PH. Analysis - UNIT 1 PART A

25/06/2024 Pharmaceutical Analysis 1
Analytical Chemistry
• Definition: The science that deals with the identification and quantification of the
components of material systems such as these is called analytical science. It is
called that because the process of determining the level of any or all components in
a material system is called analysis.
• It can involve both physical and chemical processes. If it involves chemical

processes, it is called chemical analysis or, more broadly, analytical chemistry. For
example, Fluoride content in water.
• Qualitative Analysis: The identification of one or more chemical species present in

a sample
• Quantitative Analysis: The determination of the exact amount of a chemical species

present in a sample
Analytical Chemistry
• Scope and Applications :
 Quality control
 Monitoring and control of pollutants.
 Clinical and biological studies
 Geological assays
 Fundamental and applied research
 If a material is known by a particular name and an analysis is carried out to

determine the level of that named substance in the material, the analysis is called an
assay for that named substance.

Analysis using physical properties
• It involves no chemical reactions and at times relatively simple devices (although
possibly computerized) to facilitate the measurement. Physical properties are
especially useful for identification.
 Melting point
 Boiling point
 Specific gravity
 Viscosity
 Refractive index,
 Solubility
 Particle size
 Optical rotation
Wet Chemical Analysis
 Volumetric Analysis: Analysis by volume
 Gravimetric Analysis: Analysis by mass
• Volumetric analysis refers to any procedure in which the volume of reagent needed
to react with the analyte is being measured.
• To perform a volumetric analysis is necessary to have a solution at known

concentration a glass vessel, a burette (calibrated tube able to measure volume,
equipped with a tap) and an indicator (chemical species able to change colour when
change the composition of the solution.
• One method in volumetric analysis is titration
• In titration: substance to be analysed is known as the analyte, the solution added to

the analyte is known as the titrant.Titrant is usually delivered from a buret

Titration
• A titration is a chemical reaction which allows to obtain the unknown concentration
of a reagent, A, by adding the reagent B and by stopping the addition when the
equivalent number of A and B are exactly equal.
• The point corresponding to meq* A = meq B is called equivalent point or point of

equivalence.
*meq = milli equivalents = VACA = VB CB

• Reaction must be:
 Quick
 Stoichiometric with known coefficients
 Collateral reactions must be absent
 Complete

Titration
1. Acid-Base
HCl + NaOH → H2O + NaCl
2. Redox
5NaC2O4 + 2 KMnO4 + 6H+ → 10CO2 + 2Mn2+ +8H2O
3. Precipitation
Ag+ + X- → AgX(s)
4. Diazotisation
The formation of diazonium ion
5. Complex formation
Ethylenediaminetetraacetic acid (EDTA) and
Metal ion
Pharmaceutical Analysis
Titration
 Equivalence point: Ideal theoretical result
• Quantity of added titrant is the exact amount necessary for stoichiometric reaction
with the analyte
• Equivalence point occurs when 2 moles of MnO4- is added to 5 moles of Oxalic

acid
Analyte Titrant (colorless) (colorless)
Oxalic acid (purple)
(colorless)
 End point
• It occurs from the addition of a slight excess of titrant
• Endpoint does not equal equivalence point

Titration
Analyte Titrant (colorless) (colorless)

Oxalic acid (purple)
(colorless)
After equivalence point occurs, excess MnO4- turns solution purple  Endpoint

Methods of expressing Concentration
• Chemical methods of expressing concentration are based upon chemical formula
or combining power, The word "Concentration" is frequently used as a general
term referring to a quantity of substance in a defined volume of solution. But for
quantitative titrimetric analysis use is made of standard solutions in which the base
unit of quantity employed is the "mole".
• Solution containing very small amounts of solute may be expressed is millimolar

(mM) concentration defined as the number of millimole/ml of solution.
(1 mM = 1x10-3 M)
• Normality (N) : The normality of a solution expresses the number of equivalents

(gram equivalent weight) of the solute in one litre of solution.This is generally a
much more useful expression since it is directly related to reactive concentrations
of various species in solution.
Methods of expressing Concentration
• Molarity (M) : The molarity of a solution expresses the number of moles (gram-
molecular weights) of solute contained in 1000 ml (1 Litre) of solution.
A solution containing 1 mole of solute in each litre of total solution is said to be a
one molar (M) solution.
• Molality (m) : The molality of a solution expresses as the number of moles of a

solute contained in 1000 gm of a solvent. This method of denoting concentration is
used in many equations to express thermodynamic properties of solutions.
• Formality (F) : Formality may be defined as the number of gram formula weight
(GFW) of the solute dissolved per litre of solution.
Formality (F) = GFW/Litres of solution

Standardization
• It is very hard to perform a volumetric analysis by comparing a solution with
another, without a reference point. It is necessary to have solutions at known
concentration, prepared by dissolving a known weight in a measured volume.
Compounds having such property are called mother substances or primary
standards.
• Process where the concentration of the titrant is determined exactly using "Primary
Standard" = ultrapure reagent where the number of moles is known exactly so it
can be used to accurately measure the titrant concentration.e.g.
2HCl + Na2CO3 → CO2 + H2O + 2NaCl
?? M Primary standard
(MW = 105.99)
99.99% pure
Primary standards
 A primary standard should:
• Be readily available
• Be available in a pure form
• Not readily react with the atmosphere
• Be easily stored
• Have a high molar mass
• Be inexpensive
 Common acidic and basic substances cannot be used as standard primary standards
because KOH, NaOH, HCl and H2SO4 are either impure or their exact
concentration may not be specified. The bases tend to absorb water as they react
with carbon dioxide in the air.

Standardization
 Preparation and standardization
• Oxalic acid
• 1M Sodium hydroxide
• 1M Hydrochloric acid
• 0.1M Sodium thiosulphate
• 0.5M Sulphuric acid
• 0.02M Potassium permanganate
• 0.1M Ceric ammonium sulphate
 Equivalent weight of Acid

• Equivalent weight of the substance is that weight which contains 1 gm of
replaceable hydrogen ion (1.008 gm).
 Equivalent weight of Base

• Equivalent weight of base is that weight which contains one gram of replaceable
hydroxyl groups i.e., 17.008 gm of hydroxyl ion
Preparation
• Stock bottle of 37% HCl
Molarity of 37% HCl V/V (37 ml of solute/100 ml of solution)
• HCl - 37% v/v. Specific gravity: 1.19 g/ml
37ml/100 ml or 370 ml/1000 ml x 1.19 g/ml = 440.3 g/L
• HCl Molecular weight = 36.5
Molarity: 440.3 grams /36.5 grams = 12.06 M or ~12M
• Compounding 1 liter of 0.1N Solution
M1V1 = M2V2
(0.1)(1000) = (12) (x)
• x = (0.1) (1000) / 12 = 8.3 ml
• Therefore add 8.3 ml of 37% HCl to 1 liter of DW to create a 0.1N HCl solution.

Standardization
Titrant /Secondary Titre/Primary standard Indicator Type of Titration
standard (Conical flask)
(Burette)
1M Hydrochloric Acid/ Anhydrous Methyl red Acidimetry-
0.5M Sulphuric Acid Sodium carbonate Acid-Base Titration
1M Sodium Hydroxide Potassium hydrogen Phenolphthalein Alkalimetry -
phthalate Acid-Base Titration
0.1M Ceric Ammonium Arsenic trioxide, Ferroin sulphate Redox Titration-
Sulphate Sodium Hydroxide, Ceriometry
(Ceric Ammonium Sulphuric acid, Osmic
Sulphate and Sulphuric acid
Acid)
0.1M Sodium Thiosulphate Potassium bromate and Starch Redox Titration
(Sodium Thiosulphate and Potassium Iodide
Sodium carbonate)
0.02M Potassium Potassium Starch Redox Titration
Permanganate permanganate and
Potassium Iodide

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25/06/2024 Pharmaceutical Analysis 1

• It can involve both physical and chemical processes. If it involves chemical

• Qualitative Analysis: The identification of one or more chemical species present in

• Quantitative Analysis: The determination of the exact amount of a chemical species

 Monitoring and control of pollutants.

 Clinical and biological studies

 Fundamental and applied research

 If a material is known by a particular name and an analysis is carried out to

25/06/2024 Pharmaceutical Analysis 3

 Gravimetric Analysis: Analysis by mass

• To perform a volumetric analysis is necessary to have a solution at known

• One method in volumetric analysis is titration

• In titration: substance to be analysed is known as the analyte, the solution added to

25/06/2024 Pharmaceutical Analysis 5

• The point corresponding to meq* A = meq B is called equivalent point or point of

*meq = milli equivalents = VACA = VB CB

 Stoichiometric with known coefficients

 Collateral reactions must be absent

25/06/2024 Pharmaceutical Analysis 7

• Equivalence point occurs when 2 moles of MnO4- is added to 5 moles of Oxalic

• It occurs from the addition of a slight excess of titrant

• Endpoint does not equal equivalence point

25/06/2024 Pharmaceutical Analysis 9

Analyte Titrant (colorless) (colorless)

25/06/2024 Pharmaceutical Analysis 10

• Solution containing very small amounts of solute may be expressed is millimolar

• Normality (N) : The normality of a solution expresses the number of equivalents

• Molality (m) : The molality of a solution expresses as the number of moles of a

Formality (F) = GFW/Litres of solution

25/06/2024 Pharmaceutical Analysis 12

2HCl + Na2CO3 → CO2 + H2O + 2NaCl

25/06/2024 Pharmaceutical Analysis 15

 Equivalent weight of Acid

 Equivalent weight of Base

25/06/2024 Pharmaceutical Analysis 19

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