WORKSHEET

Calculations of exact normality of the standard solution

Let the weight of oxalic acid transferred to
100 ml standard measuring flask = ------------ g
Since, 100 ml of the solution contains = ------------ g of oxalic acid
The amount of oxalic acid in 1litre of
the solution will contain = ------- x
1000 = --------- g
100
We know that,
Strength = Weight of the substance in one liter × Equivalent weight

Weight of the substance in one liter

Normality =
Equivalent weight

= -------- N

1
 Expt.No.: PREPARATION OF N/10 OXALIC ACID AND M/10
Date: SODIUM CARBONATE SOLUTION

AIM
To prepare N/10 oxalic acid and M/10 sodium carbonate solution. You are provided with
distilled water, oxalic acid and sodium carbonate salts.
PREREQUISITE KNOWLEDGE
1. Difference between solute and solution.
2. Measures to represent the concentration of the solution.

GENERAL OBJECTIVE
Students will be able to analyze and apply the required amount of salts for the preparation
of N/10 and M/10 concentration solutions respectively.
SPECIFIC OBJECTIVES:
Student will be able to
1. Determine the amount of oxalic acid for its N/10 solution preparation
2. Estimate the amount of sodium carbonate for its M/10 solution preparation.
3. Understand the preparation of standard solution preparation.

APPARATUS/REAGENTS REQUIRED

Standard flask, funnel, weighing bottle, distilled water, oxalic acid and sodium carbonate
salts.
PRINCIPLE
Standard Solution
A solution of known concentration is called as standard solution. A standard solution is
prepared by dissolving a definite weight of substance in a definite volume. The substances are
classified as primary standards and secondary standards.
Primary Standards
The substances whose solution can be prepared by direct weighing is known as primary
standards.
Primary standard has the following characteristics:
1. It is easily available in pure state
2. It is not affected by atmospheric conditions
3. It is highly soluble in water
4. It does not dissociate or decompose on keeping the solution
E.g Oxalic acid, anhydrous sodium carbonate, potassium dichromate, potassium chloride
Secondary Standards
The substances whose standard solution cannot be prepared by direct weighing is known
as secondary standards. Secondary standard has the following characteristics:
1. Secondary standard are available only in the impure form.
2. They are poor soluble in water.
2
 WORKSHEET

Calculation of molarity for standard solution

Let the weight of sodium carbonate transferred to
100 ml standard measuring flask = ------------ g
Since 100 ml of the solution contains = ------------ g of sodium carbonate
The amount of sodium carbonate in
1litre of the solution will contain = ------- x
1000 = --------- g
100
We know that,
Weight of the substance in one liter = Molarity × Molecular weight

Weight of the substance in one liter

Molarity =
Strength
Molecular weight

= -------- M

3
 3. They are hygroscopic in nature.
4. They sublime like iodine.
E.g. NaOH, HCl, H2SO4, HNO3.
The solution of secondary standards are prepared by dissolving approximately the
required amount and then the strength and concentration (Normality or Molarity) of
the solution is determined by titrating against a standard solution.
PREPARATION OF N/10 OXALIC ACID SOLUTION (100 ml)
Normality
Concentration of a solution can be expressed in terms of Normality which is defined as
the number of gram equivalents of solute per litre of solution. It is denoted by N.
Number of gram equivalent of solute
Normality =
Volume of solution in litre

Weight of solute/Equivalent mass

=
Volume of solution in litre

Weight of solute per litre of solution

N =
Equivalent
mass
Oxalic acid is a primary standard. It crystallizes from water as a dihydrate. The
formula for crystalline oxalic acid is (COOH) 2.2H2O. The ionic equation for the
oxidation of oxalic acid is

Thus, two electrons are involved in the oxidation of one molecule of oxalic acid.

Molecular weight
Hence, Equivalent weight of oxalic acid =
Number of electrons lost by one molecule

126
= = = 63
2
For preparation of 1 litre of N/10 oxalic acid solution the amount of oxalic acid
required is 6.3 g. Hence, for the preparation of 100 ml of N/10 oxalic acid solution,

6.3
The amount of oxalic acid required = x 100 = 0.63 g
1000

4
WORKSHEET

5
 PROCEDURE
0.63 g of analar oxalic acid is weighed accurately using a digital electronic balance and
carefully transferred to a 100 ml standard measuring flask. Distilled water is added to
dissolve and then to reach the mark. For the last portion to reach the mark, water can be
added using a pipette. Then the flask is closed using a stopper and shaken well for
uniform concentration.
(b) PREPARATION OF M/10 SODIUM CARBONATE SOLUTION (100 ml)
Molarity
Concentration of a solution can also be expressed in terms of Molarity which is defined
as number of gram moles of solute per litre of solution. It is denoted by M
Number of gram moles of solute
Molarity =
Volume of solution in litre

Weight of substance/Molecular
= mass
Volume of solution in litre

Weight of solute in grams per litre of solution

M =
Molecular mass

Molecular weight of sodium carbonate = 106

Weight of sodium carbonate in one litre of solution
M =
Molecular mass of sodium carbonate

Weight of sodium carbonate in one litre of solution

M/10 = 106

Weight of sodium carbonate in one litre of solution = 10.6 g

For preparation of 1 litre of M/10 sodium carbonate solution, the amount of Na 2CO3
substance required is 10.6 g. Hence, for the preparation of 100 ml of M/10 sodium carbonate
solution
10.6
The amount of sodium carbonate salt = x 100 = 1.06 g
1000
PROCEDURE
1.06 g of analar sodium carbonate is weighed accurately using a digital
electronic balance and carefully transferred to a 100 ml standard measuring flask.
Distilled water is added to dissolve and then to reach the mark. For the last portion
to reach the mark, water can be added using a pipette. Then the flask is closed using
a stopper and shaken well for uniform concentration.

6
WORKSHEET

7
RESULT
1. The normality of oxalic acid = N
2. The molarity of sodium carbonate = M
APPLICATIONS
1. In all the analytical studies, preparation of standard solution is one of the
essential requirements.
2. Different strength solution preparation is the key aspect in the synthesis of
nanomaterials.
3. Any element or compounds quantity in solution should be expressed in any
concentration terms for the further evolution.
VIVA VOCE QUESTIONS
1. Recall the definition of solute.
2. Give example for primary standards.
3. Secondary standards can be standardized only by using primary standard solution.
Reason out.
4. Find the equivalent weight for HCl and NaOH.

STIMULATING QUESTIONS
1. To reduce swelling of any injury, hot salt massage is advised. Give reason.
2. Mention the principle of reverse osmosis processes.

FORMATIVE ASSESMENT
1. A mixture of that has uniform composition is called (U)
a. Saturated solution
b. Super saturated solution
c. Solution
d. Solvent
2. Which one of the following is an example of primary standard ? (Ap)
1. NaOH b. H2SO4 c. HNO3 d. Na2CO3

3. At a particular temperature solution which cannot dissolve more solute is called (U)

a. Saturated solution
b. Unsaturated solution
c. Aqueous solution
d. Supersaturated solution

8
WORKSHEET

9
 Expt. No
MEASUREMENT OF GRAIN SIZE USING OPTICAL
METALLURGICAL MCIROSCOPE
Date

AIM

To understand the methodology of studying the microstructure in a metallurgical

microscope for grain size and secondary phase observation.

GENERAL OBJECTIVE

To determine the grain size and secondary phase in an optical metallurgical

microscope.

SPECIFIC OBJECTIVE

Students will be able to

1. Observe the microstructure of a metal sample in a metallurgical microscope.
2. Explain the method to determine the grain size.
3. Identify the presence of secondary phase in the microstructure of a metallic
sample.

EQUIPMENTS AND TOOLS REQUIRED

1. Metallurgical microscope.
2. Polished/Prepared sample.
3. Computer to interface with microscope for grain size and secondary phase
observation.

PREREQUISITE QUESTIONS:
1. Why do we measure the grain size?
2. Mention the type of software used in the laboratory to measure the grain size?
3. Mention different equilibrium phases in steel.
OVERVIEW:
Observation and Measurement of Grain size
ASTM E112 is the standard procedure by which grains are analyzed. Usually, most
quality-control laboratories analyze grains via the "Chart Comparison" method. Here,
operators perform a visual estimation of the grain size by comparing a live image under
an optical microscope to a micrograph chart, often posted on the wall near the
microscope.

Example of a microscope eyepiece reticle used to compare against a live image.

10
or, instead of comparing to a micrograph poster, one can insert an eyepiece reticle
containing images of predefined grain size patterns, directly into the microscope's optical
path. This way, the comparison is performed directly in the microscope, where the
operator can see both the sample at question as well as a "golden" image simultaneously.
Intercept Method (Using Digitized Software)

Here, a pattern (i.e. circles, cross-and-circles, lines, etc) is overlaid atop the digital image
(live or captured). Each time the overlaid pattern intercepts with a grain boundary, an
intercept is drawn on the image and recorded (hence the name "Intercept Method").
Taking the system calibration into consideration, the image-analysis software
automatically calculates the ASTM "G-Number" and mean intercept length, as a function
of the intercept count and pattern length.

Planimetric method (Using Digitized Software)

Unlike the Intercept method, the Planimetric method determines the grain size on an
image (live or captured) by calculating the number of grains per unit area.

PROCEDURE:

1. Do all the polishing operations on the given sample.

2. Apply etching agent for 20 secs, and wash it with water.
3. Place the eyepiece 15 monocular tube. Also fix the objective.
4. Place the metallurgical sample specimen on the stage plate.
5. Rotate the objectives of the microscope into the optical axis to a magnification of
10. Now the total magnification is 150.
6. Viewing through the eyepiece, move the stage up or down until an image appears.
7. Focus the microscope to full sharpness of image by means of fine focusing
movement.
8. „Envision‟ software is used to measure grains and phase measurement.

11
Select measurement grains in source video average grain
Set threshold hayn linear intercept No.of lines 3 min
Find grain size

Select measurement phase Source image phase mode

Click new phase enter element name in histogram click on add
phase New phase Enter element Report click

APPLICATIONS
This can be used to
 study the microstructure of metals and alloys, upto a magnification of 1000X.
 measure the grain size of materials.
STIMULATING QUESTIONS:

1. Is it possible to measure the grain size of polymers?

RESULT:

S.No. Name of the material (Microstructure Analyzed) Average Grain

Size

VIVA QUESTIONS:

1. Define grain and grain boundary.

2. List the three different methods of estimating the grain size measurement.

3. What are the factors are to be considered for size of grains in casting?

4. Does the effect of grain change will take place at recrystallization temperature?

5. Indicate the ASTM standard used for grain size measurement.

6. List the types of software used to measure the metallographic microstructure.

7. What will be the effect of grain size when subjected to annealing heat treatment?

12
 WORKSHEET

Titration - I Standardization of EDTA solution

Burette solution : EDTA solution
Pipette solution : Standard ZnSO4 solution

Indicator : Eriochrome black-T (EBT)

Additional solution : Ammonia buffer

End point : Color change from wine red to steel blue

Standard ZnSO4 Vs EDTA solution

Volume of Burette reading (mL) Volume of Concordant

S.No. ZnSO4 EDTA solution value
solution V1 Initial Final V2 (mL) V2 (mL)
(mL)

Calculation
Volume of ZnSO4 solution V1 = ---------- mL
Normality of ZnSO4 solution N1 = ---------- N
Volume of EDTA solution V2 = ---------- mL
Normality of EDTA solution N2 = ---------- ?
According to the law of volumetric analysis, V1N1 = V2N2
V1x N1
N2 =
V2

x
=

Normality of EDTA solution N2 = ---------- N

13
 Expt.No.: ESTIMATION OF COPPER CONTENT IN BRASS BY EDTA
Date: METHOD
Aim
To estimate the amount of copper present in the given solution standard
zinc sulphate solution and a link solution of EDTA.
PREREQUISITE KNOWLEDGE
1. Two major ores of copper.
2. Applications of copper in alloying technique.
3. Role of copper in the preparation of Brass
GENERAL OBJECTIVE
To estimate the amount of copper present in the given brass solution by EDTA method.
SPECIFIC OBJECTIVES
Students will be able to
1. Standardize EDTA solution using ZnSO4 solution
2. Determine the strength of copper ion present in the given brass solution
3. Calculate the amount of copper ion present in the brass solution
4. APPARATUS/REAGENTS REQUIRED
Brass shavings, conc. HNO3, 4N H2SO4, 0.1 N EDTA solution, fast sulphone
black-F (FSB-F), NH4Cl, NH4OH, ZnSO4.
PRINCIPLE
Brass is an alloy of copper. It contains different percentage of copper (60 –
90 %). Along with copper, brass is having some other metal like Zn, Fe, Sn, Mg and
Pb. The purpose of alloying copper with these metals is to improve the strength
and mechinability. Copper is estimated in presence of these metals in brass using
standard EDTA solution and FSB-F. Accurately weighed sample of brass is
dissolved in concentrated nitric acid and the mixture is boiled to expel the oxides
of nitrogen. Copper present in the brass is brought into the solution containing
cupric ion. Then, the cupric ions are determined using EDTA in the presence of
FSB-F

Cu2+ + FSB-F [FSB-F-Cu] complex

Purple color
[FSB-F-Cu] complex + EDTA [Cu-EDTA] complex + FSB-F
(Colorless) Dark green color
PROCEDURE
1. Standardization of EDTA solution
20 mL of the ZnSO4 solution is pipetted out into a clean conical flask. 2 mL of
ammonia buffer (NH4Cl+NH4OH) solution and a 1 drop of EBT indicator are added
and titrated against EDTA solution taken in the burette.

14
 WORKSHEET

Titration - II Estimation of copper in the brass solution

Burette solution : Standard EDTA solution
Pipette solution : Brass solution
Indicator : Fast sulphone black-F (FSB-F)
Additional solution : Ammonia buffer
End point : Color change from purple to dark green
Standardized EDTA solution Vs Copper solution

Volume of brass Burette Reading (mL) Volume of Concordant

S.No. solution EDTA solution value
V4 (mL) Initial Final (mL) V3 (mL)

Calculation
Volume of EDTA solution V3 = ---------- mL
Normality of EDTA solution N3 = ---------- N
Volume of brass solution V4 = ---------- mL
Normality of brass solution N4= ----------
? According to the law of volumetric analysis,
V3N3 = V4N4
V3 x N3
N4=
V4

= ---------- N

Amount of copper present in 1 litre = Normality of brass solution x

of the given brass solution Eq.wt. of copper
= N x 63.54
= ---------- g/L
The percentage of copper in brass = [Wt.of copper/Wt.of brass] x 100

= x 100

= -------------%

15
The end point is the change of color from wine red to steel blue. The titration is
repeated for concordant value.
2. Estimation of copper in the given solution
20 mL of the prepared brass solution is pipetted out into a clean conical flask. 2
mL of ammonia buffer (NH4Cl+NH4OH) solution and a 1 drop of FSB-F indicator are
added and titrated against EDTA solution taken in the burette. End point is change
of color from purple color to dark green. The titration is repeated for concordant
value. From the titre value the amount of copper content present in the brass
solution is determined.
RESULT
1. The amount of copper present in the whole of given brass solution = ---------- g/L.

2. Percentage of copper in the given brass sample = ------%

APPLICATIONS
1. The strength of the brass alloy can be varied with respect to the copper content.
2. Electrical and magnetic properties can be enhanced by addition of Copper content.
3. Copper in alloy making process facilitate the corrosion resistance properly.
4. Copper present in brass and other copper alloys can kills the microbes.
VIVA VOCE QUESTIONS
1. Correlate chelation and complexometric titration.
2. Which type of ligand is EDTA?
3. Why there is a color change occurring from purple to dark green in this titration?
4. The pH range is to be maintained around 8 – 10 in EDTA
complexometric titrations. Reason out.
5. Write the structure and chemical name of fast sulphone black-F indicator.
STIMULATING QUESTIONS
1. How copper is helpful to the human body?
2. Why copper bottom utensils are mainly preferred rather than stainless steel.
3. What is Menkes kinky hair syndrome?

FORMATIVE ASSESSMENT
1. The metal composition of brass alloy is
(a) Zn & Cu (b) Fe & Cu
(c) Ni & Cu (d) Zn & Fe
Germicidal activity of brass is mainly because of
2.
(a) Cu (b) Fe
(c) Zn (d) Pb
3. Find the ingredient which increase the machinability of brass,
(a) Mo (b) Pb (c) Fe (d) Zn

16
WORKSHEET

17
 Expt. No
MICROSTRUCTURE ANALYSIS OF STEEL/CAST
Date IRON

AIM
To observe the microstructure of a cast iron sample (spheroidal graphite iron/grey cast
iron/malleable cast iron/white cast iron).

GENERAL OBJECTIVE

To identify the microstructure of various types of cast iron.

SPECIFIC OBJECTIVE

Students will be able to

1. Select the appropriate etching agent for cast iron.
2. Identify the different types of phases present in the microstructure of cast irons.
3. Compare the microstructure with suitable Standards. (ASM Vol.9-P.565-587)

EQUIPMENTS AND TOOLS REQUIRED

1. Metallurgical microscope.
2. Polished/Prepared sample.
3. Computer to interface with microscope for grain size and secondary phase
observation.

PREREQUISITE QUESTIONS:

1. What is the percentage of carbon present in cast iron?

2. List the types of cast iron?

3. Mention 3 applications of cast iron.

PROCEDURE

1. Do all the polishing operations on the given sample.

2. Apply etching Agent Nital for 20 secs, and wash it with water.
3. Place the eyepiece 15 monocular tube. Fix the objective.
4. Place the metallurgical specimen on the stage.
5. Rotate the objectives of the microscope into the optical axis to a magnification of
10. Now the total magnification is 150.
6. Viewing through the eyepiece, move the stage up or down until an image appears.
7. Focus the microscope to full sharpness of image by means of fine focusing
movement.
8. Observe the microstructure and draw it.

18
 OBSEVATION:

Description Chemical composition Microstructure Observation

Carbon - 3.1%
Silicon - 2.1%
Gray Cast Iron Manganese - 0.6%
Sulphur - 0.1%
Phosphorous - 0.2%
Carbon - 3.5 to 4%
Silicon - 1 to
3%
Magnesium - 0.02 to 0.1 %
S.G.Iron Manganese - 0.1 to 6%
Phosphorous - 0.02 to 0.05%
Sulphur below - 0.02%
Remaining - Fe.

Carbon-3.5%
Sulphur-0.12%
White Cast Iron Phosphorouus-0.028%

Silicon-0.9%
Manganese-0.65%
Carbon - 2.4%
Silicon - 0.1%
Malleable Cast
Manganese - 0.4%
Iron Sulphur - 0.1%
Phosphorous - 1.2%

19
APPLICATIONS

Grey cast iron is used to make machine beds, engine frames, pump housing, cylinders
and pistons of
IC engines, flywheels.

S.G. Iron is used to make crank shafts, gears, discs, pistons, pipes, bearing blocks and
cylinder
blocks.

Malleable cast iron is use for pipe fittings, valves, chains, bearing blocks and automobile
parts.

STIMULATING QUESTION:
1. Why is gray cast iron used for lathe bed/frames?

2. Why cast irons are not used in aircraft engines?

RESULT:

VIVA QUESTIONS:

1. What is the difference in percentage of carbon between steels and cast irons?

2. In Fe-C diagram, considering steel and cast iron, which is eutectic and which is
eutectoid reaction?

3. How is S.G. Iron obtained from gray cast iron?

4. Mention the applications of gray cast iron.

5. List the applications of S.G Iron.

6. How is malleable Iron obtained from white cast iron?

7. Mention the applications of white cast iron.

8. List the applications of malleable Iron.

9. What is the etchant used for gray cast iron?

10. What is the form of carbon present in the white cast iron?

20
WORKSHEET

21
 Expt. No
MICROSTRUCTURE ANALYSIS OF STAINLESS
Date STEEL SAMPLE

AIM
To observe the microstructure of a stainless steel sample and identify its
microstructure.

GENERAL OBJECTIVE

To identify the microstructure of stainless steel.

SPECIFIC OBJECTIVE

Students will be able to

1. Select the appropriate etching agent for stainless steel.
2. Identify the different types of phases present in the microstructure of the stainless
steel.
3. Compare the obtained microstructure with suitable Standards. (ASM Vol.9-P.608-
627)

EQUIPMENT’S AND TOOLS REQUIRED

1. Metallurgical microscope.
2. Polished/Prepared sample.
3. Computer to interface with microscope for grain size and secondary phase
observation.

PREREQUISITE QUESTIONS:

1. Mention the types of stainless steels.

2. What are the equilibrium phases present in the Iron-Carbon Equilibrium diagram?

PROCEDURE

1. Do all the polishing operations on the given sample.

2. Apply etching agent 2% for 20 secs. Wash it with water.
3. Place the eyepiece 15X in the monocular tube. Also fix the objectives.
4. Place the metallurgical specimen on the stage plate.
5. Rotate the objectives of microscope into the optical axis to a magnification of 10X.
Now the total magnification is 150X
6. Viewing through the eyepiece move the stage up or down until an image appears.
7. Focus the microscope to full sharpness of image by means of fine focusing
movement.
8. Observe the microstructure and draw it.

22
OBSERVATION :

Description Chemical composition Microstructure

Carbon - 0.06%
Manganese -1.4%
Silicon -0.8%
Chromium -17%
Stainless Steel Nickel -13%
Molybdenum -2.4%

Microstructure Observation [For Stainless Steel]:

The microstructure shows fine austenitic grains with annealing twins. No carbide
precipitation is seen at the grain boundaries. This type of steel is austenitic steel,
essentially non magnetic in the annealed condition and do not harden by heat treatment.
The total content of Ni and Cr is at least 23%. When chromium is added to steel it first
combines with carbon and forms complex chromium carbides and the remaining
chromium goes in the solid solution form.

