000

Figure 8.
Explanation of the diagram:

4.8 Experimental validation

Optimum parameters Model predication Experimental Result %Eror

Corrosion rate
Weight loss
Conclusion: