Practical Notebook for Chemistry (CHE 112)

Experiment No: 01. PRACTICE OF LABORATORY RULES AND RECORD KEEPING

Theory: Laboratory rules are the guidelines that must follow in the laboratory to avoid
accident. Everybody should be taught from teacher by following proper manuals. A number
of guidelines are summarized herewith to avoid accidents and injuries. On the other hand,
the laboratory authority must provide the first aid box, fire extinguisher, fire alarm, waste
disposal cans, shower, eye washer and a telephone to create a safe environment in the
laboratory.
A. Rules for clothing:
• One should enter in the laboratory with proper clothing; otherwise splashing of harmful
liquids may damage the expensive dress.
• A laboratory apron should always be worn while working in the laboratory.
• Protecting measures like gloves, safety glass and shoes should be used.
• Shorts and skirts dress should never be worn.
• Using sandal, open toed shoes and cloth shoes should be avoided.
B. Rules for handling apparatus and glass wears
• Broken and cracked glass wares should not be used.
• One should not be handled the apparatus unless s/he is thoroughly acquainted with
different parts, its assembling and operation.
C. Rules for handling chemicals
• Before handling chemicals, one should read the instruction manuals and labels.
• An exceptional precaution should be taken in working with chemicals of toxic,
poisonous, explosive, corrosive, inflammable characteristics (Fig. 1 Hazardous
pictograms)
D. Rules for handling flammable chemicals
• One should not heat a flask containing flammable substances like alcohols, benzene,
carbon-di-sulfides, ether etc. on a burner, heater, hot plate or sand bath.
E. Rules for handling corrosive and toxic reagents
• While working with corrosive reagent like acids, alkalis and bromides etc. gloves should
be worn.
• The affected area of the skin should be washed immediately with liberal quantities of
water.

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• Care should be taken to avoid the ingestion, inhalation and absorption of toxic chemicals
by skin, mouth or body.
F. Rules for handling irritant and lachrymatory chemicals
• The reagent like halogen containing compounds and acetyl chloride which affect the
eyes and respiratory system should be handled in the fume hood.
G. Rules for protection of eyes
• Splashing, flying objects or dusts, vapors and fumes should be controlled at it origin or
source.
• Laboratory safety glasses must always be worn while doing an experiment.
• Don't use ordinary glasses at the time of experiment.
H. Rules for disposal of chemicals and solid wastes
• Water soluble chemical should not be thrown in the sink because it creates serious
environmental problems.
• The solid waste like filter papers, drying agents, broken glass wares etc. should be
packed in suitable containers and disposed properly.
• For disposal of the toxic chemicals special treatment procedure must be applied.
I. Guidelines in case of accidents or injury:
• When accident or injury occurred in the chemical laboratory, in spite of taking above
guidelines, then one should know what to do.
• One should not panic due to any accident or injury, rather immediately informed to the
instructor for medical assistance.
• Minor cuts from broken glass wares and burns from hot equipment or chemicals should
be thoroughly flashed with tap water and then covered with an appropriate bandage
and ask for medical assistance.
• If fire is limited to small container like beaker due to burning chemicals then it should be
covered with gauze. Water should never be used to extinguish fire because all
inflammable solvents are less dense than water. Sand may be used to extinguish this
fire. For large fires, a fire extinguisher is required. For fire beyond the control, the fire
alarm should be sounded and authority should call the fire services for help.

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• If one's cloth catching fire, the victim should roll over on the ground to extinguish the
fire or should be covered with a fire blanket. A fire extinguisher should not be used on a
person.
• Affected area may wash with 10% sodium chloride solution.
• Simultaneously more than one work never be done in the laboratory.
• All power points should be off before leaving the laboratory.
J. Rules for keeping records in the Laboratory notebook:
• For record keeping of the laboratory work on should maintain a notebook carefully,
faithfully and well-planned way.
• A permanently bound book with numbered pages should be used.
• First few pages should be reserved for a table of contents and should be filled in as the
work of the courses progresses.
• The first pages for each experiment should be used for an outline of the procedure and a
mathematical statement for methods of calculation.
• The procedure should not be copied from elsewhere but should be written in your own
words to suit your own particular situation.
• Sources of information should be included.
• All data should be recorded immediately and entered directly into the notebook with
pen.
• The incorrect entry should be crossed out with a single line should not erased or
otherwise obliterated and the corrected value entered nearby to it.
• Pages should not be removed from the notebook, it is sufficient to draw a single line
diagonally across the page to be disregarded. A brief notation of the reason for striking
out the page is useful.
• The right-hand page should contain title of the experiment and must be write in capital
letters and also brief statement of the principles of analysis, data, table, description and
result should be in the right-hand page.
• The left-hand page should contain equations, calculation, graph, charts etc.
• A reference of the information should be included at the end of notebook.
Hazard symbols (pictograms): Hazard symbol (pictograms) alert us to the presence of a
hazardous chemical. The pictograms help us to know that the chemicals we are using might

