Dr. M.

A Kazi Institute of Chemistry, University of Sindh, Jamshoro

Analytical Chemistry
Practical Scheme
For
B.S Part-III & M.Sc. (Prev.)
Course No. 507-507P

1
 GENERAL GUIDLINES

Before coming to the laboratory session, you should be aware of CHEMISTRY LABORATORY
SAFETY RULES and should be comprehensively familiar with the experiment.

1. Chemistry Laboratory safety Rules

 Protect Your Eyes

 Wear appropriate protective clothing
o Your clothing should cover your legs to the knees – shorts are not appropriate for
the Laboratory
 Lab aprons can be used to protect good clothing
o Loose clothing should not be worn because it may dip into chemicals or fall into a
flame and catch fire
 Wear shoes that cover your feet.
o Sandals and open-toed shoes do not protect your feet from broken glass that is
frequently found in the lab
 Do not apply cosmetics, eat, or drink in the lab
o These activities are ways by which you can accidentally ingest harmful chemicals
 Do not taste any chemical!
 Pour from large containers to smaller ones.
 Always ADD ACID to water
 Hold your hand over the label while pouring
 Work with volatile chemicals under a fume hood
 Check glassware for cracks.
 Heat test tubes at an angle
 Handle hot glassware with gloves or beaker tongs.
 First light the match then turn on the gas
 Do not smell any chemicals directly!
o Smell chemicals only if your teacher specifically tells you to do so, then use your
hand to fan the vapor to your nose.
 Do not pipet solutions by mouth!
o Use a rubber suction bulb or other device to fill a pipet.
o Wash your hands with soap and water before leaving
o This rule applies even if you have been wearing gloves!
 Know the hazards of the materials being used.
o Read and reread labels carefully to make sure that you are using the right chemical.
 Tie Back Loose Hair
o Dangling hair can fall into the Bunsen burner and catch fire or can fall into a
chemical solution
 Know the safety equipment and know how to use it.
o Eye wash fountain
o Safety shower
o Fire extinguisher
 Carry out only the experiments assigned by your teacher
 Never remove chemicals from the laboratory

2
  Never work alone in the lab
o In case of a problem, you may need another person to prevent injury or even save
your life!
 Remember that the lab is a place for serious work!
o Careless behavior may endanger yourself and others and will not be tolerated
 Demonstrate safe behavior
o Obey all safety instructions given by your teacher or found in you experimental
procedure.
o Clean up spills immediately; IF you know how. If you are uncertain how to clean
up a spill or if a large spill occurs, notify your teacher immediately
 Before leaving the lab:
o Return equipment and chemicals to their proper places
o Be sure to replace the lids to all containers
o Clean up your work area
 Know how to dispose of waste
o Dispose of all waste materials according to your instructional procedure or your
teacher’s instructions
 Report any accidents or unsafe conditions immediately!

2. Guidelines regarding preparation of Laboratory report:

Lab report is to be prepared for each experiment you perform. Follow the guidelines
mentioned below.

1. Title: Write down the title of the experiment that was performed.
2. Procedure: In paragraph form, give a brief synopsis of the process (Optional)
3. Data & Calculations: Use tables and graphs. Label them carefully and clearly, making
sure that the units are included.
4. Result & Discussion: Report the results. Discus in your own words the outcome of
your experiment.
5. Conclusion: Summarize your results and include comments on possible sources of error.

Prepared By:
Aijaz Ahmed Bhutto
Assistant Professor

3
 PART 01
CALIBRATION OF VOLUME MEASURING GLASSWARE

EXPERIMENT 01

CALIBRATION OF VOLUMETRIC PIPETTS AND TO ESTIMATE THE

MAGNITUDE OF ERROR ASSOCIATED WITH MEASUREMENT

CHEMICALS AND GLASSWARE

1. Analytical balance
2. Distilled water
3. Pippete
4. Thermometer
5. Pippete filler

PROCEDURE

Volumetric pipets (also called transfer) are calibrated to deliver a specific volume of water.
They are allowed to drain freely, and the last drop is not blown out.

