Karl Fischer Coulometric Titration

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INTRODUCTION. Developed by Karl Fischer, 1935Foul smelling, not widely usedModified by Eugene Schulz, 1979Pyridine replaced by imidazole, widespread useVolumetric method5% to 100% water samples, basic titrationCoulometric method0.0001% (1-ppm) to 5%, electroanalytical technique. INSTRUMENT.

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Karl Fischer Coulometric Titration

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1. Karl Fischer Coulometric Titration Adam G. Thomas CHE 480

2. INTRODUCTION Developed by Karl Fischer, 1935 Foul smelling, not widely used Modified by Eugene Schulz, 1979 Pyridine replaced by imidazole, widespread use Volumetric method 5% to 100% water samples, basic titration Coulometric method 0.0001% (1-ppm) to 5%, electroanalytical technique

3. INSTRUMENT Sold as an instrument: mix, press button ? data Two compartment system, keeps iodine from reducing too fast at cathode – faster, more accurate. Anolytic compartment contains SO2, I-, ROH, imidazole and sample Catholytic compartment contains an acidic oil

4. ELECTROCHEMISTRY Anolyte and catholyte solutions premixed Methanol or ethanol solvent Known volume sample, voltage required to ox. I- generate I2, voltage drops at equiv. pt. (excess I2)

5. LITERATURE EXAMPLES Examples of use widespread As an impurity or input variable, water content is important in many fields Polymerization in ionic solutions Water content of solutions Input variable for the polymerization Coulometric method Pyrolysis of bio-fuels using portable augers Used to measure %water of wood derived py-oil Also, after storage – no change Water content – greatest affect on viscosity Coulometric method

6. WORKS CITED: 1. Basics of Karl Fischer Titration. Sigma Aldrich Website. Accessed Mar 01, 2011. <http://www.sigmaaldrich.com/analytical-chromatography/titration/hydranal/learning-center/theory.html> 2. Harris, Daniel. Quantitative Chemical Analysis. 6th Ed. W.H. Freeman and Co. New York. 2003 3. Free Radical Polymerization of n-Butyl Methacrylate in Ionic Liquids. Veronika Strehmel, André Laschewsky, Hendrik Wetzel and, Eckhard Görnitz. Macromolecules. 2006 Vol. 39. 923-930 4. Pyrolysis of Wood and Bark in an Auger Reactor: Physical Properties and Chemical Analysis of the Produced Bio-oils. Leonard Ingram, Dinesh Mohan, Mark Bricka, Philip Steele, David Strobel, David Crocker, Brian Mitchell, Javeed Mohammad, Kelly Cantrell, Charles U. Pittman Jr. Energy & Fuels 2008 Vol 22. 614-625

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