Applications

Stainless Steel - engine parts of aircrafts, heating element for furnances, food
processing, transportation industry, pumps and valves parts, turbine buckets, surgical
instruments, chemical processing .

STIMULATING QUESTION:

1. In what form is carbon present in steel?

2. Why are stainless steels „stainless‟?

RESULT:

23
VIVA QUESTIONS:

1. Mention the range of carbon present in stainless steel.

2. What is the maximum carbon content in steels?

3. Mention the difference in the carbon composition between austenitic stainless steel
and ferritic stainless steel.

4. Name the etchant used for stainless steel.

5. What type of steel do you prefer for the chemical processing and food processing
industry?

6. State one specific property of stainless steel.

7. Why is Ni added to stainless steels?

8. Why is chromium added to stainless steels?

24
WORKSHEET

25
 Expt. No
MICROSTRUCTURE ANALYSIS OF ALUMINIUM/COPPER
Date

AIM
To observe the microstructure of aluminium/copper.

GENERAL OBJECTIVE

Students will be able to identify the microstructure of non-ferrous metals.

SPECIFIC OBJECTIVE

Students will be able to

1. Select the appropriate etching agent for stainless steel.
2. Identify the different types of phases present in the microstructure of the stainless
steel.
3. Compare the obtained microstructure with suitable Standards.

EQUIPMENTS AND TOOLS REQUIRED

1. Metallurgical microscope.
2. Polished/Prepared sample.
3. Computer to interface with microscope for grain size and secondary phase
observation.

PREREQUISITE QUESTIONS:

1. Al, Mg, Cu, Ni are called „non-ferrous‟ metals. Why?

2. Arrange the non-ferrous metals Al, Mg, Cu, Ni in the order of increasing density
(lightest metal first).

PROCEDURE

1. Do all the polishing operations on the given sample.

2. Apply etching agent for 20 secs, and wash it with water.
3. Place the eyepiece monocular tube. Fix the objective.
4. Place the metallurgical specimen on the stage.
5. Rotate the objectives of the microscope into the optical axis to a magnification of
10.
Now the total magnification is 150.
6. Viewing through the eyepiece, move the stage up or down until an image appears.
7. Focus the microscope to full sharpness of image by means of fine focusing
movement.
8. Observe the microstructure and draw it.

26
 OBSERVATION:

Description Chemical composition Microstructure Observation

Aluminium

Copper

Magnesium

STIMULATING QUESTION:

1. Why are Al-alloys and Mg-alloys preferred in auto/aero industry?

2. Why is Ni-alloys used in aircraft engines?

RESULT:

27
VIVA QUESTIONS:

1. What is the density of Al, Mg, Cu and Ni?

2. What are the melting temperatures of Al, Mg, Cu and Ni?

3. Mention 2 alloy systems of Copper.

4. List 3 alloys of Nickel.

5. Alloys of nickel are called „Super alloys‟. Why?

6. Can Al be added to Mg to form a Mg alloy. Give an example.

7. Mention 3 applications of aluminium alloys.

8. Mention 3 applications of magnesium alloys.

9. Mention 3 applications of copper alloys.

10. Mention 3 applications of nickel alloys.

28
WORKSHEET

29
 Exp.
No. DETERMINATION OF HARDENABILITY USING
JOMINY END QUENCH TEST
Date

AIM
To study the hardenability of steel using Jominy end quench test.

GENERAL OBJECTIVE
To understand the property of hardenability in steel using Jominy end quench test.

SPECIFIC OBJECTIVES
Students will be able to
 Explain the Jominy end quench test apparatus.
 Explain the experimental procedure to conduct the test.
 Determine the hardenability of steel after the test.

APPARATUS REQUIRED
A. Jominy end quench test apparatus
B. Sample to be tested
C. Hardness Tester

INTRODUCTION:
This apparatus is used to determine the hardenability of steel by a quench test method. It
is
designated as per Indian standards – (BS4437:1969) & (IS: 3848-1996).
The austenitised standard specimen from furnace is placed in the apparatus for quick
end quench
under water jet.

PREREQUISITE QUESTIONS
1. Define hardness.
2. Define Hardenability.
3. What is the difference between „hardness‟ and „hardenability‟.

DIAGRAM:

Fig. 1.

30
1. ON/OFF Switch for Motor Pump.
2. Bottom Sump for water.
3. Top Pressure Head.
4. Top Lid.
5. Quick Releasing Valve.
6. Specimen Loading Lid
7. Specimen.
8. Drain Plug.

