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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.

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