Inorg Chem Lab Manual PDF

LABORATORY MANUAL
CHE 114
INORGANIC CHEMISTRY LABORATORY-I
(For Private Circulation)
Name of the Student: ……………………………………………….
Registration Number/Roll No……………………………………….
Section and Group…………………………………………………....
School of Chemical Engineering and Physical Sciences
Session: 2018-19 (Spring Term)

GENERAL INSTRUCTIONS:
1. Safety in the Chemical Laboratory:

• Lab apron and safety glasses are mandatory while working in the lab.
• In the laboratory due care and caution must be exercised to avoid accidents. Correct handling of
apparatus and chemicals is the only insurance against hazards. In particular- Do not throw away
lighted match-sticks without extinguishing them.
• Do not touch any unknown chemical by hand.
• Ensure that gas taps are securely closed while putting-off burners.
• In the event of any exposure to corrosive chemicals such as strong acids, wash the effected part
in flowing water, and contact the instructor for further help.
• Never try to neutralize the corrosive substance chemically, as this may result in burns.
• In case of any exposure, move away from the source of exposure (or remove the source).
2. Maintenance of Laboratory Records:
• In any experiment, the result is to be faithfully recorded and analyzed. The maintenance of
laboratory records is an essential part of all scientific work.
• The experimental observations must be taken down in a work sheet attached in lab manual and
not in loose sheets and certainly not ion the margins of the instructions sheets.
• There should be no erasure in the observation book.
• If any entry needs to be corrected, it must be crossed out neatly and a new entry be made.
• After the day’s experimental work is over, get the observations initiated by the instructor, if the
time is left over, do the necessary calculations and get them checked too. Write up the work in
the work sheet with details mentioned.
• The maintenance of a day to day observation book, complete in all details, is an essential part
of any scientific work at any level and is a habit that you must cultivate.
TABLE OF CONTENTS
S. No. Title of the Experiment Page No.
1. To calibrate and use of apparatus (pipette, burette and volumetric flask). 4-9
2. To prepare solutions of different molarity and normality of titrants and to 10-13

estimate strength of HCl using strong base.
3. To estimate free alkali present in different soap and detergents. 14-17
4. To estimate carbonate and hydroxide present together in mixture. 18-21
5. To estimate carbonate and bicarbonate present together in mixture. 22-26
6. To estimate orthophosphoric acid using sodium hydroxide. 27-30
7. To estimate Fe(II) and oxalic acid using standardized KMnO4 solution 31-34
8. To estimate oxalic acid and sodium oxalate in a given mixture. 35-38
9. To estimate Fe(II) with K2Cr2O7 using internal (diphenylamine, anthranilic 39-43

acid) and external indicator
10. To estimate hydrogen peroxide using KMnO4 . 44-47
3
Experiment No. 1
Aim: To calibrate and use of apparatus (pipette, burette and volumetric flask).
Equipment and Apparatus Required: Pipette, burette, volumetric flask, beaker, weighing balance,
beaker.
Learning Objectives:
1. In order to avoid introducing systematic errors into our measurements, each of these
instruments must be properly calibrated.
2. The reduction of random errors can be done while using the instruments with proper and
thoroughly understanding.
3. The quality of the measurements obtained from these tools depends heavily on the care taken in
calibrating and in using each instrument.
Theory:
Calibration is usually performed by weighing the amount of water delivered by or contained in the
volumetric apparatus. This mass is then converted to the desired volume using the tabulated density of
Water:
Volume = mass / density
Pipette: The pipette is used to transfer a volume of solution from one container to another. Once the
pipette is cleaned and ready to use, make sure the outside of the tip is dry. Then rinse the pipette with
the solution to be transferred. Insert the tip into the liquid to be used and draw enough of the liquid into
the pipette to fill a small portion of the bulb. Hold the liquid in the bulb by placing your fore finger over
the end of the stem. Now place the tip of the pipette against the container from which the liquid has
been withdrawn and drain the excess liquid such that the meniscus is at the graduation mark. Move the
pipette to the receiving container and allow the liquid to flow out (avoiding splashing) of the pipette
freely. When most of the liquid has drained from the pipette, touch the tip to the wall of the container
until the flow stops and for an additional count of 10.
Volumetric Flasks: The Volumetric Flask is used to prepare Standard Solutions or in diluting a sample.
When using a flask, the solution or solid to be diluted is added and solvent is added until the flask is about
two-thirds full. It is important to rinse down any solid or liquid which has adhered to the neck. Swirl the
solution until it is thoroughly mixed. Now add solvent until the meniscus is at the calibration mark. If
any droplets of solvent adhere to the neck, use a piece of tissue to blot these out. Stopper the flask
securely and invert the flask at least 10 times.
Burette: The burette is used to accurately deliver a variable amount of liquid. Fill the burette to above the
4
zero mark and open the stopcock to fill the tip. Work air bubbles out of the tip by rapidly squirting the
liquid through the tip or tapping the tip while solution is draining. The burette should be opened and
allowed to drain freely until near the point where liquid will no longer be added to the flask. Smaller
additions are made as the end- point of the addition is neared. Allow a few seconds after closing the
stopcock before making any readings. At the end-point, read the burette in a manner similar to that above.
As was noted above, volumetric glassware is calibrated by measuring the mass of Water that is contained
in or delivered by the device.
The weight is then converted to volume data using the tabulated density of Water at the temperature of
calibration.
Finally, this volume data is corrected to the standard temperature of 20°C. This can be accomplished using
the thermal expansion coefficient of Water; 0.00025/°C:
V20 = V [1 + 0.00025 (20 - t)]
Table 1: Density of Water
Outline of the Procedure:

