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
Sample size and temperature used in Gravimetric Method
10g, Dry at 105C for 5 hours
Used when the loss sustained on heating may not be entirely water
Loss on Drying
Determination of amount of VOLATILE SUBSTANCES driven off under conditions specified
Loss on Drying
Sample size used on Loss on Drying
1-2g
Temperature and duration applied on Loss on Drying
110-120C +/-2C
As specified in indiv monograph
Specifications for capsules in Loss on Drying
Cap - Mixed contents of >4 capsules
Tab - Use powder from >4 tablets
The moisture content of a drug may be
Water of hydration
Water in the absorbed form
TF: The amount of extractive a drug yields to a solvent is a measure of the amount of a certain constituents or group of related constituents the drug contains.
True
TF: Solvents used for Extractives should only dissolve the target substances during the extraction
True