EXPERIMENT-01

1. Objective: when it's exposed to

To analyze the corrosion behaviour of steel and copper metals,
Oxidizing and corrosive environment.
2. Theory: substances it will rust at a
1, When steelrod and copper is exposed to oxidizing
slow ratc. substances it will rust at an
2. When steelrod and copper is exposed to corrosive
accelerated rate.
warmer water the rate of rusting
3. When steel wool or copper are exposed to
should increase. increase the
should greatly
4. When steel woolor copper are exposed to bleach it
rate of corrosion.
3. Materials and equipments:
tap water, boiled water, NaCI. HCI.
Steel rod and copper strip (5 pieces of2 cm long), spoon, measuring
bleach, glass beakers, safety glasses, apron, rubber gloves, marker,
cylinder, tweezers, desiccators.
Optical microscope, weighing machine and FTIR.
4. Procedure:
preparation for the experiment.
1. Put on your Personal Protection Equipments (PPE) in the appropriate
2. Take the marker and label 12 (6 set x 2) of the glass beakers with well
labels (aforementioned exposing environment) for each of yourtest solutions as
the last one with control. Keep one steel rod and copper strip sample as
as label
reference.
approximately 2 cm long and
3. Then cut the steel rod and copper strip into 5 pieces
record the weight of each sample.
5 of the steel rod into the appropriate glass
beakers that are labelled for the steel
4. Place
approximately 50%o :area of the
rod. Similarly, repeat for copper strip. Make sure'
metal should be dipped.
after 24 hours exposure and keep
5. Take out the steel rod and copper strip samples
proper labeling. Then,dispose of the imaterials safely and
samples in desiccators with
clean up your work area.
6. Record the physical appearance using optical microscope. loss (If any ).
weight
7. Record the weight of each sample and calculate the analyzes the data.
8. Record FTIR of exposed and reference samples and
5. Results and Observations:

(). Physical Appearance

Observations/Appearance of the sample
Sr. Sample Details
No.
1. Steel Rod (tap water)
 Stcel Rod (boiled water)
Steel Rod (NaCl)
4
Steel Rod (HCI)
Steel Rod (bleach)
6
Steel Rod (Reference)
7
Copper Strip (tap water)
8.2:>CopierStib (boiled water)
Copper Strip (NaCl)
TO:Copper Strip (HCI)
12.
Copper Strip (bleach)
Copper Strip (Reference)
(ii).Surface Analysis
(ii). Weight Loss Analysis
(iv). FT0R Analysis
6. Summary (Outeomes of the experiment)
End

Note: Student must read and strictiy foiiow the safety precautions!
Safety precautions:

1. Wear your PPE to conduct the lab.

2. Food and drinks are not allowed inside the
3. Clean work area. laboratory.
4. When lab is complete dispose of all
substances safely.
Read MSDS and safety precaution for each chemical and
6. Tape metal edges. Do not use acid during
follow it.
any part of this experiment due to the danger of
7.
generating
If
cyanide gas.
have any doubt discuss with the lab
instructors.
 Experiment: 02

Objective:
ahserve and record the corrosive nature of oxidation-reduction reactions on metal surface

