SANJEEV AGRAWAL GLOBAL EDUCATIONAL (SAGE) UNIVERSITY, BHOPAL

“SCHOOL OF SCIENCE”

SAGE University, Bhopal

School of Sciences
M. Sc. Chemistry

Laboratory Manual
1st Semester
Course Code: CH20M108

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List of Instruments in Chemistry Lab:

1. Digital Stirrer
2. Digital Balance
3. Digital pH Meter
4. Digital Potentiometer
5. Digital Conductometer
6. Melting Point Apparatus
7. UV- Visible Spectrophotometer
8. Hot Air Oven
9. Water Bath
[Link] Chamber
[Link] Evaporator with chiller and vacuum pump
[Link] distillation Assembly
[Link] Viscometer-I
[Link] Viscometer-II
[Link] Open Cup Apparatus
[Link] Martens Closed Cup Apparatus
17. Column Chromatography Setup
[Link] Setup
[Link] Setup
[Link] Setup
[Link] Pump

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Chemistry Lab Do’s and Don’ts

The chemistry laboratory must be a safe place in which to work and learn about chemistry. Most
of these involve just using common sense.

1. Wear chemical splash goggles at all times while you are in the laboratory.
2. Wear a chemical-resistant apron.
3. Be familiar with your lab assignment before you come to lab. Follow all written and
verbal instructions carefully. Observe the safety alerts in the laboratory. If you do not
understand a direction or part of a procedure, ask the teacher before proceeding.
4. When entering the lab/classroom, do not touch any equipment, chemicals, or other
materials without being instructed to do so. Perform only those experiments authorized
by the instructor.
5. No student may work in the lab without an instructor present. Work only with your lab
partner(s). Do not venture to other lab stations for any reason.
6. Do not wear bulky or dangling clothing.
7. Never eat or drink in the laboratory.
8. Wash acid, base, or any chemical spill off of yourself immediately with large amounts of
water. Notify your teacher about the spill.
9. Clean up spills immediately. If you spill a very reactive substance such as an acid or base,
tell the people in the area and obtain assistance from your teacher. Acid spills should be
neutralized with baking soda, base spills with vinegar before cleaning them up.
10. If chemical substances get in your eye, wash the eye out for 15 minutes with cold water.
Hold your eye open with your fingers while washing it.
11. If you take more of a chemical substance from a container than you need, you should not
return the excess to the container. This might cause contamination of the substance
remaining. Dispose of the excess as your teacher directs.

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12. Never smell anything in the laboratory unless your teacher tells you it is safe. Do not
smell substance by putting your nose directly over the container and inhaling.
13. Do not directly touch any chemical with your hands. Never taste materials in the
laboratory. 14. If you burn yourself with a hot object, immediately put the burnt area
under cold water for 15 minutes. Inform your teacher.
14. Observe good housekeeping practices. Work areas should be kept clean and tidy at all
times. Only lab notebooks or lab handouts should be out on the table while performing an
Experiment. Books, bags should not be on the lab table. Passageways need to be clear at
all times.
15. Always replace lid of bottles and jars.
16. If your Bunsen burner goes out, turn off the gas immediately.
17. Always add acid to water and stir the solution while adding the acid. Never add water to
an acid.
18. Report all accidents to your teacher.
19. Absolutely no running, practical jokes, or horseplay is allowed in the Laboratory.
20. Thoroughly clean your laboratory work space at the end of the laboratory session, Make
sure that all equipment is clean, and returned to itsoriginal Place.
21. Wash your hands before leaving the lab.

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LABORATORY SAFETY
Laboratory instructors are required to see that students know and follow established safety rules,
have access to and know how to use appropriate emergency equipment, and are aware of hazards
of hazards associated with specific experiments. The lab instructor alone cannot prevent
laboratory accidents, however. You also have a responsibility to follow safe laboratory practices
while performing experiments and to be ready to respond in case of accident.

Protecting yourself

Just as construction workers protect themselves from accidents by wearing hard hats and steel-
toed boots, people who work with chemicals should wear appropriate clothing and personal
protective equipment (such as safety goggles) that reduce the likelihood of injury in case of an
accident.

