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VIDYA PRATHISHTHANS COLLEGE OF ENGINEERING

LAB MANUAL
OF
CHEMISTRY
(APPLIED SCIENCE II)
SECOND SEMESTER
FOR FIRST YEAR ENGINEERING DEGREE COURSES

Approved By HoD
Dr. A. P. Hiwarekar

Approved By Principal
Dr. S. B. Deosarkar
PREPARED BY

Dr. APARNA G. SAJJAN

CHEMISTRY LAB MANUAL - II

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CONTENTS
Scope & Objectives

Common laboratory glassware

II

Safety rules

III

1. Determination of Alkalinity in given water sample by volumetric method.

14

2. To determine chloride (Cl ) content of water sample by Mohrs method.

56

3. To determine temporary & permanent hardness of water sample by EDTA method.

710

4. Spectrophotometric/colorimetric estimation of ferrous ions (Fe2+) from the given


solution.

1114

5. To Study of corrosion of metals in medium of different pH.

1517

6. Analysis of mixture of phosphoric acid and hydrochloric acid using indicators and
pH meter.

1821

7. To determine moisture, volatile matter & ash content of a given sample of coal.

2225

Appendix

2627

References

28

Skills developed

28

Grid table

29

CHEMISTRY LAB MANUAL - II

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SCOPE & OBJECTIVES


Water is one of the vital requirements for life on earth. The drinking water should be pure
and free of pollutants. Water is a good solvent and picks up impurities easily. Pure water -tasteless, colorless, and odorless - is often called the universal solvent. As water moves
through soil and rock, it dissolves very small amounts of minerals and holds them in solution.
Calcium & magnesium dissolved in water are the two most common minerals that make water
"hard."
One can test the water for its alkalinity, hardness and chloride content in the laboratory. These
water tests, make you understand the nature of the test, the water condition being measured,
and the significance of the test results.
When doing laundry in hard water, soap curds lodge in fabric during washing to make fabric
stiff and rough. Also causes graying of white fabric and the loss of brightness in colors.
Continuous laundering in hard water can shorten the life of clothes. In addition, soap curds
can deposit on dishes, bathtubs and showers, and all water fixtures. Hard water also
contributes to inefficient and costly operation of water-using appliances. Heated hard water
forms a scale of calcium and magnesium minerals that lead to inefficient operation or failure
of water-using appliances. Pipes can become clogged with scale that reduces water flow and
ultimately requires pipe replacement.
High Chloride content in water imparts a pungent taste and also irritates the mucous
membrane. Also leads to the bleaching (yellowing) of leaves of plants. If water with high
chloride content is used in industries, the chloride reacts with the metals leading to corrosion.
Of the eight experiments stated, three involve volumetric titrations for water analysis.
A phase diagram is a map that tells us what phases will be stable at what conditions. One
will understand & be able to find how these diagrams follow from plots of free energy curves.
Corrosion is deterioration of essential properties in a material due to reactions with its
surroundings. Weakening of iron due to oxidation of the iron atoms is a well-known example
of electrochemistry (a branch of chemistry that studies the reactions that take place when an
ionic and electronic conductor interfere) corrosion. This is commonly known as rust. This
type of damage usually affects metallic materials, and typically produces oxide(s) and/or
salt(s) of the original metal. Most structural alloys corrode merely from exposure to moisture
in the air, but the process can be strongly affected by exposure to certain substances.
By carrying out experiments in lab one can find the conditions as well as the rate of corrosion
of different metals. Then it can be prevented by treatments such as passivation and chromateconversion will increase a material's corrosion resistance.
The coal analysis for its moisture, volatile matter, ash and fixed carbon contents is carried
under proximate analysis. It is useful to find out heating value (GCV) and also gives quick
information about the quality of coal using which the suitability of the coal for a particular job
can be assessed.
I
CHEMISTRY LAB MANUAL - II

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COMMON LABORATORY GLASSWARES

Burette

Pipette

Conical flask

Test-tube

Silica crucible with vented lid

Beaker

Desiccator
II

CHEMISTRY LAB MANUAL - II

Measuring cylinder

Volumetric flask

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SAFETY RULES
1) Keep your bags in the cupboards below the
working table
2) Keep your hands away from your face, while
working.
3) Wash your hands with soap while leaving
the lab.
4) Keep your working table neat and clean.
5) Read the procedure thoroughly
starting the experiment.

before

6) Know what to do in case of emergency.


7) Handle the
carefully.

apparatus

and

chemicals

8) Leave plenty of tap water after discarding the


waste in the sink.
9) Do not waste the reagents/chemicals.

CHEMISTRY LAB MANUAL - II

III

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EXPERIMENT NO. 1
Aim: Determination of Alkalinity in given water sample by volumetric method.
Apparatus: Burette, Pipette, Conical flask, Dropper, measuring cylinder, Beaker etc.
Chemicals: 0.02 N HCl, phenolphthalein indicator & methyl orange indicator.
Theory: Pure water is neutral in nature with pH 7. Due to the presence of those minerals,
which increase the concentration of OH ions in water, the pH of water increases & it
becomes alkaline. These substances undergo dissociation or hydrolysis to form OH ions &
the total amount of such titrable bases in water expressed as equivalent of CaCO3 are
referred to as total alkalinity. Alkalinity is divisible into bicarbonate alkalinity, carbonate
alkalinity & in some cases hydroxide alkalinity. In most waters bicarbonates (HCO3-) and
carbonates (CO3=) are the major bases, but others can also be important under particular
conditions. Total alkalinity of natural waters may range from 5mg to several hundreds per
litre (as CaCO3). For biological purposes a total alkalinity over 40 mg of CaCO3/litre is
considered to indicate hard waters.
Alkalinity refers to the capability of water to neutralize acid. The presence of calcium
carbonate or other compounds such as magnesium carbonate contribute carbonate ions to
the alkalinity. Alkalinity is often related to hardness because the main source of alkalinity is
usually from carbonate rocks (limestone), which are mostly CaCO3. If CaCO3 actually
accounts for most of the alkalinity, hardness in CaCO3 is equal to alkalinity. Since hard water
contains metal carbonates (mostly CaCO3) it is high in alkalinity.
Environmental Impact: Alkalinity is important for aquatic life because it protects against rapid
pH changes. Aquatic life functions best in a pH range of 6.0 - 9.0. Higher alkalinity levels in
surface waters will buffer acid rain & other acid wastes & prevents pH changes that are harmful
to aquatic life.
Effect on boilers: If water having high alkalinity is used for steam generation in boilers, it will
lead to boiler troubles like caustic embrittlement, scale & sludge formation.
The above alkalinities can be determined volumetrically by titrating water sample against
standard acid using methyl orange and phenolphthalein indicators.
Detected by
Phenolphthalein Indicator

OH + H+

H2O (one step neutralization, P =M)


Detected by
Methyl orange Indicator

HCO3 + H+

H2 CO3 (one step neutralization, M)