WORKING PRINCIPLE
Hardenability describes how deep the steel may be hardened upon quenching from
high temperature (i.e. depth of hardening). One end of the heated steel specimen is
quenched using a water jet. The water jet cools this end (i.e. exposed end) of the specimen
faster. The cooling rate reduces from the quenched end along the length of the specimen
(i.e. away from the water jet). Upon quenching, the hardness obtained is dependent on
cooling rate. The instantly cooled (i.e. rapidly cooled) end shows higher hardness than the
areas/regions away from the quenched end. Hardenability indicates the distribution
(variation) of hardness along the length of the specimen from the quenched end. By
heating to a specific temperature, steel becomes austenite completely. Upon quenching,
austenite transforms to martensite. Martensite is the hardest phase in steel.

For e.g. a specimen with 55 HRc „throughout the section/length‟ has higher hardenability
(high depth of hardness), i.e. the value of hardness remains same for almost the entire
section/length of the sample), when compared to a specimen with quenched end
hardness of 62 HRc, and which reduces to 40 HRc along its length (low depth of
hardness).

APPARATUS:
After heating the test specimen, it is kept on the specimen holder where it is
automatically centered with respect to water jet. The quick action valve starts impinging
the water jet on the specimen end, instantly. By choosing one of the standard nozzles
provided and its corresponding water head, a well-defined water jet is achieved. Selection
of pump, tank, pipe etc., enables to obtain correct water jet for specific nozzles. The
nozzles are of quick change type and can be replaced instantly. Different set of nozzles,
specimen holders, water head adjusting pipes are available to suit different test specimen.
The electrical controls for pump motor are supplied and the entire apparatus is tightly
closed.

PROCEDURE

1. Prepare a test specimen as per I.S/B.S standards, 25 mm diameter and 100 mm

length as per drawings. The specimen should have a collar for seating in the
apparatus.
2. Set the temperature for austenizing in the furnace and switch on the furnace to
reach the set temperature.
3. Load the specimen in the furnace chamber that is set at the austenizing
temperature and close the furnace. Let the specimen get austenitised completely.
This can be achieved by giving correct soaking time depending on the composition
of the specimen.
4. Meanwhile, fill water in the end quench apparatus from the top tank, till the water
reaches the bottom sump and overflows through the side over flow tap.
5. See that quick releasing valve is at closed position while filling the water.

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 6. Switch on the motor and check whether the pump is working.
7. Open the quick releasing valve by keeping in the position “ON”.
8. If the operations from 3 to 6 are over, close the valve.
9. Keep the specimen chamber open and let the motor be running.
10. Transfer the specimen from the furnace to the end quench apparatus
through the specimen holder and then immediately open the quick releasing valve.
The specimen gets quenched at one end under specified conditions of flow rate.
11. Take the specimen out after cooling and conduct the hardness test using a
hardness tester.

STIMULATING QUESTIONS

1. Can there be applications that require only high surface hardness and not along
the full length? If yes, mention at least one application.

RESULT:

VIVA QUESTIONS:

1. What are the equilibrium phases in steel?

2. What are the non-equilibrium phases in steel?

3. How is martensite formed?

4. What is the structural requirement for martensite formation?

5. List 3 hardness testing methods.

6. Why is hardenability test done only to steels?

7. What is the purpose of quenching?

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WORKSHEET

33
 Ex.No. ESTIMATION OF IRON (THIOCYANATE METHOD) IN THE
Date: GIVEN SOLUTION BY SPECTROPHOTOMETRIC METHOD

AIM
To determine the amount of Fe3+ ion present in the given water sample using
spectrophotometer.
PREREQUISITE KNOWLEDGE
1. Electromagnetic spectrum
2. Difference between absorbance and transmittance
3. Complexing agent
GENERAL OBJECTIVE
Students will be able to estimate the unknown concentration of iron using
spectrophotometer.
SPECIFIC OBJECTIVES
Students will be able to
1. Prepare standard ferrous ammonium sulphate (FAS) solutions
2. Find the absorbance/transmittance for the prepared standards and unknown
solution
3. Construct a calibration curve from the observed values
4. Determine the unknown concentration of the Fe2+ ion
APPARATUS/REAGENTS REQUIRED
Spectrophotometer, pipette, measuring jar, standard flask, FAS solution, potassium
thiocyanate solution, dilute HNO3 solution.
PRINCIPLE
When a monochromatic light passes through a homogenous colored solution, a portion of
incident light is reflected, a portion is absorbed and the remaining light is transmitted.
Io = Ir + Ia + It
Where Io, Ir, Ia and It are the intensities of the incident, reflected, absorbed and
transmitted light respectively. Ir is usually eliminated and hence Io = Ia+It. The
mathematical statement of Beer Lambert‟s law is given by
log Io/I = εCt (or) A = εCt
Where, log Io/I = A
Io = intensity of incident light
I = intensity of transmitted light concentration
C = of the solution in moles/lit
t = thickness of cell in cm
ε = molar absorption coefficient
A = absorbance or optical density of solution