Eye protection is essential at all times and it should be the rule in every chemistry laboratory.
Safety glasses provide only limited protection because they have no side shields, so it is best to
wear safety goggles that protect your eyes from chemical splashes and flying particles from any
direction.

In any chemistry lab, you should wear clothing that is substantial enough and covers enough of
your body to offer some protection against accidental chemical spills and flying glass or other
particles. Long-sleeved shirts or blouses and long pants or dresses are recommended, especially
when they are made of denim or other heavy materials . Some synthetic fabrics can be dissolved
by chemicals such as acetone and could melt in contact with a flame or another heat source.
Wear shoes that protect you from spilled chemicals and broken glass – not open sandals or cloth-
topped athletic shoes.

Always wear appropriate gloves when handling caustic chemicals, which can burn the skin, or
toxic chemicals that can be absorbed through the skin. No single type of glove protects against
all chemicals, but neoprene gloves offer good to excellent protection against many commonly
used chemicals, and disposable nitrile gloves are adequate for use in most undergraduate labs.
Latex gloves aren't recommended, because some people are allergic to latex because they are
permeable to many hazardous chemicals.

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Preventing laboratory accidents

Most organic lab courses are completed without incident, apart from minor cuts or burns, and
serious accidents are rare. Nevertheless, the potential for a serious accident always exists. To
reduce the likelihood of an accident, you must learn the following safety rules and observe them
at all times. Additional safety rules or revisions of these rules may be provided by your
instructor.
1. Wear approved eye protection in the laboratory at all times. Even when you aren't working
with hazardous materials another student's actions could endanger your eyes, so never
remove your safety goggles or safety glasses until you leave the lab. Do not wear contact
lenses in the laboratory because chemicals splashed into an eye may get underneath a contact
lens and cause damage before the lens can be removed. Determine the location of the
eyewash fountain nearest to you during the first laboratory session, and learn how to use it.
2. Never smoke in the laboratory or use open flames in operations that involve lowboiling
flammable solvents. Anyone found smoking in an organic chemistry laboratory is subject to
immediate expulsion. Before you light a burner or even strike a match, inform your
neighbors of your intention to use a flame. If anyone nearby is using flammable solvents,
either wait until he or she is finished or move to a safer location, such as a fumehood. Diethyl
ether and petroleum ether are extremely flammable, but other common solvents, such as
acetone and ethanol, can be dangerous as well. When ventilation is inadequate, the vapors of
diethyl ether and other highly volatile liquids can travel a long way; lighting a burner at one
end of a lab bench that has an open bottle of ether at its other end has been known to start an
ether fire. Learn the location and operation of the fire extinguishers, fire blankets, and safety
showers at the first laboratory session.
3. Consider all chemicals to be hazardous and minimize your exposure to them. Never taste
chemicals, do not inhale the vapors of volatile chemicals or the dust of finely divided solids,
and prevent contact between chemicals and your skin, eyes and clothing. Many chemicals
can cause poisoning by ingestion, inhalation, or absorption through the skin. Strong acids and
bases, bromine, thionyl chloride, and other corrosive materials can produce severe burns and
require special precautions, such as wearing gloves and labcoats. Some chemicals cause
severe allergic reactions, and others may be carcinogenic (tending to cause cancer) or
teratogenic (tending to cause birth defects) by inhalation, ingestion (swallowing) or skin
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absorption. To prevent accidental ingestion of toxic chemicals, don't bring food or drink into
the laboratory or use mouth suction for pipettng, and wash your hands thoroughly after
handling any chemical. To prevent inhalation of toxic or carcinogenic chemicals, work
under an efficient fume hood or use a gas trap to keep chemical fumes out of the laboratory
atmosphere. To prevent contact with corrosive or toxic chemicals, wear appropriate gloves
and a labcoat. Clean up chemical spills immediately – use a neutralizing agent a plenty of
water for acids and bases, and an absorbent for solvents. In case of a major spill, or if the
chemical spilled is very corrosive or toxic, notify your instructor before you try to clean it up.
4. Exercice great care when working with glass and when inserting or removing
thermometers and glass tubing. Among the most common injuries in a chemistry lab are
cuts from broken glass and burns from touching hot glass. Protect your hands with gloves or
a towel when inserting glass tubes or thermometers into stoppers or thermometer adapaters,
and when removing them. Grasp the glass close to the stopper or thermometer adapter and
gently twist it in or out.
5. Wear appropriate clothing in the laboratory. Wear clothing that is substantial enough to
offer some protection against accidental chemical spills, and shoes that can protect you from
spilled chemicals and broken glass. Human hair is very flammable, to tie up your hair or
wear a hair net while using a burner if you have long hair.
6. Dispose of chemicals properly. For reasons of safety and environmental protection, most
organic chemicals shouldn't be washed down the drain. Except when your instructor or an
experiment's directions indicate otherwise, place used organic chemicals and solutions in
designated waste containers. Some aqueous solutions can be safely poured down the drain,
but consult your instructor if there is any question about the best method for disposing of a
particular chemical or solution.
7. Never work alone in the laboratory or perform unauthorized experiments. If you wish to
work in the laboratory when no formal lab period is scheduled, you must obtain permission
from the instructor and be certain that others will be present while you are working.