Detected by
Phenolphthalein Indicator

CO3 2 + H+

H CO3 (first step)


Detected by

(Two step neutralization, 2P)

Methyl orange Indicator


+

HCO3 + H

H2 CO3 (second step)

CHEMISTRY LAB MANUAL - II

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Procedure:
Part A: Preparation of solutions
1) Standard 0.02 N HCl solution: Dilute 1.72 ml of concentrated AR grade hydrochloric acid
(11.6N) to 1 litre with distilled water in a volumetric flask.
2) Phenolphthalein indicator: Dissolve 500 mg of phenolphthalein in 50 ml ethanol & 50 ml
distilled water (100 ml 50%ethanol).
3) Methyl orange indicator: Dissolve 50 mg of methyl orange in 100 ml distilled water.
Part B: Determination of alkalinity
0 ml
V1 ml (phenolphthalein
end point)

V2 ml (Methyl orange
end point)

Check the pH of water sample at the beginning to find whether


the sample is alkaline or not. If pH of the sample is above 8.00
then follow the procedure given below.
Pipette out 50 ml of filtered water sample in a conical flask &
add 4 drops of alcoholic phenolphthalein indicator to it. If the
solution turns pink then titrate it with 0.02N HCl until
colourless. Let this burette reading be V1. To the same solution
or to the solution, which remains colourless even after adding
phenolphthalein indicator, add about 4 drops of methyl orange
indicator. If the solution becomes yellow then continue titration
till orange pink colour is obtained at the end point. Let this
burette reading be V2 from the beginning. This is called methyl
orange end point. Repeat the titration for 2 more times & find
out the constant burette reading.

Reference table:
Alkalinity (ppm)
Relation between

Hydroxide

V1 & V2 / P & M

(OH )

(CO3 2 )

(HCO3 )

alkalinity

alkalinity

alkalinity

---------

--------

V1 = 0 / P = 0
V1 = V2 / P = M

Condition
If phenolphthalein end point is zero, then
alkalinity is due to only bicarbonate.

If methyl orange end point is zero & only


there is phenolphthalein end point, then the M
alkalinity is due to hydroxide alone.

If phenolphthalein end point is exactly half


the total titration, then only carbonate
V1= V2 / P = M
alkalinity is present.

---------

-------

If phenolphthalein end point is greater than


half the total titration, then alkalinity is due
V1 > V2 / P > M
to both carbonate & hydroxide.
2P M

CHEMISTRY LAB MANUAL - II

Carbonate Bicarbonate

2P
2( M P )

M
--------

-------

-------

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V1 < V2 / P < M If phenolphthalein end point is less than half
the total titration, then alkalinity is due to
both carbonate & bicarbonate.

------2P

M 2P

Observations:
Readings (ml)
Sample No.

Phenolphthalein end point, V1 = P

Methyl orange end point, V2 = M


(Yellow to Orange pink)

(Pink to Colourless)

Constant

Constant

1)
2)
3)
Calculations:
All kinds of alkalinity are expressed in terms of CaCO3 equivalents as parts per million.
1000 ml of 1N HCl 50 g of CaCO3
1 ml of 1N HCl
50 mg of CaCO3

V ml of 0.02 N HCl 50 x V x 0.02


= V mg of CaCO3
V mg of alkalinity is present in 50 ml of water sample
For 1000ml of water sample i.e., 106 mg of water, alkalinity = (1000 x V)/50 = 20 V ppm
Phenolphthalein alkalinity, P = 20 V1 ppm & Methyl orange alkalinity, M = 20 V2 ppm
1) Calculation for condition 1: water sample having only bicarbonate alkalinity, V1 = 0
Methyl orange end point, V2 = _____ ml
Methyl orange alkalinity, M = 20 V2 ppm = ________ ppm
Alkalinity due to HCO3 = M = ______ ppm
2) Calculation for condition 2: water sample having only hydroxide alkalinity, V1 = V2
Phenolphthalein end point, V1 = _____ ml
Phenolphthalein alkalinity, P = 20 V1 ppm = ________ ppm

Alkalinity due to OH = P = ______ ppm


3) Calculation for condition 3: water sample having only carbonate alkalinity, V1= V2
Phenolphthalein end point, V1 = ____ ml = Methyl orange end point, V2 = _____ ml
Phenolphthalein alkalinity, P = 20 V1 ppm = _______ ppm

Alkalinity due to CO3 2

= 2P = ______ ppm

CHEMISTRY LAB MANUAL - II

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4) Calculation for condition 4: water sample having both CO3 2 & OH alkalinity, V1 > V2
Phenolphthalein end point, V1 = _____ ml
Phenolphthalein alkalinity, P = 20 V1 ppm = ________ ppm
Methyl orange end point, V2 = _____ ml
Methyl orange alkalinity, M = 20 V2 ppm = ________ ppm
Alkalinity due to OH = 2P M = ___________________ =
Alkalinity due to CO3 2 = 2 ( M P ) = _________________ =

________
________

ppm
ppm

5) Calculation for condition 5: water sample having both CO3 2 & HCO3 alkalinity, V1 < V2
Phenolphthalein end point, V1 = _____ ml
Phenolphthalein alkalinity, P = 20 V1 ppm = ________ ppm
Methyl orange end point, V2 = _____ ml
Methyl orange alkalinity, M = 20 V2 ppm = ________ ppm
Alkalinity due to CO3 2 = 2P = ___________________ = ________ ppm
Alkalinity due to HCO3 = M 2P = ___________________ = ________ ppm
Result:
Water sample

Hydroxide (OH )
alkalinity, ppm

Carbonate (CO3 2 )
alkalinity, ppm

1)
2)
3)

Related Questions:
1) Define Alkalinity.
2) What are the types of alkalinities of water?
3) What are the pH transition ranges of the indicators used?
4) What are the ill effects of alkaline water on boilers?

CHEMISTRY LAB MANUAL - II

Bicarbonate (HCO3 )
alkalinity, ppm

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EXPERIMENT NO. 2
Aim: To determine chloride (Cl ) content of water sample by Mohrs method.
Apparatus: Measuring cylinder, conical flask, volumetric flask, burette, pipette, dropper, etc.
Chemicals: Standard 0.02N Silver nitrate solution & 5 % potassium chromate solution as
indicator.
Theory: Chlorides are present in water usually as NaCl, MgCl2 & CaCl2. Chlorides are not
harmful but their concentrations above 250 ppm impart a peculiar taste to the water thus
making the water unacceptable for drinking purposes. High concentration of chloride in a
water sample indicates pollution. MgCl2 & CaCl2 are responsible for permanent hardness of
water.
Mohrs method is used for the determination of chloride ions in water sample, which is neutral
or slightly alkaline. This method determines the chloride ion concentration of a solution by
titration with silver nitrate. As the silver nitrate solution is slowly added, a precipitate of silver
chloride forms.

