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Weight per millilitre

The weight per millilitre of a liquid is the weight


in g of 1 mL of a liquid when weighed in air at
20C, unless otherwise specified in the
monograph.
The weight per millilitre is determined by dividing
the weight in air, expressed in g, of the quantity
of liquid that fills a pycnometer at the specified
temperature by the capacity, expressed in mL, of
the pycnometer at the same temperature.
The capacity of the pycnometer is ascertained from the
weight in air, expressed in g, of the quantity of water
required to fill the pycnometer at that temperature.
The weight of a litre of water at specified temperatures
when weighed against brass weights in air of density
0.0012 g per mL is given in the following table.
Ordinary deviations in the density of air from the
above value, here taken as the mean, do not affect the
result of a determination in the significant figures
prescribed for Pharmacopoeial substances.

DETERMINATION OF WATER / MOISTURE
IT IS DONE BY;
Karl Fischer titration
Karl Fischer titration is a classic titration
method in analytical chemistry that uses
coulometric or volumetric titration to
determine trace amounts of water in a
sample.

Coulometric titration
The main compartment of the titration cell
contains the anode solution plus the analyte. The
anode solution consists of an alcohol (ROH), a
base (B), SO
2
and I
2
. A typical alcohol that may be
used is methanol .
The titration cell also consists of a smaller
compartment with a cathode immersed in the
anode solution of the main compartment. The
two compartments are separated by an ion-
permeable membrane.
Volumetric titration
The volumetric titration is based on the same
principles as the coulometric titration except
that the anode solution above now is used as
the titrant solution. The titrant consists of an
alcohol (ROH), base (B), SO
2
and a known
concentration of I
2
.
Method I
The semi-micro determination of water is
based upon the quantitative reaction of water
with sulfur dioxide and iodine in a suitable
anhydrous medium in the presence of a base
with sufficient buffering capacity.
Apparatus:
The apparatus consists of a titration vessel with:
2 identical platinum electrodes;
tight inlets for introduction of solvent and titrant;
an inlet for introduction of air via a desiccant;
a sample inlet fitted with a stopper or, for liquids,
a septum.
Inlet systems for introduction of dry nitrogen or for
aspiration of solvents may also be fitted.
The titration is carried out according to the instrument
supplier's instructions. Care is taken throughout the
determination to avoid exposure of reagents and solvents
to atmospheric moisture. The end-point is determined
using 2 identical indicator electrodes connected to an
electrical source that maintains between the electrodes
either a constant current or a constant voltage. Where
direct titration is used , addition of titrant causes either a
decrease in voltage where constant current is maintained
or an increase in current where constant voltage is
maintained, until the end-point is reached. Instruments
with automatic end-point detection are commonly used.
Method IA:
Introduce into the titration vessel methanol R, or
the solvent indicated in the monograph or
recommended by the supplier of the titrant.
Where applicable for the apparatus used,
eliminate residual water from the measurement
cell or carry out a pre-titration. Introduce the
substance to be examined rapidly and carry out
the titration, stirring for the necessary extraction
time.
Method IB:
Introduce into the titration vessel methanol R, or the
solvent indicated in the monograph or recommended by
the supplier of the titrant. Where applicable for the
apparatus used, eliminate residual water from the
measurement cell or carry out a pre-titration. Introduce the
substance to be examined rapidly and in a suitable state of
division. Add an accurately measured volume of the titrant,
sufficient to give an excess of about 1 mL or the prescribed
volume. Allow to stand protected from light for 1 min or
the prescribed time, with stirring. Titrate the excess of
reagent using methanol R or the prescribed solvent,
containing an accurately known quantity of water.
The accuracy of the determination with the
chosen titrant must be verified for each
substance to be examined. The following
procedure, given as an example, is suitable for
samples containing 2.5-25 mg of water.
The water content of the substance to be
examined is determined using the
reagent/solvent system chosen. Thereafter,
sequential known amounts of water R are
added in an appropriate form (at least 5
additions) and the cumulative water content
determined after each addition. Calculate the
percentage recovery (r) at each point using the
following expression:
Method II: Determination of water by
distillation
The apparatus consists of a glass flask (A)
connected by a tube (D) to a cylindrical tube (B)
fitted with a graduated receiving tube (E) and
reflux condenser (C). The receiving tube (E) is
graduated in 0.1 mL. The source of heat is
preferably an electric heater with rheostat control
or an oil bath. The upper portion of the flask and
the connecting tube may be insulated.

Method: Clean the receiving tube and the condenser of the
apparatus, thoroughly rinse with water, and dry. Introduce 200 mL
of toluene R and about 2 mL of water R into the dry flask. Distil for 2
h, then allow to cool for about 30 min and read the water volume
to the nearest 0.05 mL. Place in the flask a quantity of the
substance, weighed with an accuracy of 1 per cent, expected to give
about 2 mL to 3 mL of water. If the substance has a pasty
consistency, weigh it in a boat of metal foil. Add a few pieces of
porous material and heat the flask gently for 15 min. When the
toluene begins to boil, distil at the rate of about two drops per
second until most of the water has distilled over, then increase the
rate of distillation to about four drops per second. When the water
has all distilled over, rinse the inside of the condenser tube with
toluene R. Continue the distillation for 5 min, remove the heat,
allow the receiving tube to cool to room temperature and dislodge
any droplets of water which adhere to the walls of the receiving
tube. When the water and toluene have completely separated, read
the volume of water and calculate the content present in the
substance as millilitres per kilogram, using the formula:

Method III (Coulometric titration)
Principle:
The coulometric titration of water is based upon the quantitative reaction
of water with sulfur dioxide and iodine in an anhydrous medium in the
presence of a base with sufficient buffering capacity. In contrast to the
volumetric method, iodine is produced electrochemically in the reaction
cell by oxidation of iodide.
The iodine produced at the anode reacts immediately with the water and
the sulfur dioxide contained in the reaction cell. The amount of water in
the substance is directly proportional to the quantity of electricity up until
the titration end-point. When all of the water in the cell has been
consumed, the end-point is reached and thus an excess of iodine appears.
Apparatus:
The apparatus consists of a reaction cell,
electrodes and magnetic stirrer. The reaction cell
consists of a large anode compartment and a
smaller cathode compartment.
Depending on the design of the electrode, both
compartments can be separated by a diaphragm.
Each compartment contains a platinum
electrode. Liquid or solubilised samples are
introduced through a septum, using a syringe.
Method:
Fill the compartments of the reaction cell with electrolyte
reagent for the micro determination of water R according
to the manufacturer's instructions and perform the
coulometric titration to a stable end-point. Introduce the
prescribed amount of the substance to be examined into
the reaction cell, stir for 30 s, if not otherwise indicated in
the monograph, and titrate again to a stable end-point. In
case an oven is used, the prescribed sample amount is
introduced into the tube and heated. After evaporation of
the water from the sample into the titration cell, the
titration is started. Read the value from the instrument's
output and calculate if necessary the percentage or amount
of water that is present in the substance.
Verification of the accuracy:
Between two successive sample titrations,
introduce an accurately weighed amount of
water in the same order of magnitude as the
amount of water in the sample, and perform the
coulometric titration. The recovery rate is within
the range from 97.5 per cent to 102.5 per cent
for an addition of 1000 g of H
2
O and in the
range from 90.0 per cent to 110.0 per cent for
the addition of 100 g of H
2
O.
LOSS ON DRYING
Test determines the amount of volatile matter of any
kind that is driven of under specified conditions.
Take 1-2g of substance, reduce particle size if necessary
and place in already dried (for 30 min) glass stoppered
shallow bottle .
Weigh the bottle containing the sample.
Shake the bottle to evenly distribute the test
substance.
Remove the stopper of bottle and Place the loaded
bottle and stopper in drying chamber.
Dry the sample at temperature specified in
monograph, close the bottle. Cool in desiccator &
weigh

If the substance melts at a lower temperature
than that specified for the determination of
Loss on drying, maintain the bottle with its
contents for 1 to 2 hours at a temperature 5 to
10 below the melting temperature, then dry
at the specified temperature.

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