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List of Experiment:

Inorganic Chemistry Practical

1. Preparation of [Ni(NH3)6]Cl2 and [Ni(en)3]Cl₂

2. UV-vis spectroscopy of [Ni(H2O)6]Cl2, [Ni(NH₃)₆]Cl₂, and [Ni(en)3]Cl₂ : Analysis of ligand field
strength
3. Demonstration of cis-trans isomerisation in Cobalt(III) complexes
4. Chemistry of a five-coordinate d1 complex: case of vanadyl acetylacetonate, VO(acac)2

Physical Chemistry Practical (any 4 experiments)

1. Conductometric titration of a weak acid with strong base.

2. Conductometric titration of a mixture of weak and strong acids.
3. Potentiometric titration of a strong acid with strong base using quinhydrone electrode.
4. Conductometric titration of KCl with AgNO3.
5. Degree of hydrolysis of urea hydrochloride by kinetics method.
6. Equilibrium constant of KI + I2 ⇌ KI3 by distribution method.

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Inorganic Chemistry Practical

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Experiment-1
Aim: To Preparation of [Ni(en)3]Cl2. 2H2O, [Ni(NH3)6]Cl2 and [Ni(en)2]Cl2.2H2O.

Apparatus: Beaker ( 100 mLx2)( 50 mLx2) (25 mLx1),measuring cylinder (10 mL&50 mL), ice
bath, dropper, glassrod,Buchner funnel, filtration flask,conical flask (100 mLx2), magnetic
bar,spatula,graduatedpipette,glass funnel, test tubes,test tube stand,G4 crucible, sample vial( 3
Nos.), volumetric flask ( 10 mLx3 ),gloves.

Chemical: NiCl2, 6H2O, ethylenediamine, methanol, acetone, ethanol, concentratedNH4OH.

Theory: The term coordination chemistry is generally applied to transition metal complexes.

However, the term “coordination compound” can be extended to any LewisAcid-Base complex
and thus to the vast majority of compounds known in inorganicchemistry. As applied to the
transition metals, coordination compounds are among themost extensively investigated areas in
the field of inorganic chemistry; and in fact, the first inorganic chemist to win a Nobel Prize,
Alfred Werner, won the prize for work oncoordination compounds. These compounds exhibit
extensive and interesting spectraland magnetic properties in addition to widely varying structures
and stoichiometries. Inthis experiment you will prepare several nickel salts and determine the
spectrochemicalordering of several ligands using visible spectroscopy. Magnetic measurements
will bemade which will aid in the determination of their structure.