Ag+(aq) + Cl (aq)

AgCl(s)

(White ppt)

The indicator used is dilute potassium chromate solution. When all the chloride ions have
reacted, any excess silver nitrate added will react with chromate ions to form a red-brown
precipitate of silver chromate. This procedure is known as Mohrs method.

2AgNO3(aq) + K2CrO4(aq)

Ag2CrO4(s) +

2KNO3

(Red-brown ppt)

The pH of the water sample should be between 7 - 8.5. At pH higher than 8.5, silver ions get
hydrated to form silver hydroxide. And at pH below 7 (acidic), potassium chromate is
converted to potassium dichromate.
Procedure:
Preparation of solutions:
1) Standard 0.02N silver nitrate solution: Dissolve exactly 3.3978g of dry solid AgNO3 in
distilled water & dilute it to 1 liter with distilled water in a volumetric flask, then store in a
brown bottle.
2) 5% Potassium chromate solution: Dissolve 5g of solid K2CrO4 in 100 ml distilled water.
Determination of chloride:
Back titration: Pipette out 50 ml of given water sample into a 250 ml conical flask & add 5
6 drops of potassium chromate as indicator. Now titrate this yellow coloured solution against
standard 0.02N silver nitrate solution taken in burette. Initially white precipitate of silver
chloride is formed which appears yellow due to the indicator. When all the chloride ions in
water sample gets precipitated then addition of an extra drop of silver nitrate forms a reddishbrown precipitate of silver chromate. Thus formation of reddish-brown precipitate indicates
the end point. Note down the burette reading & repeat the same titration for 2 more times.
Let the constant burette reading be X ml.
CHEMISTRY LAB MANUAL - II

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Blank titration: A blank titration is also carried out as above with distilled water. In a 250 ml
conical flask pipette out 50 ml distilled water & add 5 6 drops of potassium chromate as
indicator. Now titrate it against standard 0.02N silver nitrate solution until the formation of
reddish-brown precipitate at the end point. Note down the burette reading & repeat the same
titration for 2 more times. Let the constant burette reading be Y ml.
Observations:
Blank titration
Reading in ml

II

III

Constant reading (X)

II

III

Constant reading (Y)

Initial
Final
Difference
Back titration:
Reading in ml
Initial
Final
Difference
Calculations:
Volume of water sample taken for titration = 50ml.
Volume of 0.02 N silver nitrate that has reacted with the chloride ions = Y X = ____ = Z ml.
1 mole of AgNO3
1 mole of AgCl

1 mole of AgCl

1 mole of AgNO3
1000 ml 1N AgNO3

1 mole of Cl

1 mole of Cl

Z ml 0.02 N AgNO3
Weight of chloride ions

35.5 g of Cl
Z x 0.02 x 35.5 g of Cl
Z x 0.02 x 35.5
50

Strength of chloride ions per litre = 1000 x A


Or

= _______ = A gm/ liter


= _______ mg chloride ions / litre
= _______ ppm of chloride ions

Result: The given water Sample contains __________ of chloride ions.


Related Questions:
1)

What is the type of titration used to determine the chloride content?

2)

Name the salts that contribute for the chloride content in water.

3)

What are the ill effects of chloride in water?

4)

Name the indicator used in the above method.


CHEMISTRY LAB MANUAL - II

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EXPERIMENT NO. 3
Aim: To determine temporary & permanent hardness of water sample by EDTA
method.
Apparatus: Burette, Pipette, Conical flask, Dropper, Beaker etc.
Chemicals: Ethylene diamine tetra acetic acid (EDTA) solution, zinc sulphate solution,
ammonia buffer of pH 10 & Eriochrome black-T indicator.
Theory: Hardness of water can be defined as the soap consuming capacity of water
resulting in the formation of white curdy PPT due to the presence of salts of Ca & Mg salts.
Ca/Mg + sodium stearate (C17H35COONa)
Salts
Soap

Ca (C17H35COO)2 / Mg(C17H35COO)2
Calcium/Magnesium stearate (curd)

Total hardness = It is due to the presence of all the salts of Ca & Mg.
= Temporary hardness + Permanent hardness
Temporary hardness: It is due to the presence of bicarbonates and soluble carbonates of
Ca & Mg. Also called as carbonate hardness & can be removed by boiling. Ca(HCO3)2,
Mg(HCO3)2, MgCO3.
Permanent hardness: It is due to the presence of sulphates, chlorides and nitrates of Ca &
Mg. Also called as non-carbonate hardness, which cannot be removed by boiling. It requires
lengthy treatment. CaCl2, MgCl2, CaSO4, MgSO4, Ca(NO3)2, Mg(NO3)2 etc.
For determining suitability of water for domestic and industrial purpose, type of hardness and
the amount of hardness is important. For the estimation of total hardness of a sample,
disodium salt of EDTA is used. Na2EDTA forms 1:1 complex with divalent metal ions like
Ca2+, Mg2+, Fe2+, Zn2+, etc.
NaOOCH2C

CH2COOH
N CH2 CH2 N

HOOCH2C

CH2COONa
Disodium-EDTA Structure

The anion of EDTA (H2Y4-) is a strong chelating agent, which forms a stable anionic complex
with divalent metal ions in basic medium.
Therefore alkaline buffer of NH4OH & NH4Cl of
pH-10 is used. In this complexometric titration, Eriochrome black -T is used as an indicator.
This indicator forms unstable wine red coloured complex with metal ions, which dissociates
on titration with EDTA solution. On dissociation, a strong metal ion- EDTA complex is formed
and indicator is set free which gives blue colour to the solution at the end.

CHEMISTRY LAB MANUAL - II

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M2+

HIn2

Metal ion

MIn

MIn

Indicator

Metal-Indicator complex

Blue

Wine red

H2Y4

MY2

HIn2

EDTA

Metalion-EDTA

Indicator

Ionic form

Complex

Blue

O
||

H+

C
O
||
C

O
CH2
CH2

N
CH2

Ca/Mg + EDTA

M = Ca / Mg
CH2

N
C
||
O

CH2
CH2
O
C
||
O

Metal +2 EDTA4 complex


The following table gives the relation between the type of water sample & the degree of hardness
Nature of water

Hardness in ppm (CaCO3 equivalent)

Soft

Below 50 ppm

Moderately hard

50-150 ppm

Hard

150-300 ppm

Very hard

Above 300 ppm

CHEMISTRY LAB MANUAL - II

H+

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Procedure: Part A: Preparation of solutions


