Development of Karl Fischer Reagents

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Chapter II: Applications - 1 [Examples of Measurement] (1) Volumetric titration Reagents used: Karl Fischer Reagent SS-Z (or SS) Dehydrated Solvent GEX (or MS) 25-50ml Substance Chloral hydrate Hydrazine hydrate Dehydrated solvents General-use " Sample quantity (g) 0.1752 0.0732 Measurement value (mg) 19.27 25.68 Moisture content (%) 11.0 35.1 95
II-1 Organic Compounds 12. Amines 96 Key Points Some amines exhibit unusual behavior during Karl Fischer titration. That behavior falls into two categories; that caused by basicity and that caused by other chemical interference reactions. The titration conditions must be modified in accordance with the nature of the behavior that is involved. In terms of basicity, substances can be divided into two groups using benzylamine with a pKa value of 9.4 (Ka=2.4 x 10 -5 ) as the dividing line. 1) Amines below pKa9.4 Titration can be carried out without difficulty using standard procedures and behavior is comparable with hydrocarbons. In the case of volumetric titration, the substances are dissolved in a general-use dehydrated solvent and titrated directly. With coulometric titration, the sample is introduced into a general-use electrolyte (anolyte) and titrated directly. 2) Amines with strong-basicity (above pKa9.4) Aside from the Karl Fischer reactions with water, interference reactions caused by the strong basicity of these substances gradually consume the Karl Fischer reagent and are known to cause the following phenomena. a. Poor end point stability b. Failure to reach end point c. Abnormally high analytical results To suppress these interference reactions, the substances must be neutralized with acids before titration and the Karl Fischer titration system must be kept in a state that is close to neutrality. Salicylic acid is normally used for this purpose as it causes almost no esterification reaction with titration solvents which have methanol as their main ingredient. If acetic acid is used, the esterification reaction must be suppressed by chilling the system to 15 � C or below during the Karl Fischer titration. For volumetric titration the titration solvent is prepared by dissolving 10g of salicylic acid in 50ml of Dehydrated Solvent GEX (or MS). For coulometric titration the electrolyte is prepared by dissolving 10g of salicylic acid in 100ml of general-use electrolyte (anolyte). Note: Up to 70mmol of amine can be neutralized with 10g of salicylic acid. This is why titration is normally carried out continuously with a quantity that corresponds to a sample of 70mmol.
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Introduction The methods used to an
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eagents and analytical methods. As
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5. Officiak Testing Methods and Doc
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8 6.Goument Foods, etc. III-3.Pharm
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Chapter I: Basic Knowledge Chapter
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Chapter I: Basic Knowledge at a tim
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following formula: Chapter I: Basic
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[Procedures] Chapter I: Basic Knowl
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Chapter I: Basic Knowledge electrod
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! Electrolysis cell Titration syste
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1. Karl Fischer Reagent SS-Z, SS Ch
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! Helpful hint - 4 Chapter I: Basic
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[Characteristics] Chapter I: Basic
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[Characteristics] [Applications] Ch
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[Characteristics] [Applications] Ch
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Chapter I: Basic Knowledge a) No es
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2. Electrolytes for use with Ketone
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3. Applicability of Karl Fischer Ti
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Q9 Chapter I: Basic Knowledge What
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Chapter I: Basic Knowledge Na2S2O5+
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Chapter I: Basic Knowledge (3) Sila
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Substance Dehydrated solvents [Insu
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7. Plastics Key Points Chapter III:
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[Examples of Measurement] (1) Moist
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Raw rubber NR SBR BR CR NBR Vulcani
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Substance 10. Dyestuff Intermediate
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(2) Coulometric titration Reagents
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Chapter III: Applications - 2 such
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Chapter III: Applications - 2 (2) M
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Substance Epoxy resins (powder) Iso
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(4) Moisture vaporization - Coulome
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Substance Sample Quantity (g) Measu
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III-2. Foodstuffs Chapter III: Appl
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2. Cereals and Dried Vegetables Key
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3. Sugars and Condiments Key Points
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Chapter III: Applications - 2 [Exam
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Substance Heating Temperature ( �
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Chapter III: Applications - 2 [Exam
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Substance Dehydrated solvents Sampl
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Substance Dehydrated solvents Sampl
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[Examples of Measurement] (1) Volum
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2. Natural Products Key Points Subs
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Chapter IV: List of Karl Fischer Re
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ChapterV: Summary of Selection Proc
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Index 202
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Index B: Bakelite paper ��
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Index Cyclohexanol ��
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Index (L-) Histidine ��
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Index (p-) Nitrophenol ��
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Index Sodium 5'-guanylate ��
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218 copyright©2004by API Corporati
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Printed in Japan Rev. 3
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Development of Karl Fischer Reagents

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