Procedure:

The preparation of [Ni(en)3]Cl2. 2H2O. Dissolve 6.0g of NiCl2 .6H2O in3mL of H2O in 100 mL
beaker. A little warming improves the rate of dissolution. Cool thesolution in ice while adding
5.0g (5.6 mL) of ethylenediamine. Add theethylenediamine slowly because the reaction is quite
exothermic. Cool. Add10 mL of cold ethanol to initiate crystallization. Keep cold for 10 min.
Thecollect the product on a Büchner funnel and wash with three3 mL portions ofethanol. Dry in
air. Record the yield.

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b. The preparation of [Ni(NH3)6]Cl2. Dissolve 3.0g of NiCl2.6H2O in 5 mLof warm H2O in a

100 mL Erlenmeyer flask and add 5.8mL of concentratedNH 4OH. Cool with an ice bath and
observe the precipitation of large violetcrystals. Add 10 mL of cold ethanol to complete the
precipitation. Collect thecrystals on a Büchner funnel and wash with three3 mL portions of
[Link] in air. Record the yield.

c. The preparation of [Ni(en)2]Cl2.2H2O. 1.25 g of NiCl2.6H2O and 3.02 gof [Ni(en)3]Cl2.2H2O

are gently warm( in 100 mL beaker on Mag. Stirrer) in a mixture of 22 mL of methanoland 1.0
mL of H2O for five minutes. Keep the solution hot and gravity filterinto a 100 mL conical. Rinse
the flask twice with 1.5 mL of hot methanol. Inorder to initiate crystallization cool the blue
solution on ice seed crystals areobtained by the following method: Take 1 mL of the cold
solution in a testtube and add 1 or 2 mL of acetone dropwise. Scratch by glass rod or shake until
crystalsform. The separation of two layers indicated too much acetone was [Link] the bulk
chilled solution. Add 10 mL of acetone dropwise for about twominutes. Add 5 mL of acetone
and an occasional seed [Link] the seed crystals no longer dissolve add all of the seed
[Link] to stir for about 10 min. Collect the blue crystals using a sintered glass filter.
Wash twice with 2-5 mL ofacetone and allow to dry, record the yield.

Result: -
Yield of compound (1)------------------ gm.
Yield of compound (2)------------------ gm.
Yield of compound (3)------------------ gm.

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Experiment-2
Aim: Characterization of [Ni(en)3]Cl2. 2H2O, [Ni(NH3)6]Cl2 and [Ni(en)2]Cl2.2H2O by using
UV-vis spectroscopy.

Apparatus: Beaker, UV-vis spectrophotometer.

Chemical: Hexaminenickel(II) chloride 0.1 Min50% NH4OH, bis- and tris-

ethylenediaminenickel(II) chloride 0.1 M in H2O, Nickel(II) chloride hexahydrate0.1 M in H2O.

Procedure:
From these data you shoulddetermine the energy of the three transitions and the spectrochemical
orderingof the ligands NH3, H2O, and en. (See textbookfor adiscussion on Crystal/LigandField
Theory).The magnetic susceptibilities of each compound will be measured usingthe Johnson and
Matthey susceptibility balance.[Ni(en)2]Cl2 appears to be a 4- coordinate Ni(II) complex
(tetrahedral orsquare planar?) although it could be octahedral wih the two chloride ions inthe
coordination sphere. Show how the magnetic data might permit you toeliminate some of the
structural possibilities. Is the structure uniquely definedby the magnetic moment in this case?
Why or why not?

Discussion:

Result:

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Experiment-3
Aim: Demonstration of cis-trans isomerisation in Cobalt (III) complexes.

Apparatus: Beaker ( 100mlx2, 50 ml,250 mlx1), measuring cylinder ( 10 mLx1),graduated

pipette 5mL,spatula,glassrod,dropper, magnetic bead, ice bath, thermometer, water bath,
Buchner funnel, test tube( 2 nos.), test tube stand, filtration flask, volumetric flask ( 10 ml x2).

Chemicals: CoCl2.6H2O, 1, 2-diaminoethane, H2O2 (30%), Conc. HCl, Ethanol, Methanol,

Litmus paper.

