Development of Karl Fischer Reagents
Development of Karl Fischer Reagents
Development of Karl Fischer Reagents
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II-1 Organic Compounds<br />
[Examples <strong>of</strong> Measurement]<br />
(1) Volumetric titration --neutralization using salicylic<br />
<strong>Reagents</strong> used: <strong>Karl</strong> <strong>Fischer</strong> Reagent SS-Z (or SS)<br />
Dehydrated Solvent GEX (or MS) approx. 50ml<br />
Salicylic acid approx. 10g<br />
(2) Coulometric titration<br />
<strong>Reagents</strong> used: Aquamicron AX (or AS) 100ml<br />
or with approx. 10g <strong>of</strong> Salicylic acid added<br />
Aquamicron CXU 5ml<br />
98<br />
Substance<br />
n-Butylamine<br />
Diethylamine<br />
Diethanolamine<br />
Piperidine<br />
Tri-n-butylamine<br />
Di-isopropyl amine<br />
2-Methylaminopyridine<br />
Triethanolamine<br />
N-Ethyl morpholine<br />
N,N-Dimethyl benzylamine<br />
N-Ethyl aniline<br />
Aniline<br />
Dehydrated<br />
solvents<br />
General-use+Salicylic acid<br />
"<br />
"<br />
"<br />
"<br />
"<br />
"<br />
"<br />
"<br />
"<br />
"<br />
Ketone-type<br />
Sample<br />
quantity(g)<br />
0.7335<br />
0.7234<br />
1.0240<br />
0.9034<br />
1.6367<br />
1.5010<br />
1.0520<br />
1.1240<br />
0.9050<br />
0.9000<br />
0.9580<br />
1.0185<br />
Measurement<br />
value (mg)<br />
1.45<br />
1.02<br />
2.62<br />
1.00<br />
1.27<br />
1.21<br />
0.47<br />
0.70<br />
0.88<br />
1.55<br />
0.55<br />
1.49<br />
Moisture<br />
content (%)<br />
0.200<br />
0.140<br />
0.260<br />
0.110<br />
0.077<br />
0.081<br />
0.120<br />
0.170<br />
0.260<br />
0.170<br />
0.057<br />
0.150<br />
Note: Salicylic acid crystals are bulky and difficult to handle. To<br />
overcome this problem, place 10g <strong>of</strong> salicylic acid in an empty<br />
titration flask and add Dehydrated Solvent GEX. The salicylic<br />
acid will dissolve readily and can be rendered moisture-free<br />
through a <strong>Karl</strong> <strong>Fischer</strong> titration that prepares for the main<br />
titration.
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