1. Take a clean dry beaker and weigh in analytical balance.
2. Using a clean dry pipette transfer measured volume of distilled water into the beaker and
reweigh.
3. Record the temperature of the water used.
5
4. From the difference in mass, and the density of water at the given temperature, calculate
the volume of the water delivered. Correct the volume to 20°C.
5. Repeat the same procedure for the burette and the volumetric flask.
6. Calculate the Correction Factor by subtracting the apparent volume delivered, as given by the
readings, from the actual volume delivered.
Results: Calibration of different glassware at room temperature.
Scope of the result: In order to avoid introducing systematic errors into our measurements, each of the
volumetric instruments must be properly calibrated.
Relationship to be determined: Density
Cautions: 1. All the glass apparatus should be cleaned and dried properly before use.
Requirement for Lab Technician: Provide clean glass-wares
Suggested reading for students: Books:
1. Practical Inorganic Chemistry by Shikha Gulati, J L Sharma, Shagun Manocha, CBS Publishers &
Distributors.
2.An Advanced Course in Practical Chemistry by Ananta Kumar Nad, Bimal Mahapatra, Amalendu
rd
Ghoshal, New Central Book Agency Pvt Ltd, 3 Edition, (2011)
Weblinks:
1. http://www.titrations.info/pipette-burette
2. http://infohost.nmt.edu/~jaltig/VolumetricWare.pdf
6
Worksheet of the student
Date of performance: Registration number:
Aim: To calibrate and use of apparatus (pipette, burette, volumetric flask and weighing balance).
Observation Table:
Burette:
Volume of water taken:
S. No. Initial weight Final weight Actual volume Corrected volume at

(in gm) (in gm) (in ml)
20 °C
Correction Factor = Actual volume delivered - apparent volume delivered
Pipette:
S. No. Initial weight Final weight Actual volume Corrected volume

at 20 °C
7
Volumetric flask:
S. No. Initial weight Final weight Actual volume Corrected volume

at 20 °C
Result and Discussion:
8
Error Analysis
Learning outcome (What I have learnt)
To be filled by Faculty
S. No Parameter Max. Marks Marks

Obtained
1 Understanding of the student about the 20

procedure/apparatus.
2 Observations and analysis including 20
learning outcomes
3 Completion of experiment, Discipline and 10
Cleanliness
Signature of Faculty Total marks
obtained
9
Experiment No. 2
Aim: To prepare solutions of different molarity and normality of titrants and to estimate strength of HCl
using strong base.
Equipment and Apparatus Required: Pipette, burette, volumetric/measuring flask, conical flask,
weighing balance, beaker.
Material Required: Hydrochloric acid, sodium hydroxide, and phenolphthalein
1. In volumetric analysis, the amount of a substance (acid, base or salt) is estimated using a standard
solution.
2. The preparation of solution of different normality.
Theory
A solution of known concentration (Normality or Molarity) is called a standard solution. Some of the
standard solutions are prepared by weighing out accurately and dissolving the weighed solute in a suitable
solvent and making up the solution to a known volume. An approximate concentration is first prepared and
then standardized by titrating against a suitable standard solution.
Standardization of HCl is based on the neutralization of HCl by NaOH solution.
HCl + NaOH → NaCl + H2O
A known volume of standard NaOH solution is titrated against HCl using phenolphthalein as indicator.
Since we know the volume and normality of NaOH and the volume of HCl required to neutralize the
NaOH, the normality of HCl can be calculated.
1. A burette is washed and filled with the given HCl solution.
2. A pipette is washed with water and rinsed with the NaOH solution. Pipette out 20 mL of NaOH
solution into a clean conical flask. Added one or two drops of phenolpththalein to the solution in
the conical flask. The solution turned pink.
3. Hydrochloric acid from the burette is added to the NaOH solution in the conical flask, little by
little. Meanwhile the flask is kept gently shaking. The addition of the acid is stopped when the
pink color is just discharged. This is the end point of the titration.
4. The final reading of the burette is noted and the titration is repeated to get concurrent values.
10
Calculations:
As we know N1V1 = N2V2
N1= Normality of NaOH solution= x N
V1=Vol of NaOH solution = 10 mL

V2= Vol of HCl solution = ……….mL
N2=Normality of HCl solution=(N1V1) / V2 = (x N x 10) / (………) =…y N
Results: The solutions were prepared according to different normality.

Scope of the result: Preparation of standard solution.
Cautions:
1. The glass apparatus should be cleaned and dried properly before use.
2. Standard solutions should be prepared carefully. Measuring flask should be used for preparing
standard solution not measuring cylinders.
Requirement for Lab Technician: Standard solution of NaOH
Suggested reading for students:
Books:
Distributors.
2. An Advanced Course in Practical C h e m i s t r y by Ananta Kumar Nad, Bimal Mahapatra,
Amalendu Ghoshal, New Central Book Agency Pvt Ltd, 3rd Edition, (2011)
Weblinks:
1. http://amrita.olabs.co.in/?sub=73&brch=7&sim=109&cnt=1
2. http://vlab.amrita.edu/?sub=2&brch=193&sim=352&cnt=4
11
Aim: To prepare solutions of different molarity and normality of titrants and to estimate
strength of HCl using strong base.
Observation Table:
Std NaOH Vs HCl using phenolphthalein
Sr . No. Burette reading Volume of HCl used

(in mL)
Initial Final
(mL) (mL)
Titre Value=……….mL
Calculations:
12
Error Analysis
S. No Parameter Max. Marks

Marks Obtained

learning outcomes
Cleanliness
obtained
13
Experiment No. 3
Aim: To estimate free alkali present in different soap and detergents.
Equipment and Apparatus Required: Pipette, burette, volumetric flask, conical weighing balance, flask,
beaker.
Material Required: Soap, 0.1N hydrochloric acid, phenolphthalein, distilled water.
Learning objectives:
1. The formation of soap is via esterification reaction of fatty acid with alcohol
2. Every soap has different power of cleaning depending upon amount of fatty acid esters present.
Theory:
A detergent is a surfactant or a mixture of surfactants with cleaning properties in dilute solutions. These
substances are usually alkylbenzenesulphonates, a family of compounds that are similar to soap but are
more soluble in hard water, because the polar sulfonate (of detergents) is less likely than the polar
carboxylate (of soap) to bind to calcium and other ions found in hard water.
Soaps are compounds formed by the reaction of bases with fats, chemically known as fatty acid esters. The
three most important fatty acid esters are Palmitin (C15H31COO)3C3H5], Stearin [(C17H35COO)3C3H5] and
Olein [(C17H33COO)3C3H5] They are found in lard, tallow, olive oil, cotton seed oil, and other animal and
vegetable fats or oils. Soap is usually made by the reaction of animal fat or vegetable oil with sodium
hydroxide. The process of treating fats with bases or is called ‘Saponification’.
Active alkalinity: The total alkaline content except carbonates present in a sample is known as active
alkalinity
Procedure: Weigh 0.5g of detergent in powder form in a 100ml beaker and add distilled water to make up
weight to 50g (1% w/w solution). Stir it till all the detergent got dissolved. Pipette out 10ml of this
detergent solution in 100ml conical flask, add phenolphthalein indicator and titrate it 0.1 N HCl solution till
we got end point (pink to colorless). Repeat the titration till we got two concurrent readings.
Calculation: N1V1 (Standard acid) = N2V2 (Soap sol/Base)
N2 = N1V1/V2
14
1000 mL 1 N NaOH =40 g NaOH
1 mL 1N NaOH =40/1000 g NaOH
50 mL 1N NaOH= (40×50/1000) g NaOH
50 mL N2 NaOH=(40×50×N2/1000) g NaOH=x gm
0.5 g Detergent contain x gm NaOH
% free alkali = x /0.5 (wt of soap) x 100 %
Results: The total alkali content of the given soap sample was found to be
Scope of the result: Estimation of alkali in soap.
Cautions:
2. Standard solutions should be prepared carefully.
3. Measuring flask should be used for preparing standard solution not measuring
cylinders
Requirement of Lab Technician:
Standard solutions of HCl, indicators
Distributors.
2. An Advanced Course in Practical Chemistry by Ananta Kumar Nad, Bimal Mahapatra, Amalendu
Ghoshal, New Central Book Agency Pvt Ltd, 3rd Edition, (2011)
Weblinks:
1. https://www.classle.net/book/estimation-total-alkali-content-soap
15
Aim: To estimate free alkali present in different soap and detergents.
Observation table:
Standard HCl Vs soap sample
S. No. Volume of Burette reading Volume of

soap solution Initial Final HCl (mL)
(mL) (mL) (mL)
Calculation:
16
Error Analysis

Marks Obtained

learning outcomes
Cleanliness
obtained
17
Experiment No. 4
Aim: To estimate carbonate and hydroxide present together in mixture.

Equipment and Apparatus Required: Pipette, burette, conical flask
Material Required: 0.1N Hydrochloric acid, phenolphthalein, methyl orange
1. The carbon dioxide that is dissolved by naturally circulating waters appears in chemical analysis
principally as bicarbonate and carbonate ions and can be estimated experimentally.
2. Learning about titration using two different indicators in same experiments.
Theory:
To understand the basis of two consecutive titrations at different pH range: OH-, CO2- (caustic 3alkalinity)
-
and HCO can be estimated separately by titration against standard acid using phenolphthalein and methyl
orange as indicators.
The determination is based on the following reactions:
OH- + H+ H2O
HCO3- + H+ H2O + CO2
Thus, titration of a given mixture in presence of phenolphthalein (pink color above pH 8.5 and below pH
8.5 it becomes colorless) as an indicator indicates completion of reaction 1 and 2 whereas the same sample,
if titrated in presence of methyl orange (yellow color orange-red below pH 3.1) as an indicator indicates
the completion of reaction 1, 2 and 3.
Outline of the Procedure
1. Transfer exactly 20mL of mixture provided into a 100mL conical flask using a pipette.
2. Add 1 or 2 drops of methyl orange indicator and one drop of phenolphthalein.
3. Titrate against the 0.1N HCl solution and record the volume.
4. Do not discard the mixture and wash the flask
Calculation:
Volume of 0.1N HCl for the 1st end point using phenolphthalein = V1 mL
18
Volume of 0.1N HCl for the 1st end point using methyl orange = V2 mL
In 20 mL solution Na2CO3 present =2(V2-V1) mL of 0.1N HCl

=2(V2- V1) x 0.1 x 0.053 g Na2CO3
=2(V2- V1) x 0.1 x 0.053 x 1000 g/L Na2CO3
20
In 20 mL solution NaOH present = V2 - 2(V2- V1) mL of 0.1N HCl
= V2- 2(V2- V1) x 0.1 x 0.04 g NaOH
= V2 - 2(V2- V1) x 0.1 x 0.04 x 1000 g/L NaOH
20
Results: Amount of carbonate is g/L and hydroxide is g/L
Scope of the result: Estimation of mixture
Relationship to be determined: Acid-base titration
Cautions:
Requirement for Lab Technician:
0.1N HCl, mixture of carbonate and hydroxide
1. Practical Inorganic Chemistry by Shikha Gulati, J L Sharma, Shagun Manocha, CBS
Publishers & Distributors.
2. An Advanced Course in Practical Chemistry by Ananta Kumar Nad, Bimal Mahapatra,

Weblinks: 1. http://egyankosh.ac.in/bitstream/123456789/43326/1/Exp-5.pdf
19
Aim: To estimate carbonate and hydroxide present together in mixture.
Observation Table:
Titration of mixture using phenolphthalein:
S. No. Volume of Burette reading Volume of HCl

mixture (mL) Initial Final V1(mL)
Titration of mixture using methyl orange:

Calculation:
20
Error Analysis
Learning outcomes (what I have learnt)

Marks Obtained

learning outcomes
Cleanliness
obtained
21
Experiment No. 5
Aim: To estimate carbonate and bicarbonate present together in mixture.
Equipment and Apparatus Required: Pipette, burette, conical flask

Material Required: 0.1 N Hydrochloric acid, phenolphthalein, methyl orange, sample solution
1. Carrying out acid-base titration
2. Determination of the amount of sodium carbonate and sodium bicarbonate in a mixture by
titration
3. Role of indicator in the titration
Theory:
The pKa1 and pKa2 values of H2CO3 are quite distinct and so when a carbonate solution is titrated against
hydrochloric acid, there occur two distinct regions of sharp pH change. The first corresponding to the
-
formation of HCO3 (pH 8 to 10) and the second due t o complete neutralization at pH 4-6. The first is
roughly in the pH range in which color of phenolphthalein changes from red to colourless and the second is
that at which methyl orange changes from yellow to orange red. This end point, however, is not very sharp
in the titration of the strong base NaOH. The sharp change of pH occurs over a range of pH that
includes the regions of color change of both the indicators, so both of them give the end point correctly. When
we have both sodium carbonate and sodium hydroxide present together in a solution, a titration using
phenolphthalein gives the titer (volume at the equivalence point) corresponding to sodium hydroxide plus
half the carbonate and the titer obtained with methyl orange corresponds to the total alkali. The
individual sodium carbonate and hydroxide concentrations may be calculated from the data.
Carbonate ion reacts with hydrogen ions in steps:
CO32- + H+ HCO3-
HCO3- + H+ H2CO3 H2O + CO2

1. Pipette out 25 mL sample in a 250 mL conical flask.
2. Add 2-3 drops of phenolphthalein as an indicator. The solution becomes pink.
3. Titrate this solution with 0.1 N HCl until color of the solution changes to colorless.
4. Add 2 drops of methyl orange indicator into the same solution. Solution becomes yellow.
5. Continue the titration without refilling the burette till the color of solution turns to orange.
22
Calculation:
Volume of 0.1 N HCl for the 1st end point using phenolphthalein = V1 mL Volume
of 0.1 N HCl for the 2nd end point using methyl orange = V2 mL
In 25 mL solution Na2CO3 present = 2V1 mL of 0.1 N HCl
=2V1 x 0.1 x 0.053 g Na2CO3

= (2V1 x 0.1 x 0.053)/25 x 1000 g/L Na2CO3
In 25 mL solution NaHCO3 present = (V2 - 2V1) mL of 0.1 N HCl

= (V2 - 2V1) x 0.1 x 0.04 g NaHCO3
= (V2 - 2V1) x 0.1 x 0.04 x 1000 g/L NaHCO3
25
Results: Amount of carbonate is g/L and bicarbonate is g/L
Scope of the result: Volumetric estimation
Cautions:
3. Initial reading should be same for both the titrations.

Requirement for Lab Technician: Required reagents will be provided by lab technician and all the
solutions will be prepared by student.
Suggest ed reading for students: Books:

Distributors.
Weblinks:
1. http://www.chm.uri.edu/jdwyer/chm212_fall_10/CHM212_Exp3_2010_Final.pdf
23
Aim: To estimate carbonate and bicarbonate present together in mixture.
Observation Table:
Titration of mixture using phenolphthalein:

Titration of mixture using methyl orange:

Calculation:
24
Error Analysis
25

Marks Obtained

learning outcomes
Cleanliness
obtained
26
Experiment No. 6
Aim: To estimate orthophosphoric acid using sodium hydroxide.
Equipment and Apparatus Required: Pipette, burette, conical flask, glass rod
Material Required: Phosphoric acid, calcium chloride, 1N sodium hydroxide solution, phenolphthalein
Learning objective:
1. Titration curve contains only two inflection points and phosphoric acid can be titrated either
as a monoprotic acid or as a diprotic acid.
2. Difference in direct and indirect titration.
Theory:
Titration of the phosphoric acid H3PO4 is an interesting case. Although often listed together with strong
mineral acids (hydrochloric acid, nitric acid and sulfuric acid) phosphoric acid is relatively weak, with
pKa1 = 2.15, pKa2 = 7.20 and pKa3 = 12.35. In the first case acid has to be titrated against indicator
changing color around pH 4.7 (for example methyl orange), in the second case - against indicator changing
color around pH 9.6 (for example thymolphthalein). Phenolphthalein can't be used, as it starts to change
color around pH 8.2, when phosphoric acid is titrated in about 95%. Therefore, H3PO4 is indirectly titrated
by estimating the HCl it liberates, reacting quantitatively with CaCl2 solution. The HCl is estimated
by titrating with a standard NaOH solution using phenolphthalein indicator.
2H3PO4 + 3CaCl2 = Ca3(PO4)2 ↓ + 6HCl

1. Pipette 5 mL aliquot of phosphoric acid solution into 100 mL Erlenmeyer flask.
2. Add 2 mL of 20% CaCl2 and mix thoroughly.
3. Dilute to 25 mL with distilled water
4. Add 1-2 drops phenolphthalein indicator.
5. Titrate with NaOH solution till pink color appears.
Calculation:
1 mL of 1N NaOH ≡ 0.033 g H3PO4
V1 mL of 1N NaOH ≡ V1 x 0.033 g H3PO4
≡ (V1 x 0.033 x 1000)/5 g/L H3PO4
Results: Amount of H3PO4 is g/L
27
Scope of Result: Estimation of polybasic acid
Relationship to be determined: Back titration of released HCl
Cautions:
2. Standard solutions should be prepared carefully. Measuring flask should be used for
preparing standard solution not the measuring cylinders.
1N NaOH, 20% CaCl2
1. Practical Inorganic Chemistry by Shikha Gulati, J L Sharma, Shagun Manocha, CBS

Publishers & Distributors.
2. An Advanced Course in Practical Chemistry by Ananta Kumar Nad, Bimal Mahapatra,

Weblinks:
1. http://www.titrations.info/acid-base-titration-phosphoric-acid
28
Aim: To estimate orthophosphoric acid using sodium hydroxide.

Observation table:
Titration of released HCl using phenolphthalein:
S. No. Volume of Burette reading Volume of

mixture (mL) Initial Final NaOH V1(mL)
Calculation:
29
Error Analysis

Marks Obtained

learning outcomes
Cleanliness
obtained
30
Experiment No. 7
Aim: To estimate Fe(II) and oxalic acid using standardized KMnO4 solution.
Equipment and Apparatus Required: Beaker, glass rod, dropper, heating mental, stirrer, funnel, burette,
water bath, stirrer.
Material Required: Potassium permanganate, sulphuric acid, Mohr’s salt [FeSO4 (NH4)2SO4.6H2O] solution,
phenolphthalein
1. Importance of redox titration in chemistry
2. Concept of self-indicators.
3. Concept of primary standard solution (Oxalic acid)
4. Concept of secondary standard solution (KMnO4)
Theory: The Potassium permanganate is a powerful oxidizing agent has the formula KMnO4 in which
Manganese is in +7 oxidation state and Fe(II) acts as a reducing agent. These two reacts in presence of
sulphuric acid as given below. In this reaction Mn+7 is reduced to Mn+2 and Fe+2 is oxidized to Fe+3.
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5(O)
10FeSO4 + 5H2SO4 + 5(O) → 5Fe2(SO4)3 + 5H2O
--------------------------------------------------------------------------------------
2KMnO4 + 10FeSO4 + 8H2SO4 → K2SO4 + 2MnSO4 + 5Fe2(SO4)3 + 8H2O
According to the above chemical reactions, one mole of potassium permanganate is reacting with five
moles of Fe(II). In this reaction, all the reactants and products are colorless except potassium permanganate.
So the colour of the permanganate is used to locate the end point. When all the Fe(II) ions are completely
reacted, the excess trace amount of potassium permanganate can give sufficient color to the solution i.e.
color change at the end point is colorless to pale pink. Potassium permanganate acts as a self-indicator, so it
is called self-indicator reaction.
The potassium permanganate is previously standardized against sodium oxalate in acid solution:
2MnO4- + 5HCO3- + 6H+ → 2Mn2+ + 10CO2 + 8H2O

1. Take 10 mL of standard oxalic acid solution into a conical flask.
2. Add 5 mL of dilute H2SO4 into the flask.
3. Warm the mixture to 60-70 °C. Do not boil.
4. Titrate in the warm condition with KMnO4 solution. Appearance of faint pink colour indicates end
point.
31
5. In a separate flask take 10 mL of the provided Fe(II) solution.
6. Add 5 mL of dilute H2SO4.

