Laboratory Manual CHE102 Chemistry Lab

LMCHE 102: Chemistry Lab
LABORATORY MANUAL
CHE102
CHEMISTRY LAB
Page 1
Some rules to be followed in the Lab:
General Rules:
1. Entry without lab coat in chemistry lab is strictly prohibited.
2. Mobile phones should be switched off and kept in the bag during lab hours.
3. No group discussions are allowed in the lab.
4. Clean the apparatus as well slab after your experiment is finished.
5. Do not do any undisciplined activity in lab as you are under strict cc-TV
surveillance.
6. Always bring the lab manuals with you.
7. Do not use laptop while performing the experiments.
8. Switch off electrical apparatus after their use.
9. Do not throw filter papers in sink, dispose all waste in dustbin.
Precautionary Rules:
1. Never pipette out strong acids and base with your mouth, it can be
dangerous, therefore use measuring cylinders for such chemicals.
2. Never try to smell the chemicals as it can be dangerous for you.
3. Cap the bottles after taking chemical as uncovered bottles can be a source of
harmful fumes.
4. In case of any accidental spill over of any chemical on you, report your
teacher or lab technician immediately.
5. Report your lab technician if any breakage of glass apparatus takes place.
Page 2
Table of Contents
S.No Title of Experiment Page No.

With the help of complexometeric titration how you will determine the
1 4-6
hardness of given hard water sample by using EDTA. Provided standard
hard water.(1ml of S.H.W.=1mg of CaCO3)
Preparation of Sodium trioxalatoferrate(III) Na2[Fe(C2O4)3] .9H2O
2 7-9
compound.
To find the distribution coefficient of benzoic acid between benzene and
3 10-13
water.
Determination of the dissociation constant of acetic acid using pH-meter.
4 14-17
Determination of Strength of hydrochloric acid solution(approximately N/10)
5 18-21
by titrating it against sodium hydroxide solution conductometrically
To test the validity of Beer-Lambert’s law using colorimeter and to
6 22-25
determine unknown concentration of solution
Estimation of nickel in the given sample using dimethyl glyoxime.
7 26-27
Determination of the rate constant of hydrolysis in case of ethyl acetate
8 28-31
using an alkali.
Determine the strength of given solution of ferrous ammonium sulphate by
9 32-33
titrating against potassium dichromate solution
Separation of a mixture of amino acids by thin layer chromatography.
10 34-37
To determine the surface area of given solid by adsorption of acetic acid
11 38-42
from its aqueous solution.
Some important instruments in chemistry lab

12 43-44
Textbook: 1. J. Mendham, R. C. Denney, J. D. Barnes, and R. C. Denney, Vogel’s

th
Quantitative Chemical Analysis, 6 Edition, Prentice Hall, 2000. (Physical
Chemistry)
Other Reading:
th
2. J. B. Yadav, Advance Practical chemistry, Krishna Publications, Merrut 12
Revised Edition
3. Basset J Denny. R. C., Jeffery C. H. and Mendham J., Vogel’s Textbook of
Quantitative Inorganic analysis, ELBS, 1978. (Inorganic)
4. N. K. Vishnoi Advanced Practical Organic Chemistry, Vikas Publications, New
nd
Delhi, 2 edition
5. M.S. Saini, Senior practical chemistry-Vol-III, Modern Publishers-2006
Page 3
Experiment No. 1
Title: To determine the hardness of the given hard water sample by EDTA method.
Provided Standard Hard Water (1 ml of SHW =1 mg of CaCo3).
Equipments to be used: Burette, Burette stand, Titration flask, Pipette, Beakers,

funnel etc.
Chemicals Used: Standard Hard water, EDTA solution, Eriochrome black-T (EBT),
Buffer Solution, Sample hard water.
Learning Objectives:
i. The purpose of this experiment is to determine the hardness of water by

measuring the concentrations of calcium and magnesium in water samples by
titration.
ii. To know about use of buffer solution: The buffer being used has composition
NH4Cl and NH4OH. Its pH is the order of 10.5.
iii. How the indicator works: When indicator is added to hard water it combines
with free metal ions present in water.
HIn-2 + M+2 → MIn- + H+ {M = Mg or Ca}

(Wine red)
When EDTA solution is added to the titration flask it combines with the free metal
ions giving metal EDTA complex, which is stable and colorless.
H2Y2- + M+2 → MY-2 + 2H+
When all the free metal ions are exhausted, next drop of EDTA removes the metal
ion engaged with indicator and the original blue color is restored.
H2Y2- + MIn+ → MY-2 + HIn+2 + H+
Procedure:
(a) Standardisation of EDTA solution:
 Pipette out 10ml of standard hard water in the titration flask. Add to it 2-3ml of
buffer solution and two drops of Eriochrome Black-T indicator. A wine red
color appears.
 Titrate this solution against EDTA solution taken in a burette till wine red
colour changes to blue color.
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 This is the end point. Recovered the volume of EDTA consumed as A ml.
Repeated the procedure to get at least three concordant readings.
(b) Determination of Total Hardness:-
 Pipette out 10ml of sample hard water in the titration flask. Add to it 2-3ml of
buffer solution and two drops of Eriochrome Black-T indicator.
 A wine red colour appears. Titrate this solution against EDTA solution taken in
a burette till wine red colour changes to blue color.
 This is the end point. Recovered the volume of EDTA consumed as B ml.
Repeated the procedure to get at least three concordant readings
Calculations:
(a).Standardisation of EDTA solution:-
1 ml of standard hard water = 1 mg of CaCO 3
10 ml of S.H.W. = 10 mg of CaCO3 = A ml of EDTA
A ml of EDTA = 10 mg of CaCO 3
1 ml of EDTA = 10/A mg of CaCO 3
(b).Calculation of total hardness:
10 ml of hard water sample = B ml of EDTA
Now 1 ml of EDTA = 10/A mg of CaCO3
10 ml of hard water sample = B x 10/A mg of CaCO 3.
1 ml of hard water sample = B x 10/A x 1/10 mg of CaCO3.
1000 ml of hard water sample = B x 10/A x 1/10 x 1000 mg of CaCO3.
Hence total hardness = 1000 x B/A ppm
Result: The hardness of water is...........
Scope of result: The determination of water hardness is a useful test that provides
a measure of quality of water for households and industrial uses. Originally, water
hardness was defined as the measure of the capacity of the water to precipitate
soap.
Error Analysis: %Error = (1 – observed value/actual value) x 100
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Precautions:
i. The burette, pipette and conical flask should be washed and then rinsed with
distilled water.
ii. Redistilled water should be employed for preparing the EDTA solution.
iii. The color change near the end point is very slow and thus should be observed
very carefully.
Requirement for Lab Technician:
1. EDTA solution 0.1 M.