1) Standard 0.01 M ZnSO4. 7H2O solution: Weigh accurately 0.718 g of pure zinc sulphate &
dissolve it in distilled water in a beaker. Then transfer it to a 250 ml volumetric flask & take
washings of beaker into the volumetric flask. Dilute this solution upto the mark with distilled
water and make it homogeneous.
2) 0.01m EDTA solution: Dissolve 3.723 g of Disodium EDTA in one litre distilled water as above.
3) Buffer solution of pH-10: Dissolve 68 g of NH4Cl in distilled water. Add 572 ml of liquor
ammonia and dilute to 1 litre with distilled water.
4) Eriochrome black-T indicator: Add 0.2 g of solid dye in 15 ml of triethanol amine & 5ml of ethanol.
Part B: Standardisation of EDTA solution:
Fill the burette with approximately 0.01m EDTA solution. Pipette out 25 ml of above standard ZnSO4
solution in a conical flask, add 5ml of pH 10 buffer solution using measuring cylinder & then add 5
drops of Eriochrome black-T indicator. Titrate this wine red coloured solution against EDTA solution
till the colour changes to blue at the end point. Repeat the same titration for 2 times and note the
constant burette reading as X ml. Using this value calculate the exact molarity of EDTA solution.
Observations and Calculations:
Reading in ml

II

III

Constant reading (X)

Initial
Final
Difference
M1V1 (ZnSO4) =
M2V2 (EDTA)
0.01 x 25
=
M2 x X
M2
= ( 001 x 25 ) /X
Molarity of EDTA = M2 = ______ M.
Part C: Total hardness of water sample:
Pipette out 50 ml of water sample in a conical flask, add 5ml of pH 10 buffer solution & then add 5
drops of Eriochrome black-T indicator. Titrate the wine red coloured solution against EDTA solution
taken in burette till the colour changes to blue at the end point. Repeat the same titration for 2 times
and note the constant burette reading as Y ml. Using this value calculate the total hardness of water
sample.
Observations and Calculations:
Reading in ml

II

Initial
Final
Difference

CHEMISTRY LAB MANUAL - II

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Constant reading (Y)

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EDTA and Ca2+/Mg2+ ions form 1:1 complex


1 mole EDTA

1 mole Ca2+/Mg2+
1 mole EDTA

100 g CaCO3
Thus 1000 ml 1M EDTA
100 g CaCO3
1ml 1M EDTA

1g CaCO3
1ml 0.01M EDTA

1mg CaCO3
Y ml M2 M EDTA

1 mole of CaCO3

( Y x M2 ) / 0.01 mg of CaCO3
_______ mg of CaCO3 = A

50 ml water sample contains A mg of CaCO3


1000 ml water sample contains (A x 1000) /50
= 20 A mg of CaCO3
But 1 mg of CaCO3 per litre of water is 1 parts per million (ppm) of CaCO3
Thus total hardness of water sample is = 20 A = _______ ppm.
Part D: Permanent hardness of water sample:
Take 250 ml of hard water sample into a 500 ml beaker & boil it for about 30 minutes. Then cool &
transfer the water into a 250 ml volumetric falsk and make the volume upto the mark with distilled
water. Pipette out 50 ml of this water sample, add 5ml of pH 10 buffer, 5 drops of Eriochrome blackT indicator & titrate it against standard EDTA solution as given in part C. Repeat the same titration
for 2 times and note the constant burette reading as P ml. Using this value calculate the permanent
hardness of water sample.
Observations and Calculations:
Reading in ml

II

Constant reading (P)

III

Initial
Final
Difference
1ml 0.01M EDTA

1mg CaCO3

P ml M2 M EDTA

(P x M2) / 0.01

mg of CaCO3

_______ mg of CaCO3
50 ml water sample contains B mg of CaCO3

= B

1000 ml water sample contains


(B x 1000) / 50 = 20 B mg of CaCO3
Thus Permanent hardness of water sample is = 20 B = _______ ppm.
Temporary hardness = Total hardness permanent hardness
Temporary hardness = 20 A 20B = _________ ppm

CHEMISTRY LAB MANUAL - II

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Result:
Determinations

Value

1) Strength of EDTA solution

molar

2) Total hardness of given water sample

ppm of CaCO3

3) Permanent hardness of water sample

ppm of CaCO3

4) Temporary hardness of water sample

ppm of CaCO3

Conclusion: The water sample analysed has_____ppm of hardness hence it is __ __


Related Questions:
1) Define hardness. What are the types of hardness of water?
2) What type of titration is used in the above method? Name the indicator used.
3) What are the ill effects of hard water on boilers?

CHEMISTRY LAB MANUAL - II

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EXPERIMENT NO. 4
Aim: Spectrophotometric / colorimetric estimation of ferrous ions (Fe2+) from the given
solution.
Apparatus: Spectrophotometer or colorimeter, 50 ml volumetric flasks, Beaker etc.
Chemicals: 0.25% ortho-phenanthroline solution, 10% hydroxylamine hydrochloride solution,
ammonium acetate buffer solution, 0.2% sodium acetate solution, concentrated HCl,
standard 0.1, 0.2, 0.3, 0.4 & 0.5 N iron solutions.
Theory: Colorimetry is the science of measuring colors. One useful and often used way of
determining the concentration of a chemical in a solution, if it has a color, is to measure the
intensity of the color and relate the intensity of the color to the concentration of the solution.
Several useful factors are very important.

The BeerLambert law, also known as Beer's law or LambertBeer law is an empirical
relationship that relates the absorption of light to the properties of the material through which
the light is traveling. It states that the optical absorbance of a chromophore in a transparent
solvent varies linearly with both the sample cell path length & the chromophore
concentration.
Absorbance is measured in a colorimeter or spectrophotometer by passing a collimated
beam of light at wavelength through a plane parallel slab of material that is normal to the
beam. For liquids, the sample is held in an optically flat, transparent container called a
cuvette. Absorbance (A) is calculated from the ratio of light energy passing through the
sample (I0) to the energy that is incident on the sample (I):

A = -log (I/I0)
Beer's Law follows:

A = bc

= molar absorptivity or extinction coefficient of the chromophore at wavelength (the


optical density of a 1-cm thick sample of a 1 M solution). is a property of the material and
the solvent. b = sample pathlength in centimeters & c = concentration of the compound in
the sample, in molarity (mol L-1)
The reaction between ferrous ion and 1,10-phenanthroline to form a red complex serves as a
sensitive method for determining iron (II). The molar absorptivity of the complex,
[(C12H8N2)3Fe]2+, is 11,100 at 508 nm. The intensity of the color is independent of pH in the
range 2 to 9. The complex is very stable and the color intensity does not change appreciably
over long periods of time. Beer's law is obeyed. Hydroxylamine hydrochloride is used to
reduce any ferric ion that is present. The pH is adjusted to a value between 6 & 9 by adding
ammonia or sodium acetate. 1,10-phenanthroline is a bidentate ligand and only has 2 active
sites to bond with iron, so the oxidation state it prefers to bond with is the Fe2+ or Fe(II).
CHEMISTRY LAB MANUAL - II

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Fe2+ + 3phen

1,10-phenanthraline

(phen)3Fe(II)

