EXPERIMENT - 2 Properties - Separation of a Mixture INTRODUCTION- Separation of the components of mixtures is performed in chemistry laboratory. Each component in a mixture retains its own set of physical properties. You will use the differences in properties to separate silicon dioxide (SiO2, sand), sodium chloride (NaCl, table salt), and ammonium chloride (NH4Cl), from a mixture of these compounds. A description of some common properties used in separating mixtures follows. (a) SUBLIMATION: Sublimation is the process by which a solid changes from the solid to the gaseous state directly without forming a liquid. Melting is a process by which a solid changes to a liquid by heating. In this experiment you will use sublimation to separate a solid which sublimes from other solids, namely, SiO2 and NaCl which do not. (b) SOLUBILITY: The extent to which a substance is soluble in a solvent depends upon the chemical structure of both the substance and the solvent. In general, polar compounds, such as sugar and alcohol, and ionic compounds, such as KCl, NaCl, NH4Cl, and NH4NO3 which have ions of low charge density, are soluble in polar solvents such as water. Nonpolar substances, such as grease, wax, and oil, are soluble in nonpolar solvents such as toluene or kerosene. Extracting (dissolving) a soluble substance out of a mixture with a solvent is a common separation technique. In this experiment you will use solubility to separate(extract) a solid, NaCl, which is dissolved in water from another solid, SiO2, which does not. (c) DISTILLATION: If two components have very different boiling points, the substance with the lower boiling point will evaporate more rapidly at a given temperature than the substance with a higher boiling point, and so they can be separated by evaporation. Solid NaCl with a very high boiling point can be separated from a salt solution (salt- H2O solution) by evaporating the water, which has a much lower boiling point. If the vapor condenses as a liquid and is collected, the process is called distillation. The properties of sublimation, solubility, and evaporation usually do not change the chemical composition of a substance. You will use these properties to separate three components of a mixture. You will also use the techniques for decantation (or filtration) and evaporation. 1 Experimental Procedure Part I Obtain a sample of “unknown mixture” from your instructor; record its identity number or letter on the report form. Weigh a clean, dry 150-ml beaker to the nearest 0.01 g. Record the mass on the report form. Measure approximately 2.00 g mixture on a weighing paper and transfer it into the beaker. Part II Heat the beaker and its contents on a hot plate. Ammonium chloride, NH4Cl, will sublime from the mixture and produces a white gas. Continue the heat until no more white gas is produced from the mixture. Allow the beaker to cool to room temperature; then weigh the cool beaker and residue to the nearest 0.01 g and record this mass on the report form. Determine the mass of ammonium chloride and calculate the percentage of NH4Cl. Part III Add about 30 ml of distilled water to the residue in beaker to dissolve (extract) the NaCl. Heat gently (warm solution- DO NOT boil) and stir for at least 5 minutes to loosen and extract salt completely in with water. Decant (or filter) liquid, salt water, to a pre-weighed large evaporating dish to separate salt and sand. Heat the beaker with sand residue on a hot plate to dry the sand. Allow the beaker to cool to room temperature; then weigh the cool beaker and residue to the nearest 0.01 g and record this mass on the report form. Determine the mass of sand and calculate the percentage of SiO2. Part IV Heat the evaporating dish with salt water content on a hot plate to evaporate all water and dry the salt completely. Allow the evaporating dish to cool to room temperature; then weigh the cool evaporating dish and residue to the nearest 0.01 g and record this mass on the report form. Determine the mass of the table salt and calculate the percentage of NaCl. Part V Calculate the total percentage of mixture recovered in this experiment. The accuracy of the experiment is such that the total percentage of your three components should be in the neighborhood of 99 percent. If your percentage recovery is less than hundred percent or more than hundred percent, give an explanation for you errors. 2 EXPERIMENT – 2 REPORT FORM Name ___________________________ Instructor ________________________ Date ______________ Part I 1) Sample Identification ______ 2) Mass of empty beaker ________ g 3) Mass of beaker + mixture ________ g 4) Mass of mixture ________ g Part II 5) Mass of beaker + sand + salt ________ g 6) Mass of ammonium chloride [(3) – (5)] ________ g 7) Percentage of NH4Cl = [ (6) / (4) ] x 100 ________ % (show your calculation) Part III 8) Mass of beaker + dry sand ________ g 9) Mass of sand [ (8) – (2) ] ________ g 10) Percentage of SiO2 = [ (9) / (4) ] x 100 ________ % (show your calculation) Part IV 11) Mass of empty evaporating dish ________ g 12) Mass of evaporation dish + dry salt ________ g 13) Mass of dry salt [ (12) – (11) ] ________ g 14) Percentage of NaCl = [ (13) / (4) ] = ________ % (show your calculation) Part V - Total percentage of mixture recovered ________ % Explanation: 3 EXPERIMENT – 2 Name Pre- laboratory Questions and Exercises Due before lab begins. Answer in space provided. 1. Define the following terms; a) Evaporation- b) Sublimation- 2. A student used 20 ml water instead of 30 ml for extraction of salt from mixture. How would this change effect on the percentage of NaCl. 3. Naphthalene sublimes easily upon heat. How do you separate a mixture of naphthalene and NaCl? 4. Define the process of boiling. 5. A mixture was found to contain 1.50 g NH4Cl, 0.80 g NaCl, and 1.20 g SiO2. What is the percentage of sand in this mixture? 4 EXPERIMENT – 2 Name Post- laboratory Questions and Exercises Due after completing lab. Answer in space provided. 1. Define the following terms: a) Filtration- b) Decantation- 2. During heating, some solution of NaCl splattered out of the evaporating dish. How would this observation effect the total calculated percent of mixture? 3. How would you distinguish between mixture and a pure substance? 4. Define the process of melting. 5. A student reported the following combination of unknown mixture “X”: 25% NH4Cl, 30% NaCl, and 50% SiO2. Assuming these calculations are correct, explain the student's error in this experiment. 5