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cause harm to people or the environment. One or more pictograms might appear on the
labelling of a single chemical. Some hazardous symbols (pictograms) are given below-

Explosive Corrosive Flammable Extremely Flammable

(Symbol: Exploding (Symbol: Corrosion) (Symbol: Flame) (Symbol: Flame with
bomb) F+ superscript)

Oxidizing Toxic Very Toxic Radioactive

(Symbol: Flame (Symbol: Skull and (Symbol: Skull and crossbones (Symbol: Ionizing
over circle) crossbones) with T+ superscript) radiation trefoil)

i
Biohazard Harmful Irritant Health
(Symbol: Three - (Symbol: Cross mark) (Symbol: Cross mark hazard/Hazardous to
sided trefoil) with subscript i) the ozone layer (Symbol:
exclamation mark)

Serious Health hazard Hazardous to the Gas under pressure

(Symbol: Health hazard) environment (Symbol: Gas cylinder)
(Symbol: environment)

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Experiment No: 02. AN ORIENTATION WITH CHEMICALS AND APPARATUS

Grades of chemicals: One of the most important considerations of laboratory chemicals is

the quality (grades) of the chemicals. In preparing standard solutions for quantitative
analysis, the analytical grade chemicals should be used. For spectrophotometer analysis, the
best grade is ‘spectrosol’. Several manufacturers of Germany, United Kingdom, United
States of America, India and some other countries manufactures chemical. The chemical
company, BDH (British Drug House) of England terms one of their best grades of chemical as
‘AnalaR’. On the other hand, Merck of Germany terms the same grade as ‘Extra pure’, while
some other manufacturers mark it as AR (Analytical Reagent). Some other grades like CP
(chemically pure), GPR (General Purpose Reagent), LR (Laboratory Reagent), Technical or
commercial etc. are commonly available for general purpose. Some specially purified
chemicals are also available with trade mark as GR, ACS, and GOLD LEVEL etc.
Apparatus: The common apparatus used in laboratory are as follows:
A. Volumetric apparatus are the volume measuring apparatus. Depending on the types of
work and analysis, volumetric apparatus are as follows:
Burette: A burette consists of a cylindrical glass tube with graduations along its side and
with provision for withdrawing liquid through a small opening at the end. It is used to
measure definite volume at control delivery.
Pipette: Pipettes are narrow cylindrical glass tubes either graduated or not. Pipettes are of
two types:
a) Graduated or Measuring Pipette: It is used to draw and deliver the solution by suction
and employed to deliver various volume.
b) Transfer or Volumetric Pipettes: it is employed to deliver constant volume. Micro pipettes
are used to deliver a different constant volume at micro liter levels.
Volumetric flask: Different types of volumetric flask are used like, round bottomed, flat
bottomed, long necked, bolt head and pear-shaped flask. It is used to contain specified
volume and not suitable for measuring exact volume.
Measuring Cylinder: It is cylindrical graduated glass tube provided base stands one end and
spout on other end of the tube. It is used for the rough measurement of volume.
Beaker: Beak like structured graduated glass apparatus. It is used for general purpose.

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Conical flask or Erlenmeyer flask: Glass flask having flat bottom and narrow mouth is known
as conical flask. It is especially used for mixing and titration purpose.
B. Funnels: There are different types of funnels used in the laboratory such as ordinary
funnel, separator funnel, dropping funnel, Buchner funnel etc. Ordinary funnel and
separator funnel is used for the extraction of a product from reaction mixture. Dropping
funnel employed for the addition of a reactant to a reaction mixture. Buchner funnel is used
for filtration of a solid product.
Glass funnel: Glass funnel is used to transfer the liquids and filtration.
Buckner funnel: Employed for filtering large quantities of materials.
Separator funnel: Suspending solid or liquid is separated from the mixture.
C. Heating apparatus are the warming, heating, drying, destructing apparatus.
Burner: Employed for heating moderately at high temperature.
Water bath: Employed for heating solution just below boiling pont, especially for the slow
evaporation of flammable liquids or digestion of precipitates etc.
Hot plate: The electrically heated plate with thermostat control. Used as a general heating
apparatus.
Sand bath: A hot plate covered with sand, used for indirect heating in digesting the sample.
Electric ovens: An electrically heated, thermostatically controlled drying equipment having a
temperature ranges from room temperature to about 250-300OC
Muffle furnaces: An electrically heated furnace of heating capacity at 1200 OC
D. Filtration apparatus: To separate solid from liquid, the following apparatus is used.
Filter paper: Filter papers are made of varying grades. The appropriate type must be chosen
depends on size, porosity, retention capacity, speed etc.
Gooch Crucibles: It is used for the filtration by suction.
Centrifuge machine: It is used for separation of solid from a liquid.
E. Stirring apparatus are the mixing and stirring instruments.
Stirring rod: A glass rod of 3-5 mm in diameter used for mixing two or more reagents
Magnetic stirrer: A rotating field of magnetic force is employed to induce stirring.
F. Reagent containing apparatus these are chemical preserving bottles.
Narrow mouth amber reagent bottle: It is for preserving g liquid reagent or chemicals
which is sensitive to light.
Narrow mouth colourless reagent bottle: It is used for preserving ordinary liquid reagent.

