UNIT 1 INORGANIC QUANTITATIVE AND QUALITATIVE ORGANIC ANALYSIS

Structure
1.1 1.2 Introduction
Objectives

Inorganic Quantitative and Qualitative Organic Analysis

Experiment No. 1 : To Determine the Strength of an Unknown Solution of Mohrs Salt Volumetric Analysis Redox Titration
1.2.1 1.2.2 1.2.3 1.2.4 1.2.5 1.2.6 Principle Requirements Procedure Observations Calculations Result

1.3

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

1.3.1 1.3.2 1.3.3 1.3.4 1.3.5 Principle Requirements Procedure Observations Result

1.4

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

1.4.1 1.4.2 1.4.3 1.4.4 1.4.5 Principle Requirements Procedure Observations 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. 5

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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 MOHRS 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 Mohrs salt solution with potassium permanganate solution. Mohrs salt, i.e. ferrous ammonium sulphate [FeSO4. (NH4)2SO4. 6 H2O] behaves as a reducing agent whereas potassium permanganate (KMnO4) acts as an oxidising agent. 5 [Fe+ 2 MnO4 Fe+ 3 + e] +8H +5e
+

(Oxidation reaction) Mn
+2

+ 4H2O (Reduction reaction)

MnO4 + 5 Fe+ 2 + 8 H+

5 Fe+ 3 + Mn+ 2 + 4H2O

In this titration, the end point can be detected by the colour change of a redox indicator. Here, KMnO4 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) (ii) (iii) Self indicator Internal Indicator External indicator

Self Indicator It is one of the reacting species itself which changes the colour at the equivalence point, e.g. KMnO4. 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. 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, K3[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, KMnO4 will be behaving as a strong oxidizing agent.

Inorganic Quantitative and Qualitative Organic Analysis

SAQ 1
(a) (b) (c) What are the basic criteria for selecting a substance to be a primary standard? Why cannot FeSO4 salt be used as a primary standard instead of Mohrs salt? Why is redox titration Mohrs salt vs KMnO4 carried out in an acidic medium?

1.2.2

Requirements
Apparatus Burette (50 mL) Pipette (20 mL) Conical flasks (250 mL) Volumetric flask (250 mL) Weighing bottle Beaker (250 mL) Funnel Test tube Burette stand Quantity 1 1 1 1 1 2 1 1 1 Chemicals Mohrs salt Sulphuric acid Potassium permanganate

Solution Provided (i)

M Standard Mohrs Salt Solution : Weigh accurately 1.96 g of Mohrs 50 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 H2SO4 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. H2SO4 is mandatory otherwise the solution will turn brownish in colour due to the arial oxidation of Fe+ 2 to Fe+ 3 ions.
M KMnO4 Solution : 0.79 g of KMnO4 is dissolved in 250 mL of 250 distilled water and stored in a cool place.
Indicator : KMnO4 acts as a self indicator.

(ii)

(iii)

1.2.3

Procedure
(a) Mount the burette on the burette stand and fill it with the prepared M KMnO4 solution. Note down the initial reading in Observation 250 Table 1.1 in the initial reading column.

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

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(b)

M Pipette out 20 ml of standard Mohrs salt solution into a 250 mL 50 conical flask and add 10 to 20 mL of dil. H2SO4 to it to make the medium acidic.
Titrate the Mohrs salt solution by adding KMnO4 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 Mohrs salt solution of unknown strength with KMnO4 salt solution and record the readings in observation Table 1.2.

(c)

(d) (e)

1.2.4

Observations

Approximate mass of the weighing bottle = m1 = ---------------g Mass of bottle + mohrs salt (before transfer) = m2 = ---------------g Mass of bottle (after transfer) = m3 = ---------------g Actual mass of mohrs salt = m2 m3 = m4 = ---------g Molar mass of mohrs salt = 392.15 g mol 1 Volume of mohrs salt solution prepared (V ) = 250 mL Molarity of mohrs salt solution (m1) = =

m4 1000 mol L1 molar mass 250

m4 mol L1 = . . . mol L1. 392.15

Observation Table 1.1

Standard Mohrs Salt Solution vs KMnO4 Solution Sl. No. Volume of Mohrs Salt Solution in mL Burette Reading Initial 1 2 3 20 20 20 Final Volume of KMnO4 Consumed in mL (Final Initial)

Observation Table 1.2

Given Mohrs Salt Solution vs KMnO4 Solution Sl. No. Volume of Mohrs Salt Solution in mL Burette Reading Initial 1 2 3 20 20 20 Final Volume of KMnO4 Consumed in mL (Final Initial)

1.2.5

Calculations

Molarity of Mohrs salt solution= M1 = ------- mol L 1 Vol. of mohrs salt solution = V1 = -------- 20 mL Vol. of KMnO4 solution consumed (from Table 1.1) = V2 = -------- mL 8 Molarity of KMnO4 solution = M2 = -------- ?

From the principle, it is known that one mole of KMnO4 reacts with 5 moles Mohrs salt solution ions, i.e. ferrous ions. Therefore.

Inorganic Quantitative and Qualitative Organic Analysis

M1 V1 = 5M 2 V2

M2 =

M1 V1 = . . . mol L 1 5V2

The estimation of strength of ferrous ions solution from the given solution. Molarity of KMnO4 = M3 = M2 = ---------- mol L 1 Vol. of KMnO4 solution used = V3 = ------- mL From observation Table 1.2 Vol. of mohrs salt solution (given) = V4 = 20 mL Molarity of mohrs salt solution = M4 = ? or,

M 4 V4 = 5M 3 V3
M4 = 5M 3 V3 = . . . mol L 1 V4

Then the strength of the mohrs salt solution = Molarity Molar mass = ------- g L 1.

1.2.6

Result

The strength of the given mohrs 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 Thermometre Melting point determination apparatus (Thieles tube) Capillary tubes Bunsen burner Mortar and Pestle (to grind) Stand to hold the m. p. apparatus Quantity 1 1 3 1 1 1 Chemicals Paraffin oil or Sulphuric acid Any organic compound

1.3.3

Procedure
(i) The compound whose melting point is to be determined is thoroughly powdered using the mortar and pestle. 9

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

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(ii) (iii) (iv)

A capillary tube of suitable length is sealed at one end by heating in a Bunsen burner. The powdered compound is filled up to 1 cm length in the capillary tube. The capillary tube and the thermometer are placed in a Thieles tube filled with paraffin oil or concentrated H2SO4 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. The flask is gently heated to raise the temperature. Observe carefully the temperature in the thermetre and the compound. The temperature at which the substance begins to liquefy is noted.

(v) (vi)

(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. 1. 2. 3. Solid Begins to Liquefy (in oC) Solid Completely Liquefied (in oC)

1.3.5
SAQ 2

Result

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

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
Apparatus Ignition tube Capillary tube Thermometre Stand to hold thermometre and ignition tube Rubber cork Bunsen burner Pyrex test tube Quantity 1 1 1 1 1 1 1 Chemicals Substance (liquid) for which boiling point is to be determined. Conc. H2SO4

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1.4.3

Procedure

For experimental work, the following steps are to be followed : (i) (ii) (iii) (iv) A few drops of the liquid, for which the boiling point is to be determined, is taken in an ignition tube. The capillary tube, sealed at one end, is put inside the ignition tube such that the sealed end should be at the upper side. This ignition tube is attached to the lower part of the thermometre with the help of a rubber thread (Figure 1.1). 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. H2SO4 which is taken in the test tube. The test tube is heated slowly to raise the temperature. 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.

Inorganic Quantitative and Qualitative Organic Analysis

(v) (vi)

(vii) Repeat the above procedure for getting a consistent value of the boiling point.
Thermometer

Pyrex test tube Ignition tube Capillary Testing Liquid Conc. H2SO4

Figure 1.1 : Boiling Point Apparatus

1.4.4

Observations
Table 1.4 : Boiling Point of the Liquid
Sl. No. 1. 2. 3. (in oC)

1.4.5 SAQ 3

Result

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

Define boiling point and give its importance.

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