7. Titrate against KMnO4 solution until faint pink colour persists.
Calculation:
Volume of KMnO4 for reduction of 0.1N oxalic acid = V1 mL
Volume of KMnO4 for reduction of Fe (II) = V2 mL
Normality of KMnO4 = 10 x 0.1N = x N
V1
1000 mL 1 N KMnO4 =56 gm Fe

1 mL 1N KMnO4 =56/1000 gm Fe
V2 mL 1N KMnO4= (56×V2/1000) gm Fe
V2 mL xN KMnO4=(56×V2×x/1000) gm Fe=y gm
Results: The amount of iron present (y/10) g/mL

Scope of the result: Estimation of iron.
Relationship: Redox equivalence
Cautions:
1. Maintenance of proper pH condition during titration
2. Handle the acids with care
2N H2SO4, Oxalic Acid (K2C2O4), 0.1N KMnO4, 0.1N Mohr’s salt
1. Practical Inorganic Chemistry by Shikha Gulati, J L Sharma, Shagun Manocha, CBS Publishers
& Distributors.
Weblinks:
1. http://www.lahc.edu/classes/chemistry/arias/exp%208%20-%20redox.pdf
32
Aim: To estimate Fe(II) and oxalic acid using standardized KMnO4 solution.
Observation Table:
Standardization of KMnO4:
S. No. Volume 0.1 N Burette reading Volume of

oxalic acid Initial Final KMnO4
(mL) V1(mL)
Titration of Iron (II) with KMnO4:
S. No. Volume iron(II) Burette reading Volume of

solution (mL) Initial Final KMnO4
V2(mL)
Calculation:
33
Result and Discussion
Error Analysis

Marks Obtained

learning outcomes
Cleanliness
obtained
34
Experiment No. 8
Aim: To estimate oxalic acid and sodium oxalate in a given mixture.
Equipment and Apparatus Required: Pipette, burette, conical flask, hot plate, glass rod
Material Required: 0.1N Potassium permanganate solution, 0.1N sodium hydroxide solution, oxalic acid,
sulphuric acid, phenolphthalein.
1. To find strength of oxalic acid is determined by titration with NaOH solution and the amount of
oxalate ions
2. Use of redox reactions by titrating with potassium permanganate.
Theory:
The strength of oxalic acid is determined by titration with NaOH solution and the amount of oxalate ions is
determined by titration with potassium permanganate. The mixture is first titrated with NaOH when only
oxalic acid reacts with NaOH and the other component sodium oxalate does not react at all with sodium
hydroxide.
C2O4H2 + 2NaOH → Na2C2O4 + 2 H2O

When the mixture is titrated with KMnO4 then both oxalic acid and sodium oxalate are oxidized and give
the combined normality of the mixture. Thus, the normality of sodium oxalate may be evaluated by
subtracting the normality of oxalic acid from that of the mixture.
2KMnO4 + 5H2C2O4 + 3H2SO4 → K2SO4 + 2MnSO4 + 8H2O + 10CO2
Or, ionically
2MnO4- + 5C2O42- + 16H+ → 2 Mn2+ + 8H2O + 10CO2
Outline of the Procedure

1. Take 10 mL of the sample into a conical flask.
2. Add 5 mL of dilute sulphuric acid.
3. Heat the solution to 60- 70 °C. Do not boil.
4. Titrated with KMnO4 until faint pink color persists
5. In a separate flask add 10 mL of the mixture.
6. Add 1 drops of phenolphthalein indicator and titrate against 0.1N NaOH until pink colour appears.
35
Calculations:
m eq of oxalic acid ≡ m eq of NaOH = V1 x N1 (NaOH) (1)
N x V = V1 x N1
Wt. of oxalic acid = V1 x N1 (NaOH) Eq. Wt. of oxalic acid
Strength. of oxalic acid = V1x N1 (NaOH) x eq wt of oxalic acid×1000 = x g/L
10
∴ Strength of oxalic acid = ……g/L

m eq of oxalic acid + m eq of sodium oxalate = m eq of KMnO4 = N2 × V2 (KMnO4) (2)
∴ m eq of sodium oxalate only = eq. 2 – eq. 1
Strength of sodium oxalate = (2-1) x eq wt of sodium oxalate×1000 = y g/L

10
∴ Strength of Sodium oxalate= ….g/L
Results: Strength of oxalic acid …………..g/L and sodium oxalate ……………..g/L

Scope of the result: Estimation of oxalic acid and oxalate in a mixture.
Cautions:
Requirement for Lab Technician: Required reagents will be provided by lab technician.
Suggested reading for students:
Books:
Distributors.
Weblinks. 1. https://www.scribd.com/doc/228321112/Oxalic-Acid-and-Sodium-Oxalate
2. http://qu.edu.iq/el/pluginfile.php/75800/mod_resource/content/0/Lucture%208.pdf
36
Aim: To estimate oxalic acid and sodium oxalate in a given mixture.