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Wide mouth amber reagent bottle: It is used for preserving light sensitive solid or powder
chemicals.
Wide mouth colourless reagent bottle: It is used for preserving ordinary solid or powder
reagent.
G. Miscellaneous apparatus are the non-specific general purpose apparatus.
Wash Bottle: It is necessary apparatus used to wash precipitate and rinse off reagents from
glassware’s.
Crucible: It is small porcelain, platinum or silica dish used to ignite the substance or
precipitate. It is heat resistant and can be heated directly over naked flame.
Crucible tongs: It is a metallic holder to hold the hot crucible or porcelain dish crucible. Hot
crucible should always be taken out or kept in with the help of the crucible tongs only.
Test tube: It is used for taking samples.
Test tube holder: It is used to hold the test tube when heated or when concentrated
reagent is added.
Test tube brush: It is used for cleaning the glass apparatus.
Glass rod: Glass rod is used to stir the solution in beaker or to transfer the liquid from
beaker to funnel.
Wire gauze: It is wire net fixed asbestos fiber in the center. Glass ware heated over wire
gauze to distribute the heat through out.
Dropper: It is used for delivering liquids drop by drop.
Weighing bottle: It is used for weighing the sample for preparing solution.
Porcelain crucible: It is utilized for igniting precipitates and heating small quantities of solids
up to 1200OC
Platinum crucible: It is used for fusion with most of the chemicals up to 1700 OC
Desiccators: It is used for maintaining a dry (moisture free) and CO2 free atmosphere in
which to place the object that might be affected by moisture or CO2 while cooling.
H. Analytical instruments are the modern sophisticated electric and electronic equipments
used for measuring any physical parameters.
Balance: Balance is the most important tool for analysis. The accuracy of any analysis
depends on precision capacity of a balance. The value of sensitivity determines the precision
capacity of a balance. The sensitivity of a balance is the magnitude of deflection in the scale
produced by one unit of weight. The calibration of a balance is carried out by a set of

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standard weights. Each set of weight is calibrated by comparing against the corresponding
piece from a standard set (calibrated by a nationally recognized institution).
Spectrophotometer: Used for determining the concentration of solution.
Flame photometer: It is used for the determination of metal ions.
Atomic absorption spectrophotometer: It is employed for the determination of metal ions.
All types of spectrophotometers are calibrated by a series of standard solution.
pH meter: Applied for the determination of hydrogen ions concentration in a solution. It is
calibrated by standard buffer solutions of pH 4, pH 7 and pH 9.
Electric conductivity meter (EC meter): Employed for the determination of salt
concentration in solution. It is calibrated by a series of standard salt solution.
Digestion and distillation apparatus: These are steam forming and oxidizing equipment.
Kjeldahl apparatus: Employed for the digestion and distillation of sample and mainly for the
determination of nitrogen in plant and soils.
Soxhlet apparatus: Used for the separation of different liquids at various boiling point.
Distilled water plant: It is used for making distilled water by evaporation and condensation
techniques.
Deionizer plant: Used to make distilled water free from any types of ions.
Gas liquid chromatography: Analysis done by adsorption.

Buchner funnel Electric oven Glass rod Water bath

Desiccators Filter paper Electrical balance Sand bath

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Kjeldahl apparatus Crucible Spectrophotometer Measuring Burette

cylinder

Centrifuge machine Flame photometer Conical flask Magnetic stirrer

Atomic absorption Electrical conductivity Volumetric flask Muffle furnaces

spectrophotometer meter

Gooch Crucibles Hot plate

pH meter
Volumetric Micro pipette
pipette Graduated
pipette

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Experiment No: 03. PREPARATION OF PRIMARY STANDARD SOLUTION

Theory: A solution is a perfectly homogeneous mixture of solute and solvent in which the
solute is present in the intermolecular space of the solvent.

