Lab 4 – Gravimetric Analysis of a Carbonate/Bicarbonate Decomposition Product – “Which Salt” Chemistry B1A / by Daniel & Vaughan/Summer 2015 There are many, many kinds of questions which can be answered with a well-founded understanding of moles and their use through balanced equations. The bread-and-butter calculation of a chemist predicts the amount of product to be obtained based on the amounts of reactants used. Extending that basic use to solving a problem is the focus of this lab. The experimental You will be examining the decomposition of an unknown carbonate or bicarbonate salt. The unknown compound is either sodium bicarbonate, potassium carbonate, or sodium carbonate monohydrate. Note when calculating the molar mass of a hydrate, you must include the water in your molar mass. You should be able to determine which of these three compounds your unknown is which by reacting the unknown salt with an excess of hydrochloric acid, which will cause the following reactions to occur: a. NaHCO3 + HCl ⟶ NaCl + H2O + CO2 b. K2CO3 + 2HCl ⟶ 2KCl + H2O + CO2 c. Na2CO3⋅H2O + 2HCl ⟶ 2NaCl + 2H2O + CO2 The extra HCl, the H2O, and the CO2 will be removed by evaporation (the CO2 will mostly disappear without any help, as it will bubble out of solution). This will leave behind only the product salt (NaCl or KCl). By keeping track of the mass of unknown you begin with, you should be able to predict how much product would be made if it matched any of the salts above. The one you actually come closest to should be the identity for that unknown. Please take good notes in your lab notebook for this experiment. Procedure 1. Obtain a clean, dry 125 mL Erlenmeyer flask, label with you and your partner’s initials, unknown letter, and your lab section, weigh it on the balance and record the mass. To this add 1 g. (±0.2 g) of an unknown salt; record the mass to 3 decimal places. Record the unknown letter/number identifier. Record any observations made of the unknown and any of the following reactions. 2. Back at your bench, add about 10 mL of distilled water and gently swirl your flask to dissolve the solid. Be careful not to get solid on the walls of the container. Your instructor will show you how to rinse and fill a buret with 1.5 M HCl. This is 1.5 molar HCl, which is 1.5 moles of HCl solute dissolved in enough water to make one liter of solution. Lab_4_Which_Salt_Stoichiometry_v5 Page 1 3. Slowly add about 8 mL of the HCl solution to your unknown. Gently swirl the Erlenmeyer flask to mix the substances. Record your observations that show a reaction is taking place. Now slowly add more HCl, drop by drop, until you no longer see bubbles produced. With a stirring rod and about 1 cm (~1/4”) of pH paper test your solution to be sure it is acidic with a pH less than 7. You should not need more than a total of 11 mL of HCl. 4. Attach the flask with a clamp to a ring stand so the flask can be heated with a hot plate. Attach the stem of a funnel to the hose coming out of the side arm on a sink aspirator, and clamp the funnel so that it is upside down above the Erlenmeyer flask. Be sure the hose does not sit on the hot plate to avoid burning the hose. Place a beaker under the faucet. (Warning, item within 17 cm (~1 foot) of the sink may get wet). Heat the Erlenmeyer flask with a setting on the hot plate of about 1/3 of the maximum dial setting. You want a gentle boil. If you smell an irritating odor while heating, turn on the faucet to vacuum the gases above the flask. When the flask contents are about dry, turn off the hot plate. 5. Wait until the hot plate has cooled and your flask contents appear dry. Remove the funnel, carefully remove the Erlenmeyer, and allow it to cool. Measure and record it’s mass. Place the flask in the drying oven for at least 30 minutes, then cool it and record its mass again. If the mass has changed by more than 0.020 g, repeat the oven heating. Data You will be doing 3 calculations for you unknown. Using the balanced equations above, determine the theoretical yield in grams of product salt that could be made from each reactant salt. For example, assuming your unknown is sodium bicarbonate: g NaHCO3 reactant X 1 𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3 84.01 𝑔 1 𝑁𝑎𝐶𝑙 𝑋 1 𝑁𝑎𝐻𝐶𝑂3 𝑋 58.44 𝑔 𝑁𝑎𝐶𝑙 1 𝑚𝑜𝑙 𝑁𝑎𝐶𝑙 = g product (NaCl) This calculates the theoretical yield of NaCl produced if your unknown was NaHCO3. You will also calculate the theoretical yield of NaCl if Na2CO3 H2O was the unknown and the theoretical yield of KCl if K2CO3 was the unknown. You will then compare these theoretical yields with your actual experimental yield. This should help you to decide which compound your unknown is, sodium bicarbonate, sodium carbonate monohydrate, or potassium carbonate. Lab_4_Which_Salt_Stoichiometry_v5 Page 2 Table 1 – Example of data table Trial 1 – Unknown A Mass Empty Erlenmeyer Xxxxxxxxxxxxxxxxxxxxxxxx Flask Mass empty Erlenmeyer Xxxxxxxxxxxxxxxxxxxxxxxx Flask with Unknown A Other things here Xxxxxxxxxxxxxxxxxxxxxxxx …… Percent Error if Unk A is NaHCO3 Percent Error if Unk A is Na2CO3 Identity of Unk A Xxxxxxxxxxxxxxxxxxxxxxxx Xxxxxxxxxxxxxxxxxxxxxxxx Xxxxxxxxxxxxxxxxxxxxxxxx Xxxxxxxxxxxxxxxxxxxxxxxx 1. Calculate the three percent errors for each unknown using the three theoretical yields and your actual yield. Your table should have a title stating what is in the table. (e.g., Mass analysis of unknown carbonate/bicarbonate reaction with HCl) 𝐴𝑐𝑡𝑢𝑎𝑙 𝑌𝑖𝑒𝑙𝑑−𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑 𝐾𝐶𝑙 % Error if Unk A is K2CO3 = | | 𝑥 100% = 𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝐾𝐶𝑙 2. One problem with potassium carbonate is it must be heated before use because it absorbs water from the air. If your unknown was potassium carbonate and it had water in it when you weighted it, how would this affect your calculated yield? How could this change your identification of your unknown. (One way to think about this is in your theoretical yield calculation, how would water change the actual mass of potassium carbonate weighed out, and how would that change the mass of your theoretical product.) 2. Discuss sources of error and how they would change the actual yield. Be specific. Lab_4_Which_Salt_Stoichiometry_v5 Page 3
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