Development of Karl Fischer Reagents

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7. Sulfates, Sulfites Key Points Chapter II: Applications - 1 Differences in reactivity to Karl Fischer reagent mean that the choice of direct titration method must be made with reference to the individual substance. In most cases we recommend the measurement of moisture content using the moisture vaporization method. Sulfates crystallize as hydrates. In general, hydrates with six or more molecules of water of crystallization dissolve in methanol and remain in solution during titration. This means that they can be measured directly using a general-purpose solvent. Some examples of this type of substance are listed below. Na2SO2 � 10H2O, MgSO4 � 7H2O, NiSO4 � 6H2O, ZnSO4 � 7H2O, Al2(SO2)2 � 18H2O,KAl(SO4)2 � 12H2O, FeSO4 � (NH4 )2SO4 � 6H2O Water is strongly bonded in zinc sulfate 1-hydrate and manganese sulfate 1-hydrate and cannot be measured. Karl Fischer titration cannot be used for calcium sulfate 2-hydrate at normal room temperatures as the water is released very slowly. Total moisture content can be measured by using the moisture vaporization method at a temperature above 200 � C. Copper sulfate causes interference by oxidizing hydrogen iodide, the reactive substance in Karl Fischer reagent. This reaction frees 0.5 moles of iodine. CuSO4+2HI � CuI+0.5I2+H2SO4 As the resulting free iodine acts as a reagent, the measurement results will be low. In general, the weakly acidic salts of alkaline metals react in the same way as oxides. Sulfites and pyrosulfites react quantitatively. Sodium sulfite and sodium pyrosulfite react as shown in the following formulae. Na2SO3+I2+CH3OH � 2NaI+HSO4CH3 Na2S2O5+I2+CH3OH � 2NaI+SO2+HSO4CH3 Accordingly, the moisture vaporization method is used with these salts. 125
II-2. Inorganic Compounds [Examples of Measurement] (1) Moisture vaporization - Volumetric titration Reagents used: Karl Fischer Reagent SS-Z (or SS) Dehydrated Solvent GEX (or MS) 50-100ml 126 Substance Sodium metabisulfite Potassium metabisulfite Gypsum Heating temperature( � C) 150 150 250 Sample quantity (g) 0.1926 0.2215 0.2060 (2) Moisture vaporization - Coulometric titration Reagents used: Aquamicron AX (or AS) 150ml Aquamicron CXU 10ml Substance Sodium dithionite (Sodium hydrosulfite) Sodium sulfite Aluminum sulfate 100�C dried 200�C dried Sodium sulfate Calcium sulfate " " Heating temperature( � C) 200 250 700 700 250 200 600 900 Sample quantity (g) 0.4796 4.0301 0.0229 0.0515 3.1305 0.0521 0.0684 0.0612 Measurement value (mg) 11.39 3.85 14.76 Measurement value (µg) 2671 247 8787 8139 375 3310 4337 3868 Moisture content (%) 5.91 1.74 7.17 Moisture content (%) 00.557 61ppm 38.400 15.800 120ppm 06.3500 06.3400 06.3200
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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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Page 80 and 81: (2) Coulometric titration Reagents
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 96 and 97: Chapter II: Applications - 1 [Examp
Page 98 and 99: Chapter II: Applications - 1 Substa
Page 100 and 101: Substance pKa Sample quantity (g) C
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 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
Page 134 and 135: Chapter III: Applications - 2 Chapt
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 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
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Page 172 and 173: 2. Cereals and Dried Vegetables Key
Page 174 and 175: 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 (2) M
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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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