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Karl Fischer Titration PDF
Karl Fischer Titration PDF
Determination of Water
BP 2012
Method 1 (Ph.Eur.method 2.5.12)
Volumetric KF Titration
7
KF reagent
Automatic
Burette
Platinum
electrodes
Methanol
Titration flask
Iodine
I2
Sulfur dioxide
Buffer
Imidazol
Solvent
Methanol
SO2
10
11
2 Steps
12
Standardization USP34
13
Standardization BP2012
14
Substance
Purified water
Remarks
Water
content
100.00%
Ideal if technician
knows how to proceed
Certified water standards Not hygroscopic
10 mg/g &
Balance essential with 1 mg/g
test certificate
15
17
19
FCV/KF
F = the water equivalency factor of the Reagent, in mg/mL
C = the used volume, in %, of the capacity of the buret
V = the buret volume, in mL
KF = the limit or reasonable expected water content in
sample, in%
C is generally between 10%-100% for the instrument method endpoint.
20
21
SF
22
SF x 100
mg of Test Preparation
23
Bivoltametry
Ipol = 50 A
Current applied to a double Pt electrode
During titration:
Excess H2O
High voltage between the Pt wires
Drift in
l/min
Stop at 6 l/min
Basis Drift
e.g. 6 l/min
Time in s
25
1000-2000 (1.0-2.0mg)
2000-5000 (2.0-5.0mg)
5000-15000 (5.0-15.0mg)
Maximal permitted
RSD%
Not reported
5.0%
3.0%
2.0%
1.50%
28