Sn4 Synthesis Lab Report

The synthesized product, SnI4 was found to have a yield of 0.0227 g which corresponded to a 4.63 % yield. The synthesizing process of SnI4 showed distinctive changes. After the addition of dichloromethane the solution turned to a purple color, this then turned into a purple-burgundy colour after gravity filtration; the desired colour was observed only when vacuum filtration was applied. The purple solution turned into damp orange crystals and after thorough drying the crystals were a bright, dry and dusty orange. The average melting point range of the final product was 142 °C - 143 °C which corresponded to the melting range of SnI4 143 °C 1. This range was found by doing three trials and then tabulating the average between them (Table
A percent yield of 4.63% was determined (see appendix for calculations). The low yield was due to various sources of error in the performed experiment. Sources of error that led to a loss of product were filtering of the product with the gravity filter and the Hirsch funnel, as it was difficult to obtain the entire product from the filter paper and the sides of the funnel. As the experiment follows a semi microscale technique even a small amount of lost product yields a great loss in the yield 4. These sources of error could be minimized by doing a larger reflux in order to increase the yield. However, as the purpose was to simply synthesis SnI4 in order to identify the stable oxidation states (the melting point range requires very little product) it would be advantageous to use the current method. This is due to the smaller quantity of materials needed for this type of reflux, thus making less of an environmental impact (using smaller quantities means that the material is saved for other reactions and therefore lessening the amount needed to be bought) when conducting the experiment. The solvent temperature is also a factor in good yield. The SnI4 dissolves in hot dichloromethane, this is very important when the gravity filtration is done as the impurities should be insoluble in the hot solvent allowing for the filter paper to catch them. After recrystallization, the product was washed twice with cold solvent, as the product is insoluble it
Both the SnI2 and SnI4 have a bright orange colour to them, therefore formation of the product would not indicate which compound was formed 2. The melting point however is a powerful method to use in order to distinguish the two compounds as SnI2 has a literature melting point value of 320 oC 2 and SnI4 has a melting point of 144.5 oC 1.The prepared product had an average melting point range of 142 °C - 143 °C. This range includes the melting point of SnI4 and not SnI2. Thus, the prepared product was identified as SnI4. The range was lowered by a few degrees due to impurities in the prepared compound. Impurities in a compound will decrease the melting point and increase the range at which the compound melts 4. However, since the range of the product is quite small and close to the literature value it can be said that the product contained few