Molar Mass by Freezing Point Depression Adapted from Vonderbrink, Laboratory Experiments for AP Chemistry A procedure that allows the determination of the molar mass of a substance is very useful to chemists. The molar mass is an important value that must be known in order identify an unknown substance or to characterize a newly prepared compound. There are a number of ways of determining the molar mass of a substance. One of the simplest involves finding the change in the freezing point of a solvent when an unknown substance is dissolved in it. It has been found that the change in freezing point is directly proportional to the molality of the solution. This change in freezing point is one of several "colligative" properties of solutions, properties that depend only on the number of dissolved particles in solution, and not on the type of particle. Other colligative properties include change in boiling point, vapor pressure and osmotic pressure. Measurements of these properties also can be used to find molecular mass of solute. The relation to change in freezing point is: ∆Tfp = kfpm where Tfp is the change in freezing point, kfp is the freezing point depression constant for the solvent, and m is the molality of the solution. The value of kfp must be determined for each solvent. The solvent that will be used in this experiment is a nonpolar solvent with the common name butylated hydroxytoluene. This compound is abbreviated BHT and is frequently used as an antioxidant in foods. The IUPAC name for the compound is 2,6-di-tert-butyl-4-methylphenol. Its structural formula is: The figure below shows a cooling curve for a pure solvent and for a solution. Notice that supercooling may occur in both the solvent and the solution. If it does, as the crystals begin to form the temperature will rise slightly and then remain constant as the pure solvent freezes or will slowly fall as the solution freezes. Experiment Overview The purpose of this experiment is to determine the molar mass of an unknown substance by measuring the freezing point depression of a solution of the unknown substance and BHT. Part 1. The freezing point of BHT is first determined by analyzing a cooling curve for BHT. Even though the freezing point of BHT is known, it is necessary to determine it with the thermometer that will be used in the experiment. Even if the thermometer reading is slightly off, the change in temperature should be accurate. It is important that the same thermometer is used to determine both the freezing point temperature of the solvent and that of the solution. Part 2. A known amount of stearic acid (285 g/mol) is then added to a measure quantity of BHT. The freezing point depression (∆Tfp) of this solution is found and the freezing point depression constant (kfp) is calculated. Part 3. The unknown is added to BHT, the freezing point depression of this solution is measured, and the molar mass of the unknown is then determined. To save time, Parts 1 and 2 will be done as a “dry lab”; i.e. you will be given the data. You will need to analyze the data to determine kfp. You will then use a microscale technique to redo Part 2 (melting point of BHT) and to do Part 3 (melting point of a mixture of BHT plus an unknown). From the freezing point depression of the mixture, you will calculate the molar mass of the unknown. Part 2-3 Procedure 1. Pulverize a small amount (about 0.5 g) of BHT with a mortar and pestle. 2. Pack the BHT in a capillary tube to a depth of about 1 cm. Fasten the capillary tube to a digital thermometer. The BHT should be level with the bulb of the thermometer. 3. Immerse the thermometer+capillary tube assembly in a Thiele melting point tube filled with water and heat. Heating can be rapid in the beginning, but as the temperature approaches the melting point, 67°C, heat very slowly in order to get an accurate value. 4. Record the temperature at which the BHT melts. If repeating the melting procedure, use a new sample and capillary tube. 5. Use an analytical balance to accurately measure about 0.5 g ( 1 mg) BHT into a small beaker. Accurately measure about 0.1 g ( 1 mg) of unknown into the beaker. Heat the beaker gently over a small flame. When the substance melts, mix it well with a stirring rod until it is homogeneous. Allow the mixture to cool and solidify. 6. After it solidifies, pulverize a small amount of the mixture and determine the solution melting point. Cooling Cuves Data for BHT kfp Determination Mass of BHT, g 7.990 g Mass of stearic acid, g 1.656 g Time, s 0 20 40 60 80 100 120 140 160 180 200 220 240 260 300 360 Temperature, °C BHT + BHT stearic acid 85.0 76.8 80.0 74.7 75.8 74.5 72.0 72.2 69.0 69.8 68.8 67.8 69.0 65.9 68.8 64.3 68.6 62.9 68.4 61.6 68.2 60.4 61.1 61.5 61.6 61.2 60.5