1. Obtain 5 and 10ml volumetric pipets from your lab assistant. Inspect the tips—if you see a
flaw, bring the pipet to your lab assistant for evaluation.
2. Clean your pipets, using soap and water until they drain without leaving any droplets
behind, other than the usual volume left in the tip.
3. Tare a 50 mL beaker or flask.
4. Pipet 5.00 mL deionized (DI) water into the flask and determines the mass of water added.
5. Measure the temperature of the water and use the table to determine the density of water at
that particular temperature.
6. Using density formula determine the exact volume delivered by the pipette

4
OBSERVATION

S.No Volume Mass Mean mass Standard

deviation

1 5 mL

2 10 mL

After determining the mean mass we can convert this mass into volume delivered by the pipet by
using this density formula.

Density of water can be determined at particular temperature as shown in table,

D=M
V
So
V= M
D
This is an actual volume taken through the pipette.

ERROR = Volume of the pipet - Actual volume taken by pipet

RESULTS

Mention the results by using following formula.

ERROR = Volume of the pipet - Actual volume taken by pipet

DISCUSSION
Discuss the source of error in the results

5
 EXPERIMENT 02

CALIBRATION OF THE BURETTE

CHEMICALS AND GLASSWARE

1. Analytical balance
2. Distilled water
3. Pippete
4. Thermometer
5. Pippete filler

PROCEDURE

1. Obtain and clean a burette. Set it up and fill it with water.

2. Tare a clean 50-mL beaker.
3. Create a table in your lab notebook to record the reading of the burette and mass of water
dispensed.
4. Record the initial reading on the burette. You can generally estimate between graduations.
5. Drain out 5.00 mL deionized (DI) water into the tared beaker and determines the mass of
water added.
6. Take 10 readings over the entire range (0-50 mL, approximately every 5mL) of the burette.
7. Using density formula determine the exact volume delivered by the pipette

OBSERVATION

S.NO Initial Final Difference Mass of Mean Standard

Reading Reading of Volume Transferred Liquid Mass Deviation
1
2
3
4
5
6
7
8
9
10

6
After determining the mean mass we can convert this mass into volume delivered by the burette
using the density formula.

D=M
V
So
V= M
D

This is an actual volume taken through the pipette.

ERROR = Volume of the pipet - Actual volume taken by pipet

RESULTS

Mention the results by using following formula.

ERROR = Volume of the Burette - Actual volume taken by Burette

DISCUSSION
Discuss the source of error in the results.

7
 PART 02
ESTIMATION OF AMOUNT OF IONS THROUGH
PRECIPITATION

Types of Gravimetric Methods of Analysis

Gravimetric Methods of Analysis are of following types

 Particulate gravimetry
 Precipitation gravimetry
 Volatilization gravimetry
 Electrogravimetry

In particulate gravimetry the analyte is

determined following its removal from the sample matrix Particulate gravimetry:
by filtration or extraction. The determination of A gravimetric method in which
suspended solids from water released from a sewage- the mass of a particulate analyte
treatment facility is one example of particulate
gravimetry. is determined following its
separation from its matrix.
When the signal is the mass of a precipitate, we
call the method precipitation gravimetry. The indirect
determination of PO33– by precipitating Hg2Cl2 is a Precipitation gravimetry:
representative example as phosphite, PO33–, reduces Hg2+ A gravimetric method in which
to Hg22+, so in the presence of Cl– a solid precipitate of the signal is the mass of a
Hg2Cl2 forms. The direct determination of Cl– by precipitate.
precipitating AgCl is the example of direct determination
of precipitate.
When thermal or chemical energy is used to Volatilization gravimetry:
remove a volatile species, we call the method A gravimetric method in which
volatilization gravimetry. In determining the moisture the loss of a volatile species
content of food, thermal energy vaporizes the H2O. The gives rise to the signal.
amount of carbon in an organic compound may be
determined by using the chemical energy of combustion to convert C to CO2.
Finally, in electrogravimetry the analyte is Electrogravimetry:
deposited as a solid film on one electrode in an A gravimetric method in which
electrochemical cell. The oxidation of Pb2+ and its the signal is the mass of an
deposition as PbO2 on a Pt anode is one example of electrodeposit on the cathode or
electrogravimetry. Reduction also may be used in anode in an electrochemical cell.
electrogravimetry. The electrodeposition of Cu on a Pt
cathode, for example, provides a direct analysis for Cu2+.

