Karl Fisher Titration By Ruchi Bhatia & Dr S Nayak

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By: mehrankhanjeee (24 month(s) ago)

plz send it on my email plz hsa_1993@yahoo.com

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BANSAL COLLEGE OF PHARMACY Kokta , Anand Nagar, Bhopal www.bansalpharmacy.com : KARL FISCHER TITRATOR Ruchi Bhatia Lecturer Dr. S. Nayak Principal

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2 INTRODUCTION

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3 Karl Fischer titration is a widely used analytical method for quantifying water content, in the form of water of hydration or absorbed water. This method was invented in 1935 by the German chemist Karl Fischer. This Water Determination Test (Karl Fischer Method) is designed to determine water content in substances, utilizing the quantitative reaction of water with iodine and sulfur dioxide in the presence of a lower alcohol such as methanol and an organic base such as pyridine.

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4 This titration method uses coulometric or volumetric titration to determine trace amounts of water in a sample. Coulometric titrations use a constant current system to accurately quantify the concentration of a species. The volumetric titration is based on the same principles as the coulometric titration except that the anode solution above now is used as the titrant solution. The titrant consists of an alcohol (ROH), base (B), SO 2 and a known concentration of I 2 .

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5

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6 In the coulometric titration method, first, iodine is produced by electrolysis of the reagent containing iodide ion, and then, the water content in a sample is determined by measuring the quantity of electricity which is required for the electrolysis (i.e., for the production of iodine). In the volumetric titration method, iodine required for reaction with water is previously dissolved in water determination TS, and water content is determined by measuring the amount of iodine consumed as a result of reaction with water in a sample.

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7 Enhanced accuracy and reproducibility. User friendly. Eliminates use of conventional delicate & fragile Glass burette. Highly motorized dispensing system for precise control of titrant volume. Endpoint is provided by both visual as well as audible alarm. Salient Features of Karl Fischer Titrator

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8 Facility for calculating titer value automatically . Storage facility of date , time & batch number & final results of 20 titrations. Internal battery backup provision to store result even if instrument is not switched on. Provision for external printer attachment. Analyses moisture concentration of liquid samples, powder , fine particles, fiber sample etc. Salient Features contd…..

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9 Technical Specifications of Karl Fischer Titrator Measuring range 10 ppm to 100% of moisture Measuring method Karl Fischer volumetric titration method Indication of titrant volume 0.00 to 99.99 ml on display Moisture content calculation(Automatic) % age : 0.00 to 100% ppm : 10 to 999999 mg H 2 O : 0.00 to 999.99 KF Titer factor In-built automatic KF Titer Factor calculation facility End point alarm Visual LED and Audible alarm

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Wait time for end point alarm Adjustable (1 to 59 seconds) Keyboard 24 keys soft touch, membrane type Sample storage Upto 20 latest samples using FIFO memory Display 8 digit bright red, seven segment LED display Clock In-built clock with date and time display Stirrer In-built magnetic stirrer with adjustable speed Reagent bottles 3x250ml bottles for KF Reagent, Methanol and Calcium Chloride Printer interface External Dot-Matrix Printer interface available 10 Technical Specifications contd…

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11 Standard Accessories Dual Platinum Electrode Titration Vessel Built-in Magnetic Stirrer Teflon Coated Magnetic Stirring Capsule 250ml bottle for methanol 250ml Reservoir Bottle for KF Solution 25 µl Syringe 250ml bottle for Calcium Chloride Adaptor for KF Reservoir Adaptor for Methanol Reservoir Bottle Instruction Manual

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12 Principle The Pharmacopoeias all over the world prescribes the limit for the content of water to achieve uniformity in the quality of drugs. Karl Fischer titration is one such method used for quantifying water content, in the form of water of hydration or absorbed water which works using Dead -stop end point type of assembly.

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Karl Fischer Reagent Composition Karl Fischer Reagent used in the titration is composed of Iodine , Sulphur dioxide , Pyridine and methanol in following molar basis 1I 2 : 1SO 2 : 1 CH 3 OH : 3C 5 H 5 N Pyridine is used as: It forms complex with Sulphur trioxide . It neutralizes hydroiodic acid formed in the reaction and prevent oxidation of HI to I2. Prevents reverse reaction if concentration of acidic product increased

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14 The reaction of KFR is stated to proceed in following steps: I 2 + SO 2 + H 2 O 2HI+SO 3 SO 3 + C 5 H 5 N C 5 H 5 NSO 3 HI+C 5 H 5 N C 5 H 5 N.HI C 5 H 5 N.SO 3 + CH 3 OH C 5 H 5 N.HSO 4 CH 3 ROH + SO 2 + R’N [R’NH]SO 3 R + H 2 O + I 2 + 2R’N 2[R’NH]I+[R’NH]SO 4 R [alcohol] [base] [alkyl sulfite salt] [water] [iodine] [hydroiodic acid salt] [alkyl sulfatesalt] Water and iodine are consumed in a 1:1 ratio. The presence of excess iodine is detected voltametrically by the titrator’s indicator electrode

Titer Factor Determination:

Titer Factor Determination KFR Factor = (mg of sample added x 0.1566) (Quantity of KFR used) Moisture Content = 100*ml of KFR*Factor weight of samples in mg 15

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16 IP SPECIFICATIONS OF SOME DRUGS/CHEMICALS Anhyd . Citric acid :NMT 1.0% w/w determined on 2.0 g Citric acid monohydrate : 7.5-9.0% w/w determined on 0.5 g Anhyd Ampicillin : NMT 2.0% w/w determined on 0.3 g Amodiaquine HCl : Between 6.0-10.0 %w/w determined on 0.5 g Amoxicillin Na : NMT 4.0% w/w determined on 0.4 g Ampicillin Na : NMT 2.0% w/w determined on 0.3 g Betamethasone Sodium : NMT 8.0% determined on 0.5 g Phosphate Sulfacetamide Sodium : Between 6.0-8.0% w/w determined on 0.2 g

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17 Food stuff Sugar Wood Paper Textile Industry Chemicals (Alcohols, Acids) Oil, fat, wax Moisture sensitive drugs (e.g. sulfonamides) Applications For determination of moisture content in:

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18 Thank You

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