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University Of Central Lancashire School of Forensic and Investigative Sciences FZ1025 Experimental techniques

6&7. Synthesis, Characterisation and Stability of an Interhalogen Compound
INTRODUCTION The aim of this experiment is to introduce you to the synthesis and analysis of a compound containing an interhalogen ion. You will also investigate the decomposition of this interhalogen anion to another and accurately establish the stoichiometry of both interhalogen anions using volumetric analysis. Many interhalogen compounds have been synthesised and fully characterised. Stable interhalogen molecules are of the type XYn where n is an odd number and Y is usually the lighter halogen. Examples include ClF, BrF3, IF7 and ICl3. Also, a wide range of cationic and anionic interhalogen species are known. For example, [Br2]+, [I5]+, [ClF2]+, [BrF6]+, [IF8]-, [Cl3]- and [IBrCl]-. Some ions such as [I3]- are stable even in aqueous solution, but most of the larger ions exist only in crystalline salts with large counter-ions. The molecular structures of interhalogen species can be reliably predicted using VSEPR theory.

PRE-LAB QUESTIONS 1. Write balanced equations for the reaction of aqueous iodate (V) with excess iodide in the presence of acid and the reaction of molecular iodine with thiosulphate ions. (4 marks) 2. Why is potassium iodate (V) a good primary standard? (3 marks)

3. This experiment uses chlorine gas. What safety precautions should you take when using this substance? (3 marks)

COSHH ASSESSMENT: Please read the safety information carefully before beginning the practical
Chemical / Process Hazard Severity Grade 1-4 A 2 2 3 Likelihood of occurrence Grade 1-4 B 2 2 2 Risk (A x B) (Likelihood x hazard) 4 4 6 Safety

Dichloromethane Tetrabutylammonium iodide Chlorine

Wear gloves. Harmful by inhalation and in contact with skin. Harmful by ingestion and irritating to the eyes Toxic by inhalation, very irritating to eyes and respiratory system. Strong oxidising agent Extremely flammable – keep away from ignition sources. Harmful by skin contact and inhalation

Diethyl ether




Add the cold dichloromethane to the conical flask and shake gently until the solid dissolves. 15 minutes. Weigh your product accurately and keep in the dark. 40°C) but make sure your compound remains in solution by adding drops of dichloromethane should any yellow precipitate be observed. Lithium iodide Acetone 1 1 1 2 1 2 EXPERIMENTAL Part 1: Synthesis of the interhalogen compound 1. (this is to prevent oxidation of your product which can occur if there are any traces of water present). . Wash with copious amounts of water and consult a physician.0 g of your product [nBu4N][ICln] and grind the crystals to a fine powder using a mortar and pestle. 7. Prepare an ice bath. Harmful by ingestion Flammable. When precipitation from the solution has stopped. Cool 25 ml of dichloromethane in a measuring cylinder. Filter the cold solution on a Buchner funnel and suck dry for approx. remove from the chlorine supply. Wash the crystals with a small amount of diethyl ether to aid drying. Harmful to eyes and lungs Oxidising agent. Wash with copious amounts of water. 9.. 3. add water to the ice to aid heat conduction. 3. 2. 4. Place the watch glass in a vacuum desiccator and place under the light source provided and leave overnight. Spread the powder as a very thin layer on a watch glass. 1. Heat the flask gently on a water bath in the fume cupboard for approximately 5 minutes or until the bubbling due to the evolution of excess chlorine has stopped. 5. Take approx. 8. 2. Slowly pass chlorine gas over the surface of the solution which should be gently swirled in the flask. Do not boil the solution (boiling point of dichloromethane is approx. Cool the solution in the ice bath. Cool the solution in the ice bath for about 10 minutes or until crystallisation is complete. 6. Part 2: Light Decomposition 1. Weigh accurately approximately 2 g (make a note of the actual weight) of tetrabutylammonium iodide and place into a 125 ml conical flask with a stopper. Harmful by ingestion May be irritating to the eyes and skin Corrosive.Sodium thiosulphate solution Potassium iodate (V) Potassium iodide Sulphuric acid 1 1 1 2 2 2 1 2 2 2 1 4 Harmful by ingestion.

Calculate the yield of [nBu4N][ICln]. The add 12 ml of 0.15 g of your [nBu4N][ICln]. 3. Repeat the titration once more and calculate the value of n for the interhalogen anion. Using your titre figures from part 4 and the following equation. The end point of the titration corresponds to the disappearance of the iodine colour from the solution. 2.5 M potassium iodide solution and 20 ml of 1 M sulphuric acetone solution results in the quantitative liberation of iodine according to the equation below. POST-LAB QUESTIONS 1. 3. 1. Add approximately 20 ml of acetone and shake until the solids dissolve. Remove 20 ml of this solution and place in a 250 ml conical flask. The liberated iodine can then be determined by titration with the previously standardised solution of sodium thiosulphate. Using your results from part 3. 4.product into a 125 ml conical flask and add approximately 0. calculate the value of n for the interhalogen anion.05 ml. Formula weight of potassium iodate (V) is 214 g/mol.02 M solution. Repeat the titration twice until the titres agree within 0.1 M sodium thiosulphate solution provided 2. Fill your burette with the approximately 0. calculate the molarity of the sodium thiosulphate solution. 5. 4. Without any delay (to prevent air oxidation of I2) titrate the solution against your previously standardised thiosulphate solution. Titrate the liberated iodine against the thiosulphate solution. 2.5 g of lithium iodide. calculate the yield of your [nBu4N][ICln]-. 6. [nBu4N][IClm]Repeat the steps given in part 4 for your decomposition product and determine the value of m in the interhalogen anion. . [ICln]. 4. Part 5: Volumetric analysis of the decomposition product. The end point will correspond to the disappearance of the iodine colour from the solution. Prepare this solution in a 250 ml volumetric flask using deionised water.and use VSEPR theory to calculate the shape of the anion. [nBu4N][ICln]The basis of the analytical method here is that the addition of lithium iodide to [ICl n]. Using your titre figures from part 5 calculate the value m for the interhalogen anion and use VSPER theory to calculate the shape.Part 3: Standardisation of sodium thiosulphate solution 1. Record your titre figures in your notebook and calculate the molarity of the thiosulphate solution. Accurately weigh 0. Calculate the mass of potassium iodate (V) required to make 250 ml of a 0. Part 4: Volumetric analysis of the first product. Based on the weight of the tetrabutylammonium iodide starting material.+ n LiI → n/2 I2 + n LiCl + I3.

.5. Attempts to synthesise Li[ICln] result in the formation of LiCl. Make use of this fact. to explain why large cations such as [nBu4N]+ are used in the synthesis of interhalogen anions. ideally with an appropriate Born-Haber cycle.