8
 Precipitation Gravimetry

In the majority of cases; gravimetric methods rely on the use of precipitation reactions. The
quantitative determination of a substance by the precipitation method of gravimetric analysis
involves isolation of an ion in solution by a precipitation reaction (which causes the formation of
insoluble compound following the addition of precipitating reagent called “precipitant”). Once the
precipitates are formed; these are filtered, washed to make them free from contaminants, converted
to a product of known composition and finally weighed to determine its mass by difference. From
the mass and known composition of the precipitate, the amount of the original ion can be
determined.

Many metallic elements in their ionic forms react with negative counter ions to produce
stable precipitates. Silver ions form stable and highly insoluble salts with chloride, bromide or
iodide.

Determination of Calcium form natural water involves the formation of precipitates with oxalate
ion

Barium precipitates quantitatively as the sulfate. The reactions often follow the same patterns i.e.
positive and negative ions in an aqueous solution produce highly insoluble precipitates with certain
added reagents.
Most precipitation gravimetric methods were developed in the nineteenth century as a means
for analyzing ores. Many of these methods continue to serve as standard methods of analysis.

Procedure to carry out precipitation

1. Weigh the sample to be analysed.

2. Dissolve the sample in a suitable solvent, eg, water.
3. Add an excess of the precipiating agent to the solution to precipitate the analyte.
4. Heat the solution on a hot plate to increase the particle size for easier filtering (optional). This is
usually referred to as digestion.
5. Filter the mixture to separate the precipitate from the solution. It is important that the precipitate is
quantitatively transferred to the filter. If any remains in the beaker, the mass obtained will be
inaccurate.
6. Wash the precipitate to remove any impurities and dry by heating to remove water.
7. Cool the precipitate in a dessicator to prevent the precipitate absorbing moisture from the air.
8. Weigh the cooled precipitate.
9. Repeat the drying and weighing process until a constant mass for the precipitate is achieved.
10. Calculate the percent by mass of analyte in the sample.

9
Properties of Precipitates and Precipitants

Precipitates

1. Must be in the state so that readily filtered and washed free of contaminants.
2. Of sufficiently low solubility so that no significant loss of the analyte occurs during
filtration and washing.
3. Unreactive with constituents of the atmosphere.
4. Of known composition after it is dried or, if necessary, ignited.

Precipitants
Specific (rare): react only with a single chemical species.
As Dimethylglyoxime (DMG) is used for Ni2+
2 DMG + Ni2+  Ni(DMG)2(s) + 2 H+

Selective (common): react with a limited number of species.

As AgNO3 can be used for Cl-, Br-, I- & SCN-
Ag+ + X- → AgX, (X= Cl, Br, I, F)
The determinations involving the use of AgNO3 solution are referred as
“Argentometry” or “Argentrimetry”.

Calculation steps to solve the Problems related to find out percentage of Analyte

1) Write the balanced chemical equation for the precipitation reaction.

2) Calculate the moles of precipitate- (moles = mass ÷ molecular mass).
3) Calculate moles of analyte from the balanced chemical equation using the mole ratio
of analyte : precipitate
4) Calculate mass of analyte- (mass = moles x molecular mass)
5) Calculate percent by mass of analyte in sample (mass analyte ÷ mass sample) x 100

Sources of Error

1) Incomplete precipitation results in a value for the percentage of analyte in the sample that
is too low.
2) Incomplete drying of the sample results in a value for the percentage of analyte in the
sample that is too high.
3) Other ions in the sample may also be precipitated resulting in a value for the percentage of
analyte in the sample that is too high.