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 WORKSHEET

CALIBRATION GRAPH

Absorbance Vs Concentration

LAYOUT OF THE SPECTROPHOTOMETER

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Fe3+ ion does not give any color in solution. However, it develops a red color when it reacts
with potassium thiocyanate solution.
2+ 3- +
Fe + 6KSCN [Fe(SCN)6] + 6K
Red coloured complex

Spectrophotometer has a wide range of adaptability that allows selection of

monochromatic light of any wavelength in the visible spectrum. The light source is an
ordinary light bulb and monochromatic light is obtained using either a prism or a
diffraction grating. The monochromatic light is then passed through the filter and is
directed through a cell containing the sample. The light that penetrates hits the
photoelectric cell and the output of this can be seen in the display.

PROCEDURE
A standard stock solution of iron is prepared by dissolving 0.864 gm of Ferrous
Ammonium Sulphate (FAS) (AR) in distilled water in presence of 10 mL of conc.HNO3 (AR)
and made upto 1 litre in a standard measuring flask. 1 mL of this stock solution = 0.1 mg of
iron. From the stock solution, a series of standard solutions containing 2, 4, 6, 8 and 10 mL
of the ferrous ammonium sulphate stock can be prepared. To each of the solution taken in a
100 mL SMF, 3.0 mL of strong HNO3 (1:1 V) and 5 mL of potassium/ammonium
thiocyanate (10 %) solution are added and made upto the mark using distilled water. A blank
solution is prepared by taking 5.0 mL of the reagent and 3.0 mL of the acid making upto the
mark in a 100 mL SMF.

The spectrophotometer is switched on and warmed up for 15 minutes. The

monochromator is adjusted for 480 nm. The blank solution (distilled water) is kept in the cell
and the absorbance is measured for which the absorbance is zero and the transmittance is
100. Now, the absorbance of the all the standard solutions are measured. Then absorbance
of the unknown solution is also measured. A calibration graph is plotted between absorbance
and concentrations. From this graph, the concentration of Fe2+ in the unknown solution is
obtained.

RESULT:
ppm.
The amount of Fe2+ ion present in the given solution =

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APPLICATIONS
1. Spectrophotometer is used to detect even a trace amount of colored compounds.
2. It can b e u s e d to d e t e r m i n e t h e e q u i l i b r i u m c o ns t a n t o f a reaction.
3. It is a time and cost effective method.
VIVA VOCE QUESTIONS
1. Recall the wavelength range of UV and visible light in electromagnetic spectrum.
2. Identical cuvettes are used for analysis in spectrophotometer. Give reason.
3. Name two instruments employed in absorption measurements.
4. Filters are invariably used in absorption spectroscopy. Why?
5. Differentiate absorbance and transmittance.
6. Identify the role of dilute nitric acid in iron estimation using
S pectrophotometer

STIMULATING QUESTIONS
1. Using colorimetry, can we test the concentration of haemoglobin in blood?
2. Assume that your samples are meant to be pale blue colors, but the blue
colors which you have prepared are very dark and the spectrophotometer
absorbance readings are all 9999. Identify the error.
FORMATIVE ASSESSMENT
1 . According to the Beer-Lambert Law, on which of the following
does absorbance not depend?
a) Solution concentration.
b) Distance that the light has travelled through the sample
c) Color of the solution
d) Extinction coefficient of the sample
2 . The λmax value of iron complex is
a) 490nm
b) 470 nm
c) 480 nm
d) 580 nm
3 . A solution of X of concentration 0.010 mol dm–3 gives an absorbance of 0.5.
What concentration is a solution of X which gives an absorbance reading of
0.25? Assume that the same optical cell is used for both readings.
a) 0.050 mol dm–3
b) 0.0050 mol dm–3
c) 0.010 mol dm–3
d) 0.020 mol dm–3

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