Tris (1,10 phenanthraline) Iron (II) complex


A
B
S
O
R
B
A
N
C
E

A
(0,0)
CONCENTRATION, C (mg/ml)

Fig-1: Spectrum showing max at 508 nm

Fig-2: Beers plot [for standard Fe (II) solution]

Procedure: Preparation of solutions:


1) 0.25% 1,10-phenanthroline solution: Dissolve exactly 0.25 g of solid 1,10phenanthroline monohydrate in 100 ml of distilled water & slightly warm it.
2) 10% Hydroxylamine hydrochloride solution: Dissolve 10 g of solid Hydroxylamine
hydrochloride in 100 ml of distilled water.
3) 5% Sodium acetate solution: Dissolve 5 g of Sodium acetate in 100 ml of distilled water.
4) Standard Ferrous ammonium sulphate solution: Weigh accurately about 0.0702 g of
pure ferrous ammonium sulphate hexahydrate, dissolve it in distilled water & transfer the
solution to a 1liter volumetric flask. Add 2.5mL of conc. sulfuric acid & dilute the solution
to the mark with distilled water. Calculate the concentration of solution in mg of Fe / mL.
5) Unknown Fe(II) solution: Add about 0.2 g of the solid unknown & approximately 0.25 mL
conc. sulfuric acid into a 100 mL volumetric flask. Dilute to the mark with distilled water.
Determination of Fe (II): Into five 50 mL volumetric flasks, pipette out (volumetrically) 5, 10,
15, 20, and 25 mL portions of the standard iron solution. To another 50 mL volumetric flask
pipette out 1 ml of unknown solution of iron (II). Put 5 mL of distilled water into another flask
to serve as the blank. To each flask, including the "prepared unknown" (7 flasks), add 5 mL
of the hydroxylamine solution, 5 mL of the 1,10 phenanthroline solution and 5 mL of the
sodium acetate solution. Then dilute all the solutions to the 50 mL marks and allow them to
stand for 10 minutes with occasional shaking.

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Using the blank as a reference and any one of the iron solutions prepared above, measure
the absorbance at different wavelengths in the interval from 400 to 700 nm. Take reading
about 20 nm apart except in the region of maximum absorbance where intervals of 5 nm
should be used. Plot the absorbance vs. wavelength and connect the points to from a
smooth curve as shown in Fig-1. Select the proper wavelength to use for the determination of
iron with 1,10-phenanthroline. Also, calculate the molar absorption coefficient, , at the
wavelength of maximum absorption ( max) on the absorption curve (assume b = 1 cm).
Measure the absorbance of each of the standard solutions and the unknown at the selected
wavelength. Plot the absorbance vs. the concentration of the standards as shown in Fig-2.
Note whether Beer's law is obeyed. Using the absorbance of the unknown solution calculate
the % (w/w) iron in original solid sample.
Observations:
Serial No.

Volume of standard
Fe (II) solution

1.

5 ml

2.

10 ml

3.

15 ml

4.

20 ml

5.

25 ml

6.

Blank

7.

Unknown

Concentration In
mg/ml

Absorbance, A (Or %transmittance, T)


A = log T

Calculations:
Concentration of standard Fe solution = 0.01 mg/ml
Using C1V1 = C2V2, calculate the concentration of all solutions.
Now plot the graph of absorbance Vs. Concentration & from this standard graph, determine
the concentration of unknown Fe (II) solution as shown below:
A
B
S
O
R
B
A
N
C

Absorbance of
Unknown solution

A
Concentration of
Unknown solution

(0,0)
CONCENTRATION, C (mg/ml)

CHEMISTRY LAB MANUAL - II

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Result: The concentration of ferrous ion in a given solution is _______ mg/liter.


Related Questions:
1) State the BeerLambert law or Beer's law.
2) Name the ligand used to complex Fe+2 ions.
3) What is the wavelength of maximum absorbance for [(C12H8N2)3Fe]2+ complex?
4) Why Hydroxylamine hydrochloride is added?

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EXPERIMENT NO. 5
Aim: Study of corrosion of metals in medium of different pH.
Apparatus: Beakers, metal bars, pH meter, sand paper, weighing balance, etc.
Chemicals: Standard 2N hydrochloric acid and 2N sodium hydroxide (for preparing solutions
of different pH).
Theory: Corrosion is the primary means by which metals deteriorate or Corrosion is defined
as the destruction of metals through chemical or electrochemical reactions taking place at its
surface. Most metals corrode on contact with water (& moisture in the air), acids, bases,
salts, oils, aggressive metal polishes, and other solid & liquid chemicals. Metals will also
corrode when exposed to gaseous materials like acid vapors, formaldehyde, ammonia, and
sulfur containing gases.
Corrosion specifically refers to any process involving the
deterioration or degradation of metal components. The best example is that of the rusting of
iron/steel.
If a piece of metal is immersed in a polar solvent like water, some of the metal ions leave the
metal surface and go into the solution i.e., dissolution of metal starts. The metal continues to
dissolve, more and more electrons are left back and a net negative charge is built up in the
metal. Thus metal acquires a negative charge. The potential developed can be measured
under standard conditions using standard hydrogen electrode as a reference electrode. It is
called standard oxidation potential of metal. The metals having positive values are noble,
they do not dissolve readily (metals like gold, platinum, silver, etc.). The metals having
negative values of electrode potential are called active metals, which go into solution readily
(like iron, zinc, magnesium, etc.).
Metal

Electrode Potential (V)

Gold (Au2+)

+ 1.498

2+

Platinum (Pt )

+ 1.18

Silver (Ag+)

+ 0.7996

2+

Copper (Cu )
+

Hydrogen (H )
2+

Iron ((Fe )

+ 0.3419
0
- 0.447

2+

Zinc (Zn )

- 0.7618
3+

Aluminium (Al )

- 1.662

2+

- 2.372

Magnesium (Mg )

This behaviour of metals depends upon the environmental conditions to which they are
exposed. It can be studied by immersing metal plates in the solutions of different pH for a
fixed or constant time.
pH = log [ H+ ]

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Procedure: Take 5 metal plates (mild steel or zinc) of size 6cm x 2.5cm having same
thickness. Rub the metallic plates with sand paper to remove any corrosion product on it.
Weigh them separately and note down their respective weights.
Prepare solutions having different pH such as 1.5,
2.0, 3.0, 5.0 & 8.0 units by mixing standard 2N HCl
& 2N NaOH. Measure their pH using pH meter.
Take five 50 ml beakers, label them and take
about 30 ml above solutions in the beaker. Dip
the previously weighed metallic strips in the
beaker such that 4/5th portion is immersed in the
solution. Note down the time.

Beaker
Electrolyte solution
Metal plate

Corrosion assembly

After one hour take out the metallic plates from the
beaker, dry them in air and then weigh. Note
down the respective weights of the plates.

Observations:
Plate No.

pH of the
solution

1.

1.5 unit

2.

2.0 unit

3.

3.0 unit

4.