2. Standard Hard water of 1000ppm.
3. EBT(Eriochrome Black-T indicator)
4. Ammonia buffer solution.
5. Sample hard water of known strength.
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Experiment No. 2
Title: Preparation of Sodium trioxalato ferrate(III)
EQUIPMENTS TO BE USED: China dish, water bath, glass rod, Buchner funnel,
glass funnel, weighing machine, filter papers, measuring cylinder, beakers etc.
CHEMICAL REQUIRED: Mohr’s Salt ((NH4)2SO4•FeSO4•6H2O), Sodium Oxalate,

3M H2SO4, oxalic acid, water, ethanol, 30% H2O2, acetone.
LEARNING OBJECTIVES:
(i) To know about gravimetric analysis of ions
(ii) The students will learn how the transition complex formation is helpful to
determine amount of particular ion in given salt.
(iii) How to use Buchner funnel and suction pump.
THEORY: Sodiumtrioxalatoferrate (III) is a coordination compound; with a

coordination number of six and oxidation state of +3. The shape of the complex is
octahedral and it is sp3d2 hybridized. Na3[Fe(C2O4)3] •3H2O is highly photosensitive.
The bright green crystals on exposure soon become covered with a yellow powder of
ferrous oxalate.
2Na3[Fe(C2O4)3]•3H2O →2FeC2O4•2H2O + 2CO2 + 3Na2C2O4 + 2H2O
PROCEDURE:
Preparation of Ferrous Oxalate:
 Put some water in a beaker and place it on a hot plate for heating.
 Weigh 2g ferrous ammonium sulphate (Mohr’s Salt) (NH4)2SO4•FeSO4•6H2O.
Transfer the ferrous ammonium sulphate to a beaker containing 25 mL of
warm water.
 Acidify this solution with 1 mL dilute 3M H2SO4.
 To this solution add 25 mL of oxalic acid solution (5 g/50mL).
 Cautiously heat the solution to boiling on a hot plate, continuously stirring the
solution to avoid bumping.
 Remove and then allow the precipitate to settle.
 Decant and discard the clear supernatant liquid (avoid loss of precipitate). Stir
the remaining precipitate with 25 mL of hot water.
 Again decant and discard the wash liquid. Add 25 mL of hot water to the
precipitate and stir.
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 Then filter by suction using a small Buchner funnel and wash the precipitate
thoroughly with small portions (10-20 mL) of hot water. Finally rinse with acetone.
Keep these precipitates in oven for drying. Weigh the final product.
Buchner Funnel Buchner Funnel Hot Plate Weighing balance

Setup
Preparation of Sodium trioxalato ferrate(III):
 Weigh 3.5 g of Sodium oxalate (Na2C2O4•H2O) and put in 30 mL of warm

water.
 Put the washed and dried ferrous oxalate in this solution.
 Place this solution in an ice bath (a beaker or bath having ice in it) and keep it
their until it acquires the temperature of the bath.
 Add slowly with continuous stirring 10 mL of 30% H2O2 in very small
portions and stirring.
 After this heat the mixture to boiling and dissolve the precipitate by adding in
one portion 10 mL of a solution of oxalic acid (containing 2.5 g/25 mL) in very
small proportions. The liquid should be near the boiling point while
these additions are being made.
 Filter through a Buchner funnel to get the clear filtrate solution.
 Transfer the hot solution to a clean beaker and while still hot, add to the
filtrate 15 mL of 95% ethanol and redissolve any precipitated crystals by
gently heating.
Page 8
 Then store the solution in a dark cupboard for crystallization. After

crystallization has occurred, filter with suction and wash the product on the
filter paper with 20 mL of an equi-volume mixture of ethanol and water and
finally with acetone.
 Draw air through the precipitate for several minutes or keep in oven for drying.
Weigh the dry crystals.
 Preserve the crystal in a polyethene and attach to your notebook.
RESULT: Color of the compound……….
Weight of the ppt. …………….
SCOPE OF THE RESULT: Gravimetric analysis is helpful in estimation of amount of

Fe in given complex.
Precautions:
i. Stirring should be done very carefully wherever is mentioned in the procedure.

ii. Addition of H2O2 should be done when the solution acquire temperature of ice
bath.
iii. Addition of acetic acid should be done when solution is just near to the boiling
point.
Requirements for Lab Technician:
1. Oxalic acid solution (5g/50mL)
2. 3M H2SO4
3. 30% H2O2
4. Alcohol
5. Acetone
6. Ferrous ammonium sulphate and sodium oxalate
Page 9
Experiment-3
Title: To study the distribution of benzoic acid between benzene and water.
EQUIPMENTS REQUIRED: Pipette, Burette, titration flask, eight washed empty

bottles, stoppers, separating funnel.
CHEMICAL REQUIRED: Benzene, Benzoic acid, water, NaOH, HCl,

Phenolphthalein.
LEARNING OBJECTIVE: In this experiment we will use the volumetric technique of

acid-base titration to determine the distribution of benzoic acid in the water-benzene
system. From these distribution measurements we will be able to examine the two
equilibria:
(1) dimerization of benzoic acid in benzene and,
(2) distribution of benzoic acid monomers between water and benzene.
INTRODUCTION:
Distribution coefficient (D) is the ratio of concentrations of a compound in the two

phases of a mixture of two immiscible solvents at equilibrium. Hence these
coefficients are a measure of differential solubility of the compound between these
two solvents.
If an excess of liquid or solid is added to a mixture of two immiscible liquids it will
distributes itself between the two phases. So the each phase become saturated. If
the substance is added to the immiscible solvents in an amount sufficient to saturate
the solution, it will still remain distributed between the two layers in a definite
concentration ratio. If C1 and C2 are the equilibrium concentration of the substance in
the solvent -1 and solvent-2 the equilibrium expression becomes
C1/C2=K
The equilibrium constant is known as the distribution ratio of partition coefficient.
A general treatment by Moelwyn-Hughes equation (1) allows examination of the
above two equilibria from distribution measurements. In the benzoic acid(HBz )-
water-benzene system, there are three equilibria which must be considered. In the
aqueous layer, benzoic acid, being a weak acid will dissociate:
HBz ↔ H+(aq) + Bz-(aq) (1)
and we can write the acid dissociation constant, Ka for the equilibrium as
Ka = [H+] [Bz-] / [HBz] (2)
In the benzene layer, benzoic acid exists both as a monomer and dimer (i.e. two
benzoic acid molecules bonded together by hydrogen bonding to form a new
species). This dimerization is also in equilibrium:
2 HBz↔ (HBz)2
KD = [(HBz)2]/[(HBz)2]b (3)
where [HBz]b, is the equilibrium molar concentration of the monomer in benzene and
[(HBz)2]b is the equilibrium molar concentration of the dimer in benzene.
The third equilibrium is the equilibrium constant for the distribution of benzoic acid
monomers between water and benzene:
(HBz)W ↔ (HBz)b
KM = [HBz]b/[HBz]W (4)
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The total concentrations of benzoic acid in water and benzene, CW and Cb

respectively, is obtained by titration of the appropriate phase with sodium hydroxide.
CW = [HBz]W + [Bz-]W = CW(1 - α) + α CW (5)
where α is the degree of dissociation of benzoic acid; and
Cb = [HBz]b + 2 [(HBz)2]b (6)
Using Eqs.(3) and (4) as well as noting that [HBz]W = CW(1 - α) allows Eq.(6) to be
rearranged to,(7)
Cb/CW(1 - α)= KM + 2KM2KDCW(1 - α) (7)
A plot of Cb/CW(1 - α) vs. CW(1 - α) will be linear with a slope of 2KM
2KD and an intercept of KM. The value of α used in Eq. (7) is obtained from the
known value of Ka.
Ka = α2CW/1 - α= 6.3 x 10-5 for benzoic acid at 20oC
pKa= 4.1 (benzoic acid)
Cb and Cw are calculated from the titration of the respective layers.
PROCEDURE:
Prepare a 1.2 % w/v solution of Benzoic acid in benzene (stock solution).
A. Preparation of the benzene/benzoic acid/water mixtures:

