Experiment 8 EMPIRICAL FORMULA OF A HYDRATE Learning Objectives By the end of this experiment the student should have learned: 1. A method for determining the identity of an inorganic salt. 2. To determine the percent water and empirical formula of a hydrate. 3, To use a platinum wire flame tester. Text Topics ‘The mole, percent composition, empirical formula, hydrates (Malone, Chapter 8). Exercises For additional problem solving experience with the mole, percent composition and empirical formulas, see Exercises 16, 17. Discussion Many compounds decompose when heated before their melting points are reached. Decomposition of a compound results in the formation of two or more distinct substances. A particular class of compounds that undergo decomposition are the inorganics (often called salts) that contain waters of hydration in their crystal structures. In these compounds called hydrates, the water is weakly bonded to the salt and usually can be driven off with relatively mild heating. The formulas of hydrates are written in a unique fashion. The formula of the anhvdrous ealt is written firet and a dot fnilawe A enaffieient denetine the108 Experiment 8 CuS0,'5 H,0 Hydrates are the only compounds that have coefficients in the middle of their formulas. Some compounds like water so much that they absorb water from the atmosphere. These compounds are deliquescent or hygroscopic and can be used as desiccants to keep the environment of a container dry. In some hydrates, the water of hydration is bonded so weakly that it tends to escape even at room temperature when the compound is exposed to the atmosphere. These compounds are efflorescent. In the first part of this experiment you will study the efflorescence and deliquescence of two compounds and attempt to verify that copper sulfate pentahydrate loses water when heated. As stated earlier, waters of hydration can usually be driven off with mild heating. When the water can be driven off, it is possible to determine the mass percent of water that makes up the formula unit, simply by weighing the hydrate, heating it to drive off the water, then weighing the anhydrous salt, weight lost after heating x 190% = % water in the hydrate original weight If the identity of the anhydrous salt is known, then it is possible to determine the formula of the hydrate, Suppose you know you have the hydrate of barium chloride but you don't know what its formula is. You weigh a sample of it and find it has a mass of 4.13 grams. After you heat it you find the mass of the resulting anhydrous salt is 3.52 grams. The percent by mass of water would be: (: 13 2x 100% = 14.8% 4.13 You can determine how many water molecules are associated with each formula unit of the hydrate by determining the number of moles of water that were driven off and the number of moles of barium chloride left. 1 mol 208.2 grams BaCl, 3.52 grams BaCly x 1.69 x 107? mol BaCly 1 mol Thon an x -? mol 180 grams H,0 ~ °4 * 10 ‘mol Ho 0.61 grams H,0 x 0.034 moles HaO 0.0169 moles BaClz Therefore, there were 2 moles of water per mole of BaClo BaClp*2H0,) > BaClyy + 21,0, In the second part of this experiment, you will determine the identity of an unknown salt (strontium chloride, zine sulfate, or magnesium sulfate), the percent water of the unknown hydrate, and the formula of the hydrate. One of the techniques that you will use for identification purposes is called a flame test. In the flame test, a platinum wire is inserted into a solution containing the ions of interest and then inserted into a bunsen burner flame. For some cations, the energy of the flame will cause electrons to be elevated from the ground state or lowest possible energy levels to higher energy orbitals. As this results in anExperiment 8 109 often in the form of a characteristic emission of light. The color of the light is useful for the verification of the presence of certain cations (e.g., Na*, Ba**, Ca*?, Sr*?, Li*, K*). Procedure A. DELIQUESCENCE AND EFFLORESCENCE Place a few crystals of sodium sulfate decahydrate on a watch glass. Occasionally observe their appearance for about an hour and write an equation for the observed change On another watch glass, place a few crystals of potassium acetate. As above, observe their appearance. B. COPPER SULFATE PENTAHYDRATE Put 1.0 grams of CuSO, 5 H,0 into a 13 mm x 100 mm test tube. Stuff a small wad of fine glass wool into the test tube so that it holds copper(II) sulfate pentahydrate in place when the tube is tilted downward (caution: minimize contact of the glass wool with your hands - it causes splinters and itching). Clamp the test tube upside down over a watch glass. Holding the base of the burner, heat the CuSO, +5 HzO. The blue color should begin to dissipate while the vapors given off condense to a liguid (caution: if blackening occurs, reduce the heat). Heat until several drops of liquid have been collected and the residue is white. Using an eyedropper, test a drop of the liquid collected in the watch glass with a piece of blue cobalt chloride test paper (if the paper is pink, pass it quickly over the burner flame to turn it blue). Test a drop of water on a piece of blue CoClz paper. 