5.0 unit

5.

8.0 unit

Calculations:

Weight of the plate


Before

After

Loss in weight
(In 1 hr)

Loss/gm/hr

Loss in weight (in 1 hr.) = Before weight After weight = X gm


Weight loss / before weight /hr. = X gm = ______ gm
Loss of metal /gram/hr. = X / Before weight = _______ gm

Plate No. 1:
Plate No. 2:
Plate No. 3:
Plate No. 4:
Plate No. 5:

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Result:

Weight loss / gm / hour is maximum in _______ pH solution.


Weight loss / gm / hour is minimum in _______ pH solution.

Conclusion:

Related Questions:
1) Define corrosion.
2) How does pH affects the rate of corrosion?
3) Name the series in which metals and their alloys are arranged according to their
anodic or cathodic nature.

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EXPERIMENT NO. 6
Aim: Analysis of mixture of phosphoric acid and hydrochloric acid using indicators
and pH meter.
Apparatus: Burette, pipette, conical flask, burette stand, beaker, magnetic stirrer, pH-meter,
glass electrode, etc.
Chemicals: 0.1 N sodium hydroxide, standard buffer solution of Known pH and 3:1
phenolphthalein naphtholphthalein indicator mixture.
Theory: An acid or a base is quantitatively determined by titration using pH meter or acidbase indicators to detect the equivalence point/end point. pH-meter is frequently used
because the advantage that one actually monitors is the change in pH at the equivalence
point rather than just observing the colour change of a visual indicator. This eliminates any
indicator blank error.
The titration of a mixture of phosphoric acid and hydrochloric acid is complicated by the fact
that phosphoric acid is a triprotic acid with
Ka1 = 7.5x10-3, Ka2 = 6.2x10-8, and Ka3 = 4.8x10-13.
Ka1 is sufficiently large that the first proton from phosphoric acid cannot be differentiated from
strong acids like hydrochloric acid. The second dissociation of phosphoric acid is varies
significantly from the first. The second proton can be neutralized and differentiated from the
first phosphoric acid proton and the strong acid proton.
At the first equivalence point: pH = 4.7
H3PO4 (aq) + OH(aq)

H2PO4(aq) + H2O(l)

At the second equivalence point: pH = 9.3


H2PO4 (aq) + OH(aq)

HPO42 (aq) + H2O(l)

Neutralization of the third proton of phosphoric acid does not produce an appreciable break
in the titration curve. This is ultimately because Ka3 is very small and acids with small Ka' s
produce small breaks. Because Ka3 is so small, the basicity (proton accepting ability) of the
phosphate ion is large, and it undergoes hydrolysis producing hydroxide ion.
HPO42 (aq) + OH(aq)
Overall reaction: H3PO4 (aq) + 3OH(aq)

PO43 (aq) + H2O(l)


PO43 (aq) + 3H2O(l)

To express H+ ion concentration, pH scale is used. This pH can be measured directly using a
pH meter. pH = log H+ ion concentration Or pH = log [H+].
The titration curve for a mixture of phosphoric and hydrochloric acids are illustrated here.
The first break in the mixed acid curve indicates the amount of hydrochloric acid plus the
amount of the phosphoric acid. The amount of phosphoric acid in the sample is indicated by
the difference between first and second breaks in the titration curve. The first equivalence
point volume (25.0 mL) permits calculation of the total meq of HCl + (meq H3PO4)/3 since the
first proton of H3PO4 is neutralized.

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In acid-base titrations addition of base to the


acid, decreases the H+ ion concentration of the
reaction mixture.
This change in pH
(equivalence point) can be measured by pHmeter or the end point can be found out by
using visual indicators.
When a pair of electrodes namely pH sensitive
glass electrode and reference electrode are
dipped in an aqueous solution, they generate
e.m.f. which is proportional to the pH of the
solution.
This e.m.f. (E) is temperature
dependent & is given by the Nernst equation:
RT
E

ln [H+]

2.303 RT
E

log [H+]

F
2.303 RT
E

pH
F

Where -

E0
R
T
F

=
=
=
=

voltage that depends on the reactants and the products in the reaction.
Gas constant, 8.314 J mol-1 K-1
Absolute temperature in Kelvin.
Faraday, the charge on one mole of electrons (96485 coulombs).

Procedure: Preparation of solutions:

1. Standard 0.1N sodium hydroxide solution: Weigh accurately 4 g of pure NaOH in a clean watch
glass and transfer it to a beaker. Dissolve it in distilled water and collect the washings of the watch
glass in the same beaker. Then transfer it to a 1liter volumetric flask & take washings of beaker
into the volumetric flask. Dilute this solution upto the mark with distilled water and make it
homogeneous.

2. 0.01% Methyl orange indicator: Weigh 0.01 g of solid methyl orange and dissolve it in 100ml
distilled water.

3. 0.05% Phenolphthalein indicator: Weigh 0.05 g of solid phenolphthalein and dissolve it in


100ml 50% ethanol (50ml ethyl alcohol + 50ml distilled water).
Determination of mixture of HCl & H3PO4:
Measurement of pH of unknown sample consists of two steps. First step is to standardise
the pH meter using a known standard buffer solution (usually of pH 7) at room temperature.
The second step involves the measurement of pH of unknown solution.
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Standardisation of pH meter: Switch on the instrument by turning the control ON and set
the function switch to standard-by, STD BY position. Rinse the electrode pair with distilled
water and wipe them carefully with tissue or filter paper. Take the beaker containing
standard buffer solution of pH 7.00 and dip the electrodes in it. Set the function switch to the
pH position. Set the buffer value on digital display to read 7.00 by rotating the Standardise
knob. Put back the function switch to STD BY mode. Now without disturbing the
Standardise knob, complete all the pH measurements of titration.
Acid-Base titration using pH-meter: Pipette out 25ml of acid mixture (0.1N HCl + 0.05N
H3PO4) in a 100ml beaker. Rinse the glass electrode with distilled water and wipe it with
filter paper. Now dip the electrode in the beaker containing acid solution. Set the function
switch to pH mode and note down the pH of the solution displayed on the digital display of
pH meter. Fill the burette with standard 0.1N sodium hydroxide solution. Add 5 ml of NaOH
to the beaker containing acid solution and stir it using a magnetic stirrer. Note down the pH
of the solution. Similarly measure the pH of the reaction mixture after adding 10, 15, 20,
25,30,35,40 and 45 ml of NaOH from burette. Watch for the region where the pH begins to
change rapidly with each added portion of titrant. As the pH begins to change more rapidly,
add the titrant in smaller portions. When you have passed the equivalence point by several
ml, there is no reason to continue any further in the titration.
Then plot graphs of pH versus volume of NaOH added and pH/ml versus volume of
NaOH. From the graph, find out the end point of titration.
Acid-Base titration using indicator: Pipette out 25 ml of acid mixture (0.1N HCl + 0.05N
H3PO4) in a conical flask and add 2-3 drops of methyl orange indicator. Titrate this orange
red solution against standard 0.1N NaOH till the solution becomes yellow at the end point
(first).
After recording the burette reading, to the same flask add 2-3 drops of
phenolphthalein indicator and continue the titration till the solution turns pink at the end point
(second). Record the total burette reading. Repeat the titration and Compare the results
with the first method.
Observations: For pH-meter method
Volume of NaOH added, (ml)
05
10
15
20
22
24
26
28
30
35
40
45
50
CHEMISTRY LAB MANUAL - II

pH

pH

ml

pH / ml

VPCOE

Plot the following graphs:


