APPLIED CHEMISTRY LABORATORY

INTRODUCTION TO CHEMISTRY LABORATORY

Chemical analysis is carried out to understand the composition of the materials. This will enable to assess
the properties of materials and if necessary, modify the properties for technical and scientific applications.
Chemical analysis is the resolution of a chemical compound into proximate or ultimate parts. Traditional
manual chemical analysis is divided into two types.
1) Qualitative analysis.
2) Quantitave analysis.

Qualitative Analysis: It deals with the identification and confirmation of the nature of the substance or
impurities present in a given sample.

Quantitative Analysis: It deals with the estimation of amount of each component or specified components
are present in a given sample, including in trace quantities. The substance determined is analyte and the minor
or the trace quantities are impurities. The complete quantitative analysis consists of five steps: sampling,
dissolution of the sample, conversion of the analytes into a form suitable for measurement, measurement,
calculation and interpretation of data.
Quantitative chemical analysis is further divided into two types:
1) Gravimetric analysis.
2) Volumetric analysis.

Gravimetric analysis: Gravimetric analysis involves the estimation of the amount of a given compound from
the results of weighing.
Volumetric analysis: Volumetric analysis is based on the measuring the volume of the solution of a
substance.

Terms involved in volumetric analysis:

Titration: The process of finding out the volume of one of the solution required to react completely
with a definite volume of one the other solution of known concentration is called titration.
Titrant: The solution of known strength is called titrant. Titrate: The solution whose concentration to be
estimated.
Indicator: The reagent which indicates the endpoint or equivalent point of the titration. The strength
of concentration of a solution is expressed in the following ways.
Solute: In a solution, the substance present in relatively low quantity is called a solute.
Solvent: In a solution, the substance present in relatively high quantity is called a solvent.
Concentration: It is relative or absolute amount of the desired material in the company of others, especially
in solution. The relative amounts of solute and solvent present in a solution is also called concentration of the
solution. Concentration can also be defined as the number of solute particles present in unit volume of
solution. Usually, normality or molarity is used to express the concentrations.
Normality (N): It is the number of gram equivalents of the substance in a liter of the given solution.
Normality(𝑁) =
ANDHRA LOYOLA INSTITUTE OF ENGINEERING AND TECHNOLOGY Page 1
 Weight × 1000
Equivalent weight × volume∈ml

ANDHRA LOYOLA INSTITUTE OF ENGINEERING AND TECHNOLOGY Page 2

Molarity (M): It is the number of moles of the substance in a liter of the given solution.
Molarity= No. of moles/volume of the solution in liters.
Weight ×1000
Molarity(𝑀) =
Molecular weight × volume∈ml
Standard Solution: It is the solution for which the exact concentration is known. In general, graduated
flasks are used to prepare standard solutions.
Molar Solution: If one gram molecular weight of a solute is dissolved in one liter of the solvent, it is called
a Molar solution.
Standardization: Determination of the concentration of a solution by any suitable analytical method is
known as standardization.
Primary standard substance: A primary standard is a reliable, readily quantified substance. Features of a
primary standard include high purity, stability (low reactivity), low hygroscopic, efflorescence, high
solubility and high equivalent weight. Some examples of primary standards are potassium hydrogen
phthalate, sodium carbonate, sodium chloride, potassium chloride, potassium dichromate, etc.
Secondary standard substance: A secondary standard is a substance of low purity, low solubility and
more hygroscopic or high reactivity. The concentration of solution of such substance changes with time.
Examples of secondary standards are Na2B4O7.10H2O, CuSO4.5H2O, etc. Hydrated salts do not make good
standards because of difficulty of efficient drying.
Primary standard solution: If the concentration of a solution is known by dissolving a known mass of the
desired substance into a known volume of solvent, then the solution is called a primary standard solution.
Secondary standard solution: If the concentration of a solution is determined by using a suitable primary
standard solution, then the solution is called secondary standard solution.
Types of titrations: Titrations can be classified by the type of reaction. Different types of titrations
include:
1) Acid base titration is based on the neutralization reaction between the analyte and an acidic or basic
titrant. They most commonly used as pH indicator, a pH meter, or a conductometer to determine the
endpoint.
2) A redox titration is based on an oxidation reduction reaction between the analyte and titrant. They
most commonly use a potentiometer or a redox indicator to determine the end point. Frequently either
reactants or the titrant have a color intense enough that an additional indicator is not required.
3) A complexometric titration is based on the formation of a complex between the analyte and the titrant.
The chelating agent EDTA is very commonly used to titrate metal ions in solution. These titrations
generally require specialized indicators that form weaker complexes with the analyte. A common
example is Eriochrome Black-T for the titration of calcium and magnesium ions.
4) A precipitation titration is based on the formation of a product which is insoluble in solvent and forms
precipitate, by the reaction between the analyte and the titrant. A classic example is the reaction
between Ag+ and Cl- to form the very insoluble salt AgCl.

General procedure of a titration: In order to perform a titration, the basic requirements are burette,
pipette and conical flask. Before starting the titration, wash all the glass apparatus with tap water. Collect
distilled water into wash bottles provided and rinse all the glassware with distilled water. Collect the
solutions required for the titration into beakers. Rinse the burette with the solution to be taken into it. Fill
the burette with the respective solution slightly above the zero mark. Slowly open the stopper screw of the
burette, allow the solution out slowly and makeup the burette reading to zero mark by the lower meniscus of
the solution level coincided with the zero mark. Care is to be taken to avoid air bubbles in the solution of the
burette. Fix the burette to the stand at an appropriate height. Rinse the pipette with the solution to be taken
into the conical flask. Take the solution up to the mark of the pipette and transfer quantitatively into the
conical flask. Add the required reagents and indicator as given in the prescribed procedure and place the
conical flask on the glazed tile. Gently shake the conical flask with simultaneous addition of titrant from the
burette until the end point is reached. After getting end point, take the burette out of the stand and note down
the reading without parallax error. Throughout all the contents of conical flask, wash it with tap water and
rinse with distilled water. Repetition of titration is must in order to conform the accurate reading. After
completing the experiment, wash all the apparatus with tap water. Place all the apparatus and reagent bottles
in their respective places after their use.

Precautions:
1. Do not measure acids with pipette.
2. Do not waste the valuable distilled water
3. Do not place bags, note books or manual on the working table.
4. Handle all the glass apparatus with care and avoid payment of breakage fees.
5. During the titration, observe the changes taking place in the contents of conical flask instead of the
burette reading.
Expt.No.01

ESTIMATION OF HCl BY USING STANDARD SODIUM CARBONATE

(Acid –Base Titration)

Aim: To estimate the amount of HCl in a given solution using Na2CO3 solution.
Apparatus: Burette, pipette, conical flask, volumetric flask, beaker, wash bottle and burette stand.
Chemicals: Standard oxalic acid solution, Washing soda (Sodium Carbonate), hydrochloric acid and
methyl orange indicator.
Chemical equation:
Na2CO3 + (COOH)2 → (COONa)2 + CO2 + H2O

Na2CO3 + 2HCl → 2 NaCl + H2CO3

Basic principle: The neutralization method includes volumetric determinations based on the neutralization
reaction.
OH- + H+ → + H2O

By this method, standard solution of an acid can be used for quantitative determination of alkalis,
or a standard solution of an alkali can be used for quantitative determination of acids.
If a solution of any acid is titrated with an alkaline solution, the OH- ions of the latter combine with
the H+ ions of the acid and the concentration of the later gradually increases while the pH of solution also
increases. At a certain definite pH value the equivalence point is reached and no more alkali should be
added. When a solution of an alkali is titrated with an acid solution the OH- ions are removed by the H+
ions and the concentration of the latter gradually increases while the pH of solution decreases. At a certain
definite pH value, the equivalence point is reached and titration must be ended at that point.
The pH value at the equivalence point depends on the nature and the concentrations of the reacting
substances (acid and base). To detect the equivalence point, acid base indicators are used. The color of any
indicator changes only within a certain pH range which is known as the useful range of that indicator. For
any indicator to be selected in particular reaction, the pH of solution at the equivalence point should be in
the useful pH range of the indicator or in practice, we select an indicator which exhibits a distinct color
change at a pH close to that obtaining at the equivalence point.
HCl is standardized by titrating with standard solution of sodium carbonate using methyl
orange as indicator. The color change of methyl orange is from yellow in alkaline medium to orange red in
acid medium
Na2CO3 + 2HCl → 2 NaCl + H2CO3
At the equivalence point, saturated solution of H2CO3 has a pH of about 4. Useful pH range of methyl
orange is 3.1 to 4.5 and so this can be used as indicator in this titration.

Solutions:
1) Standard Oxalic acid solution (0.02M): Dissolve 1.8 g of oxalic acid in DI water and make up to 1litre.
2) Na2CO3 (0.02M): Dissolve 0.212 g of sodium carbonate in DI water and make up to 100ml.
Procedure:
Part-1: Standardization of Na2CO3 solution: Pipette out 10ml of Sodium carbonate solution in to a
conical flask. Add few drops of methyl orange indictor. The solution turns yellow. Fill the burette with
Oxalic Acid solution. Titrate sodium carbonate solution against Oxalic acid solution until the color of the
solution changes from yellow to orange red. This is the endpoint of the titration.

Part-2: Estimation of HCl solution: Pipette out 10ml of standard sodium carbonate solution in to a
conical flask. Add few drops of methyl orange indictor. The solution turns yellow. Fill the burette with
unknown HCl solution. Titrate sodium carbonate solution against unknown HCl solution until the color of
the solution changes from yellow to pale pink. This is the endpoint of the titration.

Observations and Calculations:

Part-1: Standardization of Na2CO3 solution:

Volume of Na2CO3 Burette reading (ml) Volume of Oxalic acid

S.No.
solution (ml) Solution run down(ml)
Initial Final

V 1 M1 V 2 M2
=
Formula: n1 n2

V 1 M 1 n2
M 2=
 V 2 n1 =

Where;
Oxalic acid Na2CO3
M1 = Molarity of standard Oxalic acid solution = 0.02M M2 = Molarity of Na2CO3 solution =
V1 = Volume of standard Oxalic acid solution = V2 = Volume of Na2CO3 solution = 10 ml
n1 = No. of moles of standard Oxalic acid taken part in the n2 = No. of moles of Na2CO3 taken part in the
reaction = 1 reaction = 1
 Part-2: Estimation of HCl:

Volume of Na2CO3 Burette reading (ml) Volume of HCl Solution run down
S.No.
solution (ml) (ml)
Initial Final

Formula:
V 2M2 V 3 M3
=
n2 n3

Where;
Na2CO3 HCl
M2 = Molarity of Na2CO3 solution = M3 = Molarity of HCl solution =
V2 = Volume of Na2CO3 solution = 10 ml V3 = Volume of HCl solution =
n2 = No. of moles of Na2CO3 solution taken part in n3 = No. of moles of HCl solution taken part in the
the reaction = 1 reaction = 2

V2M2n3
∴ M3 =
n2V3

Amount of HCl present in given 100 ml of solution = Molarity of HCl (M3) x M.Wt of HCl (36.5) x 100
1000

= –––––––––––– g

Result: Amount of HCl present in the given 100 ml of solution = ––––––––––

Expt.No: 2

DETERMINATION OF ALKALINITY OF A SAMPLE CONTAINING Na2CO3 and NaOH

(Acid –Base Titration)

Aim: To determine the alkalinity of sample containing Na2CO3 and NaOH using standard HCl solution.
Apparatus: Burette, pipette, conical flask, volumetric flask, beaker, wash bottle and burette stand.
Chemicals: Standard Na2CO3 solution, HCl solution, sample containing Na2CO3 and NaOH solution,
methyl orange and phenolphthalein indicator.
Chemical equations:
Na2CO3 + 2HCl → 2 NaCl + H2CO3

NaOH + HCl → NaCl + H2O

Theory: The neutralization method includes volumetric determinations based on the neutralization
reaction.
OH- + H+ → H2O
By this method, standard solution of an acid can be used for quantitative determination of alkalies,
or a standard solution of an alkali can be used for quantitative determination of acids.
HCl is standardized by titrating with standard solution of sodium carbonate using methyl orange
as indicator. The color change of methyl orange is from yellow in alkaline medium to orange red in acid
medium
Na2CO3 + 2HCl → 2 NaCl + H2CO3
At the equivalence point, saturated solution of H2CO3 has a pH of about 4. Useful pH range of
methyl orange is 3.1 to 4.5 and so this can be used as indicator in this titration.
When a known volume of the mixture is titrated with HCl in presence of phenolphthalein indicator, the
acid reacts with all the sodium hydroxide and with only half of the carbonate.
P = All hydroxides + ½ carbonates
When a known volume of the mixture is titrated with HCl in presence of Methyl Orange indicator, the acid
reacts with all the hydroxide and all the carbonate.
M = All hydroxide + All carbonate
Solutions:
1) HCl (0.3M): Dilute 25.8 ml of conc. HCl to 1 litre with DI water.
2) Sample mixture: Dissolve 15.9 g of Na2CO3 and 6 g of NaOH in DI water and make up to 1litre.
Procedure:
Determination of alkalinity: Pipette out 10 ml of the sample mixture into a conical flask, and add one or
two drops of phenolphthalein indicator. Fill the burette with standard HCl solution. Titrate the sample
mixture against HCl solution until the color of the solution changes from pink to colourless. Repeat the
titration till the concurrent values are obtained.
The volume of acid is taken as P and is equivalent to all the hydroxide and half the carbonate.

Pipette out 10 ml of the sample mixture into a conical flask, and add one or two drops of methyl orange
indicator. Fill the burette with standard HCl solution. Titrate the sample mixture against HCl until the color
of the solution changes from yellow to orange red. Repeat the titration till the concurrent values are
obtained.
The volume of acid is taken as M and is equivalent to all the hydroxide and all the carbonate.
Observations and Calculations:
Determination of alkalinity: Molarity of HCl = 0.3M

Using phenolphthalein:
Volume of sample Burette reading (ml) Volume of HCl Solution run
S.No. Initial Final
solution (ml) down (P ml)

Phenolphthalein alkalinity in terms of CaCO3 is calculated by using the formula

P Molarity of HCl 
ppm 
501000 Volume of sample
mixture

Using Methyl orange:

Burette reading (ml)

Volume of sample Volume of HCl Solution run
S.No. Initial Final
solution (ml) down ( ml)

Methyl Orange alkalinity in terms of CaCO3 is calculated by using the formula

M Molarity of HCl  501000
Volume of sample mixture
Result:
Phenolphthalein alkalinity in terms of CaCO3 = ---------------ppm
Methyl Orange alkalinity in terms of CaCO3 = ----------------ppm
Expt.No: 3

DETERMINATION OF Mn (II) USING STANDARD OXALIC ACID SOLUTION

(Redox Titrations)

Aim: To estimate the amount of Mn+2 present in given solution by using standard oxalic acid solution.
Apparatus: Burette, pipette, conical flask, volumetric flask, beaker, measuring cylinder, wash bottle,
Bunsen burner and burette stand.
Chemicals: Standard sodium carbonate solution, Oxalic acid solution, Potassium permanganate solution,
methyl orange and 10% sulphuric acid solution.
Chemical Equations:
Na2CO3 + (COOH)2 → (COONa)2 + CO2 + H2O

5H2C2O4 + 2KMnO4 +3H2SO4 → K2SO4 +2MnSO4 +8H2O +10CO2

Theory:
Oxidometry involves oxidation – reduction reactions associated with transfer of electrons. In a
reaction of this type, the oxidizing agent gains electrons and is reduced and the reducing agent loses
electrons and is oxidized. This exchange of electrons leads to changes in the valence of the corresponding
atoms or ions. The valence of an oxidized atom or ion is increased and the valence of a reduced atom or ion
is decreased.
The permanganate method is based on reactions of oxidation by the permanganate ion. In acid
solutions KMnO4 acts as an oxidizing agent. The heptavalent (+7) manganese in it is reduced to
Mn2+cations and manganese salt is formed.
Standard solution of oxalic acid is used to standardize potassium permanganate solution. When
oxalic acid is titrated with potassium permanganate the reaction is

5H2C2O4 + 2KMnO4 +3H2SO4 → K2SO4 +2MnSO4 +8H2O +10CO2

Here C2O42- ions are oxidized as C2O42- - 2e- → 2CO2

This reaction hardly proceeds at room temperature and so to make the reaction proceed at an
adequate rate this titration should be performed at 60 to 70 o C. No indicator is needed in permanganate
titrations. The pink color of the Mn2+ ion will give the color change. When all the reducing agent has been
titrated a single excess drop of permanganate colors the whole solution as distinct pink.

Solutions:
1) Standard sodium carbonate solution (0.05M): Dissolve 5.299 g of Na2CO3 in DI water and make up to
1litre.
2) Oxalic acid solution (0.05M): Dissolve 6.30 g of oxalic acid in DI water and make up to 1litre.
3) H2SO4 (2N): Dilute 55.6 ml of conc. H2SO4 to 1 litre with DI water.
Procedure:
Part-I: Standardization of Oxalic acid:
Pipette out 10ml of oxalic acid solution in to a conical flask. Add few drops of methyl orange
indictor. The solution turns pink. Fill the burette with standard sodium carbonate solution. Titrate oxalic
acid solution against sodium carbonate solution until the color of the solution changes from pink to yellow.
This is the endpoint of the titration.

Part-II: Estimation of potassium permanganate solution:

Pipette out 10ml of standard oxalic acid solution into a conical flask and add 10 ml of 10%
sulphuric acid. Heat the solution to about 70 0 C, (do not allow it to boil, because oxalic acid decomposes on
boiling). Now, titrate this hot solution with KMnO 4 from burette. The first drop of KMnO4 fades rather
slowly. However as soon as a small amount of MnSO 4 (acts as catalyst in this reaction) is formed,
subsequent fading is always instantaneous. The endpoint is obtained when one drop of permanganate colors
the whole solution pale pink which should remain for one minute.

Observations and Calculations:

Part-1: Standardization of oxalic acid solution:
Burette reading (ml) Volume of Sodium
Volume of oxalic
S.No. carbonate solution run
acid solution (ml) Initial Final
down (ml)

Formula:
V1M1 V M
2 2
n1  n2
Where
M1 = Molarity of standard sodium carbonate solution = 0.05M
V1 = Volume of standard sodium carbonate solution =
n1 = No. of moles of standard sodium carbonate taken part in the reaction = 1
M2 = Molarity of oxalic acid solution =?
V2 = Volume of oxalic acid solution = 10ml
n2 = No. of moles of oxalic acid taken part in the reaction = 1
V M n
M 2= 1 1 2
 V 2 n1 =
Part2: Estimation of potassium permanganate:
Volume of Burette reading (ml)
Volume of KMnO4 Solution
S. No. Oxalic acid
Initial Final run down (ml)
solution(ml)

Formula:
V 2 M2 V M
3 3
n2  n3
Where;
 V 2 M 2 n3
M 3=
 V 3 n2 =

Amount of Mn+2 present in the given one litre of solution

= Molarity (M3) x Atomic weight of Mn(54.94) x1000

1000

= ––––––––––––g/L

Result: Amount of Mn+2 present in the given solution= g/L.

Expt.No:4

DETERMINATION OF FERROUS IRON USING STANDARD K2Cr2O7 SOLUTION

(Redox Titration)

Aim: To estimate the amount of Ferrous iron present in the given solution using potassium dichromate.
Apparatus: Burette, pipette, conical flask, volumetric flask, beaker, measuring cylinder, wash bottle, and
burette stand.
Chemicals: Standard Mohr’s salt solution, potassium dichromate solution, ferrous sulphate solution, 10%
sulphuric acid and diphenylamine indicator.

Chemical Equation:

K2Cr2O7 +6FeSO4 +7H2SO4  K2SO4 +3Fe2 (SO4)3 + Cr2 (SO4)3 + 7 H2O

Theory:
Dichrometry titrations are based on oxidation reactions by dichromate ion. Its oxidizing action is
due to conversion of Cr2 O7- ions (containing Cr6+) into Cr3+ ions.
Cr2O72- + 14 H ++ 6e-  2Cr3+ +7H2O

Potassium dichromate acts as an oxidizing agent in the presence of sulphuric acid. It oxidizes Fe2+ ion and
itself is reduced to green chromic salt.

K2Cr2O7+6FeSO4+7H2SO4  K2SO4 + 3Fe2(SO4 )3 + Cr2 (SO4 )3 + 7H2O

To detect the end point, diphenylamine is used as indicator in the titration. Indicator used in oxidation –
reduction titrations are known as oxidation – reduction or Redox indicators. Redox indicator change color
when the oxidation potential of titrated solution reaches a define value. These indicators can be reversibly
oxidized or reduced with different color in the oxidized and reduced forms.
Indicator (ox) + ne-  Indicator (red)

Diphenylamine changes from colorless to blue – violet between 0.73V and 0.79V. Effective potential range
of Redox indicator must be within the limits of the sharp change of potential near the equivalence point.
Phosphoric acid is added to lower the Redox potential of Fe 2+ - Fe3+ ion system so that abrupt potential
change near the equivalence point nearly coincides with the potential range of the indicator.

Solutions:
1) Mohr salt solution (0.06M): Dissolve 23.52 g of Mohr salt in DI water and make up to 1litre.
2) Potassium dichromate solution: Dissolve 2.94 g of K2Cr2O7 in DI water and make up to 1litre.
3) 10% Sulphuric acid: Dilute 50 ml of conc. H2SO4 to 500 ml with DI water.
4) Diphenyl amine: Dissolve 0.5 g of diphenyl amine in 85 ml of conc. H2SO4 and make up to 100ml.
Procedure:
Part-1: Standardization of Potassium dichromate solution:
Pipette out 10ml of standard Mohr’s salt solution into a conical flask and add 5ml of 10% H 2SO4.
Add 2 or 3 drops of diphenylamine, titrate this solution with Potassium dichromate solution from a burette.
With the titration the solution becomes green and just before the endpoint it is bluish green and at the
endpoint it is bluish violet.

Part-2: Estimation of Ferrous Ion:

Pipette out 10ml of ferrous sulphate solution in to a conical flask and add 5ml of 10% H2SO4 .Add
2 or 3 drops of diphenylamine and titrate this solution with Potassium dichromate solution from a burette.
Then the resulting solution becomes green and just before the endpoint it is bluish green and at the end
point it is bluish violet.

Observations and Calculations:

Part-1: Standardization of Potassium dichromate solution:
Volume of Burette reading (ml)
Volume of K2Cr2 O7
S.No. standard Mohr’s
Initial Final Solution run down (ml)
salt solution(ml)

Formula:
V1M1 V2 M 2

n1 n2
Where;
M1 = Molarity of standard Mohr’s salt solution = 0.06 M
V1 = Volume of standard Mohr’s salt solution = 10ml
n1 = No. of moles of Mohr’s salt taken part in the reaction = 6
M2 = Molarity of potassium dichromate solution =
V2 = Volume of potassium dichromate solution =
n2 = No. of moles of potassium dichromate taken part in the reaction = 1
V 1 M 1 n2
M 2=
 V 2 n1 =
Part2: Estimation of ferrous ion:
Volume of ferrous Burette reading (ml)
Volume of K2Cr2 O7
S.No. sulphate solution
Initial Final Solution run down (ml)
(ml)

Formula:
V2 M 2 V3M3

n2 n3
Where;
 M2 = Molarity of potassium dichromate solution =
V2 = Volumeof potassium dichromate solution =
n2 = No. of moles of potassium dichromate taken part in the reaction =1
M3 = Molarity of ferrous sulphate solution =
V3 = Volume of ferrous sulphate solution = 10ml
n3 = No. of moles of ferrous sulphate taken part in the reaction =6

V 2 M 2 n3
M 3=
 V 3 n2 =

Amount of ferrous ion present in one litre of solution

= Molarity of ferrous sulphate(M3) x Atomic weight (56)x 1000

1000
=
=

Result: Amount of ferrous ion present in the given solution= g/L

Expt.No:5

DETERMINATION OF TEMPORARY AND PERMANENT HARDNESS OF WATER USING

STANDARD EDTA SOLUTION
(Complexometric Titration)

Aim: To determine the temporary and permanent hardness in water sample by complexometric
titration using EDTA solution.
Apparatus: Burette, Pipette, conical flask, beaker, measuring cylinder etc.
Chemicals: Standard EDTA solution, hard water, boiled out water sample ammonia – ammonium chloride
buffer solution (pH = 10), Eriochrome Black -T
Chemical equations:

1. Metal ions + indicator → [ Metal- indicator]complex

(Blue) (Less stable and wine red color)
2. Metal ions + EDTA → [ Metal- EDTA]complex
(Stable and colorless)
3. EDTA + [ Metal- indicator] → [ Metal- EDTA] complex + indicator
(Wine red) (Blue)
Here metal ions refer to Ca2+, Mg2+, Zn2+ or any other heavy metal ion.

Theory: The hardness of water is generally due to dissolved calcium and magnesium salts and may be
determined by complexometric titration. The total hardness of water is the sum of temporary hardness and
permanent hardness, and is expressed as parts per million of CaCO3 (ppm).
Structural formula of EDTA, ethylene diamine tetra acetic acid is

Disodium salt of EDTA is

The solution of Erichrome black – T is

Red …. Below pH 5.5 (due toH2D-)

Blue …. Between pH 7 to 11 (due to HD2-)
Yellow orange…. Above pH 11.5 (due toD3-
 Eriochrome Black -T

pH is rather critical in this titration, and for obvious reasons a value of about 10 is most satisfactory. To
maintain a pH of 10, Ammonia- ammonium chloride buffer solution is added to the water sample taken in
conical flask. Two drops of the indicator Eriochrome Black –T (complex organic compound) is added to
hard water (pH=10 ± 0.1) it gives wine red color complex, with Ca 2+ and Mg2+ ions of water sample, and
the solution is titrated with standard EDTA solution until the colour of the solution changes from wine red
to blue.

M = Ca+2 or Mg+2

The following table gives relation between the type of water sample and the degree of hardness

Nature of water Hardness in ppm (CaCO3 equivalent)

Soft Below 50 ppm
Moderately hard 50-150 ppm
Hard 150-300 ppm
Very hard Above 300 ppm

Solutions:
1) EDTA (0.01M): Dissolve 3.72 g of disodium salts of EDTA in DI water and make up to 1litre.
2) Buffer solution: Dissolve 7 g of NH4Cl and 43 ml of conc. NH3 in DI water and make up to 100 ml.
3) EBT Indicator: 0.5 g of EBT dissolved in 100 ml of ethanol.
 Procedure:
Part-1: Determination of Total Hardness of water:
Pipette out 10ml of the water sample into a conical flask. Add 1ml of ammonia- ammonium
chloride buffer solution and 2 or 3 drops of Eriochrome black-T indicator. Now the solution is wine red
in color. Titrate this solution with standard EDTA solution from a burette until the color changes from wine
red to blue. Repeat the titration until the concurrent value is obtained.

Part-2: Determination of Permanent Hardness of water:

Pipette out 10ml of the water sample (after boiling) into a conical flask. Add 1ml of ammonia-
ammonium chloride buffer solution and 2 or 3 drops of Eriochrome black-T indicator. Now the solution
is wine red in color. Titrate this solution with standard EDTA solution from a burette until the color
changes from wine red to blue. Repeat the titration until the concurrent value is obtained.

Observations and Calculations:

Molarity of EDTA = 0.01M

Part-1: Determination of Total Hardness of water:

Volume of water Burette reading (ml) Volume of EDTA Solution
S.No.
sample (ml) Initial Final run down (X ml)

Part-2: Determination of Permanent Hardness of water:

Volume of boiled Burette reading (ml) Volume of EDTA Solution
S.No.
water sample (ml) Initial Final run down (X ml)
 Calculations:
1000 mL of 1 M EDTA = 100 g of CaCO3
X ×0.1 ×100
X mL of 0.1 M EDTA = g of CaCO3
1000 ×1

= ____ x 1000 mg of CaCO3

Volume of EDTA × Molarity of EDTA × 100 ×1000

Total hardness in 10 mL of water sample = mg
1000 ×1

Volume of EDTA × Molarity of EDTA × 100 ×1000

Total hardness of 1 Litre water = mg of CaCO3/L
10

Permanent hardness of 1 Litre water =

Volume of EDTA(boil)× Molarity of EDTA ×100 ×1000
= mg of CaCO3/L
10

Temporary hardnessofwater = Total hardnessofwater – Permanent Hardness of water.

=
Result:
Total Hardness of the given water sample
Permanent hardness of water sample
Temporary hardness of water sample
= mg of CaCO3/ Lit. or ppm
= mg of CaCO3/ Lit. or ppm
= mg of CaCO3/ Lit. or ppm
Expt.No:6

DETERMINATION OF THE CONCENTRATION OF ACETIC ACID USING SODIUM

HYDROXIDE (PH-METRY METHOD)

Aim: To determine the concentration of acetic acid present in the given solution using sodium hydroxide
by pH-metry method.
Chemicals: Buffer solution, Acetic Acid, Sodium Hydroxide etc.
Apparatus: pH meter, glass electrode.
Theory:
pH of any solution depends upon the concentration of H+ or OH- ions and can be measured by using a PH
meter containing a glass electrode. When a base is added to an acid its P H value increases due to
neutralization. Similarly the PH of a base decreases when an acid is added to it

CH3COOH + NaOH → CH3COONa + H2O

By noting down various values of PH for various volumes of acid or base added, the concentration of
acid or base can be determined. The use of a p H meter permits a more accurate location of the end points in
a titration than does an indicator.

Calibration Procedure:
In order for the pH electrode to give accurate measurements, it must be calibrated with buffer solutions
having known pH values.
1) Plug the cable of the pH electrode.
2) Wash the electrode carefully with DI water by directing a stream of water and wipe with a tissue paper.
3) Switch on the pH mode. Adjust calibration knob to the value Ph 7, now switch on the STANDARD BY
mode.
4) Rinse the electrode with DI water and wipe with a tissue paper.
5) Place the electrode in enough pH buffer solution to completely cover the glass bulb. Switch on the pH
mode and adjust the value to pH4.
6) You have now completed a “two point calibration”, which means your pH readings are fairly accurate
as long as the pH is between ~4 and7.
7) Once the pH of the solution you are titrating reaches 7 you will need to recalibrate using buffer
solutions of 7 and 10, respectively.
8) Rinse the electrode again with DI water and wipe with tissue paper.

Procedure:
Titration of acetic acid solution pH metrically:
1) 10 ml of CH3COOH is pipette out in to a beaker and 100ml of distilled water is added to it.
2) Glass electrode is dipped in to it and by switching on PH meter, the PH value is noted.
3) 2ml of NaOH is added to CH3COOH solution through a burette. The solution is mixed and pHvalue is
noted.
4) This procedure is repeated by noting PH values for every addition of 2ml of NaOH. After some time,
the pH of the solution increases slowly. But at the equivalence point, the rate of change of pH is very
rapid. However, the procedure is continued with addition of NaOH for some time.

Graph: A graph is plotted between volume of NaOH on X axis and corresponding P H on Y axis. The
volume of sodium hydroxide at equivalence point corresponding to P H = 7 is noted from the graph. The
sharp break in the curve gives the equivalence point from which the strength can be evaluated, using
normality equation.

𝑝𝐻 = −log[𝐻+]
The pH of solution is defined as the negative logarithm of the hydrogen ion concentration.

Solution:
1) NaOH (0.1M) : Dissolve 4 g of NaOH in DI water and make upto 1litre.

Observations and calculations:

S.No. Volume of NaOH Added (ml) pH of the solution
Formula:
V1M1 V M
2 2
n1  n2
Where;
M1 = Molarity of CH3COOH solution =?
V1 = Volume of CH3COOH solution = 10ml
n1 = No. of moles of CH3COOH taken part in the reaction = 1
M2 = Molarity of NaOH solution =0.1M
V2 = Volume of NaOH solution (from the graph) =
n2 = No. of moles of NaOH taken part in the reaction =1

V 2 M 2 n1
M 1=
 V 1 n2 =
.

𝑀1×𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 (60)×1000

Amount of Acetic Acid present in given 1 lit of solution =
1000

= g/L

Result:
Concentration of CH3COOH present in the given solution= M
Amount of CH3COOH present in given sample solution= g /L
Expt.No:7

DETERMINATION OF THE CONCENTRATION OF STRONG ACID VS STRONG BASE

(CONDUCTOMETRIC METHOD)

Aim: Determination of strength of HCl solution by titrating it against NaOH solution

conductometrically.
Apparatus: conductivity meter, conductivity cell.

Chemicals: KCl NaOH , HCl and distilled water.

Theory: End point of a volumetric analysis can also be found by conductometric titration which involves
measurement of conductance of solution during titration. The principle of these titrations is that
electrolytic conductance varies during the course of titration as it depends upon ions in solution and their
mobility. It is measured in ‘Mhos’. The conductance of an acid like HCl depends upon the no. of H+ ions.
When a base NaOH is added, the conductance of acid decreases due to formation of H2O. The end point
is found from a plot of conductance values against volume of titrant added which gives two lines
intersecting each other. The point of intersection gives the end point of titration.

𝐻 + + 𝐶𝑙− + 𝑁𝑎+ + 𝑂𝐻− → 𝑁𝑎+ + 𝐶𝑙− + 𝐻2𝑂

On adding NaOH from burette, the conductivity goes on decreasing till the equivalence point or
neutralization point is reached, it is because fast moving H+ ions of HCl are neutralized and replaced by
slow moving Na+ ions. From equivalence point, added NaOH increases the conductance of solution due
to addition of highly mobile OH- ions, conductivity is minimum at equivalent point. On plotting
conductance vs vol. of NaOH added, a V-shaped graph is obtained (Fig 1). The point of intersection of
two lines gives end point. From volume of NaOH used at end point, the strength of HCl solution can be
determined.

Graph: A graph is plotted between conductance on Y axis and volume of NaOH added on X axis.
From the graph the volume of NaOH at equivalence point is noted.

Procedure
1) Calibrate the conductivity meter using N/10KCl.
2) Pipette out 10 mL of given HCl solution in a 100 mL beaker.
3) Add 100 ml of conductivity water to it.
4) Dip conductivity cell in HCl solution.
5) Note down the conductance value of solution.
6) Add 2 mL of N/10 NaOH solution from burette. Stir solution with a glass rod and note down the
conductance of solution when it becomes stable.
7) Add NaOH solution in 2 mL lots and note the corresponding conductance values till conductance
becomes constant.
8) Plot a graph between conductance (Y-axis) and volume of added NaOH solution (along X-axis).
9) Find out the volume of NaOH used at end point of intersection of two lines in graph.

conductance (mho)

volume of NaOH added (mL)

Fig. 1: plot of conductance vs volume of NaOH added

Observations and calculations:

S.No. Volume of NaOH Added(ml) Conductance (ms/s)
Formula:
V1M1 V M
2 2
n1  n2
Where
M1 = Molarity of HCl solution =?
V1 = Volume of HCl solution = 10ml
n1 = No. of moles of HCl taken part in the reaction = 1
M2 = Molarity of NaOH solution = 0.1M
V2 = Volume of NaOH solution (from the graph) =
n2 = No. of moles of NaOH taken part in the reaction = 1
V 2 M 2 n1
M 1=
 V 1 n2 =

Amount of HCl present in given 1 liter solution = [𝑀1× 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 (36.5) × 1000] ÷1000

= –––––––––
= g/L

Result:
Concentration of HCl present in the given solution= M
Amount of HCl present in given sample solution= g /L
Expt.No:8

DETERMINATION OF CONCENTRATION OF STRONG ACID VS STRONG BASE

(POTENTIOMETRIC METHOD)

Aim: To estimate the strength of given HCl solution by titrating against standard NaOH solution.
Requirements: Potentiometer, calomel electrode, platinum electrode, beaker, stirrer, HCl, standard NaOH
solution.
Chemical equations:
HCl +NaOH→ NaCl + H2O
Theory:
In a potentiometric titration, a suitable electrode is immersed in the solution to be titrated acts
as the indicator. The indicator electrode is paired with a reference electrode and the two electrodes are
connected to an electronic voltmeter. Since the reference electrode potential has a constant value, any
change in the indicator electrode potential is reflected by a similar change in the cell potential. Therefore
the equivalence point can be found by plotting a graph between the cell e.m.f and the volume of titrant
added from the burette.
Procedure:
The potentiometer is calibrated and kept ready along with the electrodes.10ml of HCl is pipette
out in to a beaker and 100ml of distilled water is added to it. Electrodes are dipped in to it and by switching
on potentiometer, e.m.f is noted. 2ml of NaOH is added to HCl solution through a burette. The solution is
mixed and e.m.f is noted. This procedure is repeated by noting e.m.f values for every addition of 2ml of
NaOH. After some time, the e.m.f becomes negative. However, the procedure is continued with addition of
NaOH for some time.