 Five mixtures of benzene/benzoic acid in benzene/water are to be studied so
that the distribution can be observed over a wide range of concentration.
 These mixtures are to be made according to Table 1, using the burettes for
benzene and the benzoic acid solution in benzene, the water should be
added using the 50.00 mL pipette. For example Mixture 2 can be prepared by
adding 20 mL of Benzoic acid in Benzene, 5 mL of Benzene and 25 mL of
water.
TABLE 1:Mixture of Benzoic acid in Benzene, Benzene and Water.
Mixture Benzoic acid in Benzene (mL) Water (mL)
Benzene (mL)
1 25 +0 +25
2 20 +5 +25
3 15 +10 +25
4 10 +15 +25
5 5 +20 +25
 Make up the mixtures in the stoppered bottles and allow the equilibrium
distribution to be attained over a period of about 30 minutes, shaking
frequently.
 During the equilibration period, practice the two titrations involved on samples
of benzoic acid in benzene and in water as supplied in the laboratory.
 Separate the organic and the aqueous layer using separating funnel or at the
end of the equilibration period, allow the mixture to separate into two layers.
Decant the upper benzene layer into a large, clean, dry test tube, and cork it
at once. (This separation need not be perfect).
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Separating Funnel. Setup of Separating Funnels and reagent bottles
B. Titration of the benzene layer
Pipette 10.00 mL of the benzene solution from the upper layer in a conical flask. Add
2-3 drops of phenolphthalein as indicator and titrate it against 0.1 N NaOH taken in
burette. Appearance of pink color will be the end point. Perform for all bottles.
C. Titration of the aqueous layer
Pipette out 10 mL of aqueous layer in titration flask and add 2-3 drops of
phenolphthalein as indicator and titrate it against 0.01 N NaOH taken in burette.
Appearance of pink color will be the end point. Perform for all bottles.
OBSERVATIONS AND CALCULATION:

Titration of benzene layer:
Bottle Vol. taken in Burette readings Volume of 0.1 N NaOH
No. titration flask (mL) Initial reading Final reading solution used (mL)
1 10
2 10
3 10
Concentration of Benzoic acid in bottle 1:
N1V1 = N2V2
(benzoic acid) (NaOH)
N1 x 10 = 0.1 x A
N1 = a N
Concentration of Benzoic acid in organic layer Cb:
Cb = a x Mol. Wt. Of benzoic acid = a x 122
Same calculations will be follwed for the other bottles also.
Page 12
Titration of aqueous layer:

Bottle Vol. taken in Burette readings Volume of 0.01 N
No. titration flask (mL) Initial reading Final reading NaOH solution used
(mL)
1 10
2 10
3 10
Concentration of Benzoic acid in bottle 1:
N1V1 = N2V2
(benzoic acid) (NaOH)
N1 x 10 = 0.01 x A
N1 = b N
Concentration of Benzoic acid in aqueous layer C w:
Cb = b x Mol. Wt. Of benzoic acid = b x 122
Same calculations will be follwed for the other bottles also.
Distribution coefficient K = Cb/Cw calculate K for all bottles and report in the result.
Graphical presentation of distribution law

Bottle No. Cw Cb α= (Ka/Cw)1/2 Cb/CW(1 - α) CW(1 - α)
1.
2.
A graph between Cb/CW(1 - α) Vs CW(1 - α) is plotted. The graph gives a straight line
with a slope of 2KM
Ka = 6.3 x 10-5 for benzoic acid at 20o C.
RESULT: The distribution coefficient of benzoic acid in benzene and water in bottles
1,2, 3 …….. is ............. respectively/
PRECAUTIONS:
1. Titration should be carefully performed.

2. The bottles should be shaked properly.
3. Separating funnel should be handled by care.

1. Benzene
2. Benzoic acid in benzene (0.1N)
3. 0.1 N and 0.01N NaOH.
4. Phenolphthalein indicator
Page 13
Experiment No. 4
Title: Determination of the dissociation constant of acetic acid using pH-meter.
Equipments to be used: pH meter, 100 mL beaker, pH electrode, pipette, burette,

funnel etc.
Chemicals to be used: Acetic acid, sodium hydroxide, buffer solution of pH 4 and

pH 7.
Learning objectives:
i. Students will learn the basics of pH meter and how to use pH meter.
ii. To monitor the total pH of a solution and to determine equivalence point of
titrations that involve ions.
iii. Students will learn how to use a calibration curve to determine the unknown
strength of a solution.
iv. To calculate the dissociation constant of weak acid.
Glass electrode
To set temperature To set knob at pH
pH reading Buffer Solution of pH 4 & 7
Fig: pH meter
THEORY: The strength of an acid is experimentally measured by determining its

equilibrium constant or dissociation constant (K). Since strong acids are strong
electrolytes, they are ionized almost completely in aqueous solutions. It is not
Page 14
meaningful to study the ionic equilibrium of strong acids and calculate their
equilibrium constants as the unionized form is present to such a small extent. Hence,
the study of ionic equilibrium and calculation of K is applicable only to weak acids.
e.g. Acetic acid ionizes feebly as,
CH3COOH (aq) + H2O (l) H3O+ (aq) + CH3COO- (aq)
K = [H3O+] [CH3COO-]/[ CH3COOH]
pKa is a modern method of expressing acid strengths. pK a is determined by

measuring the changes in pH of acid solution at different amounts of the base
added.
During the titration of an acid with a base, the pH of the solution rises gradually at
first, then more rapidly and until at the equivalence point, there is a very sharp
increase in pH for a very small quantity of added base. Once past the equivalence
point, the pH increases only slightly on addition of excess base. The titration curve is
obtained by plotting changes in pH at different amounts of the base added and the
equivalence point is determined.
PROCEDURE:
 Switch on the pH meter after connecting the pH electrode to it .
 With the help of temperature knob shown in the Fig set the temperature to the
room temperature.
 Make sure that pH knob is pointing towards pH as shown in Fig.
 Take buffer solutions of pH 4 and pH 7 which will be provided by the lab

technician.
 Put the pH electrode in pH 4 solution and set the pH on screen to 4 with

calibration knob present on the pH meter.
 Then wash the electrode and put it in pH 7 solution and set 7 on the screen.
 Your pH meter is now ready to to take readings of unknown solutions. Don’t

touch any of the button now onwards till the end of the experiment.
Page 15
 Pipette out 50 mL of the given weak acid into a 100 cm3 beaker. Immerse
electrode assembly into the acid. Measure the pH of the acid.
 Fill a burette with the base (0.1 N sodium hydroxide).
 Add 1 mL of the base from burette to the acid. Stir the solution thoroughly and
measure the pH after addition.
 Continue adding 1 mL of base and noting down pH at each successive

addition.
 When the pH begins to show a tendency to increase rapidly (e.g. from 6-9),
add only small increments (say 0.1 mL) of the base and measure the pH after
each addition. Continue till there is only a slight increase in pH on the addition
of the base.
 Again add 1mL of base for 3-4 time more and note down the change in pH.
Plot a graph of pH (ordinate) against the volume of sodium hydroxide added