Procedure:

(a) Preparation of Trans-Dichlorobis(ethylenediamine)cobalt(III) chloride, trans-

[CoCl2(en)2]Cl

CoCl2.6H2O (4 g) is dissolved in 4 cm3 of water in a 100 mL beaker and 2 cm 3 of 1,2-

diaminoethane (ethylenediamine, en) in 4 cm 3 ofwater is slowly added cautiously( dropwise) and
with stirring. The solution is cooled in an ice bath to 5°C( for 5 min.) and 4 cm 3 ofH2O2 (30%) is
slowly added (dropwise) while maintaining the temperature at 5°C. [CAUTION: Keep H2O2 off
theskin and eyes!]. Then the solution is gently warmed to about 60-70°C for 15-20
[Link] HCl (4 mL) is then added slowly with stirring and the solution evaporated
on a steam bath with occasional stirringto about 1/3 of volume( it will take more than 30
minutes). After cooling the solution in an ice-bath, 3 mL of ethanol is added and the mixture
cooledfor a further 20 minutes ( wait for some time at room temp.). The resultant green crystals
of trans-[CoCl2 (en)2][Link].2H2O are filtered onto asintered glass Buchner funnel, washed with
ethanol and sucked dry.

To drive off the HCl of crystallization, place the dark green crystals in a small beaker containing
5 cm3 ofmethanol and vigorously stir these with a glass stirring rod. Transfer the resultant slurry
to a large test [Link] the test tube in a 250 mL beaker of water, then heat the water ( gently at
first) until the methanol has evaporatedand no more HCl gas is driven off. (The presence of HCl
can be tested by holding a piece of moist litmuspaper at the mouth of the test tube).Boiling for 15

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minutes after the methanol has evaporated is usually sufficient. Trans-[CoCl2(en)2]Cl

thusobtained is a light green powder.

(b) Synthesis of Cis-Dichlorobis(ethylenediamine)cobalt(III) Chloride,[cis-CoCl2(en)2]Cl

Once characterization on the trans isomer is complete, place the trans isomer in a 25 mL beaker
and dissolve it in 3.0 mL of water. Heat the green solution carefully on a magnetic stirrer to
evaporate the water without violently boiling the solution. As the solution evaporates, a deep
violet sample of the cis isomer will form. Heat the mixture to dryness and isolate the sample of
[cis-Co(en)2Cl2]Cl for characterization.

Another method: Take about half of the trans isomer obtained previously, dissolve it in the
minimum volume of hot water and evaporate the solution to about one-sixth of the original
volume on a water bath with stirring. Cool the product, then filter off the purple crystals, wash
with a small amount of ethanol and air-dry.

Characterization by UV: Prepare 0.1 M solution of both isomers in 10 ml distilled water.

Result:
1. Yield of trans isomer is equal to ------------------ gm.
2. Yield of cis isomer is equal to ------------------ gm.

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Experiment-4
Aim: Chemistry of a five-coordinate d1 complex: case of vanadyl acetylacetonate,
VO(acac)2.
Apparatus: Conical flask (100mL,250 mL), beaker ( 100 mLx2,50 mLx2), Buchner funnel,
filtration flask, magnetic bar, water bath, glass rod, sample vial (2 no.), glass funnel, spatula,
heater, graduated pipette ( 10 mL), measuring cylinder ( 10 mL), dropper.

Chemicals: Vanadium (V) oxide, conc. H2SO4, ethanol, acetyl acetone, sodium carbonate,
chloroform, diethyl ether, pyridine, DCM.

