A

Mini-Project Report

on

“ FORMATION OF FERROUS SULPHATE FROM IRON NAILS’’

Submitted by

SHRIKANT DNYANESHWAR GITE

(2130331527517)

Under the guidance of

Prof. L. Y. RAWOOT

DEPARTMENT OF PETROCHEMICAL ENGINEERING

DR. BABASAHEB AMBEDKAR TECHNOLOGICAL

UNIVERSITY, LONERE
ACADEMIC YEAR 2022-2023
 CERTIFICATE
This is to certify that the seminar report, entitled “FORMATION OF FERROUS SULPHATE FROM IRON
NAILS” is bonafied work carried out by SHRIKANT DNYANESHWAR GITE (2130331527517) of third year
B.TECH in Petrochemical Engineering of Dr. Babasaheb Ambedkar Technological University, Lonere in
academic year 2022-2023.

Prof. L. Y. RAWOOT Dr. S. S. METKAR

(Mini-Project Guide) (Head,Department of Petrochemical Engg.)

Examiners:
1.

2.

Place: Lonere
Date:

ii
 ACKNOWLEDGEMENT
We would like to acknowledge our deepest gratitude to our Head of Department DR. S.S Metkar and our Project Guide Prof.
L. Y. RAWOOT for her constant attention, valuable suggestions, enthusiastic support and personal concern during the Project.
Furthermore, my appreciation also goes to our lab technicians Special thanks to the Department of Petrochemical
Engineering for the permission to use the facilities and equipment available at Department which aided us to complete this
project successfully.

SHRIKANT. D. GITE
(2130331527517)

iii
 ABSTRACT
A process is provided for converting iron, such as scrap iron, directly to ferrous sulfate monohydrate
in the absence of intermediate formation of ferrous sulfate heptahydrate, the use of pressure, vacuum
and/or excessively high operating temperatures. The above is achieved by reacting iron and a sulfuric
acid solution having a concentration within the range of between about 10-90 percent for a period of
time sufficient to reduce the free acid concentration to between about 2-35 percent, separating the
resulting solution from the unreacted iron, filtering the solution to remove any precipitation and
impurities contained therein, adding concentrated sulfuric acid to the solution to bring the free sulfuric
acid concentration up to between about 35-45 percent for precipitating pure ferrous sulfate
monohydrate and separating the pure ferrous sulfate monohydrate precipitate from the filtrate.

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 CONTENT
TITLE.......................................................................................................................................... i

CERTIFICATE..............................................................................................................................ii

ABSTRACT...................................................................................................................................iii

ACKNOWLEDGEMENT..............................................................................................................iv

CHAPTER 1……………………………………………………………………………………...1

INTRODUCTION………………………………………………………………………………...1-2

CHAPTER 2………………………………………………………………………………………3

Literature survey…………………………………………………………………………………..3

CHAPTER 3………………………………………………………………....................................4

Experimental work………………………………..………………………………………………4-9

CHAPTER 4………………………………………………………………………………………10

Analysis of product………………………………………………………………………………. 10-11

CHAPTER 5………………………………………………………………………………………11

Properties and its uses…………………………............................................................................. 11-12

CONCLUSION……………………………………………………………………………………13

REFERANCES…………………………………………………………………………….14

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 LIST OF FIGURES

Sr no Fig no Fig name Page no

1 Fig 1.1 Ferrous sulphate structure 1
2 Fig 3.1 Apparatus and chemicals requirement 5
3 Fig 3.2 Reaction carried out in beaker 6
4 Fig 3.3 Mixture of iron oxide and ferrous sulphate 6
5 Fig 3.4 Final product ferrous sulphate 6
6 Fig 3.5 Apparatus and chemicals requirement 7
7 Fig 3.6 Solution after reaction done 7
8 Fig 3.7 Ferrous sulphate solution form 7
9 Fig 3.8 Final product ferrous sulphate 8
10 Fig 3.9 Scrap iron in sulfuric acid 9
11 Fig 3.10 Ferrous sulphate solution with crystals 9
12 Fig 4.1 Identification test by using water 10
13 Fig 4.2 Identification test by using Ethanol 10
14 Fig 4.3 Identification test by using NaOH 11
15 Fig 4.4 Identification test by using Heating 11