(abscissa). Determine the equivalence point and hence the pH at half equivalence
point. This gives the pKa value of the acid.
OBSERVATIONS AND CALCULATIONS:
S. No Volume of NaOH added Observed conductivity
(ml.) (mMhos/cm)
1. 0
2. 1.0
3. 2.0
4. 3.0
- -
- -
1) Equivalence point =........................(on x-axis i.e. vol. of NaOH in mL)
2) Half equivalence point =............... (take half of the vol. of NaOH at Eq. Pt. in mL)
3) pH at half equivalence point =………………(on y-axis)
Page 16
pKa of the given weak acid = pH at half equivalence point =....................
pKa = - log Ka
Ka = Antilog10 (-pH at half equivalence point)
Ask for the original value from your instructor for error calculations.
Scope of the result:
Parameter used: pKa = - log Ka, hence the value of dissociation constant(Ka) can
be calculated
Plot:
Equivalence point
pH
Half equivalence point
Volume of alkali added(ml)
With the help of plot, Equivalence point is calculated.
PRECAUTIONS:
1. Handle the glass electrode very carefully.
2. Switch on the pH meter at least 10 minutes before the start of the measurements.
3. Stir the solution thoroughly before taking the reading.
4. Let the reading stabilize for tome time (15 seconds) before taking the reading.
1. Acetic acid 0.02M.
2. 0.1N NaOH.
Page 17
Experiment No. 5
Title: To find the strength of hydrochloric acid solution (approximately N/10) by

titrating it against sodium hydroxide solution conductometrically.
Equipments required: Conductivity Bridge, conductivity cell, beaker, funnel, burette

and pipette.
Chemicals required: 00.1 N NaOH solution and approximately HCl solution.
i. Students will learn the basics of Conductometer and how to use Conductometer.
ii. To monitor the total conductance of a solution and to determine the end points of
titrations that involve ions.
iii. Students will learn how to use a calibration curve to determine the unknown
strength of a solution.
iv. Students will get knowledge about conductometric titrations.
Value of Cell Constant
To set at the value of cell Conductivity Electrode

constant
Conductivity Electrode
Range
To set temperature
To set Cond. or Cell constant
Fig.: Conductometer
THEORY: Conductometry can be used to detect the equivalence point (end point) of
a titration. This method is based upon the measurement of conductance during the
course of titration. The conductance varies differently before and after the
equivalence point. This is due to the reason that electrical conductance of a solution
depends upon the number of icons present and their ionic mobilities i.e. speeds.
When conductance values are plotted against volume of titrant added, two straight
Page 18
lines are obtained; the point of intersection of the lines gives the end point. For
studying HCl vs NaOH titration, a know volume of HCl is taken in a beaker and
NaOH solution in the burette. The conductance of acid solution is noted initially as
well as after successive additions of small amounts of NaOH solution.Conductance
of acid solution in the beginning is very high due to presence of highly mobile H +
ions. On adding NaOH solution, the H+ ions are replaced by slow moving Na ions,
decreasing the conductance of solution.
[H+ + Cl -] + [Na + + OH-] Na++ Cl- + H2O
When neutralization is complete, further addition of NaOH will cause the

conductance to increase due to excess of highly mobile OH - ions. The conductance
will thus be minimum at the equivalence point. Thus if conductance values are
plotted against the volume of NaOH added, a curve of the type xyz is obtained.
The point of intersection (i.e. point Y) corresponds to the end point.
PROCEDURE:
 Determine the cell constant of the given conductivity cell which is written on the
neck of the cell.
 Connect the conductivity cell to the conductometer.
 Set the function switch to check position. Display must read 1.000. If it does not,
set it with CAL control at the back panel.
 Put the ‘Function Switch’ to ‘Cell Constant’ and set the value of the cell constant
determined in step-1 with the help of cell constant Knob shown in the Fig.
 Set the temperature control to the actual temperature of the solution under test.
 Rinse the conductivity cell with the solution whose conductivity is to be
measured.
 Take 20 ml of the given HCl in a 100 ml beaker.
 Wash the conductivity cell with distilled water and then rinse it with it with the
given HCl solution. Dip the cell in the solution taken in the beaker.
 Set the range with the help of “range” knob shown in the Fig to 200.
 Set the ‘Function Switch’ to ‘Conductivity’ and read the display. This will be the
exact conductivity note it down.
 Take alkali (NaOH) in the burette and 0.5 mL of it into the beaker containing HCl.
Stir and determine the conductivity.
 Repeat the procedure of addition of 0.5 mL of NaOH and noting down the
conductivity in the observation table.
 Take 12-15 readings in the ways. After each addition, stir the solution gently.
 Plot a graph between observed conductivity value along Y-axis against the
volume of alkali added along x-axis. The point of intersection gives the amount of
alkali required for neutralization of acid.
Page 19
OBSERVATIONS AND CALCULATIONS:

Volume of HCl taken = 50 ml
Normality of NaOH solution = 0.1 N
OBSERVATION TABLE
S. No Volume of NaOH added Observed conductance
(ml.) (ohm-1)
1. 0.5
2. 1.0
3. 1.5
4. 2.0
- -
- -
22. 11.0
23. 11.5
24. 12.0
From graph the volume of NaOH used is (calculated by drawing perpendicular on X-

axis from the point of intersection) = A ml (also called as equivalence point).
Applying normality equation
N1V1 = N2V2
(HCl) (NaOH)
N1 x 20 = 0.1 x A
N1 = a N
We know strength in grams per litre = Normality x Eq. Wt.
Therefore, strength of acid = a x 36.5 g/litre = Y g/litre.
RESULT: Strength of given HCl solution = Y g/litre.
% error: Ask your instructor for the actual value and the calculate error in your
result.
Page 20
Scope of result: Conductometric titrations are used to calculate conductance and

