Moisture Determination
Moisture Determination
Moisture Determination
1. Gravimetric Method – for drugs containing no constituents other than water, volatile at 105C.
2. Gravimetric Method – for drugs containing ether-soluble constituents, volatile at 105C.
3. Azeotropic Method or toluene distillation - for the determination of moisture content of many
vegetable drugs containing 2% or more of moisture
4. Titrimetric Method or Karl Fischer Method - for crystalline compounds that contain water of hydration
or absorbed water
5. Dew Point Method – for determining Water at Very Low Concentration
6. Electrolytic Hygrometric – for determining Extremely Low Concentration of Water
• This method is the most rapid, requires only a small sample and is specific for water.
• The method involves titration of the sample in reagent methanol with Karl Fischer reagent, which
consists of iodine, sulfur dioxide, pyridine, and methanol.
• The Karl Fischer reagent has a concentration such that one mL of the reagent is equivalent to
approximately five milligrams of water. (1 ml = 5 mg of water)
• The reagent deteriorates gradually; it is standardized by employing sodium tartrate (Na2C4H4O6.2H2O)
as a primary standard.
• The water equivalence (F) mg of water per mL of the reagent is given by the formula
0.1566 X W
V
• Where W is the weight in mg of sodium tartrate and V is the volume in mL of the reagent required.
BR x F
%Water Content = x 100
Wt
• Where BR (Volume of Reagent used), F (Water Equivalence) and Wt (Weight of sample)
Practice Problem
1. Moisture content of citric acid was determined by the Karl-fischer Method and the following data were
obtained
wt of citric acid …………………………4.8 g
vol of reagent used ……………………20 ml
Water equivalence factor of the reagent was determined by titrating 0.350 g of sodium tartrate with 10 ml
of KFR, determine the water content of citric acid
0.1566 x W
F=
V
0.1566 x 350 mg
F=
10 mL
F=5.841
BR x F
%Water Content= x 10 0
Wt
20 mL x 5.841
%Water Content= x 10 0
4800 mg
% Water Content = 2.43%
Online Assessment: (Email your assessment at [email protected], for questions/inquiries please free to
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1. From the assay of sodium citrate sample using Karl Fischer method, the following results were obtained:
Wt of sample 3.65 g sample
Vol of titrant 20 ml
Wt of primary standard 235 mg
Vol consumed during titration 7.46 ml
a. Determine the water equivalence factor
b. Compute for % water