LIST OF TABLE

Sr no Table no Table name Page no

1 Tab 4.1 comparison of properties of 11
our product and lab FeSO4

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 ‘‘Formation of ferrous sulphate by iron nails’’

CHAPTER 1
INTRODUCTION
Iron is a transitional element in periodic table. Iron compounds are used in medicine as an important
constituent and the ores are widely distributed which includes haematite Fe2O3, limonite
2Fe2O3.3H2O, magnetic iron is Fe3O4. The earth’s core consists largely of iron. Iron shows two
oxidation states – Ferrous and Ferric. Ferrous sulphate is otherwise known as “green vitriol” and
used as a reducing agent in chemistry. For the preparation with sulphuric acid the very first step is
to determine the amount of impurity as sulphuric acid tolerable by the crystals which may result in
chemical burns on touching if the amount of sulphuric acid content will be higher. The lab
temperature has to be kept low or below 25°C. In the experiment we can take direct iron chips or a
steel wool can be taken and iron can be extracted from it by degreasing with acetone for half an hour
and then dried completely in safe place where no light source should be present not even a lamp.
Then the degreased steel wool has to be dipped in dilute sulphuric acid to make it dissolve
completely as a result reddish-brown insoluble ferric compound formed.

Fig 1.1 Structure of ferrous sulphate

• GENERAL INFORMATION ABOUT FERROUS SULPHATE

1. Density is 2.84 g/cm³.

2. Molecular Weight/ Molar Mass is 151.908 g/mol.
3. Boiling Point is >300 °C.
4. Melting Point is 56-64 °C.
5. Appearance is Blue-green powder or crystals.
6. Soluble in water.

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• Molar Mass
1.Anhydrous ferrous sulphate- 151.91 g/mol
2.Monohydrate ferrous sulphate- 169.93 g/mol
3.Heptahydrate ferrous sulphate- 278.02 g/mol
• Color
1.Anhydrous- White crystals.
2.Monohydrate- Yellowish white crystals.
3.Heptahydrate- Bluish-green crystals.

• Refractive Index

1.Monohydrate- 1.591
2.Tetra hydrates 1.526-1.528
3.Heptahydrate- 1.471

• Hydrates of Ferrous Sulphate

Iron (II) sulfate is available in several states of hydrations, and some of these types occur
in nature. Such as;

1.FeSO4⋅H2O (relatively rare).

2.FeSO4⋅7H2O (Melanterite, blue-green, very common).
3.FeSO4⋅5H2O (relatively rare)

