Water Content Determination Flashcards
Methods used in Water content determination
Method I - Karl Fischer/Titrimetric
Method II - Azeotropic-Toluene Distillation/Modified Xyelene Method
Method III - Gravimetric Method
Advantages of Karl Fischer Method
Most rapid
Requires only a small sample
Specific for water
Widely applicable in determination of the water content of drug products
Karl Fischer Components ⭐
Pyridine
Iodine
Methanol (Anhydrous)
Sulfur dioxide
PIMS
Reduced by SO2 in the presence of water to form Hydroiodic
Iodine
Reacts with water to form sulfur trioxide
Sulfur dioxide
Forms a complex with SO3 and neutralizes hydroiodic acid and prevents reversal of reaction
Pyridine
Reacts with the pyridine-sulfur trioxide complex
Anhydrous methanol
Primary Std used in Karl Fischer titration
Na tartrate dihydrate
End point of Karl Fischer Titration Method
Canary Yellow to Amber Color
Types of Karl Fischer Method
IA: Direct Titration
IB: Residual Titration
IC: Colometric Titration
Use of Toluene Moisture Apparatus
Azeotropic / Mod. Xylene
Azeotropic - Toluene Distillation is used for what substance
For vegetable drugs (2% moisture or 2-4 mL of water)
Sample size used in Azeotropic method
50-100g
Solvent used in Azeotropic/Modified Xylene
Toluene (USP Official)
Xylene
Method used for articles of Botanical Origin
Gravimetric