10
Example (Problem)
2.00g sample of limestone was dissolved in hydrochloric acid and all the calcium present
in the sample was converted to Ca2+(aq). Excess ammonium oxalate solution, (NH4)2C2O4(aq) was
added to the solution to precipitate the calcium ions as calcium oxalate, CaC2O4(s). The precipitate
was filtered, dried and weighed to a constant mass of 2.43g. Determine the percentage by mass of
calcium in the limestone sample. (Molecular weight of CaC2O4 = 128.04)

Data : Mass of Sample = 2.0 g

Mass of precipitate = 2.43 g

Percent mass of analyte =?

Solution

1. Write the balanced chemical equation for the precipitation reaction:

Ca2+(aq) + C2O42-(aq) → CaC2O4(s)

2. Calculate the moles (n) of calcium oxalate precipitated.

n (CaC2O4(s)) = given mass ÷ molecular mass

n(CaC2O4(s)) = 2.43 ÷ 128.04

n (CaC2O4(s)) = 0.019 moles

3. Find the moles of Ca2+(aq).

From the balanced chemical equation, the mole ratio of Ca2+ : CaC2O4(s) is 1 : 1

So, n(Ca2+(aq)) = n(CaC2O4(s)) = 0.019 moles

4. Calculate the mass of calcium in grams

mass (Ca) = n x molecular weight

mass (Ca) = 0.019 x 40.08 = 0.76g

5. Calculate the percentage by mass of calcium in the original sample:

% Ca = (mass of analyte ÷ mass sample) x 100

% Ca = (0.76 ÷ 2.00) x 100 = 38%

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Example: Analysis of chloride

When mass of sample of unknown chloride after drying is 0.0984 g and mass of AgCl
precipitate is 0.2290 g, so percentage by mass of Cl- in the given solution of becomes 57.57%.

If Pb2+ had been used to precipitate the chloride, the calculation would need to be modified
to account for the fact that each mole of PbCl2 contains two moles of chloride.

Marie Curie's Measurement of the Atomic Mass of Radium

As part of her Ph.D. research (Radioactive Substances, 1903), Marie Curie measured the atomic
mass of radium, a new, radioactive element that she discovered. She knew that radium is in the
same family as barium, so the formula of radium chloride is RaCl2. In one experiment, 0.091 92 g
of pure RaCl2 was dissolved and treated with excess AgN03 to precipitate 0.088 90 g of AgCl.
How many moles of CI were in the RaCI2? From this measurement, find the atomic mass of Ra.

Marie Curie, Pierre Curie and Henri Becquerel shared the Nobel Prize in physics in 1903 for
pioneering investigations of radioactivity. The Curies needed 4 years to isolate 100 mg of
RaCl2 from several tons of ore. Marie received the Nobel Prize in chemistry in 1911 for her
isolation of metallic radium. Linus Pauling, John Bardeen, and Frederick Sanger are the only
others who received two Nobel Prizes.

12
 EXPERIMENT 03

TO ESTIMATE THE AMOUNT OF CHLORIDE IONS PRESENT IN THE GIVEN

SODIUM CHLORIDE SOLUTION BY PRECIPITATING THEM AS SILVER
CHLORIDE

THEORY
Write down about the properties of precipitates and precipitants mentioning the following
precipitation reaction.
NaCl + AgNO3 AgCl + Na NO3

PREPARATION OF REAGENTS
Chemicals required: Sodium chloride salt, Silver nitrate and Conc. Nitric acid
1. Sodium chloride solution: about 1.0 gm of sodium chloride is accurately weighed and
dissolved in distilled water in a 25 ml measuring flask and make up the volume.
2. Precipitating reagent (0.1N AgNO3) solution
3. Washing solution: 0.01N HNO3 solution.

