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University Of Central Lancashire Department of Forensic and Investigative Science FZ1025 Experimental Techniques in Chemistry

2. Preparation of tin tetraiodide
INTRODUCTION Tin tetraiodide can be prepared by the direct reaction of tin and iodine, but the reaction can be violent. The use of a solvent leads to a safer and smoother reaction, however water cannot be used because iodine is insoluble and tin tetraiodide is hydrolysed by it. Because of volatility as well as health and safety issues associated with chloroform and tetrachloromethane, dichloromethane is used as the solvent instead. PRE-LAB QUESTIONS 1) What is the ‘inert-pair effect’ and why does it occur? Which block of the periodic table is it most likely to occur? Which non-radioactive element of group 14 is most likely to be susceptible to the inert-pair effect? (6 marks) 2) Tin tetraiodide is sometimes used in organic chemistry reactions. Write a balanced equation for the reaction of CH3MgBr with tin tetraiodide, naming the products formed. (3 marks) 3) In this experiment you will be using dichloromethane as a solvent. What should you do with your waste dichloromethane? (1 marks) HEALTH & SAFETY Chemical / Process Hazard Severi ty Grade 1-4 A
1 2

Likelihood of occurrence Grade 1-4 B
1 2

Risk (A x B) (Likelihood x hazard)

Safety

Tin foil Iodine

1 4

Dichloromethane Acetone

2 1

2 2

4 2

Not hazardous. Wear gloves. Harmful by inhalation and in contact with skin. Wash with plenty of water and soap, consult a physician. Wear gloves. Harmful by inhalation and in contact with skin. Flammable. Wash with copious amounts of water.

remove heat. Calculate the theoretical yield and the % yield. When the flask is cool. with the condenser still in place. 7. Continue heating the mixture under reflux until all the tin has dissolved (record the reaction time. remove both the flask and the test tube from the ice bath and dry both.0067 mol Sn) of tin foil and tear this into small fragments. Discuss your observations and pH values when you add water to your product. 6. but it should be approximately 30 minutes). place the flask in an ice/water bath. Fill a test tube with 5 ml distilled water.81 g mol-1) iodine and 15 ml dichloromethane.8 g (M(I 2)=253. then remove the condenser. Compare the melting point of your product to the literature value (give reference) and discuss any differences. At the same time place a test tube with 15 ml dichloromethane in the ice/water bath. add another 0. 3. Fit the flask with a water-cooled condenser and heat on a hotplate until the mixture starts to boil and reflux (74°C). Observe what happens and record the pH value. Dry the crystals in a vacuum desiccator for 5 minutes and determine yield. Use some of the extra dichloromethane to transfer the product to the glass-filter. 3. Remove the condenser from the flask and filter off the product using a glass-filter (porosity 3 or 4). Drain the crystals briefly on the filter and collect the crystals in a glass container with lid (weigh the container + lid in advance). 4. Work as quickly as you can without making mistakes because tin tetraiodide is slowly hydrolysed by moisture in the atmosphere. When the tin has dissolved. cool the flask in a beaker of cold water with the condenser still in place.2 g iodine and replace the condenser before bringing the mixture back to reflux. What is the shape of the molecules of the compound and what is the predominant type of bonding in the molecule. Determine the melting point of the crystals. Place these in a dry 100 ml Quickfit conical flask together with 3. 2. 8. give an equation for the hydrolysis reaction. Weigh 0. Rinse once more with the cold dichloromethane to remove any remaining iodine. then add a small sample of your product (spatula tip). 5.8 g (0. 5. swirl flask to dissolve the crust (if any) and. If the iodine colour becomes very weak before all the tin has dissolved. check the pH value with indicator paper. 2. 4. Report: 1.EXPERIMENTAL 1. What is the oxidation state of tin in this compound? What other oxidation states of tin are predominant and how might you alter the oxidation state of the tin in tin tetraiodide to these other oxidation states? .