Theory:
Pusting of metals is a special case of metal oxidation. Iron will oxidize to form rust, Water will
eause metals to rust; this reaction can be accelerated by adding salts. In the corrosion process,
metals get oxidized. For example in mild steel (which is greater than 99% iron) the metal
corrodes according to the following:
Fe + Fe*+ 2e' (removal of electron)
These electrons are consumed by reacting with another substance (usually oxygen but it can be
H in acids) in reduction as in
Op+ 4e + 4H;0 + 40H (gain of electron)
In an acid solution, the reduction is
2H*+ 2e H2
These equations indicate that in order for metals to corrode (rust), two reactions occur: an
Oxidation that converts metal to metal ions and electrons and a second reaction which consumes
those electrons by converting oxygen and water to hydroxide ions. In order for these reactions to
occur, the electrons must be transported from the place where the metal dissolves to.the place
where the oxygen is consumed and an ionic current must also flow between the sites to complete
the circuit. This ionic current flows more easily through water containing electrolytes (i.e.
NaC),This accounts for the rapid rusting of unprotected steel in asalty environment.
The final product of iron oxidation (rust) is usually a ferric oxide (often hematite Fe203).
The initial corrosion product of the anodic reaction is ferrous (Fe2+) ion. This is subsequently
Oxidized to Fe* by exposure to oxygen. In this experiment we are looking at the initial product
only. In this experiment we can watch the corrosion reaction by using substances that produce
acolor change when they react with the products of the iron oxidation or oxygen reduction.
Recall that phenolphthalein turns pink in the presence of hydroxide and ferricyanide turns a deep
blue in the presence of iron II" (rust). (see experiment #6, Metcalfe, H. Clark, Modern
Chemistry, Holt, Reinhart and Winston, 1982, pp. 147-50).
The corrosion process may be slowed by coating the metals with other metals or
be
polymers in order to protect the metal from the corrosive environment. Examples of this can
is coated
seen in food cans which have a polymer coating and in galvanized steel where iron
with zinc.
other reduces
When we put two metals in direct contact, one can oxidize (rust) whil the
measuring
Oxygen. This reaction sets up a voltage and is the primary reaction in a.battery. By
tendencies. If metals
this voltage, it is possible to construct alistranking the metal's oxidationeach other and with an
which are far apart in oxidation tendencies are placed in contact with
some of these
electrolyte solution, severe corrosion of one metal can occur. We will examine
metal combinations in this experiment.
3.
Materials and
equipments:
01 MKaFe(CN), 01 MKife(CN),: 0.1 MNaCI solution: phenolphthalein; mild stel
galvanizcd steel sheet, polvmer coaled tin coaled steel, zinc coated steel (stze: 4x4cm).
Watch glass: dropper; fine wide-mouth
sandpaper; digital volt meter: I00-ml bottle; meter leads
Iith alligator clips;rubberstopper, hole bored; triangular file.
4. Procedures:
a) Plain Steel:
Obtain |00 ml of salt solution and add 10 drops of phenolphthalein. On a section of mild
combine 4 drops of this solution and 3 drops of potassium ferricyanide and cover with steel,a
watçhglass. Observe tor at least five minutes, What changes occur?
ne same bar do as above except use ferrocvanide. Observe for at least 5 minutes. What
CIlaliges 0cCur? Which chemical reagent (ferro or ferri) would you use to check for rust on iron?

Figure l

$ er In Figure 1, fill in the colors you see at the proper Sites.

lons are spatially separated in this salt drop experiment because the drop is thicker in the
middle than at the edges.
Electrochemical reduction reactions that produce OH- occur at the edges due to readily available
oxygen fromthe air. Electrochemical oxidation reactions occur at the middle of the drop due to
the lack ofoxygen. See Figure 2.
B ue

Rak
OH

Figure 2

b), Polymer Coated Steel:

Using the file, place a deep scratch on one area of a polymer coated steel. Place 3 drops of
ferricyanide and 4 drops of salt solution onthe scratch. On a second area of the polymer coated
lid, place the drops as above and cover with a watch glass. Observe both areas of the lid for at
least 5 minutes.

Unecrale bed
Bermlchd
 c). Tin Coated Steel:
Repeat Procedure 2 using a tin plated steel can side, tinside up. Observe for at least 8minutes.

Uron
Hirurr 4

Unscratched Scratched

d). Zinc Plated Steel:

Repeat Procedure 2using a piece of galvanized steel. Observe for Sminutes. Record in Figure 5.

Unscratched Scratched

Observe that an intense pink color forms, indicating a reaction is taking place and OH ions are
produced. No blue is seen in the drop-indicating that the iron is not rusting. Melals such as zinc
are used because these sacrificial anodes are more willing togive up electrons (oxidize) than the
iron and thus protect the iron from oxidation. Let us investigate diferent metal combinations.
e). Coin:
Following above procedures, use the salt drop technique on each of two coins with a deep
scratch on each.