Observation Table:
Titration with KMnO4:
S. No. Volume 0.1 N Burette reading Volume of

oxalic acid Initial Final KMnO4
(mL) V1(mL)
Titration with NaOH using phenolphthalein:

Calculations:
37
Result and Discussion
Error Analysis
Learning outcomes (what I have learnt):

Marks Obtained

learning outcomes
Cleanliness
Obtained
38
Experiment No. 9
Aim: To estimate Fe(II) with K2Cr2O7 using internal (diphenylamine, anthranilic acid) and external
indicator
Equipment and Apparatus Required: Pipette, burette, conical flask, measuring cylinder, hot plate.
Material Required: Potassium dichromate, N-phenyl anthranilic acid, sulphuric acid.
1. Role of electrons as they are transferred from one reactant to another and so electrons are lost from
one substance and gained by another.
2. Why K2Cr2O7 does not act as self-indicator.
Role of external indicator in redox titrations Theory:
Oxidation-reduction reactions involve exchange of electrons between the reacting substances e.g., reaction
between Fe2+ and Cr2O72-.
6Fe2+ + 14H+ + Cr2O72- → 6Fe3+ + 2Cr3+ + 7H2O
The above reaction is called as redox reaction because it could be represented by two half reactions
involving oxidation and reduction, respectively.
a) Oxidation of Fe2+ to Fe 3+
Fe2+ → Fe3+ + e
b) Reduction of Cr6+ to Cr3+
Cr2O72- + 14H+ + 6e- → 2Cr3+ + 7H2O
This disappearance of the colour of dichromate cannot be used to locate the end point because the Cr3+ ions
have green colour that makes the Cr2O72- colour indistinguishable. The end point is conveniently detected
by using a redox indicator.
Redox indicator:
The change in potential at equivalence point of a titration may be detected by the addition of a suitable
indicator. An indicator that exhibits a change in colour corresponding to a change in oxidation state is
known as redox indicator. For example, colourless diphenylbenzidine is oxidized to a coloured substance,
diphenylbenzidine (violet).
39
1. Take 10 mL of the sample into a conical flask.

2. Add 5 mL of dilute sulphuric acid
3. Add three to five drops of N-phenyl anthranilic acid solution, and titrated against the supplied
N/20 potassium dichromate solution.
4. The solution acquires a pale green colour due to the Cr3+ ions; at the end point, the colour
changes sharply to red-purple. Note the burette reading.
5. Complete oxidation can be checked by adding a drop of this solution in a test tube containing
potassium ferricyanide solution, which acts as an external indicator. If ferrous ions are present
then the solution will turn blue.
Calculations:
N1V1=N2V2
Volume of K2Cr2O7 require =V1
Normality of K2Cr2O7=N/20=0.05 N
1000 mL 1N K2Cr2O7 =56 g of Iron
1 mL 1 N K2Cr2O7 =56/1000=0.056 g of Iron

1mL of 0.05 N K2Cr2O7 = 0.056×0.05 g of iron(II)
V1 mL of 0.05 N K2Cr2O7 = V1 X 0.05 X 0.056 g of iron(II)
Amount of iron present = (V1 X 0.05 X 0.056)/10 x 1000 g/L of Iron

Results: The given solution contains g/L of iron.
Scope of the result: Redox titration using external indicator
Cautions: Maintenance of proper pH condition during titration
Handle the acids with care
40
Distributors.
Weblinks:
1. http://wwwchem.uwimona.edu.jm/lab_manuals/c10expt31.html
2. http://shodhganga.inflibnet.ac.in/bitstream/10603/45618/21/21_appendix%20ii.pdf
3. http://www.nsec.ac.in/images/bes_REDOX%20TITRATION.pdf
41
Aim: To estimate Fe(II) with K2Cr2O7 using internal (diphenylamine, anthranilic acid) and external
indicator.
Observation Table:
Titration of iron (II) with K2Cr2O7:
S. No. Volume iron(II) Burette reading Volume of

solution (mL) Initial Final K2Cr2O7
V1(mL)
Result:
Calculations:
42
Error Analysis

Marks Obtained

learning outcomes
Cleanliness
Obtained
43
Experiment No. 10
Aim: To estimate hydrogen peroxide using KMnO4.
Equipment and Apparatus Required: Beaker, filter paper, conical flask test tube, test tube stand, test
tube holder
Material Required: Potassium permanganate, hydrogen peroxide, sulphuric acid,
Learning Outcomes:
1. Hydrogen peroxide acts as source of oxygen and acts as reducing agent.
2. Role of acid on this redox reaction
Theory:
Hydrogen peroxide is usually available in form of an aqueous solution containing about 3%, 6%, 12%and
30%. hydrogen peroxide. In sulphuric acid medium hydrogen peroxide is converted into oxygen and water
when treated with potassium permanganate. The oxidation of hydrogen peroxide with permanganate in
acidic solution proceeds slowly at first, but it is catalyzed by the
manganese (II) ions formed in the reaction (like oxalate and permanganate).
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5(O)
5H2O2 + 5(O) → 5H2O + 5O2