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CHAPTER 2

LITERATURE SURVEY

1.Mohammed Ahmed University of Technology, Iraq (2021)- Iron Sulphate was resulted by
leaching method (using selective leaching corrosion phenomenon). To product the source of
iron food supplement, industrial iron waste was used here from the workshop. Food supplement
when product be ferric compound ferrous compound, both compounds be as Sulphate of iron.
To extract these compounds, extraction by leaching was used. Use Sulfuric acid (H2SO4) as
dissolvent solution to leaching process. Mitigation of sulfuric acid concentration by Distilled
water in the beakers. After mitigation of sulfuric acid in the beakers, put and diving the
industrial waste (0.25kg) from workshop in the solution of sulfuric acid, after a period from
start reaction the color of the solution converts into transparent green color. After 24 hours from
reaction the waste converts into very small black particles, precipitate in bottom of beakers.
2.Kim William Gates (2010) by Monohydrate-The invention provides a process for the
production of ferrous sulphate monohydrate which comprises: (a) reacting a source of iron with
an aqueous solution of sulfuric acid in at least a first reaction vessel, to obtain a process liquor
comprising ferrous sulphate and acid solution; and then (b) combining the process liquor with
concentrated sulfuric acid in a mixing vessel, causing the solution to crystalize thus forming a
slurry comprising crystalline ferrous sulfate monohydrate. The slurry can, if desired, then be
converted to ferric sulphate.
3.Alexander Kehrmann (2006) by Hepathydrate-In a method of producing ferrous sulfate
heptahydrate, ferrous sulfate monohydrate is converted in a crystallization reactor in the presence
of water into ferrous sulfate heptahydrate as crystallized product, and water is subsequently
isolated from the ferrous sulfate heptahydrate. Ferrous sulfate monohydrate is obtained from a
pickling solution containing ferrous chloride, hydrochloric acid and water and reacted in a
precipitating reactor in the presence of excess sulfuric acid to form ferrous sulfate monohydrate
and hydrochloric acid. The ferrous sulfate monohydrate is then dehumidified and converted in a
crystallization reactor in the presence of excess water into ferrous sulfate heptahydrate.

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 ‘‘Formation of ferrous sulphate by iron nails’’

CHAPTER 3
EXPERIMENTAL WORK
There are lots of method of production of ferrous sulphate in industry but we consider laboratory
production method for production as mention below.
• Chemicals required-Water, (conc)sulfuric acid, iron nails, beaker, cotton filter, conical flask.
• Apparatus required-iron nails, beaker, cotton filter, conical flask.
For that we do two process for production of ferrous sulphate as written below.

1.USING CONCENTRIC SULFURIC ACIDS

• PROCEDURE
1.Take 100ml sulfuric acid and 300ml water in each beaker.
2.Make electrolyte acid solution ie .add 300ml water in beaker and then add slowly sulfuric acid
in it to make electrolyte solution and mix it well.
3.Take 100mg pure iron nails in beaker and add our electrolyte solution slowly in it.
4.After addition our reaction is started leave it for 2hrs.
5.After completion of 2hrs we see bluish-green solution in beaker.
6.Then using of cotton filter, filter our solution.
9.By these we got our product (ferrous sulphate in crystal form).

• REACTION OF FERROUS SULPHATE PRODUCTION

Fe + H2SO4 ⟶ FeSO4 + H2
(Iron) (sulfuric acid conc.) (Ferrous sulphate) (Hydrogen)

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2.USING DILUTE SULFURIC ACID H2SO4

• Chemicals and Apparatus required-Water, (dilute)sulfuric acid, iron nails, beaker, cotton filter,
conical flask.
• PROCEDURE
1.Take 55ml of con. Sulfuric acid in a beaker and take 165 ml water in other beaker.
2.Take 1000ml capacity beaker and add 55ml sulfuric acid in it. After that add iron nails in that
beaker and leave it for 10-15 min for start reaction.
3.After reaction start between nails and sulfuric add 165 ml water in it to make solution dilute and
by adding water reaction rate is also increase.
4.Leave the solution for around 3 hours. After reaction complete take the solution in the beaker.
5.In solution some amount of oxide layer is present in it, so heat the solution ie we get solution
around 200ml so heat it and make it half ie 100ml and cool the solution(heat at 40°C for 20 min)
6.After heat filter the solution using filter paper or cotton filter.
7.After filter done condense the solution for around 12 hours.
8.After 12 hours complete you will see at bottom of beaker some blueish crystals are formed.
9.Filter it using filter paper and separate solution and crystal. These crystals is our final product.

• REACTION OF FERROUS SULPHATE PRODUCTION

Fe + H2SO4 ⟶ FeSO4 + H2
(Iron) (sulfuric acid dilute) (Ferrous sulphate) (Hydrogen)

• EXPERIMENTAL WORK CARRIRD IN LABORATORY

1.FORMATION OF FeSO4 USING CONC. H2SO4

1.Apparatus and chemicals requirement- Water, (conc)sulfuric acid, iron nails, beaker, cotton
filter, conical flask ,funnel.