Standard solution is a solution of exactly known concentration which is prepared by

standard grade solute. Standard solutions mainly are of two types - a) Primary standard
solution and b) Secondary standard solution.

a) Primary standard solution or reference solution: A solution which is prepared by primary

standard substance is called primary standard solution or reference solution.

b) Secondary standard solution: A solution which is prepared by secondary standard

substance and then standardized by a primary standard solution is called secondary
standard solution.

Primary standard substance: A Primary standard substance should satisfy the following
requirements:

1. It must be easy to obtain, chemically pure (impurity must not exceed 0.01-0.02%), dry
and preserve in a pure state.
2. The substance should not be hygroscopic, nor oxidized by air and nor affected by carbon
dioxides.
3. The substance should capable of being tested for impurities by qualitative and other
tests of known sensitivity.
4. The equivalent weight of the substance should be high so that weighing errors may be
negligible.
5. The substance should be readily soluble in water under the condition in which it is
employed.
6. The composition of the substance must correspond exactly to its formula.
7. The substance must be stable in both solid and liquid states.
8. The reaction with the standard solution should be stoichiometric.
Secondary standard substance: The standard substance with impurities or hygroscopic or
hydrated nature (i.e. other than the primary standard substances) is called secondary
standard substance.

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Units of concentration: There are different units which are used to express the
concentration of solutions; such as normality, molarity, parts per million (ppm), percent
solution (%) or parts per hundred (pph) etc.

Analytical normal solution (N): A solution containing gram equivalent weight of a substance
per 1000 mL solution. The equivalent weight of Na2CO3 is 53. When 53 g Na2CO3 dissolved in
1000 mL of a solution than it is called 1N Na2CO3 solution.

Analytical molar solution (M): A solution containing one mole of a substance per 1000 mL
solution. The molecular weight of Na2CO3 is 106. When 106 g of Na2CO3 dissolved in 1000
mL of a solution than it is called 1M solution of Na2CO3.

Parts per million (ppm): When 1 g solute present in 106 g or 106 mL (1 million) of solution it
is called ppm solution. It is expressed as g/106 mL, mg/L or μg/mL. i.e., If 1g Na2CO3 present
in 106 mL of solution than it is called 1 ppm Na2CO3 solution.

Percent solution (%) or parts per hundred (pph): When one gram of the substance
dissolved in 100 mL of the solution then is called percent solution. If one gram of Na 2CO3
dissolved in 100 mL solution than it is called 1% Na2CO3 solution.

Preparation of primary standard 100 mL 0.1N Na2CO3 solution

Apparatus and chemical required: a. Analytical balance (sensitivity-0.001 mg), b. Beaker

(500 mL), c. Volumetric flask (100 mL), d. Funnel (75 mm), e. Sodium carbonate (Na2CO3)-AR
grade, f. Distilled water, g. Dropper.

Procedure:

1. A quantity of primary standard grade sodium carbonate were dried for half an hour in an
oven at 260-270ºC by using beaker and watch glass arrangement.
2. The dried sodium carbonate was cooled in air for two to three minutes and in a
desiccator for at least 30 minutes before weighing the individual samples.
3. Accurately 0.53 g (equivalent weight of sodium carbonate) dry and cool sodium
carbonate was weighted with the help of analytical balance and was taken into a clean
100 mL volumetric flask which was fitted with a clean funnel at its mouth.

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4. A little quantity of distilled water was added through the funnel to wash the solid
sodium carbonate on the funnel and flowed down into the flask.
5. The mouth of the flask was closed tightly with the stopper and shaken carefully to
dissolve the solid sodium carbonate, with one hand on the stopper and other hand on
the bulb.
6. More distil water was added to make the volume up to the mark. Then tightly closed the
stopper and was shaken as before to make homogeneous solution.
7. Labelling was done with a paper sheet or marker and was kept for further experiment.
Experimental data: Weight to be taken = 0.53 g.

Normality to be made = 0.1N

Weight actually taken= W g= 0.534g

Result: Concentration of Prepared sodium carbonate (Na2CO3) solution = (Weight actually

taken X Normality to be made)/ Weight to be taken = (0.53 g X 0.1N)/W g = (0.53 g X
0.1N)/0.534 g = 0.1007 N

Alternate method of calculation:

53 g Na2CO3 dissolved in 1000 mL = 1N of Na2CO3 solution

So, 0.53 g Na2CO3 dissolved in 100 mL = 0.1N of Na2CO3 solution

So, 1 g Na2CO3 dissolved in 100 mL = 0.1N/0.53

Therefore, 0.534 g Na2CO3 dissolved in 100 mL = ( 0.534 g X 0.1N)/0.53 g = 0.1007 N

Note: you should put your class data for calculation…….

Conclusion: The concentration of prepared primary standard solution of sodium carbonate

was 0.1007 N.

Primary standard solution of Na2CO3

Concentration: 0.1007 N
Date:
Signature:

Fig. Labelling of the solution

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 Practical Notebook for Chemistry (CHE 112)

Experiment No: 04. PREPARATION OF SECONDARY STANDARD SOLUTION

Theory: A solution which is prepared by secondary standard substance and then

standardized by a primary standard solution is called secondary standard solution or
standardized solution. Substances like NaOH absorb moisture and carbon dioxide from the
atmosphere for which the preparation of solutions of secondary standard substances of
desired concentration becomes very difficult. Instead, solutions of secondary standard
substances of approximate concentration are at first made and then standardized against
the solutions of primary standard substances. Solutions thus standardized are known as
secondary standard solution. In other words, when the reagent is not available in the pure
form (as in the case of most alkali hydroxides, some inorganic acids and various deliquesce
substances), then solution of approximate concentration are first prepared from secondary
standard substance. These are then standardized against primary standard solution.

Standardization: Standardization may be defined as a method by which the concentration

of a solution of approximately prepared or approximately known concentration is
determined accurately with the help of a primary standard solution by some analytical
method like titration or other instrumental methods.

Preparation of secondary standard H2SO4 (0.1N) solution

Apparatus and chemical required: a) Analytical balance (sensitivity-0.001 g), b) Beaker (500
mL), c) Volumetric flask (1000 mL and 100 mL), d) Funnel (75 mm), e) Sulphuric acid (H2SO4),
f) Analytical Reagent Grade Sodium Carbonate.

Procedure:

Step I. Preparation of primary standard Na2CO3 (0.1 N) solution: Primary standard sodium
carbonate solution was prepared by weighing 0.53 g dry and cool sodium carbonate and
taken into a clean 100 mL volumetric flask and the volume was made up to the mark. Then
preserve the solution with proper labeling in a reagent bottle as described in experiment 3.

Step II. Preparation of approximately 0.1 N solution of sulphuric acid: Sulphuric acid always
contains some water and is not absolutely pure. It is not possible to weight out a definite
amount of H2SO4. We have to calculate it in some other way. The equivalent weight of

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sulphuric acid is 49, purity of supplied acid is 98% and density (sp. gr.) is 1.84. From this
information the amount of liquid is calculated.

Calculation: 98 g sulphuric acid present in 100 g pure acid

So, 1 g...................................... 100/98 g pure acid

So, 49 g.................................... (100 X 49)/98 g pure acid = 50 g Pure acid

We know, V = M/D = 50/1.84 = 27.17 mL; Where, V=Volume, M=Mass and D=Density

27.17 mL H2SO4 dissolved in 1000 mL = 1 N

2.717 mL H2SO4 dissolved in 1000 mL = 0.1 N

Procedure

1. Approximately 3 mL of concentrate H2SO4 was measured with the help of measuring

cylinder.
2. This volume of acid was poured down the side of a 1000 mL clean volumetric flask in
which some distilled water was taken before.
3. The flask was shaken and left for cool.
4. More distill water was added to the flask and made the volume up to the mark.
5. The concentration of the solution was approximately 0.1 N. Then this solution was
standardized with the help of standard solution of sodium carbonate (0.1 N) and then
preserved/stocked the solution in a reagent bottle.
Step III. Preparation of methyl orange indicator: It was prepared by dissolving 0.1 g of
methyl orange in 100 mL distilled water.

Step IV. Standardization of H2SO4 : Ten (10) mL of Na2CO3 solution was pipette out from the
preserved primary standard solution into a conical flask. Two drops of methyl orange
indicator was added into the solution. The solution becomes pale yellow. About 20 mL
distilled water was added to the conical flask. Then approximately prepared 0.1 N sulphuric
acid solution was added to the conical flask from the burette. The end point was pink. The
titration was repeated for three times. The initial and final burette readings were recorded
properly in a table.

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Titration Table

Sl. No. Volume primary standard Burette reading (mL)

Na2CO3 Solution (V2 )mL
Initial Final Mean

01

02

03

Calculation: We know, V1S1 = V2S2

or, S1 = V2S2 / V1 Where, V1 = Volume of the H2SO4 =......................

S1 = Concentration of the H2SO4 =?

V2 = Volume of the Na2CO3 Solution =...............

S2 = Concentration of the Na2CO3 Solution =...............

Conclusion: The concentration of prepared sulphuric acid .......................N

Approximately 0.1 N H2SO4 solutions Secondary standard solution of H2SO4

Date: ................................................... Concentration:................
Signature:.......................................... Date: ....................................
Signature:.............................

Fig. Labelling of the solution

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 Practical Notebook for Chemistry (CHE 112)

Experiment No: 05. ESTIMATION OF SODIUM CARBONATE IN SOLUTION

Theory: An alkaline solution titrates with a standard solution of an acid then at equivalence
point or stoichiometric point the amount of base can be calculated.

Method: Volumetric method (acid-base titration).

Work to be done:

1. Preparation of primary standard solution of sodium carbonate.

2. Preparation of approximately normal solution of sulphuric acid.
3. Standardization of sulphuric acid.
4. Titration of sample solution with standard sulphuric acid.
5. Tabulation and calculation of result.
Reagents:

1. Sodium carbonate (Na2CO3), AR grade.

2. Sulphuric acid (H2SO4), LR grade.
3. Methyl orange indicator.
Apparatus:

1. Analytical balance.
2. Magnetic stirrer
3. Volumetric apparatus (burette, pipette, conical flask, measuring cylinder etc.)
Preparation of primary standard solution of sodium carbonate (0.1 N):

The equivalent weight of sodium carbonate is 53. According to the definition of normality,
5.3 g sodium carbonate was dissolved in 1000 mL distilled water in a volumetric flask.

Sulphuric acid dilution:

The amount of concentrated acid needs to prepare 1000 mL 1 N dilute acid was calculated
from the % purity and specific gravity of the concentrated laboratory acid. Then the amount
of dilute acid needs to prepare 1000 mL 0.1 N acids was calculated by applying the formula
of liquid to liquid dilution.

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Standardization of sulphuric acid:

Ten (10) mL sodium carbonate (0.1 N) was taken in a conical flask and then 20 mL distilled
water and 6 drops methyl orange were added. The content was titrated with dilute
sulphuric acid (approximately 0.1 N). The standard value of the acid was calculated by
applying formula V1S1 = V2S2. The strength of H2SO4 was 0.09 N (From Exp.-04).

Titration of sample: Ten (10) mL sample was taken in a conical flask and titrated with
standard sulphuric acid (standard value after calculation) using methyl orange as indicator.

Titration table:

Volume of sample Burette reading

Sl. No. Differences Mean
solution Initial Final

01 10

02 10 9.5

03 10

Calculation: We can express our result mathematically by the following equation-

10 mL sample ≡ 9.5 mL 0.09 N H2SO4

From the basic principle of volumetric analysis-

1000 mL 1 N H2SO4 ≡ 1000 mL 1 N Na2CO3

1000 mL 1 N H2SO4 ≡ 53 g Na2CO3

1 mL 0.09 N H2SO4 ≡ g Na2CO3

9.5 mL 0.09 N H2SO4 ≡ g Na2CO3 = 0.045 g Na2CO3

That is, 10 mL sample ≡ 0.045 g Na2CO3 ≡ 9.5 mL 0.09 N H2SO4

So, 10 mL sample contains 0.045 g Na2CO3

100 mL sample contains = % Na2CO3 = 0.45% Na2CO3

Result: The supplied sample contains 0.45% Na2CO3

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Experiment No: 06. STANDARDIZATION OF OXIDIZING AGENT BY REDUCING AGENT

Method selection: Oxidation reduction (Redox) method

Theory
Oxidation: The process of loss of electron or donation of electron is called oxidation. For
example-when Na0 loss an electron to form Na+ ion. Here sodium loss an electron or donate
an electron to the system i. e., Na 0 → Na + + e . This type of loss or donation process is
called oxidation. H 0 → H + + e . It is also an oxidation process. The state Na0 or H0 is
reduced stage. The state Na+ or H+ is oxidized state. e. g., Na or H is reducing agent. So we
can say a reducing agent ( H 0 → H + + e ) losing or donating an electron become oxidized. In
other word hydrogen H0 or Na0 oxidized to H+ ion or Na+ ion. In other word oxidation is a
process of increase in oxidation number H 0 → H + + e , Here the oxidation number of H
increases from zero to one.
Reduction: The process of gains an electron or acceptance of electron is called reduction
when an element Cl0 gains an electron to form Cl- ion. This process is called reduction. When
an element Cl0 gains an electron to form Cl- ion. This process is called reduction. i. e.,
Cl 0 + e → Cl − , here Cl0 accepts an electron or gain an electron from the system. Here Cl0 is
reduced to Cl- ion. The state Cl0 is oxidized state and the state Cl- is reduced stage. Here Cl0 is
called oxidizing agent. So, we can say oxidizing agent ( Cl 0 + e → Cl − ) by gaining an electron
or accepting an electron reduces to Cl- ion. Decreases in oxidation number are reduction.
Here the oxidation number of Cl decreases from 0 to -1. e. g. SO4-- present as oxidized state,
2−
when SO42- gain electron or accept electron ( SO4 + e → S 2− ) to reduces S2-. SO42- is
oxidizing agent, accept electron then reduces S2-. The process is called reduction. Therefore
oxidizing state or oxidizing agent reduces. In case of O0, oxygen gains electron to form (
O + e → O 2− ) O2- ion. This process is reduction. O0 is oxidized state and an oxidizing agent.
An oxidizing agent reduces by accepting or gaining electron. Oxidation and reduction are
complementary process involving loss and gain of electrons. Since electric charge is
conserved, every time something is oxidized and something else is reduced.
In other word, oxidation-reduction is coupled reaction. Where there is an oxidation there is
a reduction. Ox + e Red These indicate that an oxidizing agent or oxidized state
substance by gaining electron or by accepting electron reduced and the process is called

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reduction, i. e., Ox + e → Re d . On the other hand, A reducing agent or reduced state

substance by losing electron or donating electron oxidized and the process is called
oxidation, i. e., Ox + e  Re d .
In short, oxidation is an increase in oxidation number and reduction is a decrease in
oxidation number. Amount of oxidation must be equal to reduction.
Oxidation number: The relative state of oxidation of an element in a compound is called
oxidation number. For simple monatomic ions of the elements, the oxidation number is the
charge on the ion itself. The neutral element therefore has an oxidation number of zero. The
Na+ ion has an oxidation number of +1. The oxide ion (O2-) has an oxidation number of -2.
The oxidation number of hydrogen in H2 is zero as the oxidation number of O in O2 or P in P4.
In KMnO4, oxidation number of Mn is +7.
Principle of permanganate titration
The solution which containing permanganate ions (MnO4-) are pink or purple in color but
the salt solutions containing manganous ions (Mn++) are colorless. When a reducing agent is
added to potassium permanganate (KMnO4) solution in acid medium, the MnO4- ions
reduces to Mn++ ion and the purple color disappear first slowly and then quickly with the
formation of certain amount of Mn++ ions. This is continued until the reaction between
KMnO4 and the reducing agent in presence of an acid is over. But the solution attains pink
color with even a slight excess of MnO4-. Here, KMnO4 serves as an indicator itself, so, no
indicator is added in this titration. The reaction of KMnO4 with sodium oxalate (Na2C2O4) in
acid medium (presence of H2SO4) is given below:
2 KMnO 4 + 5 Na 2 C 2 O4 + 8H 2 SO4 = 2 MnSO4 + K 2 SO4 + 5 Na 2 C 2 O4 + 10CO 2 + 8 H 2 O
The partial reaction for reduction-
−
MnO4 → Mn + +
−
MnO4 + 8H + → Mn + + + 4 H 2 O [8H+ required to balance it]
−
MnO4 + 8 H + + 5e Mn++ + 4 H2O [5e required to balance electrically]........ (i)

The partial reaction for oxidation-

−−
C 2 O4 → 2CO 2
−−
C 2 O4 2CO2 + 2e................................................................................. (ii)
By multiplying equation (i) by 2 and (ii) by 5, we get,
−
2 MnO 4 + 16 H + + 10 e 2 Mn++ + 8 H2O
−−
5C 2 O4 10CO2 + 10e
− + −−
2 MnO 4 + 16 H + 5C 2 O4 2 Mn++ + 8 H2O + 10CO2

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 Practical Notebook for Chemistry (CHE 112)

