Development of Karl Fischer Reagents
Development of Karl Fischer Reagents
Development of Karl Fischer Reagents
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I-1. Questions & Answers about <strong>Karl</strong> <strong>Fischer</strong> <strong>Reagents</strong><br />
1. Substances requiring special treatment<br />
44<br />
Compound Treatment<br />
Ammonia<br />
Ferric salts<br />
Hydrazine derivatives<br />
Hydroxylamine salts<br />
Thiol (mercaptan)<br />
Sulfuric acid<br />
Thio acid<br />
Thiourea<br />
Add acetic acid.<br />
Add 8-Hydroxyquinoline.<br />
Add acetic acid.<br />
Add sulfur dioxide:pyridine solution (1:1).<br />
Prevent interference by adding olefins (octene, etc.).<br />
If the sulfuric acid is 92% pure or higher, add a large<br />
surplus <strong>of</strong> pyridine and titrate it as a salt.<br />
Prevent interference by adding olefins (octene, etc.).<br />
Prevent interference by adding olefins (octene, etc.).<br />
2. Using <strong>Karl</strong> <strong>Fischer</strong> reagents with interference substances<br />
With ketones, aldehydes, lower carboxylic acid and amines with strong<br />
basicity, titration should be carried out using the <strong>Karl</strong> <strong>Fischer</strong> reagent in<br />
conjunction with the reagents shown below.<br />
Substance<br />
Ketones<br />
Aldehydes<br />
Low-grade<br />
carboxylic acid<br />
Strong-base amines<br />
(pKa9 and above)<br />
<strong>Karl</strong> <strong>Fischer</strong><br />
Reagent SS-Z<br />
<strong>Karl</strong> <strong>Fischer</strong><br />
Reagent SS<br />
<strong>Karl</strong> <strong>Fischer</strong><br />
Reagent SS-Z<br />
<strong>Karl</strong> <strong>Fischer</strong><br />
Reagent SS<br />
<strong>Karl</strong> <strong>Fischer</strong><br />
Reagent SS-Z<br />
<strong>Karl</strong> <strong>Fischer</strong><br />
Reagent SS<br />
<strong>Karl</strong> <strong>Fischer</strong><br />
Reagent SS-Z<br />
<strong>Karl</strong> <strong>Fischer</strong><br />
Reagent SS<br />
Reagent Used<br />
Volumetric titration Coulometric titration<br />
Dehydrated Solvent KTX<br />
Dehydrated Solvent CP<br />
Dehydrated Solvent KTX<br />
Dehydrated Solvent CP<br />
Dehydrated Solvent PP<br />
Dehydrated Solvent KTX<br />
Dehydrated Solvent CP<br />
Dehydrated Solvent GEX<br />
+ salicylic acid<br />
Dehydrated Solvent MS<br />
+ salicylic acid<br />
Aquamicron AKX<br />
Aquamicron CXU<br />
Aquamicron AKX<br />
Aquamicron CXU<br />
(suitable only for<br />
certain aromatic<br />
aldehydes)<br />
Aquamicron AKX<br />
AquamicronCXU<br />
Aquamicron AX<br />
+ salicylic acid<br />
Aquamicron CXU<br />
Note:Do not use <strong>Karl</strong> <strong>Fischer</strong> SS with Dehydrated Solvent KTX.