strength of solutions. Conductivity meters are used in conjunction with water
purification systems, such as stills or deionizers, to indicate the presence or absence
of ion-free water.
PLOT: When a graph is potted between volume of the alkali added and conductance
then a V – shaped graph is obtained. The point of intersection will give the end point.
X z
Conductance (ohm)
Conductance
Conductance
Y end point
Volume of alkali added (ml)
PRECAUTIONS:
1. The solution taken in the burette should be about ten times stronger than that
taken in the beaker so that the volume change of latter solution is negligible on the
addition of the former solution.
2. After every addition of NaOH solution, the solution must be stirred thoroughly.
1. 0.1 N NaOH.
2. 0.01 N HCl
Page 21
Experiment No. 6
AIM: To test the validity of Beer-Lambert’s law using colorimeter and to determine
unknown concentration of solution.
Equipments to be used: Colorimeter, test tubes, burette, 50 cc measuring flask,
Chemical required: Distilled Water, 0.1 M Potassium dichromate.
1. Students will learn the basics of colorimetry and how to use colorimeters
2. Students will gain practice in preparing solutions through dilution and in
calculating solution concentrations
3. Students will use algebraic representations to describe data
4. Students will learn how to use a calibration curve to determine the unknown
concentration of a solution
Filter (to set at λ)
To set O.D at zero
Fig: PhotoColorimeter
THEORY: When a monochromatic light of intensity I is incident on a transparent

medium, a part of it is absorbed, a part, I, is reflected and the remaining part, I, is
transmitted.
In case of aqueous solutions, is negligible as compared to and .
According to Beers Lambert’s law the decrease in intensity of the incident light is
proportional to the length of thickness of the absorbing medium and the
concentration of the solution.
(1)
Page 22
Where C is concentration of solute expressed in mole/litre, l is the length of the cell

and is a constant characteristic of the solute called molar extinction coefficient or
molar absorptivity. Further also called as optical density (OD) or absorbance
(A). Since absorbance A of the medium is given by
(2)
From equation (1) and (2)
A = ƐCl
Transmittance, T of a solution is the ratio of i.e., the fraction of incident light

transmitted by the solution.
A plot between absorbance and concentration is expected to the linear. Such a

straight line plot, passing through the origin, shows that Beer- Lambert’s law is
obeyed. This plot, known as calibration curve can also be also employed in finding
the concentration of a given solution.
PROCEDURE:
 Connect the instrument to the mains and put on the power switch.
 Adjust the wavelength knob to the 40 wavelength region on scale

(approximately).
 Open the lid on the cell compartment and insert a cuvette containing the
distilled water. Close the lid.
 Adjust the reading on the digital screen to zero optical density with the
knob shown in the Fig.
 Remove the cuvette and close the lid tightly again. Empty the cuvette and
rinse it with standard solution of KMnO4 (0.001 IM) [which will be
provided to you by lab technician]. Fill the cuvette this solution and note
the optical density.
 Change the wave length to the next high value using set wavelength knob
every time and note down corresponding optical density. Make table with
wavelength on L.H.S and OD at R.H.S.
Page 23
 Plot a graph between wavelength on the x-axis and O.D. on the y-axis. Find
the value of λmax ( O.D is maximum)
O.D
λmax
Wavelength (nm)
 Now set the λmax value in the colorimeter with the help of the knob used for
setting wavelength and place the cuvette containing Distilled water in the cell
compartment. Set O.D to zero again.
 Prepare KMnO4 solution in water with composition 10%, 20%, 30%,40%,--------

---- 100%. 10% composition means 10ml of KMnO4 and 90ml of water or 1ml of
KMnO4 and 9ml of water.
 Make table with Concentration on L.H.S and OD on R.H.S.
 Note down the absorbance (OD) of series of solution of KMnO 4 prepared
above (from 10% to 100%) by the method described above. Do not change
wavelength now.
 Plot a graph between O.D against composition. (If a straight line is obtained
Lambert - Beer’s a law is verified)
 Now take a solution of a unknown concentration and note down optical
density. Find out the concentration of the unknown solution from graph.
Report the results of unknown solution in gram/litre.
Scope of result: This experiment is used to study the absorbance power of different
solutions and also to find the unknown concentration of solution
Plot: A plot between absorbance and concentration is expected to the linear. Such a
straight line plot, passing through the origin, shows that Beer- Lambert’s law is
obeyed. This plot, known as calibration curve can also be also employed in finding
the concentration of a given solution.
Page 24
O.D
Composition of KMnO4 solution(%)
PRECAUTIONS:
1. Handle the glass cuvettes very carefully.
2. Switch on the colorimeter at least 10 minutes before the start of the

measurements.
3. There should be no air drop outside the cuvette.
4. Let the reading stabilize for tome time (15 seconds) before taking the reading.
1. 0.001M KMnO4
2. Distilled water.
Page 25
Experiment No. 7
Title: Estimation of nickel in the given sample using DMG.
Equipments to be used: Beakers, Suction pump, sintered glass crucible, oven,

glass rod etc..
Chemical required: Nickel ammonium sulphate, Dimethyl glyoxime, concentrated

ammonia, Ethanol, HCl etc.
(i) To know about gravimetric analysis of ions
(ii) The students will learn how the transition complex formation is helpful to
determine amount of particular ion in given salt.
(iii) How to use sintered glass crucible and suction pump.
Chemical Reaction:
Red ppts
H
O O
H3C H3C CH3
N OH C N N C
2 NiSO4 2NH4OH Ni (NH4)2SO4 2H2O
C N N C
N OH H3C CH3
H3C
O O
H
Theory:
Nickel dimethyl glyoxime is prepared by the action of alcoholic solution of dimethyl

glyoxime on soluble nickel salts such as Nickel chloride or Nickel sulphate in
presence of NH4OH solution or alkaline medium. Soluble Nickel salt is dissolved in
water and the solution acidified with dil HCl Solution is heated to 60-70oC and then
treated with alcoholic solution of dimethyl glyoxime. Precipitate of nickel dimethyl
glyoxime is carried out by adding 6N NH4OH solution (1:1) till it gives smell of
ammonia. A brilliant red precipitate of nickel dimethyl glyoxime separates out. It is
allowed to stand for 20 minutes so that precipitates settle down.
The precipitate is separated by filtration through Buchner funnel and washed. It is

dried in air oven at 110-120oC. Its color and weigh is noted.
Procedure: Note: Apparatus should be cleaned properly prior to use.
Page 26
1. Dissolve 1.0 g of nickel ammonium sulphate or Nickel chloride in distilled

water in a beaker and dilute it with 19 ml of distilled water. Add 0.5 ml of
concentrated HCl.
2. Dissolve 0.6 g of dimethyl glyoxime in 13 ml of ethyl alcohol in a seaparate
conical flask.
3. Add dimethyl glyoxime solution to nickel ammonium sulphate solution along
with stirring.
4. Heat the mixture solution to 60-70oC on water bath.
5. Add 6N NH4OH solution (1:1 NH3) or Ammonia solution slowly with constant
stirring till precipitation starts. Add excess of 6N NH4OH solution (means a few
drops more even after precipitation)
6. Allow the reaction mixture to stand for about 20 minutes so that mixture to
settle down.
7. Separate the precipitate by filtration through a sintered glass crucible (ask
for this from your lab technician) under suction and wash with cold water.
8. Remove the brilliant red precipitate formed and dry in air oven.
9. Note the colour and weight of the product formed.
Calculation:
288.69 58.69
Hence, weight of Nickel = 0.2033 X weight of the precipitate
Result: Color of the compound……….
Weigh of the ppt. …………….
Error Analysis: Calculate the actual amount of Ni in starting Nickel chloride taken
for the preparation and calculate the % error.
Scope of result: Gravimetric analysis is helpful in estimation of amount of Ni in

given salt.
1. Nickel ammonium suphate or Nickel chloride.
2. Dimethylglyoxime
3. Conc. HCL
4. Methanol or Ethanol.
5. Ammonia Solution.
Page 27
Experiment No. 8
Title: Determination of the rate constant of hydrolysis in case of ethyl acetate

catalyzed by HCl at room temperature
Equipments requirements: Six conical flasks, burette, pipette,
Chemical required: 0.1 NaOH, methyl acetate, 0.5 N HCl, Stop watch, Water bath,
Phenolphthalein.
Learning Objective: (i) To gain knowledge about chemical kinetics of

psuedounimolecular reactions.
(2) To determine the rate constant of a reaction
(3) Student will learn how to find the order of reaction with the help of rate constant at
different time intervals.
(4) To prove that order of reaction is experimental concept.
THEORY: The reaction is catalysed by H+ ions of an acid (HCl). This reaction is an

example of psuedounimolecular reactions. Since water is present in large excess, its
concentration is practically constant throughout the reaction. The concentration of
HCl (catalyst) also remains constant. Therefore, the rate of reaction depends upon
only on the concentration of ester.
Rate = -dx/dt = k [CH3COOC2H5]. Hence reaction is of first order.
During the hydrolysis of ester, acetic acid is produced. Therefore, the progress of
reaction is followed by determining the amount of acetic acid formed at different time
intervals.
H
CH3COOC2H5 + H2O CH3COOH + C2H5OH
A definite quantity of the reaction mixture is withdrawn after different time intervals
and is titrated against a standard solution of alkali. The amount of alkali used is
equivalent to the total amount of HCl present initially and the amount of acetic acid
formed. The volume of alkali used at the start of reaction is equivalent to amount of
HCl alone. Hence, the amount of acetic acid formed (x) after different intervals of time
can be calculated. The amount of acetic acid formed at the end of reaction is
equivalent of initial concentration of ester (a). Suppose the volumes of alkali used
required for the reaction, at the start, after time t and the end of reaction are V 0,Vt,Vα
Page 28
respectively, then initial concentration of ester (a) is proportional to V ∞-V0. The

concentration of ester after time t is V∞ - Vt
K = 2.303 log V∞ - V0
t V∞- Vt
If the value of K comes out constant during different intervals of time, then order of
reaction will first order.
Procedure:
 Take 50ml of 0.5 N HCl in a clean dry 250mL conical flask and about 10mL
of pure ethyl acetate in a test tube, cork both of them and place them in a
thermostat or water bath at or near room temperature. (Take water in a big
beaker and put conical flask and test tube in it).
 Keep the 0.5N HCl and ethyl acetate in the thermostat or water bath for about
10 min to allow them to acquire the temperature of the bath.
 In the mean time, fit the burette properly and fill it with 0.1N NaOH solution.
 At about 9 minutes add 25mL of ice cold water in a separate conical flask.
 After 10 minutes pipette out 5mL of the ethyl acetate from the test tube and
add it to the flask containing 50 mL of 0.5 N HCl. Start stop watch at this
moment from zero again.
 Shake the contents for 2-3 seconds and immediately pipette out 5 mL of
reaction mixture and transfer it at once to first conical flask containing ice cold
water.
 Keep the flask containing reaction mixture in the water bath again, it should
be noted that reaction mixture will be kept in the water bath at constant
temperate throughout the experiment.
 Titrate the solution in conical flask containing 25 mL ice cold water and 5 mL
of reaction mixture against 0.1 N NaOH taken in burette by using
phenolphthalein as indicator. Appearance of pink colour is end point. The
volume of 0.1 N NaOH used against the withdrawn sample of the ester and
dil. HCl mixture is taken as V0.
 After about 9 minutes add 25mL of ice cold water in a separate conical flask.
 Pipette out 5 mL of mixture and add it to the conical flask containing ice cold
water after 10 min. Titrate it against 0.1 N NaOH . This gives V t after 10 min.
Page 29
 Repeat the above procedure after every 10 min for taking readings upto 40
minutes.
 Place the remaining reaction mixture in the separate water bath at 60-70oC for
about half to one hour time. Pipette out 5 mL of mixture and titrate it against
alkali solution. This gives V∞.
Observations and Calculations:
S. No Time Volume of NaOH (ml) V∞ - V0 V∞ - Vt Log (V∞ - Vt) Log(V∞ - V0)

(min)
1. 0 V0
2. 10 V10 V∞ - V10
3. 20 V20 V∞ - V20
4. 30 V30 V∞ - V30
5. 40 V40 V∞ - V40
6. ∞ V∞
Calculations: Calculation of K at time 10, 20, 30 and 40 min will be done by the
following formula:
K = 2.303 log V∞- V0 min -1
t V∞- Vt
log(V∞- Vt ) = - Kt/2.303 +log (V∞- V0) is equation of straight line.
Scope of result: We study the kinetics of hydrolysis of esters; hydrolysis of ethyl

acetate has a very rapid rate that could be carried in short time.
Parameter used: Rate constant (K): The value of K comes out constant during
different intervals of time,then order of reaction will first order.
Page 30
Plot:
log(V∞ - Vt ) slope = - K/2.303. With the help of slope,
the value of rate constant can
be calculated.
t (min)
Precations:
i. Use the ice cold water only.
ii. Perform the titrations properly.
iii. Always take alkali in burette.
1. 0.1 N NaOH
2. 0.5 N HCl
3. Ehtylacetale
4. Icecold water
5. Phenolphthalein indicator
Page 31
Experiment No. 9
Title: Determine the strength of given solution of ferrous ammonium sulphate(Mohr’s
salt) by titrating against potassium dichromate solution.
Equipment Required: Volumetric flask, 250 mL Beakers, 50 mL Burette, pipette,
funnel etc.
Material Required:
Potassium dichromate K2Cr2O7 reagent grade, Ferrous ammonium sulphate,
Sulphuric Acid (concentrated).
i. Student will learn how to calculate the exact normality of Ferrous ammonium
sulphate (Mohr’s salt) by titrating with potassium dichromate solution.
ii. To gain knowledge about redox titration.
Theory: This experiment is an example of redox titration. The loss of electrons is
oxidation; the gain of electrons is reduction. Reduction/oxidation (redox) processes
occur when electrons are transferred from a donor species (the reducing agent
2FeSO4(NH4)2SO4) to another acceptor species (the oxidizing agent K2Cr2O7).
Reactions: The reaction between Potassium dichromate and Mohr’s salt can be
represented as:
Molecular equations:
K2Cr2O7 + 4H2SO4 → K2SO4 + Cr2(SO4)3 + 3[O]
2FeSO4(NH4)2SO4 +H2SO4 +O → Fe2(SO4)3 +2(NH4)2SO4 + H2O
Ionic Equations:
2Cr2O72– + 14H+ + 6e– → 2Cr3+ + 7H2O
Fe2+ → Fe3+ + e-
Procedure:
Titration of K2Cr2O7 soln. with Mohr’s salt solution
 Pipette out 10 mL of Mohr’s salt solution in the conical flask.
 Add approximately 4 mL of Conc. H2SO4 to the same flask.
 Add 2-4 drops of the Ferroin indicator.
 Titrate the reaction mixture with potassium dichromate solution taken in burette
till a colour change from Wine red - green is obtained.
 Repeat the titration for three concordant readings.
Observations and Calculations
Volume of Mohr’s salt solution used in each titration = 10 mL
Indicator used = Ferroin indicator
Color change at end point = Wine red - green
Equivalent weight of Mohr’s salt = 392
Page 32
Table.
S. No. Burette readings Volume of K2Cr2O7
Initial Final Consumed (R2 - R1)

