Development of Karl Fischer Reagents

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Chapter III: Applications - 2 (2) Moisture vaporization - Volumetric titration Reagents used: Karl Fischer Reagent SS-Z (or SS) Dehydrated Solvent GEX (or MS) + PG (3:1) 50-100ml Substance Coffee beans Dried beer yeast Curry roux Heating Temperature ( � C) 130 200 130 Sample Quantity (g) 0.1919 0.0840 0.1217 (3) Moisture vaporization - Coulometric titration Reagents used: Aquamicron AX (or AS) 150ml Aquamicron CXU 10ml Substance Coffee Raw coffee beans Cocoa Hops Beet Gelatine Heating Temperature ( � C) 090 150 110 130 130 180 Sample Quantity (g) 0.1282 0.0555 0.2486 0.0189 0.0913 0.0114 Measurement Value (mg) 4.11 8.86 4.31 Measurement Value (µg) 3229 5012 3973 1536 7669 1790 Moisture Content (%) 02.14 10.6 03.54 Moisture Content (%) 02.52 09.03 01.60 08.14 08.40 15.70 179
III-3 Pharmaceuticals III-3. Pharmaceuticals In this field, Karl Fischer titration is the most effective tool for precise moisture content measurement. Moisture content tends to be high, ranging from a few percent up to a few tens of percent. For this reason, volumetric titration is generally used. The examples in this section show the application of Karl Fischer titration to biochemical and pharmaceutical products. Where the chemical ingredients of these products are known direct titration can be used as it is possible to determine whether or not interference will occur. Even if products cause interference, they can still be measured using moisture vaporization and Karl Fischer titration, provided that they remain stable when exposed to heat. Special pharmaceutical items are listed in the Japanese Pharmacopoeia. Aside from volumetric titration, the coulometric titration and moisture vaporization methods can also be used. This chapter gives examples based on the actual implementation of these methods. 1. Biochemical Products Sugar-type dehydrated solvents are generally used when applying volumetric titration to biochemical products such as amino acids, nucleic acids, sugars, enzymes and lipids. Even substances that do not dissolve in general-use dehydrated solvents can be titrated directly using a general-use dehydrated solvent, provided that the moisture content of the sample can be extracted adequately. Direct coulometric titration is not suitable as many samples cannot be dissolved in the anolytes used for this type of titration. Coulometric titration is carried out using the moisture vaporization method. Some samples break down at certain heating temperatures and there must be careful consideration of the temperature used for moisture vaporization. L-cystime and vitamin C react with Karl Fischer reagent and cannot be titrated directly. Care is needed with general vitamin preparations that include vitamin C since these can also cause interference reactions. (Vitamin C reacts quantitatively with iodine. If the amount of vitamin C included in a sample is known, then the moisture content can be determined by adjusting the results. Refer to the Basic Knowledge section for more information.) Moisture vaporization is used with these substances. 180 Key Points
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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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Chapter I: Basic Knowledge Measurin
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[Procedures] Chapter I: Basic Knowl
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Chapter I: Basic Knowledge (3) Usin
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Q12 Chapter I: Basic Knowledge How
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Silicon rubber Figure 6: Sampling S
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Chapter I: Basic Knowledge (2) Syri
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Chapter I: Basic Knowledge (1) Upri
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Aquamicron CXU 5. Official Testing
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2. Japan Pharmaceutical Codex (Revi
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5. Japan LPG Association Standards
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Chapter I: Basic Knowledge Part 2:
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Chapter I: Basic Knowledge 6. Impor
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Chapter II: Applications - 1 Chapte
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Chapter II: Applications - 1 Chapte
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Chapter II: Applications - 1 [Examp
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Examples of substances that can be
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(2) Coulometric titration Reagents
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7. Aldehydes Key Points Chapter II:
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Chapter II: Applications - 1 1) Sam
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8. Organic Acids Key Points Chapter
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10. Organic Acid Salts Key Points C
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Chapter II: Applications - 1 Substa
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Substance pKa Sample quantity (g) C
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Substance Semicarbazide hydrochlori
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17. Acid Anhydrides Key Points Chap
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20. Peroxides Key Points Chapter II
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[Examples of Measurement] (1) Volum
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Chapter II: Applications - 1 1-Phen
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1. Metals and Simple Substances Key
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2. Inorganic Acids Key Points Chapt
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Chapter II: Applications - 1 b) Tit
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Substance Calcium hydroxide " Magne
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5. Halides (halogenides) Key Points
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Substance Potassium chloride " Lith
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7. Sulfates, Sulfites Key Points Ch
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8. Other Salts Key Points Chapter I
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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
Page 142 and 143: Substance LPG Ethylene Propane Buta
Page 144 and 145: 6. Petroleum Products Key Points Ch
Page 146 and 147: Substance Dehydrated solvents [Insu
Page 148 and 149: 7. Plastics Key Points Chapter III:
Page 150 and 151: [Examples of Measurement] (1) Moist
Page 152 and 153: Raw rubber NR SBR BR CR NBR Vulcani
Page 154 and 155: Substance 10. Dyestuff Intermediate
Page 156 and 157: (2) Coulometric titration Reagents
Page 158 and 159: Chapter III: Applications - 2 such
Page 160 and 161: Chapter III: Applications - 2 (2) M
Page 162 and 163: Substance Epoxy resins (powder) Iso
Page 164 and 165: (4) Moisture vaporization - Coulome
Page 166 and 167: Substance Sample Quantity (g) Measu
Page 168 and 169: III-2. Foodstuffs Chapter III: Appl
Page 170 and 171: Chapter III: Applications - 2 (2) M
Page 172 and 173: 2. Cereals and Dried Vegetables Key
Page 174 and 175: 3. Sugars and Condiments Key Points
Page 176 and 177: Chapter III: Applications - 2 [Exam
Page 178 and 179: Substance Heating Temperature ( �
Page 182 and 183: Chapter III: Applications - 2 [Exam
Page 184 and 185: Substance Dehydrated solvents Sampl
Page 186 and 187: Substance Dehydrated solvents Sampl
Page 188 and 189: [Examples of Measurement] (1) Volum
Page 190 and 191: 2. Natural Products Key Points Subs
Page 192 and 193: Chapter IV: List of Karl Fischer Re
Page 200 and 201: ChapterV: Summary of Selection Proc
Page 202 and 203: Index 202
Page 204 and 205: Index B: Bakelite paper ��
Page 206 and 207: Index Cyclohexanol ��
Page 208 and 209: Index (L-) Histidine ��
Page 210 and 211: Index (p-) Nitrophenol ��
Page 212 and 213: Index Sodium 5'-guanylate ��
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Page 218 and 219: 218 copyright©2004by API Corporati
Page 220: Printed in Japan Rev. 3
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Development of Karl Fischer Reagents

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