Procedure:
(a) Preparation of Bis(acetylacetonato)oxovanadium (IV), VO(acac)2.
To 2.5 g of pure vanadium(V) oxide in a 100 mL Erlenmeyer flask are added 6 mL
distilledwater, 4.5 mL concentrated sulfuric acid ( in fume hood) and 12.5 mL of 95% ethanol.
The mixture isheated to boiling on a steam or boiling-water bath and stirred. As the reaction
proceedsthe initial slurry of vanadium(V) oxide darkens, becomes light green and finally
turnsdark blue. The reduction of vanadium(V) is completed in 45 minutes. 10 mL of water
isaddded, and the solution is filtered by gravity and the filtrate is collected in a 250 mLconical
flask . 6.5 mL of acetylacetone (2,4-pentanedione) is added and the solution is stirredfor 10
minutes. The solution is neutralized by adding a solution of 10 g of sodium carbonate dissolved
in 60 mL of water slowly( by dropper) with continuous stirring to avoid excessivefrothing. The
precipitated product is collected by filtration on a Büchner funnel and driedby drawing air
through it.
Recrystallize the 2 g product by dissolving in the minimum amount of hot chloroform (about4
mL) in a 50 mL beaker, filtering hot by gravity through fluted filter-paper,cooling to room
temperature and adding 10 mL of diethyl ether to complete theprecipitation( wait for 10 minute).
Filter and allow drying in air.

(b) Spectroscopic study of adduct formation in [VO(acac)2]

*The operation below must be carried out in the fume cupboard.

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Prepare 0.025 M solutions (note down the actual concentrations to calculate epsilon values later
on) of[VO(acac)2] in the following solvents: (1) CH 2Cl2 (2) pyridine. Obtain thevisible spectra
of these solutions in the range 350-800 nm.
NOTE: Pyridine is highly toxic and is known to cause sterility in laboratory animals.

(c) Preparation of Pyridine Adduct.

*The operation below must be carried out in the fume cupboard.
Place about 20 mg of your [VO(acac)2] complex in the centre of a watch glass. In a FUME
HOOD, wet the solid with about 3 drops of pyridine, mixing the solid and theliquid with a glass
rod. Note the colour change. Put the watch-glass on the electric hot-plate in the fume hood and
leave it for a few minutes until the excess pyridine has evaporated. The product is the pyridine
adduct [VO(acac)2(NC5H5)]. Do not leave the dry solid on the hot-plate or the complexed
pyridine will slowly dissociate to reform the starting material. Cool to room temperature and
store it in a vial to record IR spectrum later.

(d) Infrared spectra.

Determine the infra-red absorption spectra of the complex and its pyridine adduct as outlined
below and compare the two. The band occurring at 995 cm -1 in the spectrum of the complex has
been identified as a V=O stretching mode. Determine the amount by which this band has shifted
in the spectrum of the complex and suggest the reason for this shift. Are there any other
differences between the two spectra?

Preparation of the Sample for Recording the Infra-Red Spectrum

Make sure that the compound to be investigated has been thoroughly dried.

Grind a small amount (about 10-20 mg) of sample with dry KBr in an agate mortar and
[Link] pallet by hydraulic press machine and record spectra.

Result:
1. Yield of complex is equal to ------------------ gm.

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Physical Chemistry Practical

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Experiment-1
Aim: To estimate the amount of Acetic acid present in the given solution by conductometric
titration. (Conductometric titration of a mixture of weak and strong acids)

Apparatus:-Conductivity cell, conductivity mete, beaker (100ml), burette (50ml), glass rod

Chemicals: - Acetic acid (0.1M) - 40ml, NaOH solution (0.5M).

Principle:-
In this experiment, acetic acid is a weak acid. When it is titrated with a strong base like NaOH,
initially the conductance is low due to the feeble ionization of acetic acid. On the addition of
base, there is decrease in conductance not only due to the replacement of H + by Na+ but also
suppresses the dissociation of acetic acid due to common ion acetate. But very soon, the
conductance increases on adding NaOH as NaOH neutralizes the un-dissociated CH 3COOH to
CH3COONa which is the strong electrolyte. This increase in conductance continues raise up to
the equivalence point. The graph near the equivalence point is curved due the hydrolysis of salt
CH3COONa. Beyond the equivalence point, conductance increases more rapidly with the
addition of NaOH due to the highly conducting OH − ions. You will get a titration curve which is
shown below. The point of intersection of the two lines gives the point of neutralization i.e.
equivalence point.

