Development of Karl Fischer Reagents
Development of Karl Fischer Reagents
Development of Karl Fischer Reagents
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III-1. Industrial Products<br />
(3) Gradually open valve B while stirring the anolyte (or general-use<br />
dehydrated solvent). Inject the sample for 10-15 minutes (at a rate <strong>of</strong><br />
about 1g/min.).<br />
140<br />
Note:The sample will gasify as it is injected and it will escape through<br />
the upper vent valve into a draft chamber, or to the outside air.<br />
(4) Withdraw the syringe from the sampling bottle.<br />
(5) Weigh the sampling bottle. Subtract this weight from the weight before<br />
the injection <strong>of</strong> the sample to determine the weight <strong>of</strong> the sample.<br />
(6) Titrate the moisture absorbed into the anolyte (or general-use<br />
dehydrated solvent) to the end point, using coulometric titration<br />
(volumetric titration).<br />
(7) Calculate the moisture content using the following formulae.<br />
For coulometric titration:<br />
Moisture content (ppm) = measurement value (µg)/sample quantity (g)<br />
For volumetric titration<br />
[Examples <strong>of</strong> Measurement]<br />
(1) Volumetric titration<br />
<strong>Reagents</strong> used: <strong>Karl</strong> <strong>Fischer</strong> Reagent SS-Z (or SS)<br />
Dehydrated Solvent GEX (or MS) 100ml<br />
Substance<br />
LPG<br />
Propane<br />
Methyl chloride<br />
Vinyl chloride<br />
Sulfur dioxide<br />
Aerosol<br />
Moisture content (ppm) =<br />
Sample quantity<br />
(g)<br />
25.1<br />
29.0<br />
18.3<br />
15.7<br />
53.1<br />
27.4<br />
Titration quantity<br />
(mg)<br />
1.40<br />
1.11<br />
4.95<br />
7.41<br />
17.6<br />
1.18<br />
(2) Coulometric titration<br />
<strong>Reagents</strong> used: Aquamicron AX (or AS) 150ml<br />
Aquamicron CXU 10ml<br />
Titration volume(ml)�Titer(mgH2O/ml)<br />
�100<br />
sample quantlty (g)�1000<br />
Moisture content<br />
(ppm)<br />
56<br />
38<br />
271<br />
475<br />
331<br />
35