PROCEDURE
1. Given sodium chloride solution was taken in 100 mL beaker.
2. About 0.5 ml of conc. HNO3 is added to it, the solution is heated to about 70 oC.
3. Add about 5 mL of silver nitrate to this solution with continuous stirring.
4. The precipitate is warmed for few minutes and allowed to cool in a dark place.
5. The supernatant liquid is tested for chloride ions by pouring AgNO3 solution gently by the
sides of the beakers.
6. The precipitate is allowed to settle down in a dark place for a few hours preferably overnight.
7. The supernatant liquid is passed through sintered glass crucible which is previously
cleaned, dried & weighed.
8. The precipitate is washed by decantation with 0.01N HNO3 solution.
9. The precipitate is transferred in to the sintered glass crucible and washed with 0.01N HNO3
solution and finally washed with distilled water.
10. The precipitate is dried in the test tube in a heating over at 100 oC, cooled in a desiccator
and weighed.

OBSERVATION
Write down your observations, such as color of precipitates, time taken in development
of precipitates and effect of boiling the solution.

RESULTS
For calculations, refer to class notes.

DISCUSSION
Discuss about the possible sources of errors during precipitation reactions.

13
 EXPERIMENT 04

TO ESTIMATE THE AMOUNT OF LEAD IONS PRESENT IN THE GIVEN SAMPLE

OF LEAD NITRATE OR LEAD ACETATE SOLUTION BY PRECIPITATING THEM
AS LEAD SULPHATE

THEORY
Write down about precipitations reactions including following reactions.
Pb(NO3)2+ H2SO4 PbSO4 + 2HNO3
or Pb(CH3COO)2+ H2SO4 PbSO4 +2CH3COOH

PREPARATION OF REAGENTS
Chemicals required: Lead nitrate or lead acetate, conc: sulphuric acid and ethyl alcohol.
1. Lead nitrate or lead acetate solution: Weigh about 0.5 gm of Lead nitrate [Pb(NO 3)2] or
1.0 gm of Lead acetate [Pb(CH3COO)2] and dissolve in distilled water in presence of 1 ml
of glacial acetic acid in a 25 mL flask and make up to the mark.
2. Precipitating reagent (Conc. H2SO4): Concentrated H2SO4 used as precipitating reagent.
3. Washing solution: 1.0% by volume of H2SO4.
4. Ethyl alcohol: 10% in distilled water (The function of ethyl alcohol is to reduce the
solubility of PbSO4 in water). .

PROCEDURE
1. The given solution of lead salt is taken in 100 ml beaker.
2. Add 2.0 ml of conc. H2SO4 in the beaker and then boiled the content of the beaker.
3. Cool the content and add about 25 mL of ethyl alcohol (10%) in it.
4. The precipitate is allowed to stand for about half an hour.
5. The supernatant liquid is tested for complete precipitation by adding few drops of diluted H2SO4.
6. Filter the precipitate through a sintered glass crucible which is previously cleaned dried
and weighed.
7. The precipitate is washed 3 to 4 times with 1% solution of H2SO4 and then with 10 % ethyl alcohol.
8. Dry the precipitate in an oven at about 60-70 oC for 10 min. and then calculate the mass.
9. Repeat the drying and weighing until the constant mass of precipitate.
10. Finally find out percent mass of analyte in the given sample.

OBSERVATION
Write down your observations, such as color of precipitates, time taken in development
of precipitates and effect of alcoholic washing.

RESULTS: For calculations, refer to class notes.