mL
Thus applying the normality relation NMohr VMohr = NdichrVdichr
Thus
NMohr = NdichrVdichr/VMohr
Thus strength (g/L) of Mohr’s salt solution = Normality x Eq. Wt
Result: Strength of given Ferrous ammonium sulphate solution= ……… g/litre.
Scope of the results expected: Redox titration are used to calculate strength of
solution, based on an oxidation-reduction reaction between analyte and titrant. Many
common analytes in chemistry, biology, environmental and materials science can be
measured by redox titrations.
Precautions:
(i) Always take Potassium dichromate solution in burette.
(ii) Potassium dichromate acts as oxidizing agent in acidic medium. Therefore
always add dil. H2SO4 in the reducing agent.
(iii) Read the upper meniscus while taking burette readings because K2Cr2O7 is
coloured.
1. N/20 Mohr’s salt solution.
2. N/20 potassium dichromate solution.
3. Cons. H2SO4.
4. Ferroin indicator.
Page 33
Experiment No. 10
Title: Separation of amino acids by thin layer chromatography.
Equipments Required: Glass plates, beaker, Glass rod,
Chemicals Required: Silica gel (for TLC), Glycine, Leucine, acetic acid, n-butanol,
water, alcoholic solution of ninhydrin
i. Students will learn the basis of TLC and how to prepare the TLC plates.
ii. To calculate retention factor (Rf).
iii. Students will learn how to separate the mixture of organic compounds on the
basis of Rf value
Theory: Thin Layer Chromatography (TLC) is used extensively for qualitative

analysis (tentative identification of mixture of two or more organic compounds). In
this technique a small amount of the material (to be separated), dissolved in an
appropriate solvent, is spotted near one edge of the plate covered with thin layer of
adsorbent.
The adsorbent is usually a thin layer of alumina or silica gel. After the sample
has been deposited on the adsorbent, the coated plate is placed in a beaker
containing small amount of solvent in such a manner that the lower end of plate dips
1-2 cm below the surface of solvent. The solvent rises through the adsorbent by
capillary action and the various components of the mixture ascends at different rates,
depending on their different affinities to the adsorbent.
This results in the separation from one another. When the solvent front has
almost reached the top of the adsorbent layer or three-fourth of it, the plate is
removed from the beaker, dried and examined.
TLC involves the following steps:
(a) Preparation of a thin layer plate

(b) Application of the materials to be separated on the plate
(c) Development of the chromatogram plate in a solvent
Page 34
(d) Visualization or Location of components

(e) Calculation of Rf values.
Retention Factor: The movement of any substance relative to the solvent front in a
given chromatographic system is constant and characteristic of a substance.
Rf value =
= b/a
Procedure:
 Take small amount of silica gel in a beaker and dissolve it in distilled water
with constant stirring by a glass rod. Continue to stir until a uniform paste free
from air bubbles is formed. Add some more water to obtain slurry of suitable
consistency. (OR this slurry may be provided to you by the lab
technician).
 Mark the base line on the glass plate about 1 cm from the bottom edge of the
glass plate. (Mark only at edges with pencil). This line is just to take an idea
that where is 1 cm distance lies from the bottom where sample mixture is to
be applied.
 Pour the slurry on to the clean and dry plate and prepare a uniform thin layer
by glass rod.
Page 35
 Allow the layer to dry for 5-10 minutes and then heat the plates in an electric
oven at 100-120oC for about 20 min.
 Prepare solution by mixing two or more different organic compounds. (Given

to you by lab technician).
 At base line and apply small sample of the mixture with the help of thin
capillary tube in the centreu. Take care the spots must be as small as
possible.
 Allow the spot to dry. Place the glass plate in a beaker containing solvent to a
depth of about 1 cm or less than that and allow the solvent to flow up until it
nearly reaches the top of the plate. ( take due care that spot must not
touch the solvent)
 Remove the plate from the beaker, mark the position of the solvent front (on
edge of the plate with pencil) and allow the solvent to evaporate.
 Spray with alcoholic ninhydrin and dry TLC plate in the oven for 2 min.
 Spots will develop on the plate. Take measurements of the distance moved by
solvents and each component from the 1 cm mark.
 Calculate the Rf values of the components in the mixture.
Apparatus for TLC TLC plate in solvent in development phase
Page 36
TLC plate in solvent in development phase Ninhydrin Spray apparatus
Scope of Result: Thin Layer Chromatography (TLC) is used extensively for

qualitative analysis and tentative identification of mixture of two or more organic
compounds.TLC is a useful screening technique in clinical chemistry; for example, it
can be used to detect the presence of drugs in urine.
Parameter used: Retention Factor (Rf): The movement of any substance
Precautions:
i. Make the slurry very carefully; it should not be very thick or very thin.
ii. Always prepare fresh silica slurry.
iii. Make sure that sample dot is always outside the solvent layer.
iv. Spots of mixture must be as small as possible.
v. Dry TLC plates carefully.
1. Glycine and Leucine mixture.
2. Silica gel
3. TLC solvent Butanol (5):Acetic acid (2):Water (4)
4. Ninhydrin spray
Page 37
Experiment No. 11
Title: Determine the adsorption of acetic acid from aqueous solution by active
charcoal at room temperature.
Equipment Required: Conical flasks with corks, beakers, pipette, funnel, filter
paper, glazed paper.
Material Required: Activated charcoal, 0.5 M acetic acid, 0.1 M NaOH
1. Students will learn about the adsorption phenomenon.
2. Students will gain practice of preparing volumetric solutions.
3. Students will learn how to verify Freundlich isotherm.
4. Students will get knowledge about volumetric titrations.
Theory: Adsorption is phenomenon of higher concentration in the surface as
compared to bulk. The substance which adsorbs is called the adsorbent while the
one which gets adsorbed is called adsorbate.
A graph between the amount of substance adsorbed (adsorbate) per gram of
the adsorbent versus equilibrium concentration at the particular temperature is
known as adsorption isotherm. According to Freundlich isotherm:
x = k C1/n where x = weight of the adsorbed substance
m m = weight of the adsorbent
C = equilibrium concentration of the solute
The value of k and n depends upon the nature of solute, solvent and adsorbent.
Taking the log of the above equation:
log x/m = log k+ 1/n log C. It is an equation of the straight line between logx/m
vs. logC with slope 1/n and intercept log k.
Page 38
Slope = 1/n
Intercept= log k
Procedure:
 Take six clean and dry stoppered conical flasks and label them 1 to 6.
 Fill the flasks as given below:
Flask No. Volume of water (ml) Volume of acetic acid
(ml)
1 --- 50
2 10 40
3 20 30
4 30 20
 Stopper the flaks and shake the solutions thoroughly.
5 40 10
 Weigh 2g of activated charcoal each on six different glazed papers. Transfer
6 contents of one paper
the 50 each, to each of the conical ---
flasks without much
loss of time.
 Cork the flasks, shake them well and keep them at room temperature for 30-
40 minutes. As far possible, each flask should be shaken for equal time.
Page 39
 Filter the solutions in flasks separately but simultaneously. Reject the first 4-5
ml of the filtrate in each case and receive the rest in six other clean and
numbered flasks (or beakers).
 Now titrate 10ml of each filtered solution against 0.1 M NaOH using
phenolphthalein as indicator. Repeat the experiment to get a set of
concordant readings.
Observations:
Room temperature = -----oC
Mass of activated charcoal in each flask, m = 2g
Volume of acetic acid solution in each case = 10ml
Bottle Initial Final Volume of 0.1 Mean

