Aquame
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Aquametry
AQUAMETRY
AQUA- means water METRY- means measurement
Aquametry is an analytical process to measure the water present in
any product.
Determining micro quantities of water by the use of Karl Fischer Reagent
by the application of current is known as aquametry. It is also been known
as amperometry.
Importance of water determination
Quantitative determination of water is important because many drugs
contain water:
As a solvent
As absorbed water
As water of crystallization
As an adulterant
Physical properties of a drug or a raw material are modified by its water
content. Pharmaceutical procedures of granulation, tablet formation & coating
operations are affected by water content.
Methods of Water Determination
Methods of Water determination can be of two types:
1. Thermal Methods:
Loss on drying
Azeotropic Distillation Method
2. Chemical Methods:
Karl Fischer Titration
Importance of aquametry
[Link] Determination of Water in pharmaceutical products is
important, because H2O may be present in the products as – Solvent,
Absorbed water. water of Crystallization
[Link] is important, because – Physical properties of a drug or raw material is
modified by the presence of H2O
3. Physical stability of the product may be hampered in presence of water.
So, we should determine whether it possesses water or not.
4. Water content of drugs may also be important for other reasons i.e- when
crude drugs
The principle of Karl Fischer titration
Fundamental Reaction
The fundamental principle behind the Karl Fischer Titration is based on the
Bunsen reaction between iodine and sulphur dioxide in an aqueous medium
shown below:
I2+ SO2+2H2O → 2HI+ H2SO4
Karl Fischer discovered that this reaction could be modified to be used for the
determination of water in a non-aqueous system containing an excess of
sulphur dioxide. He used a primary alcohol (methanol) as the solvent, and a
base (pyridine) as the buffering agent. So the reaction changed into:
py. I2 + py·SO2 + H2O + py → 2py· HI + py· SO3
Preparation of Karl Fischer titration
Into a glass- stoppered flask (about 750 ml capacity) anhydrous methanol
(400 ml,containing not more than .03% water ) is placed and pure dry
pyridine(80 g) is taken.
Flask is immersed in a freezing mixture and slowly sulphur dioxide is passed
into the cold solution , with continuous agitation, until the increase in weight
is 20 g .
Finally iodine is added (45 g) , and shaked well to dissolve and the mixture
is allowed to stand for 24 hr before use.
Advantages of Karl Fischer Titration
Karl Fischer Titration Method is very popular for a large practical advantage which it
holds over other moisture determination technique,
These includes:
Easy Sample Preparation
High Accuracy and Precision
Independence of presence any volatile materials
Nearly Unlimited Measuring Range
Short Analysis Duration
Small Sample Quantities required
Suitability for analysing-
Solids Liquids
Gases
Application
Soil quality: The appearance of large information banks on soil properties
in Europe was provoked by necessity of increasing of agricultural
production economics, i.e. the commercial price of soil as the production
medium.
Quality of food materials and products: Moisture content affects food
quality,
i.e. texture, taste, appearance and stability of foods depends on the amount
of water they contain. A knowledge of the moisture content is often
necessary to predict the behavior of foods during processing, e.g. mixing,
drying, transportation, flow through a pipe or packaging, storage stability or
shelf-life