Fig 3.1 Apparatus and chemicals requirement

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 ‘‘Formation of ferrous sulphate by iron nails’’

2.Reaction doing in beaker when we add chemical and iron nails in beaker. And upper
blackish layer is oxide layer of iron.

Fig 3.2 Reaction carried out in beaker

3.After reaction complete our product and some amount of iron oxides present in liq.
Form and at bottom ferrous sulphate is present.

Fig 3.3 Mixture of iron oxide and ferrous sulphate

4.After filter the mixture using filter paper we get our product that is ferrous sulphate.

Fig 3.4 Final product ferrous sulphate

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• FORMATION OF FeSO4 USING DILUTE H2SO4

1.Apparatus and chemicals requirement- Water, (dilute)sulfuric acid, iron nails, beaker,
cotton filter, conical flask ,funnel.

Fig 3.5Apparatus and chemicals requirement

2.Reaction carried out in beaker of dilute sulfuric acid, water and nails for 3 hours.

Fig 3.6 Solution after reaction done

3.Filter the solution using filter paper which contain in beaker.

Fig 3.7 Ferrous sulphate solution form

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 ‘‘Formation of ferrous sulphate by iron nails’’

4.Let heat the solution and make it half to increase the concentration of ferrous sulphate
solution and after that condense it. Condensation is done with solution at least 12 hours, after
that we see at bottom of beaker some blue crystals are form they are nothing but our product
ferrous sulphate.
.

Fig 3.8 final product ferrous sulphate

• NON-LABORATORY PRODUCTION PROCESS
PRODUCTION OF FERROUS SULPHATE BY SELECTIVE LEACHING METHOD
These is another production method at industrial scale by using scrap industrial iron waste.
These taken from Mohammed Ahmed article.
• Materials and Chemical Solution required
1. Industrial Iron Waste: The product from industrial processes (lathing process and filing
process), this waste be on small balls and reticulate shapes. 1.5 kg Industrial iron waste was
taken from work shop, this considered as sample. This waste considered as source to iron.
2. Sulfuric acid (H2SO4): It’s concentration of 99% purity and 99.09 g/mole molecular
weight was use in leaching solution and was purchased from the local market and be colorless
3. Laboratory tools: Which includes beakers that use as container for leaching solution with
the materials (industrial waste), The suitable solution was pulled by a pipette, sensitive balance
to scale the weight of the materials.
4. Distilled water : Used to mitigate the acid.
• PROCEDURE
1.The good absorbability of blood to metals in food supplement for that must be metals as
Sulphates model,Iron Sulphate was resulted by leaching method (using selective leaching
corrosion phenomenon)

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 ‘‘Formation of ferrous sulphate by iron nails’’

2.To product the source of iron food supplement, industrial iron waste was used here from the
workshop. Food supplement when product be ferric compound ferrous compound, both
compounds be as Sulphate of iron. To extract these compounds, extraction by leaching was
used.
3.Use Sulfuric acid (H2SO4) as dissolvent solution to leaching process. Mitigation of sulfuric
acid concentration by Distilled water in the beakers.
4.After mitigation of sulfuric acid in the beakers, put and diving the industrial waste (0.25kg)
from workshop in the solution of sulfuric acid, after a period from start reaction the color of
the solution converts into transparent green color, as shown in the figure below

Fig 3.9 scrap iron in sulfuric acid

After 24 hours from reaction the waste converts into very small black particles, precipitate
in bottom of beakers, as shown in the figure below,

Fig 3.10 Ferrous sulphate solution with crystals

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CHAPTER 4
ANALYSIS OF PRODUCT
For analysis of our product we do different identification test of product, for that we do test with OH
as NaOH, KOH and with other chemicals. But we do some test in laboratory as written below
• IDENTIFICATION TEST OF OUR PRODUCT
1.By using water-Water is using for our product identity ie ferrous sulphate is completely soluble
in water.

Fig 4.1 water and ferrous sulphate mixture

2.By using ethanol(95%)- To identify of product ie ferrous sulphate we perform another test by
using ethanol. In ethanol our ferrous sulphate is not soluble.

Fig 4.2 Ethanol and ferrous sulphate mixture

3.By using NaOH-When ferrous sulphate and NaOH are mix in test tube then dirty green
precipitate of ferrous hydroxide is formed.

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Fig 4.3 NaOH and ferrous sulphate mixture

4.By heating test-When ferrous sulphate crystal are heated in and test tube then ferric oxide,
sulfur dioxide, and sulfur trioxide are produced.

Fig 4.4 decomposition of ferrous sulphate

Also we do some comparison of properties of our obtain product and lab. Ferrous sulphate as
written in below table
Tab 4.1 comparison of properties of our product and lab FeSO4
Sr no Properties Our product Lab FeSO4 sample
1 Appearance Blue-green crystals Blue-green crystals
2 Odour Odourless Odourless
3 Melting Point 64 °C 64 °C
4 Boiling Point 300 °C 300 °C
5 Heptahydrate Blue crystals Blue crystals
6 Purity Above 95% 98.5%

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CHAPTER 5
PROPERTIES AND USES OF FERROUS SULPHATE
• Physical Properties
1. Odour-Odourless.
2. Appearance-Blue-green crystals.
3.Solubility-Soluble in water.

• Chemical Properties
1.Molecular Weight/ Molar Mass-151.908 g/mol.
2.Boiling Point-300 °C.
3.Melting Point-56-64 °C.
4.Chemical Formula-FeSO4
5.Anhydrous – White crystals.
6. Monohydrate – Yellowish white crystals.
7. Heptahydrate – Bluish-green crystals.

•USES OF FERROUS SULPHATE

1.Chemical industry use-Industrially, ferrous sulfate is mostly useful as a precursor to other iron
compounds. It is a reducing agent and is also for the reduction of chromate in cement to a less toxic
Cr (III) substance.

2.Medical Use-It is use as therapeutically at higher doses to cure or avoid iron-deficiency anemia.

3. Plants Growth-Iron (II) sulfate or ferrous sulfate, is a soil alteration to lower the pH of high
alkaline soil so that plants can absorb soil’s nutrients. It is useful for treating iron chlorosis in
horticulture.

• Other uses
1.Ferrous sulfate introduction into the cooling water running through the turbine condenser tubes to
create a corrosion-resistant protective layer.
2. It is useful in gold refining for precipitating metallic gold from auric chloride solutions (gold
dissolved in solution with aqua regia).
3. It is useful as an iron catalyst element of the Fenton reagent.
4. It’s one of the most necessary ingredients in the ink of iron gall.
5. Green vitriol is also a useful reagent for the detection of mushrooms.

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CONCLUSION
From this topic of mini-project (Formation of ferrous sulphate using iron nails) we understand
its manufacturing process on laboratory scale and industrial manufacturing process also. By
these we studied two manufacturing process of manufacturing of ferrous sulphate (1) using
(conc)sulfuric acid (2) using (dilute) sulfuric acid. Also we studied rate of reaction and how it
varies with time from these.
Also we seen properties of product (Melting, Boiling point, Odor, Appearance).
By these topic we studied lot of information regarding with ferrous sulphate and its different
manufacturing techniques.

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REFERENCES
1. Mohammed Ahmed (2021): Mohammed Ahmed University of Technology, Iraq
published article.
2. Kim. W. gate (2010) :Kim William Gates by Monohydrate published article.
3. Alexander Kehrmann,(2006): published article regarding with heptahydrate.
4.With help of google search engine.

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