Advanced Pharmaceutical analysis
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The book contain essential information about subjects based on analytical methods such as titrations, principles and procedures of functional groups and reagents, method developments and more.
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Advanced Pharmaceutical analysis - NELLORE DHARANI SAI SREEKANTH
UNIT:01
PRINCIPLES AND PROCEDURES OF THE FOLLOWING:
NON AQUEOUS TITRATION:
PRINCIPLE:
The Bronsted Lowery theory of acid and bases can be applied equally well to reactions occurring during acid
base titrations in non-aqueous solvents. This is because this approach considers an acid as any
substance, which will tend to donate a proton, and a base as any substance, which will accept a proton.
Substances which give poor end points due to being weak acids or bases in aqueous solution will frequently
give far more satisfactory end point when titrations are carried out in non-aqueous media. An
Additional advantage is that many substances, which are insoluble in water, are sufficiently soluble
in organic solvents to permit their titrations in these non-aqueous media.In the Bronsted Lowery
theory, any acid, (HB) is considered to dissociate in solution to give a proton(H+) and a conjugate base(B-)
where as any base (B) will combine with a proton to produce a conjugate acid (HB+):
HB ↔ H+ + B-
B+H+↔ HB+
The ability of substances to act as acids or bases will very much depend on the choice of solvent system.
PROCEDURE:
Dissolve the substance being examined in a suitable volume of the solvent previously neutralized to
the indicator, warming and cooling if necessary, or prepare a solution as specified in the monograph.
Titrate to the appropriate colour change of the indicator. Carry out a blank determination and make
any necessary corrections. The titrant is standardized using the same solvent and indicator as
specified for the substance.
When the equivalence point is established potentiometrically, the indicator is omitted and
neutralization of the solution and standardization of the titrant are also carried out potentiometrically.
––––––––
EXAMPLE:
Perchloric acid:
Preparation of 0.1N perchloric acid: The accurate 8.5 ml of perchloric acid is dissolved in the
100 ml glacial acetic acid and 30 ml of acetic anhydride is added. Then the volume to 1000 ml is
made with glacial acetic acid.
Standardization of 0.1N perchloric acid: 200 mg of potassium hydrogen phthalate is mixed with the 10 ml of acetic anhydride and the solution is refluxed until the salt is dissolved. Then the solution is cooled to room temperature and little quantity, that is, two to three drops of crystal violet indicator is added. The resulting solution is titrated with the 0.1 N perchloric acid.
COMPLEXOMETRIC TITRATIONS:
PRINCIPLE:
Initially the metal ions are solvated that is, they are dissolved in the appropriate solvent and then these solvent ions are replaced by the ions or other solvent molecules to form the complex. The replacing solvent or ions are known as ligands.
The main principle is the reaction between the ligand and the metal ion to form a complex. The metal ion acts as Lewis acid and the ligand acts as Lewis base which is the complexing agent
The following steps play an important role in the complexometric titrations:
Selection of the complexing agent.
Detection method employed for the detection of the end point.
Maintaining of the experimental conditions.
––––––––
PROCEDURE:
Aluminium
Dissolve the quantity of substance, accurately weighed, as specified in the monograph, in 2 mL
of hydrochloric acid (1 mol/l) VS and 50 mL of water, unless other conditions of solution are
given in the monograph. Add 50 mL of disodium edetate (0.05 mol/l) VS and neutralize to
methyl red/ethanol TS with sodium hydroxide (1 mol/l) VS. Heat the solution to boiling and
maintain in a boiling water-bath for at least 10 minutes, cool, add about 50 mg of xylenol orange
indicator mixture R and 5 g of methenamine R and titrate the excess edetate with lead nitrate
(0.05 mol/l) VS until the yellow solution turns pink-violet.
Zinc
Dissolve the quantity of substance, accurately weighed, as specified in the monograph, in 5-10
mL of water, acidified with a minimum quantity of acetic acid (~300 g/l) TS if necessary, and
then dilute to about 50 mL with water. Add about 50 mg of xylenol orange indicator mixture R
and sufficient methenamine R (about 5 g) to turn the solution pink-violet and titrate with
disodium edetate (0.05 mol/l) VS until the solution turns from pink-violet to full yellow.
The end point is determined by plotting the PM value which is the negative logarithm of the metal
ion concentration versus volume of the titrant. The end point is detected by using an indicator or
by applying an instrumental method.
Complexometric titration curveComplexometric titration curve.
OXIDATION-REDUCTION:
PRINCIPLE:
Reactions in which electrons are transferred from one species to another are called oxidation-
reduction (redox) reactions. When one species loses electrons by an oxidation process another
species simultaneously gains electrons by a reduction process in a chemical reaction. The
balanced chemical reaction can be written as the combination of two half-reactions representing
the oxidation reaction and the reduction reaction , respectively.
––––––––
PROCEDURE:
Preparation of the permanganate solution: The accurate amount of the potassium
permanganate is weighed on a watch glass and then it is transferred into the beaker. Then
this is dissolved in the three-fourth portion of the distilled water and the mouth of the beaker is
covered with the appropriate stopper. The resulting solution is boiled for 15-30 minutes and is
allowed for cooling to room temperature. The solution is filtered through a cotton plug and is
made to desired volume by adding distilled water.
Standardization