AP Chemistry The Determination of the Percent Water in a Compound The polarity of the water molecule, which makes it a great solvent for ionic compounds, causes water molecules to cling to the structure of solid substances. When this occurs, the trapped water molecules are called water of hydration and they become an integral part of the crystal structure. There are many compounds that have a tendency to absorb water vapor from the air. These compounds are said to be hygroscopic, and can be used as moisture-reducing agents. Other compounds absorb such large quantities of water vapor that they will actually dissolve in their own water of hydration, a property known as deliquescence. In this experiment, you will test a hygroscopic ionic compound to determine its water of hydration. Although the water molecules are securely attached to the ionic solid that you will test, they are susceptible to removal by heat. You will gently heat a sample of the compound to drive off the water of hydration. By measuring the mass of the sample before and after heating, you can determine the amount of water in the sample and calculate its water of hydration. OBJECTIVES In this experiment, you will Carefully heat a measured sample of a hygroscopic ionic compound. Determine the water of hydration of the compound. Complete the chemical formula of the compound. MATERIALS crucible with cover one of the following compounds: crucible tongs magnesium sulfate, MgSO4•nH2O spatula barium chloride, BaCl2•nH2O ring stand, ring, and clay triangle manganese (II) sulfate, MnSO4•nH2O lab burner sodium carbonate, Na2CO3•nH2O desiccator balance PROCEDURE Part 1 Preparation 1. Obtain and wear goggles and apron. 2. Place a clean, dry crucible with a cover in a pipestem triangle mounted on the iron ring. Leave the cover slightly off so that the heating will drive off any water that remains in the crucible. Adapted from Advanced Chemistry with Vernier, Zumdahl, World of Chemistry, 2002 and Heath and Company, 1987 2-1 Heat with Bunsen burner for two to three minutes to make sure that the crucible is dry. See setup on the next page in Figure 1. 3. From this point on, you should not touch the crucible with your hands. Use only the crucible tongs. Allow the crucible to cool for at least ten minutes, then measure the combined mass of the empty crucible and its cover. Record the mass in your Data Table. 4. Place enough of the hydrate that you are assigned into the crucible to that it is one-fourth to onethird full. Use a spatula or similar implement to break up any large pieces of the substance by pressing the pieces against the wall of the crucible. Measure and record the combined mass of the crucible, cover, and hydrate. Part 2 Evaporation of Water 1. Place the crucible, with the cover slightly off, on the pipestem triangle and begin heating. 2 - 2 Adapted from Advanced Chemistry with Vernier, Zumdahl, World of Chemistry, 2002 and Heath and Company, 1987 The Determination of the Percent Water in a Compound Gradually increase the heat until the bottom of the crucible is a dull red. Maintain this temperature for five minutes. 2. Turn off the burner and place the crucible, with the cover, in a desiccator for cooling. Allow the crucible to cool for about 15-20 minutes, then measure and record the mass of the crucible, cover, and contents. 3. Reheat the crucible for another five minutes to make sure that all of the water is driven off. Again, cool it in the desiccator, then find and record the mass. If the masses that you determined in steps 2 and 3 do not agree within 0.03 g, repeat the heating and desiccating process one more time before finding and recording a third mass. Adapted from Advanced Chemistry with Vernier, Zumdahl, World of Chemistry, 2002 and Heath and Company, 1987 2-3 Cleaning Up 1. Carefully clean the crucible and dry it. Return it to its proper location. 2. Place the samples of hydrate in the waste containers on the reagent shelves between benches. 3. Clean up your lab station, returning all equipment to its proper location. 3. Wash your hands thoroughly before leaving the laboratory. DATA TABLE Compound selected for analysis Mass of crucible and cover (g) Mass of crucible, cover, and hydrated sample (g) Mass of hydrated sample (g) Mass of crucible, cover, and dehydrated sample – 1st weighing (g) Mass of crucible, cover, and dehydrated sample – 2nd weighing (g) Mass of crucible, cover, and dehydrated sample – 3rd weighing (g) Mass of dehydrated sample (g) Mass of water evolved (g) DATA ANALYSIS 1. What was the mass of the anhydrous salt? 2. How many moles of the anhydrous salt did you have? 3. How much water was lost from your salt? 4. How many moles of water were lost from your salt? 5. How many moles of water were there per mole of anhydrous salt? 2 - 4 Adapted from Advanced Chemistry with Vernier, Zumdahl, World of Chemistry, 2002 and Heath and Company, 1987 The Determination of the Percent Water in a Compound 6. What is the formula for the hydrated salt? CONCLUSIONS 1. Can you suggest reasons why the procedure used in this experiment might not be appropriate for all hydrates? 2. A substance was found to have the following percentages: Zinc 23% Sulfur 11% Oxygen 22% Water 44% What is the empirical formula of this compound? 3. If a sample of 2.56 g of this substance were heated in a crucible as in this experiment, calculate the mass of anhydrous compound that would remain in the crucible. 4. Many different drying agents could have been in your desiccator. What characteristics should these compounds have? Adapted from Advanced Chemistry with Vernier, Zumdahl, World of Chemistry, 2002 and Heath and Company, 1987 2-5