Development of Karl Fischer Reagents

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Electrolysis cell
Titration system
Helpful hint - 3
Moisture vaporization system
Oven
Chapter I: Basic Knowledge
Figure 5: A Moisture Vaporization System (for Lubricating Oils)
How can we check for accuracy when a moisture vaporization apparatus is
added to the system?
The accuracy of capture is an important concern, since moisture vaporized
in the moisture vaporization apparatus is carried through the heating tube
and blowing tube by means of dried nitrogen gas before being absorbed
into a dehydrated solvent (or into an electrolyte in an electrolysis cell). The
capture ratio (recovery ratio) can be checked using the following three
methods.
(1) Using water
With the water method, which is usually the simplest, 5 or 10ul (5 or
10mg) of water is placed directly into the sample boat using a
microsyringe (capacity: 10ul).
(2) Sodium tartrate dihydrate method (theoretical moisture content:
15.66%)
When using this method, the sodium tartrate dihydrate must first be dried
at 105 � C.
(3) Glass capillary pipette method
The glass capillary pipette method is simple and is suitable for checking
amounts in the order of 1,000ug. Glass capillary pipettes are commonly
used in biotechnology fields, and their capacities are extremely precise.
They provide an easy way to obtain a required volume of water by
means of the capillary phenomenon.
Reference:Bunseki, p587, 1995
Temperature regulation system
Flowmeter
Drying agent (silica gel, etc.)
Nitrogen gas
(300ml/min.)
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