5. Results and Observations:

1. Record the changes occur for at least 5 minutes on plain steel substrate polymer coated
substrate, tin coated, Zn coated and coin.
2. Record the pictures and place in the appropriate results section.
3. Which chemical reagent (ferro or ferri) would you use to check for rust on iron?

6. Summary (Outcomes of the experiment)

7. State in brief what you learnt from this experiment
End

Note: Student must read and strictly follow the safety precautions!
Safety precautions:
I. Wear your PPE to conduct the lab.
2. Food and drinks are not allowed inside the laboratory.
3. Clean work area.
4. When lab is complete dispose of all substances safely.
S. Read MSDS and safetyprecaution for each chemical and follow it.
6. Tape metal edges. Do not use acid during any part of this
experiment du to ne
danger of generating cyanide gas.
7. If have any doubt discuss with the lab instructors.
 EXPERIMENT-03
1. Objective: Detection of Stecl Corrosion with a Fe"-Enhanced Fluorescence Probe

2. Theory: We study a rhodamine-based fluorescent compound (FD2) as

corrosion
steel in 3% NaCl solution. FD2 has a desirable property of"turn-on" fluorescence indicator
for
emission via
forming a complex with Fe ions. The varying of fluorescence intensity is linked to that
weight-loss of steel. Early attack on steel was detected using fluorescence microscopy. This nonof
destructive method of initial corrosion detection can be used during maintenance before serious
damage happens.
Usually, corrosion is a dissolving of metal caused by an electrochemical reaction.
involving the clectron loss and ionization of metal. For iron-based alloy corroding in water
solution, the anodic reactions can be represented as
Fe ’ Fe' + 2e ..(1)
Fe?* + Hz0 ’ Fe(OH)* + H* ...(2)
3Fe(OH)* + H;0 ’ FesO4 + SH + 2e ...(3)
The cathodic reaction in a near neutral solution involves reduction of the dissolved oxygen
according to
0, + 2H20 + 4e’ 40H7 .i(4) :
The cathodic reaction in the acidic solution is as follows
O2 + 4H*+ 4e' ’ 2H,0
2H* + 2e ’ H2‘
.(5)
:.(6)
Metal loses electron at the anode and ionization leads to corrosion dissolution. At the:cathode,
electrons are captured and damage such as hydrogen embitterment can. occur.Early corrosion
detection by fluorescent compounds is non destructive and sensitive itechniquei: As:for steel
substrates, the ferric ion is well known as fluorescence quencher owing to its paramagnetic
nature. In this experiment, a rhodamine-based compound (FD2) is designed to: detect steel
corrosion. Figure 1shows the proposed FD2-Fe" bonding structure. The' polarizatiön cunves are
used to study the electrochemical property of steelwith and without FD2 in 3%NaCl solution.

