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Karl Fischer titration: difference between revisions

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10The method matters to readers of a [[Certificate of analysis|certificate of analysis]] for a specific and frequently misunderstood reason: a chromatographic purity figure is a statement about the ''relative'' composition of the material that dissolved, not about ''how much'' peptide the vial contains. Water, counterions and residual salts occupy mass. A vial of material reported at 99% purity by [[High-performance liquid chromatography|HPLC]] may nevertheless be 6% water and 8% [[Trifluoroacetate counterion|trifluoroacetate]] by mass, in which case its [[Peptide content|peptide content]] is closer to 85%.{{r|usp1503}}10The method matters to readers of a [[Certificate of analysis|certificate of analysis]] for a specific and frequently misunderstood reason: a chromatographic purity figure is a statement about the ''relative'' composition of the material that dissolved, not about ''how much'' peptide the vial contains. Water, counterions and residual salts occupy mass. A vial of material reported at 99% purity by [[High-performance liquid chromatography|HPLC]] may nevertheless be 6% water and 8% [[Trifluoroacetate counterion|trifluoroacetate]] by mass, in which case its [[Peptide content|peptide content]] is closer to 85%.{{r|usp1503}}
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+12Two variants are in routine use. Volumetric titration delivers iodine from a burette and suits samples containing milligram quantities of water; coulometric titration generates iodine electrochemically at the anode and suits the microgram-to-low-milligram range typical of a 10 mg peptide sample.{{r|scholz1984}}
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12== Chemical basis ==14== Chemical basis ==
13The underlying reaction is the oxidation of sulfur dioxide by iodine, which consumes water stoichiometrically:15The underlying reaction is the oxidation of sulfur dioxide by iodine, which consumes water stoichiometrically: