OKORJI

DAVID
HONTORIA
LATUMBO
PAMA
Water content is generally determined by three
methods:
(1)Gravimetric, for drugs that containing no
constituents, other than water, volatile at 105°C;
(2)Gravimetric, for drugs containing ether soluble
constituents volatile at 105°C;
(3)Azeotropic (toluene distillation);
(4)and Titrimetric (Karl Fisher).
 For drugs which contain no constituents volatile at 105°C,
other than water,

about 10 g of drug is accurately weighed and then

dried in an oven at 105°C for 5h.

After 5h the sample is weighed and again dried at

1-h intervals until the loss in weight is not more than
0.25% in 1 h of drying.

The weight loss of the drug represents the

moisture present in the sample.
However, most vegetable drugs
contain variable amounts of
volatile substances other than
water, such as essential oils, ethers,
esters, and amines.

This method is not generally

applicable.
 When the drug contains matter, other than
water, which is volatile at 105°C,

N.F. directions: require the volatile ether

soluble extractive be determined,

 and the weight of the latter subtracted

from the weight lost by the drug upon drying.

the difference to be taken as the moisture

content of the drug.
Even this procedure is not
free from error.
 A better method, known as the xylene method, and developed
by the US Forestry Service.

 It has been modified and is one of the official methods for

moisture determination.

 It is referred to as the azeotropic method in the U.S.P and the

moisture method by toluene distillation in the N.F.

 This method is specified for the determination of moisture

content of many vegetable drugs containing 2% of moisture.
 Azeotropic method refers to a specific technique of adding another
component (called the entertainer) to generate a new, lower boiling
point azeotrope that is heterogenous (e.g. producing two, immiscible
liquid phases)
 Examples: addition of benzene to water and ethanol.

 An azeotrope is a mixture of liquids that maintains its composition

and boiling point during distillation.

 The purpose of deliberately adding the entertainer is either to

separate one component of a closely boiling pair or to separate
one component of azeotrope.
 Karl Fischer Titration Procedure

 The Karl Fischer titration experiment can be performed in two

different methods. They are:

 VOLUMETRIC DETERMINATION – This technique is suitable

to determine water content down to 1% of water. The sample
is dissolved in KF methanol and the iodine is added to KF
Reagent. The endpoint is detected potentiometrically.
 Karl Fischer Titration Procedure

 The Karl Fischer titration experiment can be performed in two

different methods. They are:

 COULOMETRIC DETERMINATION – The endpoint is

detected in this experiment electrochemically. Iodine required
for KF reaction is obtained by anodic oxidation of iodide
from solution
It is a destructive technique.
The solvent consumption is high as the manual
volumetric titration demands reloading during
each determination.
Coulometric titration is fitted only for samples
which contain a small amount of water.
It takes extremely long periods to determine.