Development of Karl Fischer Reagents

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(2) Coulometric titration Reagents used: Aquamicron AKX (or AX) 100ml Aquamicron CXU 5ml Substance Electrolyte Formic acid Acetic acid Propionic acid Dichloroacetic acid Salicylic acid Stearic acid Oxalic acid 9. Esters Key Points Ketone-type " " " General-use " " Sample quantity(g) 1.2200 1.0500 0.9930 1.5630 1.6222 2.1418 0.0222 Chapter II: Applications - 1 Measurement value (µg) Not measurable 0687 1321 1313 0341 0130 6645 Moisture content (ppm) 0655 1330 0840 0210 0061 29.9% Esters are substances for which moisture content can be measured very easily using standard Karl Fischer titration procedures. There are no significant interference reactions and behavior is similar to that of hydrocarbons. Both volumetric and coulometric titration can be used without any problem. For volumetric titration, a general-use dehydrated solvent is used. Solubility will be a problem with long-chain aliphatic esters and a dehydrated solvent formulated for oils is recommended. With coulometric titration, measurements are carried out by adding the sample directly to the electrolyte (anolyte). Examples of substances that can be measured directly: Esters Methyl formate, ethyl formate, methyl acetate, ethyl acetate, aryl formate, methyl acrylate, methyl methacrylate, ethyl malonate, methyl valerate, methyl adipate, methyl sebacate, methyl glycolate, 2,3-butylene di-acetate, ethyl citrate, cyclohexyl acetate, methyl benzoate, methyl salicylate, phenyl acetate Inorganic esters Ethyl carbonate, ethyl chlorocarbonate, butyl nitrite 91
II-1 Organic Compounds Lactones �-butyrolactone Carbamic acid esters Methyl carbamate, ethyl carbamate [Examples of Measurement] (1) Volumetric titration Reagents used: Karl Fischer Reagent SS-Z (or SS) Dehydrated Solvent GEX (or MS) 25-50ml (2) Coulometric titration Reagents used: Aquamicron AX (or AS) 100ml Aquamicron CXU 5ml 92 Substance Methyl acetate Ethyl acetate Methyl acrylate �-Butyrolactam Substance Methyl acetate Methyl isoamyl n-Butyl acetate Isopropyl isovalerate Di-isopropyl malonate Benzyl benzoate Dehydrated solvent General-use " " " Sample quantity (g) 2.5250 0.8548 2.4589 0.9186 1.0740 1.5825 3.1695 Sample quantity (g) 0.9467 4.3557 2.8098 5.6364 Measurement value (µg) Measurement value (µg) 105 1280 195 1256 449 319 512 2.15 0.86 5.31 1.18 Moisture content (ppm) 2224 197 1890 210 Moisture content (ppm) 42 1494 79 1367 418 202 162
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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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Page 58 and 59: Chapter I: Basic Knowledge (1) Upri
Page 60 and 61: Aquamicron CXU 5. Official Testing
Page 62 and 63: 2. Japan Pharmaceutical Codex (Revi
Page 64 and 65: 5. Japan LPG Association Standards
Page 66 and 67: Chapter I: Basic Knowledge Part 2:
Page 68 and 69: Chapter I: Basic Knowledge 6. Impor
Page 70 and 71: Chapter II: Applications - 1 Chapte
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Page 74 and 75: Chapter II: Applications - 1 [Examp
Page 76 and 77: Examples of substances that can be
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Page 86 and 87: 7. Aldehydes Key Points Chapter II:
Page 88 and 89: Chapter II: Applications - 1 1) Sam
Page 90 and 91: 8. Organic Acids Key Points Chapter
Page 94 and 95: 10. Organic Acid Salts Key Points C
Page 98 and 99: Chapter II: Applications - 1 Substa
Page 100 and 101: Substance pKa Sample quantity (g) C
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Page 104 and 105: Substance Semicarbazide hydrochlori
Page 106 and 107: 17. Acid Anhydrides Key Points Chap
Page 108 and 109: 20. Peroxides Key Points Chapter II
Page 110 and 111: [Examples of Measurement] (1) Volum
Page 112 and 113: Chapter II: Applications - 1 1-Phen
Page 114 and 115: 1. Metals and Simple Substances Key
Page 116 and 117: 2. Inorganic Acids Key Points Chapt
Page 118 and 119: Chapter II: Applications - 1 b) Tit
Page 120 and 121: Substance Calcium hydroxide " Magne
Page 122 and 123: 5. Halides (halogenides) Key Points
Page 124 and 125: Substance Potassium chloride " Lith
Page 126 and 127: 7. Sulfates, Sulfites Key Points Ch
Page 128 and 129: 8. Other Salts Key Points Chapter I
Page 130 and 131: 9. Inorganic Gases Key Points Chapt
Page 132 and 133: Chapter III: Applications - 2 Chapt
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Page 136 and 137: 2. Agricultural Chemicals Key Point
Page 138 and 139: [Examples of Measurement] (1) Volum
Page 140 and 141: Chapter III: Applications - 2 (4) C
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Substance LPG Ethylene Propane Buta
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6. Petroleum Products Key Points Ch
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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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216
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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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