No. reading reading M NaOH used Value
(ml)
(ml)
1 (i) V1
(ii)
2 (i) V2
(ii)
3 (i) V3
(ii)
4 (i) V4
(ii)
5 (i) V5
(ii)
6 (i) V6
(ii)
Calculation of equilibrium concentration, C:
Volume of 0.1N NaOH used for 10 ml of filtrate taken from bottle 1= V 1 ml
Applying normality equation,
N1 V1 = N2 V2
Page 40
(oxalic acid) (0.1N NaOH)
N1 X 10 = 0.1 V2
N1 = V2/100
i.e. equilibrium concentration in bottle 1 = V 2/100 g/litre
Equilibrium concentration (C) in bottles 2-6 can be calculated similarly.
Various observations and calculations may be tabulated as follows:
Flask Original conc. Equilibrium Amount of acetic

No. Of oxalic acid concentration acid adsorbed in
(Co) moles/litre
(C)
x=(Co-C)x50/1000 x/m logc logx/m
1 0.5 N 0.01V1
2 0.5x40/50 0.02 V2
=0.4N
3 0.5x30/50 0.03 V3
=0.3N
4 0.5x20/50 0.04 V4
=0.2N
5 0.5x10/50 0.05 V5
=0.1N
6 0.5x0/50 0.06 V6
=0
Plot of graph: To verify Freundlich isotherm, plot logx/m vs log C.
Page 41
A straight line is obtained which proves the validity of Freundlich isotherm.
Cautions:
1. Handle the apparatus carefully.
2. Alkali should be taken in the burette.
3. Cork the flask properly while shaking solutions.
Page 42
Some Common Apparatus used in Chemistry lab:
Burette with stand How to read the burette
Pipette with filler

Graduated Pipette
Page 43
Conical Flasks Measuring Cylinders
Droppers Beakers
Water bath
Spatula
Page 44

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LMCHE 102: Chemistry Lab

Some rules to be followed in the Lab:

1. Entry without lab coat in chemistry lab is strictly prohibited.

3. No group discussions are allowed in the lab.

4. Clean the apparatus as well slab after your experiment is finished.

6. Always bring the lab manuals with you.

7. Do not use laptop while performing the experiments.

8. Switch off electrical apparatus after their use.

9. Do not throw filter papers in sink, dispose all waste in dustbin.

2. Never try to smell the chemicals as it can be dangerous for you.

S.No Title of Experiment Page No.

Some important instruments in chemistry lab

Textbook: 1. J. Mendham, R. C. Denney, J. D. Barnes, and R. C. Denney, Vogel’s

Equipments to be used: Burette, Burette stand, Titration flask, Pipette, Beakers,

i. The purpose of this experiment is to determine the hardness of water by

HIn-2 + M+2 → MIn- + H+ {M = Mg or Ca}

H2Y2- + M+2 → MY-2 + 2H+

H2Y2- + MIn+ → MY-2 + HIn+2 + H+

(b) Determination of Total Hardness:-

1 ml of standard hard water = 1 mg of CaCO 3

10 ml of S.H.W. = 10 mg of CaCO3 = A ml of EDTA

1 ml of EDTA = 10/A mg of CaCO 3

(b).Calculation of total hardness:

10 ml of hard water sample = B ml of EDTA

Now 1 ml of EDTA = 10/A mg of CaCO3

10 ml of hard water sample = B x 10/A mg of CaCO 3.

1 ml of hard water sample = B x 10/A x 1/10 mg of CaCO3.

1000 ml of hard water sample = B x 10/A x 1/10 x 1000 mg of CaCO3.

Hence total hardness = 1000 x B/A ppm

Result: The hardness of water is...........

Error Analysis: %Error = (1 – observed value/actual value) x 100

Requirement for Lab Technician:

1. EDTA solution 0.1 M.

Title: Preparation of Sodium trioxalato ferrate(III)

CHEMICAL REQUIRED: Mohr’s Salt ((NH4)2SO4•FeSO4•6H2O), Sodium Oxalate,

(iii) How to use Buchner funnel and suction pump.

THEORY: Sodiumtrioxalatoferrate (III) is a coordination compound; with a

2Na3[Fe(C2O4)3]•3H2O →2FeC2O4•2H2O + 2CO2 + 3Na2C2O4 + 2H2O

Preparation of Ferrous Oxalate:

Buchner Funnel Buchner Funnel Hot Plate Weighing balance

Preparation of Sodium trioxalato ferrate(III):

 Weigh 3.5 g of Sodium oxalate (Na2C2O4•H2O) and put in 30 mL of warm

 Then store the solution in a dark cupboard for crystallization. After

RESULT: Color of the compound……….

Weight of the ppt. …………….

SCOPE OF THE RESULT: Gravimetric analysis is helpful in estimation of amount of

i. Stirring should be done very carefully wherever is mentioned in the procedure.

Requirements for Lab Technician:

1. Oxalic acid solution (5g/50mL)

6. Ferrous ammonium sulphate and sodium oxalate

EQUIPMENTS REQUIRED: Pipette, Burette, titration flask, eight washed empty

CHEMICAL REQUIRED: Benzene, Benzoic acid, water, NaOH, HCl,

LEARNING OBJECTIVE: In this experiment we will use the volumetric technique of

Distribution coefficient (D) is the ratio of concentrations of a compound in the two

The total concentrations of benzoic acid in water and benzene, CW and Cb

A. Preparation of the benzene/benzoic acid/water mixtures:

Separating Funnel. Setup of Separating Funnels and reagent bottles

B. Titration of the benzene layer

C. Titration of the aqueous layer

OBSERVATIONS AND CALCULATION:

(benzoic acid) (NaOH)

Concentration of Benzoic acid in organic layer Cb: