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UNIT 1

INORGANIC QUANTITATIVE AND QUALITATIVE ORGANIC ANALYSIS

Inorganic Quantitative and Qualitative Organic Analysis

Structure

1.1 Introduction

Objectives

1.2 Experiment No. 1 : To Determine the Strength of an Unknown Solution of Mohr’s Salt Volumetric Analysis – Redox Titration

1.2.1 Principle

1.2.2 Requirements

1.2.3 Procedure

1.2.4 Observations

1.2.5 Calculations

1.2.6 Result

1.3 Experiment No. 2 : Determination of Melting Point of a Given Organic Compound

1.3.1 Principle

1.3.2 Requirements

1.3.3 Procedure

1.3.4 Observations

1.3.5 Result

1.4 Experiment No. 3 : Determination of Boiling Point of a Given Organic Compound

1.4.1 Principle

1.4.2 Requirements

1.4.3 Procedure

1.4.4 Observations

1.4.5 Result

1.1

INTRODUCTION

The determination of the amounts of the individual components of a substance is the primary concern of quantitative analysis whereas qualitative analysis aims at the detection of the constituents (elements, ions etc.) present in a substance based on the study of physical and chemical properties.

Volumetric analysis estimates the quantities of chemical species indirectly by measuring the volume of the solution of that particular species in a suitable solvent. The law of equivalence principle is generally applied to all volumetric estimations. According to the Law of equivalence, the masses of the species which react are always in ratio of their chemical equivalent weights. The basic rule in titration is the standardisation of a given solution with a standard solution. For standard solution preparation, a chemical substance called a primary standard is used. The following criteria is used for choosing a substance as a primary standard :

It must be easily available in highly pure state.

It must be easily soluble in the desired solvent.

It must not decompose in presence of solvent, i.e. it should be stable.

It must not be a hygroscopic in nature.

Its composition must not change on standing.

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Those substances which do not fulfill the above requirements, cannot be used as a primary standard.

The identification of organic compounds by qualitative analysis involves a series test of a chemical characteristics and then a careful correlation of observed facts. In this unit, you will perform the redox titration for inorganic quantitative analysis and melting and boiling point determination under organic qualitative analysis.

Objectives

After performing the experiments, you will be able to :

define oxidation-reduction and redox titration,

define the melting point and boiling point of an element,

explain the use of various types of redox indicators,

state the basic criteria for standard solutions, and

differentiate the qualitative and quantitative tests.

1.2 EXPERIMENT NO. 1 : TO DETERMINE THE STRENGTH OF AN UNKNOWN SOLUTION OF MOHR’S SALT VOLUMETRIC ANALYSIS – REDOX TITRATION

1.2.1

Principle

A redox titration is based upon the oxidation-reduction reaction between a titrand and a

titrant. In this experiment you will titrate Mohr’s salt solution with potassium permanganate solution. Mohr’s salt, i.e. ferrous ammonium sulphate [FeSO 4 . (NH 4 ) 2 SO 4 . 6 H 2 O] behaves as a reducing agent whereas potassium permanganate (KMnO 4 ) acts as an oxidising agent.

(Oxidation reaction)

5 [Fe + 2

Fe + 3 + e]

MnO 4 + 8 H +

+ 5 e

Mn + 2 + 4H 2 O

(Reduction reaction)

MnO 4 + 5 Fe + 2 + 8 H +

5 Fe + 3 + Mn + 2 + 4H 2 O

In this titration, the end point can be detected by the colour change of a redox indicator.

Here, KMnO 4 acts as a self indicator. In the redox titrations, a chemical substance which

changes colour when the potential of the solution reaches a definite value is termed as redox indicator. In general, there are three types of indicators which are as follows :

(i)

Self indicator

(ii)

Internal Indicator

(iii)

External indicator

Self Indicator

It is one of the reacting species itself which changes the colour at the equivalence point, e.g. KMnO 4 .

Internal Indicator

There are certain indicators need to be added to the solution which change the colour at the equivalence point is known as internal indicator. For example, phenolphthalein which acts as an indicator in acid-base titrations.

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External Indicator

External indicators are not added into the solution but are kept outside the solution. At various stages of the titration, a drop of the reaction mixture is taken out and

tested for the colour change. For example, potassium ferricyanide, K 3 [Fe(CN) 6 ], is used in titration of ferrous ions with dichromate.

Here, the titration will be carried out in acidic medium because in the acidic medium, KMnO 4 will be behaving as a strong oxidizing agent.

SAQ 1

Inorganic Quantitative and Qualitative Organic Analysis

(a)

What are the basic criteria for selecting a substance to be a primary standard?

(b)

Why cannot FeSO 4 salt be used as a primary standard instead of Mohr’s salt?

(c)

Why is redox titration Mohr’s salt vs KMnO 4 carried out in an acidic medium?

1.2.2 Requirements

Apparatus

Quantity

Chemicals

Burette (50 mL)

1

Mohr’s salt

Pipette (20 mL)

1

Sulphuric acid

Conical flasks (250 mL)

1

Potassium permanganate

Volumetric flask (250 mL)

1

Weighing bottle

1

Beaker (250 mL)

2

Funnel

1

Test tube

1

 

Burette stand

1

 

Solution Provided

 

M

(i)

50

Standard Mohr’s Salt Solution : Weigh accurately 1.96 g of Mohr’s

salt and transfer it to a clean and dry 250 ml volumetric flask with the help

of a funnel. To this, add 10 to 20 ml of dilute H 2 SO 4 and about 50 ml of distilled water. Shake and dissolve the salt completely. Finally, make the volume up to the mark by adding distilled water. Addition of dil. H 2 SO 4 is mandatory otherwise the solution will turn brownish in colour due to the arial oxidation of Fe + 2 to Fe + 3 ions.

M

(ii)

250

KMnO 4 Solution : 0.79 g of KMnO 4 is dissolved in 250 mL of

distilled water and stored in a cool place.

(iii)

Indicator : KMnO 4 acts as a self indicator.

1.2.3 Procedure

For experimental work, the following steps are to be followed.

(a) Mount the burette on the burette stand and fill it with the prepared

M

250

KMnO 4 solution. Note down the initial reading in Observation

Table 1.1 in the initial reading column.

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(b)

(c)

(d)

(e)

Pipette out 20 ml of standard Mohr’s salt solution

M

50

into a 250 mL

conical flask and add 10 to 20 mL of dil. H 2 SO 4 to it to make the medium acidic.

Titrate the Mohr’s salt solution by adding KMnO 4 solution drop wise from the burette with constant shaking till the colour changes from colourless to pink. This is the end point. Note this reading and record it in Observation Table 1.1 under final reading column.

Repeat the above steps, i.e. (a) to (c) to get a concordant reading.

Follow the same procedure to titrate the given Mohr’s salt solution of unknown strength with KMnO 4 salt solution and record the readings in observation Table 1.2.

1.2.4 Observations

Approximate mass of the weighing bottle = m 1 = ---------------g

Mass of bottle + mohr’s salt (before transfer) = m 2 = ---------------g

Mass of bottle (after transfer) = m 3 = ---------------g

Actual mass of mohr’s salt = m 2 m 3 = m 4 = ---------g

Molar mass of mohr’s salt = 392.15 g mol 1

Volume of mohr’s salt solution prepared (V ) = 250 mL

Molarity of mohr’s salt solution (m 1 ) =

m

4

×

1000

molar mass

×

250

=

m ×

4 molL

392.15

1

=

Observation Table 1.1

molL

1

molL

1

.

 

Standard Mohr’s Salt Solution vs KMnO 4 Solution

Sl. No.

Volume of Mohr’s Salt Solution in mL

Burette Reading

Volume of KMnO 4 Consumed in mL (Final – Initial)

 

Initial

Final

1

20

     

2

20

     

3

20

     

Observation Table 1.2

 

Given Mohr’s Salt Solution vs KMnO 4 Solution

Sl. No.

Volume of Mohr’s Salt Solution in mL

Burette Reading

Volume of KMnO 4 Consumed in mL (Final – Initial)

 

Initial

Final

1

20

     

2

20

     

3

20

     

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1.2.5 Calculations

Molarity of Mohr’s salt solution= M 1 = ------- mol L 1

Vol. of mohr’s salt solution = V 1 = -------- 20 mL

Vol. of KMnO 4 solution consumed (from Table 1.1) = V 2 = -------- mL

Molarity of KMnO 4 solution = M 2 = -------- ?

From the principle, it is known that one mole of KMnO 4 reacts with 5 moles Mohr’s salt solution ions, i.e. ferrous ions. Therefore.

M V = 5MV

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2

2

M

2

=

M

1

V

1

5 V

2

=

mol L 1

Inorganic Quantitative and Qualitative Organic Analysis

The estimation of strength of ferrous ions solution from the given solution.

Molarity of KMnO 4 = M 3 = M 2 = ---------- mol L 1

Vol. of KMnO 4 solution used = V 3 = ------- mL

From observation Table 1.2

Vol. of mohr’s salt solution (given) = V 4 = 20 mL

Molarity of mohr’s salt solution = M 4 = ?

M

or,

M

V

44

4

=

= 5M

V

33

5M

3

V

3

V

4

=

mol L 1

Then the strength of the mohr’s salt solution = Molarity × Molar mass = ------- g L 1 .

1.2.6 Result

The strength of the given mohr’s salt solution is = ------- g L 1 .

1.3 EXPERIMENT NO. 2 : DETERMINATION OF MELTING POINT OF A GIVEN ORGANIC COMPOUND

1.3.1 Principle

Melting point is the temperature at which the solid state of an element or a compound starts melting and gets converted into the liquid state. This temperature remains fixed till the whole compound (or the element) has melted. Melting point is the most important criterion in the identification of an organic compound as the pure organic compounds have fixed and sharp melting points.

1.3.2 Requirements

Apparatus

Quantity

Chemicals

Thermometre

1

Paraffin oil or Sulphuric acid

Melting point determination apparatus (Thiele’s tube)

1

Any organic compound

Capillary tubes

3

 

Bunsen burner

1

Mortar and Pestle (to grind)

1

Stand to hold the m. p. apparatus

1

1.3.3 Procedure

For experimental work, the following steps are to be followed :

(i) The compound whose melting point is to be determined is thoroughly powdered using the mortar and pestle.

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(ii)

A capillary tube of suitable length is sealed at one end by heating in a Bunsen burner.

(iii)

The powdered compound is filled up to 1 cm length in the capillary tube.

(iv)

The capillary tube and the thermometer are placed in a Thiele’s tube filled with paraffin oil or concentrated H 2 SO 4 such that the liquid covers the filled length of the capillary. If the electrical melting point apparatus is available then you can directly put thermometre and capillary tube in the apparatus which is then heated electrically.

(v)

The flask is gently heated to raise the temperature. Observe carefully the temperature in the thermetre and the compound.

(vi)

The temperature at which the substance begins to liquefy is noted.

(vii)

The temperature at which the solid compound has completely changed into the liquid state is also noted.

(viii)

This range of temperature is recorded as melting point range of the substance. Repeat the steps to get a constant value for the melting point.

1.3.4 Observations

Table 1.3 : The Melting Point of a Substance

Sl. No.

Solid Begins to Liquefy (in o C)

Solid Completely Liquefied (in o C)

1.

   

2.

   

3.

   

1.3.5 Result

The melting point temperature of the given substance is = ----------- o C.

SAQ 2

Define the melting point of a given organic compound.

1.4 EXPERIMENT NO. 3 : DETERMINATION OF BOILING POINT OF A GIVEN ORGANIC COMPOUND

1.4.1 Principle

Like melting point, the boiling point is also an important criterion in the identification of a substance. The pure substance (e.g. organic compound) has a fixed boiling point. The boiling point is the temperature at which the liquid state changes into vapour state.

1.4.2 Requirements

10

Apparatus

Quantity

Ignition tube

1

Capillary tube

1

Thermometre

1

Stand to hold thermometre and ignition tube

1

Rubber cork

1

Bunsen burner

1

Pyrex test tube

1

Chemicals

Substance (liquid) for

which boiling point is to be determined.

Conc. H 2 SO 4

1.4.3 Procedure

For experimental work, the following steps are to be followed :

Inorganic Quantitative and Qualitative Organic Analysis

(i)

A few drops of the liquid, for which the boiling point is to be determined, is taken in an ignition tube.

(ii)

The capillary tube, sealed at one end, is put inside the ignition tube such that the sealed end should be at the upper side.

(iii)

This ignition tube is attached to the lower part of the thermometre with the help of a rubber thread (Figure 1.1).

(iv)

The thermometre along with the ignition tube is placed inside a pyrex test tube in such a way that the liquid inside the ignition tube is covered by conc. H 2 SO 4 which is taken in the test tube.

(v)

The test tube is heated slowly to raise the temperature.

(vi)

Observe the capillary carefully. Note that, after sometime, a regular and speedy stream of bubbles begins to rise inside the capillary. This temperature is the boiling point of the liquid. Note down this temperature in the Observation Table 1.4.

(vii)

Repeat the above procedure for getting a consistent value of the boiling point.

1.4.4 Observations

consistent value of the boiling point. 1.4.4 Observations Thermometer Pyrex test tube Ignition tube Capillary

Thermometer

Pyrex test tube Ignition tube Capillary Testing Liquid Conc. H 2 SO 4

Figure 1.1 : Boiling Point Apparatus

Table 1.4 : Boiling Point of the Liquid

Sl. No.

(in o C)

1.

 

2.

 

3.

 

1.4.5 Result

The boiling point of the given liquid substance is = ---------- o C.

SAQ 3

Define boiling point and give its importance.

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