1.0 gram CuS04°5H20 h Bunsen burner Glass woo! piog 13160 mm test tube SS Watch glass110 Experiment 8 c. ANALYSIS AND PERCENT WATER OF AN UNKNOWN HYDRATE 1. Your unknown is a hydrate of strontium chloride, magnesium sulfate, or zine sulfate. Dissolve a little of your sample (about 0.1 gram) in a small amount of water (about 5 mL) in a test tube to use for 1 and 2. Clean a platinum wire in a bunsen burner by dipping it into dilute HCI and inserting it into the flame until little color is observed. Perform flame tests sequentially (clean the wire between each solution) on known solutions of ZnSO, Mg8O,, and SrClz, and finally the solution of unknown. 2. If your unknown is not SrClo, drop a short piece of magnesium ribbon into your unknown solution. Allow 30 seconds for a reaction to take place. If the magnesium ribbon tarnishes, your unknown is ZnSO,. If no reaction other than bubbling occurs, the unknown is MgSO,. The bubbling is due to a side reaction of the magnesium with water (Mg + 2 H,O = Mg(OH), + H,). Mgia, + ZnSOiagy = MgSOgagy + Zrie) Mg « + MgSO, (ag) = no reaction Based on the flame test and/or the attempted reaction, identify your unknown, 3. Weigh a clean, dry crucible and cover to at least the nearest 0.01 gram. Place about 4 grams (3,5-4.5) of your hydrate crystals in the crucible and weigh to the nearest 0.01 g. Suspend the crucible in a clay triangle over a bunsen burner. Heat gently with the top slightly ajar for eight minutes and then vigorously (the crucible should glow a dull orange) for an additional eight minutes. Allow the crucible to cool (about 5 minutes), and weigh it to the nearest 0.01 g. Heat the crucible vigorously again for about 5 minutes, cool, and weigh again. If the weight difference between the first and second heatings was greater than 0.05 g perform a third heating, cooling, weighing cycle. Repeat the process until two successive weighings agree to 0.05 g.5MPrelaboratory Exercises—Experiment 8 EMPIRICAL FORMULA OF A HYDRATE For additional problem solving experience with the mole, percent composition and empirical formulas, see Exercises 16, 17. 1. Complete and balance the following reaction: CaCla+ 2 HzO.) 2. What is the percent by mass of water in CuSO, +5 H,0? 3. A 4.00 gram sample of a hydrate of nickel(II) bromide loses 0.793 grams of water when heated. Determine the mass percent water in the hydrate and the formula of the hydrate.114 Experiment 8 Solutions to prelaboratory exercises 1. CaCly:2 H,0,)—*+ CaCl, + 2,0 5(18.0 g/mole) 249.68 g/mole 0.793g 4.008 x 100% = 36.0% x 100% = 19.8%water Lmole NiBry 218.5 gNiBry mole HO. 0.793gH,0 gg gH. ~ 0-0441molesH.0 0.0441 moles H,0 0.0147 moles NiBry B.21gNiBry x = 0.0147 moles NiBrz = 3.00 moles H,O/mole NiBr, So the formula is NiBr,-3H 0RESULTS AND QUESTIONS:~—Experiment 8 EMPIRICAL FORMULA OF A HYDRATE Date Name Lab Sec. —. Desk No. Observations Reaction A. 1. Na,SO,+10 H,0 —_— 2. KC;H3O2 B. 1. condensate + CoCl, paper 2. water + CoClz paper (hint: forms cobalt chloride hexahydrate) 3. condensate + Cuso, 4, water + CuSO, 5. What compound do you suspect the condensate is? Explain your answer.116 Experiment 8 Cc. 1 2. Unknown #. Flame test: Solution _ SrCly ZnSO, MgSO, unknown Mg + UNKNOWN Flame Color Observations Unknown (circle one): SrClz,_— ZnSQ,, — MgSOy a. Mass crucible and cover + Mass crucible and cover c. Mass crucible and cover after first heating d. Mass crucible and cover + unknown after second heating e. Mass crucible and cover + unknown after third heating (if necessary) f. Mass crucible and cover + unknown after fourth heating (if necessary) unknown unknown + Mass of original unknown h. Mass of water lost from unknown i, Mass percent of water in unknown j. Mass of unknown salt remaining after heating k. Moles of unknown salt 1, Moles of water lost m, Ratio of moles of water to moles of unknown (use appropriate number of significant figures) Sl.