Observations and Calculations:

S.No. Volume of NaOH Added (ml) e.m.f.of the cell (mV)
Graph:
Plot a graph by taking e.m.f along y – axis and volume of NaOH added along x – axis. The
volume corresponding to the steepest curve is the equivalence point.

Formula:
V1M1 V M
2 2
n1  n2
Where;
M1 = Molarity of HCl solution =?
V1 = Volume of HCl solution = 10ml
n1 = No. of moles of HCl taken part in the reaction = 1
M2 = Molarity of NaOH solution = 0.1M
V2 = Volume of NaOH solution (from the graph) =
n2 = No. of moles of NaOH taken part in the reaction = 1

V 2 M 2 n1
M 1=
 V 1 n2 =

Amount of HCl present in given 1 lit. of solution = M1 x Molecular weight (36.5) x1000
1000
=
= ––––––––– g

Precautions:
1. Stirring should be done after each addition of titrant.
2. All precautions regarding the handling of the instrument should be observed.
3. Electrodes should be used with great care.

Result:
Concentration of HCl present in the given solution = _________M
Amount of HCl present in given sample solution= g /L
 Expt.No:9
ESTIMATION OF VITAMIN C
(Iodometric titration)

Aim: Estimation of vitamin C in juices and real lemon using iodometric method.
Apparatus: Conical flask, burette, pipette, beaker, volumetric flask, burette stand.
Chemicals: potassium iodide, iodine crystals, sulphuric acid, starch, vitamin C and Test solution.
Theory:
Many vegetables also contain large quantities of vitamin C, but ascorbic acid is commonly destroyed by
many cooking processes, and hence citrus fruits are regarded as the most reliable source of vitamin C.
Vitamin C can be determined in food by use of an oxidation-reduction reaction. The redox reaction is
preferable to an acid-base titration because a number of other species in juice can act as acids, but relatively
few interfere with the oxidation of ascorbic acid by iodine. The solubility of iodine is increased by
complexation with iodide to form tri iodide:
-
I2 (aq) + I− → I3
Tri iodide then oxidizes vitamin C to dehydro ascorbic acid:

C6H8O6 + I3 - + H2O → C6H6O6 + 3I− + 2H+

The endpoint is indicated by the reaction of iodine with starch suspension, which produces a blue-black
product. As long as vitamin C is present, the tri iodide is quickly converted to iodide ion, and no blue-black
iodine-starch product is observed. However, when all the vitamin C has been oxidized, the excess tri iodide
(in equilibrium with iodine) reacts with starch to form the expected blue-black color.

Solutions:
1) Iodine solution: Dissolve 2 g of potassium iodide (KI) and 1.3 g of Iodine crystals in 1000 ml
volumetric flask and make up to the mark.
2) Vitamin C standard solution: Dissolve 0.250 g of vitamin C in DI water and make up to 250ml.
3) Starch: Dissolve 1 g of starch in 100ml of water.

Procedure:
Part – 1: Standardization of the iodine solution:
Add 10 ml of vitamin C solution into a conical flask. Add 10 drops of 1 % starch solution. Rinse the
burette twice with 5 -10 ml of iodine solution, and then fill it. Titrate the solution until the solution turns
to blue colour. (That remains after at least 20 seconds of swirling). Record the final volume. Repeat this
titration at least three times. Results should agree to 0.1ml.

Part – 2: Titration of test samples:

Add 10 ml of your beverage sample into a conical flask. Add 10 drops of 1 % starch solution. Rinse the
burette twice with 5 -10 ml of iodine solution, and then fill it. Titrate the solution until the solution turns
to blue colour. (That remains after at least 20 seconds of swirling). Record the final volume. Repeat this
titration at least three times. Results should agree to 0.1ml.
Observations and Calculations:
Part-1: Standardization of iodine solution:
Volume of vitamin Burette reading (ml) Volume of iodine Solution
S.No.
C solution (ml) Initial Final run down (ml)

V 1 M1 V 2 M2
=
n1 n2

Where
Vitamin C Iodine solution
M1 = Molarity of standard Vitamin C solution M2 = Molarity of Iodine solution =
=0.0056M
V2 = Volume of iodine solution =
V1 = Volume of standard Vitamin C solution
=10 ml n2 = No. of moles of Iodine taken part in the
reaction =1
n1 = No. of moles of standard Vitamin C taken
part in the reaction =1

V 1 M 1 n2
M 2=
V 2 n1 =
Part-2: Estimation of vitamin C:

Volume of test Burette reading (ml) Volume of iodine Solution

S. No.
solution (ml) Initial Final run down (ml)
 V 2M2 V 3 M3
=
n2 n3

Where
Iodine solution Test solution
M2 = Molarity of Iodine solution = M3 = Molarity of test solution =

V2 = Volume of iodine solution = V3 = Volume of test solution =10ml

n2 = No. of moles of Iodine taken part in the n3 = No. of moles of test solution taken part in
reaction =1 the reaction=1

V 2 M 2 n3
M 3=
 V 3 n2 =

Amount of ascorbic acid present in the given sample

= Molarity of test solution x Mol.Wt of ascorbic
acid x 1000 1000
= M3 x 176
=

Result: The amount of ascorbic acid present in the given sample= –––––––––––gm/lit
Expt.No:10 Date:

DETERMINATION OF PHOSPHORIC ACID CONTENT IN SOFTDRINKS

Aim: To determine the amount of phosphoric acid in the soft drinks

Apparatus: pH meter, Combined electrode.
Chemicals: Soft drink sample, 0.1 M NaOH, pH 4,7 &10 buffers.
Theory:
Phosphoric acid is one of several weak acids that exist in carbonated beverages. It is a component of all
cola soft drinks. Phosphoric acid has a much higher concentration than other acids in a container of soft
drink, so its concentration can be determined by a simple acid-base titration.

Phosphoric acid (H3PO4, a tri protic acid, is a common ingredient in cola drinks. It provides a taste that is
both sweet and sour, but does not compete with other flavors. The concentration of phosphoric acid in cola
drinks is dependent on pH:
H3PO4 + OH− →H2PO4− + H2O
H2PO4− + OH− → HPO4-2
+ H2O HPO4-2 + OH− →
PO4-3 + H2O
−
In this experiment, we will determine the H3PO4 and H2PO4 concentrations in a sample of a cola drink
using a pH titration. We choose a pH detection method over an acid-base indicator for two reasons: (1) the
color of the cola obscures indicator changes, and (2) the use of a pH meter permits a more accurate location
of the end points in a titration than does an indicator.

Solution:
NaOH (0.1 M): Dissolve 4 g of NaOH in DI water and make up to 1 litre.

Calibration Procedure:
In order for the pH electrode to give accurate measurements, it must be calibrated with buffer solutions
having known pH values.
1) Plug the cable of the pH electrode.
2) Wash the electrode carefully with DI water by directing a stream of water and wipe with a tissue paper.
3) Switch on the pH mode. Adjust calibration knob to the value Ph 7, now switch on the STANDARD BY
mode.
4) Rinse the electrode with DI water and wipe with a tissue paper.
5) Place the electrode in enough pH buffer solution to completely cover the glass bulb. Switch on the pH
mode and adjust the value to pH4.
6) You have now completed a “two point calibration”, which means your pH readings are fairly accurate
as long as the pH is between ~4 and7.
7) Once the pH of the solution you are titrating reaches 7 you will need to recalibrate using buffer
solutions of 7 and 10, respectively.
8) Rinse the electrode again with DI water and wipe with tissue paper.
Procedure:
1) Use a graduated cylinder to measure out 10 mL of a decarbonated cola beverage and 40 mL of distilled
water into a 250-mLbeaker.
2) Place the beaker on a magnetic stirrer and add a stirring bar. If no magnetic stirrer is available, you
need to stir with a stirring rod during the titration.
3) You are now ready to begin the titration.
4) Switch on the pH mode.
5) 5.Refill your burette with the 0.1 M NaOH solution, Add 1 mL of NaOH titrant to the sample. Mix well
the solution and note down the pH value.
6) Continue to add 1 mL increments, of the soda solution as you did for the NaOH standardization (except
that there is no indicator here). Once the pH of the solution you are titrating reaches 7, you will need to
recalibrate using buffer solutions of 7 and 10 respectively. Continue to pH 10.5.When the pH has
leveled off (near pH 10), stop and graph.
7) Plot a graph between the volume of NaOH added on X and pH on Y axis as displayed below the graph.
To determine the equivalence point, go to the region of the graph with the large increase in pH.
Examine the data in this section to find the largest increase in pH upon the addition of NaOH solution.
Find and record the NaOH volume just before this jump. Then record the NaOH volume after the
largest pH increase.
8) Add the two NaOH values determined above and divide by two.
9) Rinse the pH electrode and return it to the storage solution.

Observations and Calculations:

S.No. Volume of NaOH Added (ml) pH of the solution

Calculations:
V 1 M1 V 2 M2
=
n1 n2
M1 = Molarity of NaOH solution = 0.1 M
V1 = Volume of NaOH obtained from graph average = ml
n1 = no of moles of NaOH taken part in reaction =3
M2 = Concentration of H3PO4 in soft drink sample =
V2 = Volume of soft drink sample H3PO4 = 10ml
n2 = no of moles of H3PO4 reacted in reaction =1

V 1 M 1 n2
M 2=
 V 2 n1 =

Result: Concentration of H3PO4 in soft drink sample= moles /L

Expt.No:11
PREPARATION OF BAKELITE

Aim: To prepare Phenol formaldehyde (P-F) resin.

Chemicals : Phenol (2g), 40% aq. formaldehyde solution or formalin (2.5 mL), glacial acetic acid (5 mL)
and conc. HCl (8mL).
Theory: Phenol formaldehyde resin or P-F resin or phenolic resins (also called phenoplasts) are important
class of polymers which are formed by condensation polymerization of phenol and formaldehyde in acidic
or alkaline medium. Following steps are involved:

Step 1: Formation of methylol phenol derivative:

Initially the monomers combine to form methylol phenol derivative depending upon phenol to
formaldehyde ratio.

Step II:
The mono, di, and tri methylol phenols are heated to produce two types of straight chain resins by
condensation of the methylol group with hydrogen atom of benzene ring or another methylol group.
Step III: This stage of preparation includes heating of 'A' stage resin and 'B' stage
resin together, which develops cross linking and bakelite plastic resin is produced.

Procedure:
1) Place 5 mL of glacial acetic acid and 2.5 mL of 40 % aq formaldehyde solution
in a 100 mL beaker. Add 2 g phenol safely.
2) Wrap the beaker with a wet cloth or place it in a 250 mL beaker having small amount of
water in it.
3) Add conc. HCl drop wise with vigorous stirring by a glass rod till a pink
coloured gummy mass appears.
4) Wash the pink residue several times with to make it free from acid.
5) Filter the product and weigh it after drying in folds of a filter or in an oven.
Report the yield of polymer formed.
Precautions:
1) Handle phenol carefully.
2) While adding conc. HCl, it is better to stay a little distance away from the
beaker since the reaction sometimes becomes vigorous.
3) The reaction mixture should be stirred continuously.

Observations:
Weight of empty watch glass = W1 g
Weight of watch glass + poymer formed = W2 g
Weight of polymer formed = W2 – W1 g

Result: Weight of phenol formaldehyde resin =Wg