-------------------------------------------------------------------------------------------------
2KMnO4 + 3 H2SO4 + 5H2O2 → K2SO4 + 2MnSO4 + 8H2O + 5O2
In this reaction manganese in permanganate is reduced from Mn+7 to Mn+2 and hydrogen peroxide is
oxidized to oxygen. Potassium permanganate is the only colored solution, so the color of permanganate
solution will give pink color to the solution when peroxide is completely oxidized, which shows end of the
reaction.
1. Take 10 mL of the supplied H2O2 solution into a conical flask.

2. Add 20 mL of distilled water and 5 mL of dilute H2SO4 into the flask.
3. Titrate with KMnO4 solution. Appearance of faint pink colour indicates end point.
4.
Calculations:
Volume of KmNO4 required = V1 mL 1000 mL 1 N KMnO4 ≡ 17.01 g H2O2
V1 mL 1/20 N KMnO4 =17.01 x 1 x V1 g H2O2
1000 x 20
44
= 17.01 × 1 × V1 × 1000 g H2O2
1000 x 10 x 20
Results: Amount of H2O2 in given solution is g/L
Scope of the result: Estimation of peroxide concentration
Cautions:
1. Only dry apparatus should be used.
Distributors.
Weblinks:
1. http://www.titrations.info/permanganate-titration-hydrogen-peroxide
2. https://www.microsep.co.za/wp-content/uploads/2017/05/WS3_RedOx.pdf
45
Aim: To estimate hydrogen peroxide using KMnO4.
Observations Table:
Titration with KMnO4:
Volume 0.1N Burette reading Volume of

S. No. oxalic acid (mL) KMnO4
Initial Final
V1(mL)
Calculations:
Error Analysis:
46

Marks Obtained

learning outcomes
Cleanliness
Obtained
47

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LABORATORY MANUAL

(For Private Circulation)

Name of the Student: ……………………………………………….

Registration Number/Roll No……………………………………….

Section and Group…………………………………………………....

School of Chemical Engineering and Physical Sciences

Session: 2018-19 (Spring Term)

1. Safety in the Chemical Laboratory:

2. Maintenance of Laboratory Records:

S. No. Title of the Experiment Page No.

2. To prepare solutions of different molarity and normality of titrants and to 10-13

3. To estimate free alkali present in different soap and detergents. 14-17

4. To estimate carbonate and hydroxide present together in mixture. 18-21

5. To estimate carbonate and bicarbonate present together in mixture. 22-26

6. To estimate orthophosphoric acid using sodium hydroxide. 27-30

8. To estimate oxalic acid and sodium oxalate in a given mixture. 35-38

9. To estimate Fe(II) with K2Cr2O7 using internal (diphenylamine, anthranilic 39-43

10. To estimate hydrogen peroxide using KMnO4 . 44-47

Table 1: Density of Water

Outline of the Procedure:

Results: Calibration of different glassware at room temperature.

Requirement for Lab Technician: Provide clean glass-wares

Suggested reading for students: Books:

Volume of water taken:

S. No. Initial weight Final weight Actual volume Corrected volume at

Correction Factor = Actual volume delivered - apparent volume delivered

Volume of water taken:

S. No. Initial weight Final weight Actual volume Corrected volume

Correction Factor = Actual volume delivered - apparent volume delivered

Volume of water taken:

S. No. Initial weight Final weight Actual volume Corrected volume

Correction Factor = Actual volume delivered - apparent volume delivered

Result and Discussion:

Learning outcome (What I have learnt)

S. No Parameter Max. Marks Marks

1 Understanding of the student about the 20

Material Required: Hydrochloric acid, sodium hydroxide, and phenolphthalein

V1=Vol of NaOH solution = 10 mL

Results: The solutions were prepared according to different normality.

Std NaOH Vs HCl using phenolphthalein

Sr . No. Burette reading Volume of HCl used

Learning outcome (What I have learnt)

S. No Parameter Max. Marks

1 Understanding of the student about the 20

0.5 g Detergent contain x gm NaOH

% free alkali = x /0.5 (wt of soap) x 100 %

Scope of the result: Estimation of alkali in soap.

Standard solutions of HCl, indicators

Suggested reading for students: Books:

Date of performance: Registration number:

Aim: To estimate free alkali present in different soap and detergents.

Standard HCl Vs soap sample

S. No. Volume of Burette reading Volume of

Result and Discussion:

Learning outcome (What I have learnt)

S. No Parameter Max. Marks

1 Understanding of the student about the 20

Aim: To estimate carbonate and hydroxide present together in mixture.

HCO3- + H+ H2O + CO2

In 20 mL solution Na2CO3 present =2(V2-V1) mL of 0.1N HCl

Results: Amount of carbonate is g/L and hydroxide is g/L

Scope of the result: Estimation of mixture

Relationship to be determined: Acid-base titration