DISCUSSION: Discuss that How the product that you obtained could be increased

14
 EXPERIMENT 05

TO ESTIMATE THE AMOUNT OF LEAD IONS PRESENT IN THE GIVEN SAMPLE

OF LEAD NITRATE SOLUTION BY PRECIPITATING THEM AS LEAD IODIDE

THEORY
Write down about precipitations reactions including following reactions.
Pb(NO3)2+ 2KI PbI2 + 2KNO3

PREPARATION OF REAGENTS
Chemicals required: Lead nitrate, Potassium Iodide and ethyl alcohol.
1. Lead nitrate: Weigh about 0.5 gm of Lead nitrate [Pb(NO3)2] and dissolve in distilled water
in 25 ml flask and make up to the mark.
2. Precipitating reagent (KI): Prepare 0.1 N solution of KI in 25 mL distilled water.
3. Washing solution: 10 % by volume of Ethyl alcohol.
4. Ethyl alcohol: 10% in distilled water (The function of ethyl alcohol is to reduce the
solubility of PbI2 in water).

PROCEDURE
1. Take the given solution of lead salt in 100 ml beaker.
2. Add 0.1 N solution of KI (25 mL) in the beaker and wait for 5 min.
3. Add about 15 ml of ethyl alcohol (10%) in it.
4. The precipitate is allowed to stand for about half an hour (In an ice bath → optional).
5. Filter the precipitate on filter paper which is previously weighed.
6. The precipitate is washed 3 to 4 times with 10 % ethyl alcohol.
7. Dry the precipitate in an oven at about 60-70 oC for 10 min. and then calculate the mass.
8. Repeat the drying and weighing until the constant mass of precipitate.
9. Finally find out percent mass of analyte in the given sample.

OBSERVATION
Write down your observations, such as color of precipitates, time taken in development
of precipitates and effect of alcoholic washing.

RESULTS
For calculations, refer to class notes.

DISCUSSION
Discuss about the reasons behind the colouring of precipitates.

15
 PART 03
VOLUMETRIC ANALYSIS
EXPERIMENT 06
DETERMINE THE SOLUBILITY OF THE OXALIC ACID AT ROOM TEMPERATURE

BASIC PRINCIPLE
It is an acid base titration, oxalic acid can be neutralized against sodium hydroxide

H2C2O4 + 2NaOH Na2C2O4 + 2H2O

PROCEDURE
1. Prepare a saturated solution of oxalic acid at room temperature (5 mL).
2. Transfer above prepared solution to 100 mL of the volumetric flask, and make the volume
up to the mark.
3. Fill the burette with the acid up to zero mark.
4. Take 5 mL of the standard sodium hydroxide solution in titration flask, add two drops of
phenolphthalein as indicator, the initial color will be pink.
5. Titrate it against the acid and note the burette reading when the color changes to light pink.
Take five concordant readings.

OBSERVATION
Number of moles oxalic acid reacting n1 = 1 mole
Number of moles of sodium hydroxide reacting n2 = 2 moles
Volume of NaOH solution taken for each titration V2 = 5 mL
Molarity of standard NaOH solution M2 = 0.1 M
Molarity of oxalic acid solution M1 = ?

Initial reading Final reading Difference Mean Standard

S. No. of burette of burette (Final–Initial) deviation
1
2
3
4
5

M1V1 = M2V2
n1 n2
Acid Base

RESULTS: Report the concentration of oxalic acid in gram / 100 mL (Refer Sample problem).

16
HOW TO PERFORM CALCULATION

For example following results were obtained for the supposed mixture.

No. Initial reading Final Vol. of acid

1 0.0 10 10mL
2 10 20 10mL
3 20 30 10mL

Mean volume of acid V1 used = 10mL

M1V1 = M2V2
n1 n2
Oxalic Acid NaOH

By using this formula and rearranging the equation we determine the molarity of oxalic acid as
M1 = 0.05M

Amount in g/L of Oxalic acid = Molarity × Mol. wt

= 0.05×126
= 6.3 g/L
1000 mL of diluted oxalic acid contains = 6.3 g
100mL of diluted oxalic acid contains = 6.3/1000×100
= 0.63g

As initial volume of oxalic acid prepared was 5 mL

So, 100 mL of diluted solution contains = 0.63 g
5 mL of saturated oxalic acid solution contains =0.63 g
100 mL of saturated oxalic acid solution contains =0.63 g/5×100 = 12.6
Solubility of oxalic acid at room temperature = 12.6 g/100 mL

17
 EXPERIMENT 07
CONDUCTOMETRIC TITRATION OF STRONG ACID AGAINST STRONG BASE

THEORY
Know about conductomatric titrations. Mention the source of conductance in aqueous
solutions of acids and bases.