NH,

H,N

FiGURE I Chelation o FD2 via binding withFe" on

 precautions:
Safety solütion),
thegraph (ifluoresçenc solution
(iüi) Record ()
Na;SiO4.
5. test wasusing emissionat: (c) steel
concentrátion ionsweighed(b) The samples Awashed Zn(NO:) 4.emery and 3.
Note: 6.Plproduct'
ov), Nalinto (iii)conäining e*ions. (ü)hie'i Results
Recötd fte rProcedure: Materials.
Summary with set The obtained FD2 samples diethylenetriamine),
RecórdEstimate a atloy different paper,
6. 5. 3 2 1
7. Student containing fluorescence
tluorescence
and trom has to shorld and
work
area. Food Wear the and other maý determine BaCl2.
generating
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Ifgas.Tape ReadWhen Clean
have graph MnSOcan 550nim ifromwererinsed no degreased and
(Outcomes the data
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any must gotrosion fully
Al(NO;)3,equipments:
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ard
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to read of ofions. of be640nm course
observed. weight witimmersed h time, 03
Fluorescence
safety are from of following steel
discuss Do conduct weight
the of fluorescencefluorescence as CuSO4,
not used. of in
productsignal water alcohol. water,
not dispose and steel Fe* fo r of loss. the Steel
precaution allowed experiment) standard FD2 its substrate
with use the corrosion corrosion
and in NaSiO4,
strictly loss sample loss emission cationic introduced
salts- The without Record alcohol,
the acid of lab. vs in the spectrometer, alloy,
solution during emission emission The the erased
lab for all inside time with 250mL (size,
during
substances follow FeCl,, presencefluorescence
spectra. form.
process. Fe' solution andplastic
instructors. each the End excitation the rhodamine-FD2
and time into wi th
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3% MnSO4. cm I
the intensity course different different th e a brush,
cuvettes,
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intensity (corrosion plasticshould NaCl x
h, wavelength
standard1zecorrosion solution, 3cm)
ofand safety Zn(NO;)2, of
brush, solution hair
this steel (synthesized
vs 2h of time
time. and time be each clean thermostat
follow corrosion sent dryer,
experiment precautions! depends product the substrate
24 interval interval productcorrosion, th en
it. h BaCl2, the 510 is characteristic containing for it
after using balance,
process with with fluorescence nm.should upon fluorescence
of dried water from
due immersing Al(NO), other steel). followed these by
emery
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to using using dissolved 0. FcCls,rhodamine
bath,
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scan analys1s. uM paper
danger the usingcorrosion standard CuSO4, emissionexamined air, beakers,
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 4. other using drops other
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e andthe
Results toProcedure:
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Galvanic the Experimnent 4
metal Mg, of V'oltmcterof Materials
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Observations: salt Couples standard stopper, and
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 6. precai
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Safety Note: ^ummary
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not
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the of l ab. the
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Summary c analyser.
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Results new P'rocedure: 4.
Theory:
Materials Objeetive:
7. 6. 5. 4. 3. 2. 1. Student in test galvanic a alloy,paper,
danger
If of
Tape ReadWhen Clean Food Wear brief (Ag/AgCl)
and
have (Outeomes is the titanium
performed. in Book
MSDS lab work and your what Observations: diluted corrosion
In and
any metal must Reference
clectrode(
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generating
cyanide
doubt gas. is drinks PPE alloy, electrode
edges.complete
and area. you by experiment,equipments:
read Stainless
of steelTitaniumalloyAluminumalloy using The HCI wil cell,
discuss safety are to learnt the Alloy
Zinc steel
1090 Material and by Ni
Do conduct alloy Ni Brass alloy, potential
berelerence
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half-cell of
dispose from
potentiostat. bufling
constructed. a
precaution
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with Stainless
use the strictly (SCE) electrode
the of this potentials rinse electrodeclectrode
lab. the tlhenm
lab acid all inside experiment
for follow End galvanic in The steel.Analyzer, Half-CellExperiment: 05
instructors.
substances
during th
wipotentials
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electrolyte (Ag/AgC),
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it.
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 than being When second The where the
Volmer current potential
determined At deoxygenateddegree tends and Billions
is Converts 1.
in
Theory: 2.
first equilibrium
current Object:
Corrosion
gelatine.
the the contrast carbon,
to
the is f= equation is of
first the
exponential of Scale steel,
anode
overpotential nF/RT, equal (Ecorr).
dollars
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to At To
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in -
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Equation
Anodic
Tafel
large and iron, effect
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/]Hence: the and
j= Tafel density
a cheap year Experiment: 06
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measurable as the Of
+1
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 Cathodic
Scan
A5.3 Equipment
SetupS.2 3.1.2. 1.1. 2
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with iron corrosion stirrer manuals ethanolPolish
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 5.4.
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5.4.2 S.4.5 5.3.6 5.3.5
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Scan

Repeat equilibrate Changeinear

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ep Step Rate: Voltage:
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turn
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magnetic Scan. following: surface
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minutes
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on electrode Again the the
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a
 5.
Results
Analysis
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Results

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