Apparatus required
a) Burette, b) Pipette, c) Conical flask, d) Measuring cylinder, e) Volumetric flask, f) Electric
hot plate etc.
Chemicals required
a) Potassium permanganate (KMnO4) solution - Approximately 0.1 N
b) Sulphuric acid (H2SO4) solution – 2 N
c) Sodium oxalate (Na2C2O4) solution – 0.1 N
Procedure
A) Preparation of approximately 0.1 N solution of KMnO4: Potassium permanganate
(KMnO4) is a strong oxidizing agent. In acidic solution, permanganate ion (MnO 4-) reduces to
manganous (Mn++) ion. During oxidation, it losses 5 electron. So, gm equivalent weight of
39 + 55 + 16  4 158
KMnO4 = = = 31.6 g . So, 3.16 g KMnO4 was dissolved in 1000 mL
5 5
solution to prepare 0.1 N solution of KMnO4.
B) Preparation of 2 N H2SO4 solutions: Sulphuric acid always contains some water and is not
absolutely pure. It is not possible to weight out a definite amount of H 2SO4. We have to
calculate it in some other way. The equivalent weight of sulphuric acid is 49, purity of
supplied acid is 98% and density (sp. gr.) is 1.84. From this information the amount of liquid
is calculated.
98 g pure sulphuric acid present in 100 g acid
So, 1 g...................................... 100/98 g pure acid
So, 49 g.................................... (100 X 49)/98 g pure acid = 50 g Pure acid
We know, V = M/D = 50/1.84 = 27.17 mL; Where, V=Volume, M=Mass and D=Density
27.17 mL H2SO4 dissolved in 1000 mL = 1 N
So, 54.34 mL H2SO4 dissolved in 1000 mL = 2 N
C) Preparation of primary standard solution of Na2C2O4 (0.1 N): Exactly 6.701 g sodium
oxalate was weighed out in a 1 L volumetric flask and volume up to the mark with distilled
water.
D) Standardization of KMnO4 by Na2C2O4 solution: Ten (10) mL sodium oxalate (0.1 N) was
taken in a conical flask. Five (5) mL 2N sulphuric was also added to the solution. The mixture
was then heated to 60-70ºC temperature for 1-2 minutes. In the meantime, a clean burette
was filled with KMnO4 solution (approximately 0.1 N) and the initial burette reading was

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 Practical Notebook for Chemistry (CHE 112)

noted in the titration table. The Na2C2O4 solution was titration against the KMnO4 solution
from the burette and disappear the color of KMnO4 solution. It may be mention here that,
formation of a small amount of Mn++ ion acts here as an auto catalyst and results in fading
the color of KMnO4 solution instantaneously. The end point is attained when a drop of
KMnO4 solution colors the whole solution of the conical flask into pale pink for 1-2 minutes.
Three successive burettes reading which do not differ by more than 0.1 mL were taken and
recorded in the notebook.
Titration table
Sl. Volume primary standard Burette reading (mL)
No. Na2C2O4 Solution (V1 )mL Initial Final Differences Mean
01 10 0.0 10.5 10.5
02 10 10.5 21.0 10.5 10.5
03 10 21.0 31.5 10.5

E) Calculation
a) Calculation for determination of concentration of KMnO4 solution:
We know,
V1S1 = V2S2 Where, V1 = Volume of the Na2C2O4 Solution = 10 mL
or, S2 = V1S1 / V2 S1 = Concentration of the Na2C2O4 Solution = 0.1 N
or, S2 = (10 X 0.1) / 10.5 V2 = Volume of the KMnO4 solution = 10.5 mL
or, S2 = 0.095 N S2 = Concentration of the KMnO4 solution =?

Result: The concentration of prepared secondary standard solution of potassium

permanganate was 0.095 N.

Approximately 0.1 N KMnO4 solutions Secondary standard solution of KMnO4

Date: ...................................................... Concentration: 0.095 N
Signature:................................................. Date: ........................................................
Signature:...................................................

Fig. Labeling of the solution

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 Practical Notebook for Chemistry (CHE 112)

b) Calculation for determining the amount of Na2C2O4 in the supplied solution:

We can express our result mathematically by the following equation-
10 mL sample ≡ 10.5 mL 0.095 N KMnO4
From the basic principle of volumetric analysis-
1000 mL 1 N KMnO4 ≡ 1000 mL 1 N Na2C2O4
1000 mL 1 N KMnO4 ≡ 67 g Na2C2O4
67  0.095
1 mL 0.095 N KMnO4 ≡ g Na2C2O4
1000
67  0.095  10.5
10.5 mL 0.095 N KMnO4≡ g Na2C2O4
1000
= 0.067 g Na2C2O4
That is, 10 mL sample ≡ 0.067 g Na2C2O4 ≡ 10.5 mL 0.095 N KMnO4
So, 10 mL sample contains 0.067 g Na2C2O4
0.067  100
100 mL sample contains = % Na2C2O4
10
= 0.67% Na2C2O4
Result: The supplied sample contains 0.67% Na2C2O4

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