PROCEDURE

1. Take 25mL of 0.1 M HCl acid in a beaker and keep the conductivity cell in it in such a position
that the electrodes of the cell are inside the acid solution and the body of the cell would not
touch the bottom of the beaker.
2. Note down the initial conductance of the solution. Now run NaOH in small volumes (0.5 mL)
from the burette and gently stir the solution with a glass rod without striking the cell.
3. Determine the conductance of this solution. Repeat the determination of conductance of the
solution after each addition of base volume of 0.5 mL.
4. Plot a graph between conductance and the volume of base added. Extrapolate the straight line
portions of the titration curve to obtain the correct end point.

Titration curve: Figure shows the progress of titration of HCl with

NaOH. The curve AC show the specific conductance of a mixture of
acid and salt plotted against volume of NaOH added, while the curve
BD corresponds to a mixture of salt and excess NaOH after the end
point ( the point at which the two lines cross) has reached.

Figure: Conductometric titration: Progress of

titration of HCl with NaOH
Precautions:
Operation of the conductivity bridge: Switch on the instrument five minutes before the start
of the exercise. Bring the ‘function switch' to calibration position (cell constant position) and adjust
the display reading with the cell constant knob. Keep the range selector at the maximum. Rinse
the cell with the solution whose conductance is to be measured. After taking measurements, clean
the cell with distilled water.

OBSERVATION: Draw a table and mentions the conductance readings at each added volume of base.

RESULTS: Draw the graph of conductance against volume of base and locate the equivalence point.

DISCUSSION: Discuss that why initially conductance decreased and then start increasing.

Discuss the shape when sulphuric acid titrated against NaOH

18
 EXPERIMENT 08
CONDUCTOMETRIC TITRATION OF WEAK ACID AGAINST STRONG BASE

THEORY
Know about conductomatric titrations of weak acid against strong base. Such as titration
of acetic acid against NaOH.
Equation: CH3COOH + NaOH → CH3 COONa + 4H2O

PROCEDURE

1. Take 25mL of 0.1 M acetic acid in a beaker and keep the conductivity cell in it in such a
position that the electrodes of the cell are inside the acid solution and the body of the cell would
not touch the bottom of the beaker.
2. Note down the initial conductance of the solution. Now run NaOH in small volumes (0.5 mL)
from the burette and gently stir the solution with a glass rod without striking the cell.
3. Determine the conductance of this solution. Repeat the determination of conductance of the
solution after each addition of base volume of 0.5 mL.
4. Plot a graph between conductance and the volume of base added. Extrapolate the straight line
portions of the titration curve to obtain the correct end point.

Titration curve:
Figure shows the progress of titration of
oxalic acid with NaOH. The curve show the
specific conductance of a mixture of acid and salt
plotted against volume of NaOH added.

Figure: Conductometric titration: Progress of

titration of acetic Acid with NaOH
Precautions:
Operation of the conductivity bridge: Switch on the instrument five minutes before the start
of the exercise. Bring the ‘function switch' to calibration position (cell constant position) and adjust
the display reading with the cell constant knob. Keep the range selector at the maximum. Rinse
the cell with the solution whose conductance is to be measured. After taking measurements, clean
the cell with distilled water.

OBSERVATION
Draw a table and mentions the conductance readings at each added volume of base

RESULTS
Draw the graph of conductance against volume of base and locate the equivalence point.

DISCUSSION Discuss about the shape of graph.

19