Procedure:-
Clean the burette and fill with standard NaOH solution. Take 40 ml of given CH 3COOH solution
in a 100 ml beaker and dip the conductivity cell in it and measure the conductance initially. Now
add NaOH solution from burette, drop wise i.e., 1 ml for each of the addition, after each addition,
stir the solution and note down the change in conductance. The measured conductance are
recorded and 20 readings are tabulated in the table. Plot the graph between conductivity and
volume of NaOH added. Where the intersection of two straight lines gives the end point.
Calculate the strength of given CH3COOH from unknown strength of NaOH solution.

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Observation Table:
[Link] Volume of NaOH in ml Observed conductance of CH3COOH
1 0
2 1
3 2
4 3
5 4

Graph:
Plot a graph by taking volume of NaOH on x-axis and conductance of the solution on y-axis.
Two straight lines intersecting at a point is obtained. The intersection point corresponds to
volume of NaOH required for the neutralization of weak acid.

M1= Molarity of NaOH = 0.5M

M2 = Molarity of CH3COOH soln =_____M
V1= Vol of NaOH consumed = ____ ml (graph)
V2 = Vol of CH3COOH taken in beaker = ____ml

M1V1=M2V2
M2 = M1V1/V2

Result:-
[Link] end point = -------------ml
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2. The Molarity or Concentration of CH3COOH =-------M

Experiment-2
Aim: To find the concentration of HCl by titrating it against standard NaOH solution
Potentiometrically.

Apparatus: - Potentiometer, Pt electrode, Saturated calomel electrode, 100ml beaker, 50ml

Burette, Glass rod.
Chemicals: - Standard 0.5M NaOH solution, HCl solution – 40ml, Quinhydrone powder.

Principle: - A galvanic cell is a device which converts chemical energy to electrical energy. It
consists of 2 electrodes and the potential difference between 2 electrodes is called emf of the
cell. This can be measured by an instrument called potentiometer. EMF of the given cell is given
by
Ecell = Eoxi + Ered

The Nernst equation for the electrode potential of an electrode is given by

M Mn+ + ne–

R= gas constant.
F= Faraday current in coloumbs
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In potentiometric titration an electrode whose potential depends on the concentration of the ion
being titrated is useful by measuring its potential by using Quinhydrone electrode. The
concentration of H+ ions is measured by Quinhydrone which is an equimolar mixture of Quinone
and hydroquinone.
Q + 2H+ +2e- QH2

Here Q= Quinone,
QH2= Hydroquinone.
This electrode is also called as Indicator electrode.
ESCE= 0.2422v.

Procedure:-

Take 40 ml of HCl solution in a 100 ml beaker. Add a pinch of Quinhydrone [Link] the
platinum electrode in the solution along with saturated calomel electrode. These are connected to
the potentiometer. Fill the burette with standard NaOH (0.5M) from the burette into the beaker
containing HCl and stir the reaction mixture. Note down the emf values. Repeat the titration up
to17-20 readings.

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Tabular column:

[Link] Volume of NaOH emf(Volts) ∆E ∆V ∆E/∆V

1
2
3
4
5
6

Graph
Plot a graph by taking cell EMF on y-axis and volume of NaOH on x- axis. A curve showing
inflexion at the equivalence point is [Link] graph gives an inverted ‘S’ shaped curve.
Plot another graph by taking ΔE/ΔV on y-axis and volume of NaOH on xaxisgives inverted ‘V’
shaped curve..

Calculations and observations: -

The end point of titer value from graph is= -----ml.

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“SCHOOL OF SCIENCE”

The strength of acid is calculated M1V1 = M2V2

M1= Molarity of NaOH =0.5M

M2 = Molarity of HClsoln =_____M

V1= Volume of NaOH consumed = __ ml (graph)

V2 = Volume of HCl taken in beaker = ____ml

M2 = M1V1/V2

Result:-

 End point of the reaction from the graph = --------ml

 Molarity of HCl = ------M.

 Strength of HCl = M×36.5

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[Link] Chemistry Lab manual
 SANJEEV AGRAWAL GLOBAL EDUCATIONAL (SAGE) UNIVERSITY, BHOPAL

“SCHOOL OF SCIENCE”

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[Link] Chemistry Lab manual