Graph I (pH Vs volume of NaOH)

Graph II (
ml Vs volume of NaOH)
(pH/

pH
ml

pH

(0,0)

ml of NaOH

ml of NaOH

From the graphs find out the end/equivalence points of the titration = ______ & _____ ml
Observations: For Indicator method
Reading in
ml

Readings (ml)
Methyl orange end point, V1 = M

Phenolphthalein end point, V2 = P

(Orange pink to Yellow)

(Colourless to Pink)

Constant

Initial
Final
Difference
End point of titration is = X = ______ & ______ ml

1)
2)
3)
4)
5)

1.1 x 5ml = C2 x 50
For 5 ml solution, C2 = (0.01 x
For 10 ml solution, C2 = (0.01 x
For 15 ml solution, C2 = (0.01 x
For 20 ml solution, C2 = (0.01 x
For 25 ml solution, C2 = (0.01 x

5) / 50 = 0.001
10) / 50 = 0.002
15) / 50 = 0.003
20) / 50 = 0.004
25) / 50 = 0.005

Result:
Related Questions:
1) What is the pH value at the first and the second equivalence point?
2) Why standard buffer solution of pH 7 is used?
3) Name the two indicators used in this titration.
4) How end point of titration is detected using pH meter?
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Constant

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EXPERIMENT NO. 7
Aim: To determine moisture, volatile matter & ash content of a given sample of coal.
Apparatus: Silica crucible with vented lid, electric oven, Muffle furnace, spatula, desiccator,
pair of tongs, weighing balance, long legged tongs, etc.
Chemicals: Powdered coal sample.
Theory: Coal is a primary, solid, fossil fuel. Coal sample has to be analysed before using it
in any field/industry to find out its quality & suitability. Moisture, volatile matter & ash content
of coal are determined under proximate analysis. This method is simple & quick and is used
primarily to determine the suitability of coal for coking, power generation or for iron ore
smelting in the manufacture of steel. Coal comes in following main types or ranks: Peat,
lignite or brown coal, bituminous coal, anthracite & Graphite. Each type of coal has a certain
set of physical parameters which are mostly controlled by moisture, volatile content (in terms
of aliphatic or aromatic hydrocarbons) & carbon content. The carbon content is lowest in
peat and highest in anthracite.
Moisture
Moisture is an important property of coal, as all coals are mined wet. Groundwater and other
extraneous moisture is known as adventitious moisture and is readily evaporated. Moisture
held within the coal itself is known as inherent moisture & is analysed. Moisture reduces the
calorific value of coal and considerable amount of heat is wasted in evaporating it during
combustion. Moisture may occur in four possible forms within coal: Surface moisture,
Hydroscopic moisture, Decomposition moisture & Mineral moisture.
Total moisture is analysed by loss of mass of sample by Drying in air at 100 to 105 C (210 to
220 F) and relative loss of mass is determined. T otal moisture content of the coal should be
as low as possible.
Volatile matter
Volatile matter in coal refers to the components of coal, except for moisture, which are
liberated at high temperature in the absence of air. This is usually a mixture of short and long
chain hydrocarbons, aromatic hydrocarbons & some sulfur. Volatile matter of the coal is
related to the length of the flame, smoke formation & ignition characteristics. High volatile
matter coal gives long flame, high smoke & relatively low heating values. Volatile matter
content should be therefore as low as possible but minimum 20% is required for the ignition
of coal.
In Australian & British laboratories this involves heating the coal sample to 900 5 C (1650
10 F) for 7 minutes in a cylindrical silica cruci ble in a muffle furnace. American Standard
procedures involve heating to 950 25 C (1740 4 5 F) in a vertical platinum crucible.
Ash
Ash content of coal is the non-combustible residue left after coal is burnt. It represents the
bulk mineral matter after carbon, oxygen, sulfur and water (including from clays) has been
driven off during combustion. It consists of inorganic matter like silica, alumina, iron oxide,
lime, magnesia, etc. Ash reduces the heating value of coal, reduces air supply in furnaces
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and also requires labour (extra cost) for its regular disposal. Therefore ash content of coal
should be as low as possible. Analysis is fairly straightforward, with the coal thoroughly burnt
and the ash material expressed as a percentage of the original weight.
Fixed carbon
The fixed carbon content of the coal is the carbon found in the material which is left after
volatile materials are driven off. This differs from the ultimate carbon content of the coal
because some carbon is lost in hydrocarbons with the volatiles. More the fixed carbon
content, higher will be the calorific value of coal. Fixed carbon is determined by removing the
mass of volatile matter, moisture and ash determined by the above tests, from the original
mass of the coal sample.
Procedure:
A. Determination of Inherent Moisture: Transfer about 1g (known quantity) of powdered
air dried coal sample into a previously weighed silica crucible. Place the open crucible
with sample in an electric oven and heat it at about 105 110oC for an hour. Take out
the crucible after one hour from the oven and cool it in a desiccator (containing moisture
absorbing anhydrous calcium chloride). Then weigh the crucible with sample and repeat
the process of heating, cooling & weighing till constant weight is obtained. Calculate the
loss in weight.
B. Determination of Volatile matter: The dried sample of coal after determining moisture
content is closed with a vented lid. The closed crucible is then heated in a Muffle furnace
maintained at 925 20o C for exactly 7 minutes. The crucible is taken out from Muffle
furnace carefully with the help of long legged tongs. It is first cooled in air and then in a
desiccator. When the crucible attains room temperature it is weighed. Calculate the loss
in weight.
C. Determination of Ash: Transfer about 1g (known quantity) of powdered air dried coal
sample into a previously weighed silica crucible. Place the open crucible with sample in a
Muffle furnace maintained at 725 25o C for about 40 minutes or till constant weight is
obtained. Coal burns in open and the residue left is ash. Take out the crucible from
Muffle furnace carefully using long legged tongs. Cool the hot crucible first in air and then
in a disiccator. Weigh the crucible and find out the amount of unburnt residue left (ash).
D. Determination of Fixed Carbon: The percentage of fixed carbon is determined
indirectly by substrating the sum total of percentages of moisture, volatile matter and ash
from 100.
Observations and Calculations:
A. For Moisture:
1. Weight of empty crucible =

W1 = __________ g.

2. Weight of crucible + Coal sample = W 2 = ___________ g.


3. Weight of Coal sample before heating = W 2 W 1 = W 3 = ___________ g.
4. Weight of crucible + Sample after heating for 1 hr at 105 110oC = W 4 =________ g.
5. Weight of Coal sample after heating = W 4 W 1 = W 5 = ___________ g.

CHEMISTRY LAB MANUAL - II

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6. Loss in weight of sample due to moisture = W 3 W 5 OR W 2 W 4 = W M = _______ g.


% Of Moisture in coal

Weight of moisture
x 100 = W M x 100
Weight of coal (before heating)
W3

= _____ %
Observations and Calculations:
B. For Volatile matter:
1. Weight of empty crucible =

W1 (W 1 from part A) = __________ g.

2. Weight of crucible + moisture free coal sample = W 2 (W 4 from part A) = _________ g.


3. Weight of moisture free sample (before heating) = W 2 W 1 = W3 = __________ g.
4. Weight of crucible + Sample after heating for 7 mins. at 925 20o C = W 4 =_______ g.
5. Weight of Sample after heating = W 4 W 1 = W 5 = ___________ g.
6. Loss in weight of sample due to volatile matter = W 3 W 5 = W VM = ________ g.
% Of Volatile matter in coal =

Weight of volatile matter


x 100 = W VM x 100
Weight of coal (before heating)
W3

= _____ %
Observations and Calculations:
C. For Ash:
1. Weight of empty crucible =

W1

= __________ g.

2. Weight of crucible + Coal sample = W 2 = _________ g.


3. Weight of Coal sample (before heating) = W2 W 1 = W 3 = ___________ g.
4. Weight of crucible + Sample after heating for 40 mins. at 725 25o C = W 4 =_______ g.
5. Weight of Ash formed = W 4 W 1 = W A = ___________ g.
% Of Ash in coal =

Weight of Ash
Weight of coal (before heating)

x 100 =

WA
W3

= _____ %
D. For Fixed carbon (FC):
% Of Fixed Carbon = 100 (% Moisture + % Volatile matter + % Ash)
= 100 ( ________ )
= ______ %

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x 100

VPCOE

Result:
The coal sample analysed contains: Moisture

= _______ %

Volatile matter = _______ %


Ash

= _______ %

Fixed Carbon

= _______ %

Conclusion:
Related Questions:
1) Define coal. What are the types of analysis of coal?
2) What is the temperature time limit of heating for volatile matter analysis?
3) For moisture content determination heating is carried out in which equipment?
4) What is the significance of proximate analysis of coal?
5) How does ash and fixed carbon affect the quality of coal?

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APPENDIX
Table-I: pH Value (Refer Experiment No. 6)

Table-II: pH Value (Refer Experiment No. 7)


Fuel
Kcal/Kg

Higher Calorific Value


(Gross Calorific Value - GCV)
kJ/kg

Btu/lb

Anthracite

7762 - 8120

32,500 - 34,000

14,000 - 14,500

Bituminous coal

4060 - 5553

17,000 - 23,250

7,300 - 10,000

Charcoal

7069

29,600

12,800

Coal

3582 - 6448

15,000 - 27,000

8,000 - 14,000

Coke

6687 - 7404

28,000 - 31,000

12,000 - 13,500

Lignite

3893

16,300

7,000

Peat

3296 - 4896

13,800 - 20,500

5,500 - 8,800

Semi anthracite

6377 - 7762

26,700 - 32,500

11,500 - 14,000

Wood (dry)

3439 - 4155

14,400 - 17,400

6,200 - 7,500

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Table-III: Electromagnetic spectrum (Refer Experiment No. 4)


Serial No.

Radiation /Rays

Wavelength range

Radio waves

3 x 10 5 cm

Micro eaves

30 cm

Far Infrared

0.01 cm

Near Infrared

1000 nm

Visible

400 750 nm

Red

750 nm

ii

Orange

650 nm

iii

Yellow

590 nm

iv

Green

530 nm

Blue

490 nm

vi

Indigo

420 nm

vii

Violet

400 nm

Ultraviolet

200 400 nm

Vacuum UV

200 5 nm

X - rays

5 - 0.01 nm

Gamma rays

0.01 - 0.0001 nm

Table-IV: Galvanic series (Refer Experiment No. 5)


Most susceptible to corrosive attack
(Less Noble) Anodic end

Magnesium and its alloys


Zinc and its alloys
Aluminium and its alloys
Mild steel
Cast Iron
Stainless steel (active type)
Lead
Tin
Brasses
Gun metal
Copper
Monel
Titanium and its alloys
Stainless steel (passive type)
Silver

Least susceptible to corrosive attack


(More

Noble)

Cathodic

CHEMISTRY LAB MANUAL - II

Gold

end

Platinum

VPCOE

REFERENCES:
1) Laboratory Manual on Engineering Chemistry, Sudharani (Dhanpat Rai Publishing
Company).
2) Vogels Textbook of Quantitative chemical analysis, J. Mendham et.al. (Pearson
Education).
3) Advanced Inorganic Analysis, Agarwal & Keemtilal, Pragati prakashan.
4) Chemical tables, Dr N. S. Gnanapragasam, (Sultan Chand & sons).
DEVELOPMENT OF SKILLS

This Lab Manual intends to develop the intellectual and motor skills of student. The skills
mentioned below will be developed through the experiments performed in this laboratory.
Intellectual Skills:
I-1 : To understand and identify the concepts.
I-2 : To Discriminate / Classify / Identify.
I-3 : To Investigate / Test / Verify properties or characteristics.
I-4 : To Interpret test results or numerical values.
I-5 : To locate faults.
I-6 : To plan and design.
Motor Skills:
M-1 : Skill to sketch the circuit diagram / block diagram / graph.
M-2 : Skill to select, handle and operate the equipment and reagents.
M-3 : Skill to measure the values / note down the observations.
M-4 : Skill to follow systematic procedure or sequence of operations step by step.
M-5 : Skill to observe the performance.
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In order to develop these skills for each experiment, important skills have been
identified. While performing the experiment, it is necessary to focus on such important
skills. Following table shows a grid of experiments and relevant skills.
GRID TABLE

No.

Experiment No. & Title

Intellectual skills

Motor skills

I1

I2

I3

I4

I5

I6

M1

M2

M3

M4

M5

Determination of Alkalinity in
given water sample by volumetric
method.

To determine chloride (Cl )


content of water sample by
Mohrs method.

To determine temporary &


permanent hardness of water
sample by EDTA method.

Spectrophotometric/colorimetric
estimation of ferrous ions (Fe2+)
from the given solution.

To Study of corrosion of metals


in medium of different pH.

Analysis of mixture of phosphoric


acid and hydrochloric acid using
indicators & pH meter.

To determine moisture, volatile


matter & ash content of a given
sample of coal.

CHEMISTRY LAB MANUAL - II