Qualitative Analysis of Household Products (or Kitchen Qual) Introduction Chemists often find themselves faced with the question: "What the heck is it?" Sometimes “it” is a reaction that has gone astray and looks vaguely like tar. Other times “it” could be a mystery - a white powder left at the scene of a crime: sugar, talc or any variety of illegal drugs. The criminal justice system has increasingly relied on the chemical identification techniques. Often identification is a very long and tedious process of proving what the substance is NOT. Clues from the area where the substance was found typically help to narrow the list. Today you will be the investigating chemist in a perplexing mystery. You were cleaning your basement shelves and found three unmarked bottles containing white powders. Since the powders can't possibly be anything illegal, you look around the shelves to see what the bottles might Possible Unknowns Source Chemical contain. You find a bucket of white chalk pieces, a Washing Soda Sodium Carbonate - Na2CO3 box of table sugar, cornstarch, Epsom salts, Plaster of Drain Opener Sodium hydroxide - NaOH Paris from an old art project, laundry detergent, drain Plaster of Paris Calcium sulfate - CaSO4 opener, and a box of Estee fruit sugar. Since these White chalk Calcium carbonate - CaC03 substances are all white powders you consider some Cornstarch Cornstarch Fruit sugar Fructose - C6H1206 simple physical and chemical tests that will reveal Table sugar Sucrose - C12H22011 their identity by process of elimination. Technically Epsom salts Magnesium Sulfate - MgSO4 speaking, you've designed a qualitative analysis scheme. (Qualitative analysis is only concerned with what the substance is. Quantitative analysis is concerned with determining how much of each substance is present.) The scheme acts as a separation flow chart (see below) answering “If it reacts like …, then it must be X” statements. Conveniently, even the reagents you use are fairly common household products: water, vinegar, Tincture of iodine, laxative tablets, and copper test tablets. Using these simple chemical tests, you will determine the identity of several unknown powders. First, you make use of the substances’ solubility in water. Most of the chemicals will dissolve readily in water but calcium sulfate, calcium carbonate, and cornstarch are insoluble. These three compounds can be distinguished from one another with chemical tests using iodine and vinegar. Cornstarch will form a complex with iodine resulting in a dark blue color while calcium sulfate and calcium carbonate are unreactive. The cornstarch, a polymer of sugar molecules, wraps itself around I2 molecules like a constrictor wraps its prey. Cornstarch + I2 Starch-I2 Complex (dark blue) The other two white powders, calcium sulfate and calcium carbonate, can then be tested with vinegar. The vinegar (~ 5% acetic acid, CH3COOH (a source of H+)) will react with the carbonate ions to initially form carbonic acid (an acid-base neutralization reaction). The carbonic acid is unstable and eventually decomposes to water and carbon dioxide (bubbles!). CO32- + 2 H+ H2CO, (carbonic acid) H2CO3 H2O + CO2 (g) (bubbles) The next task is to differentiate the powders that are soluble in water: sodium hydroxide, sodium carbonate, sucrose, fructose, and magnesium sulfate. We can use an acid-base indicator (a substance that changes color depending on the pH) to determine if the unknown solutions are acidic, neutral or basic. Common household indicators could be plants (beet juice or red 1 cabbage) or laxatives! We will be using phenolphthalein, a compound once found in certain laxative tablets. Phenolphthalein turns from colorless to pink in basic solutions. Only two of the soluble unknowns (sodium hydroxide and sodium carbonate) form basic solutions (alkaline) when mixed with water. Of the last three (sucrose, fructose, and magnesium sulfate) only the magnesium sulfate forms a white solid with drain opener (sodium hydroxide). The precipitate is the main ingredient in Milk of Magnesia, magnesium hydroxide. MgSO4 (aq) + 2 NaOH (aq) Na2SO4 (aq) + Mg(OH)2 (s) This is considered a "double replacement" reaction since all of the ions "switch partners." Finally, copper reduction test tablets will be used to distinguish fructose from sucrose. The tablets are used for water analysis and are available in most variety stores. Fructose has the ability to reduce copper (II) to copper metal forming a red/brown precipitate: Cu2+ (aq) + 2 electrons Cu° (s). This set of “homemade” reactions is very similar to techniques used in analytical laboratories. The methods are very reliable and effective while the cost of the reagents is minimal. Experimental Procedures You will be drawing conclusions based only on your observations. Observe Carefully! First test the Known Samples to identify what a positive or negative result will look like. Then conduct the same tests with your unknowns. Be careful of contamination of the samples - always use a clean spatula when switching powders and rinse the testubes well. A. Solubility Test 1. Obtain a test tube and put a microspatula TIP (about 1/8th teaspoon) worth of the solid unknown in the test tube. 2. Fill the test tube about ½ full with water. Cap the test tube with a stopper and shake. 3. If the powder does not dissolve (indicated by a cloudy solution), it is insoluble - go to step B. If the powder dissolves or begins to dissolve it is soluble -go to step D. B. Iodine Test (Done with the insoluble powder test tube from the solubility test.) 1. Add 2-3 drops of Tincture of Iodine to the test tube from the solubility test. 2. Observe the color. (Blue = Cornstarch, Brown = CaCO3 or CaSO4) C. Vinegar Test (Done with NEW test tube and samples.) 1. Place a spatula tip of the insoluble powder into a clean test tube. 2. Add about 2 - 3 mL of vinegar. 3. If bubbles form the solid is CaCO3. If bubbles do NOT form the solid is CaSO4. D. Phenolphthalein Test (Done with the resulting solution from A. Solubility Test) 1. Add 3 - 5 drops of phenolphthalein to the test tubes. 2. Observe the color. 2 3. A dark pink color indicates a basic solution and the powder is either NaOH or Na2CO3 - go to step E. A colorless solution indicates a slightly acidic solution and the powder may be Sucrose, MgSO4,or Fructose - go to step F. E. Vinegar Test #2 (Done with NEW test tube and samples.) 1. Place a spatula tip of powder into a clean test tube. 2. Add about 2-3 mL of vinegar. 3. If bubbles form the solid is Na2CO3. If bubbles do NOT form the solid is NaOH. F. Sodium Hydroxide Test (Done with NEW test tube and samples.) 1. Place a spatula tip of powder into a clean test tube. 2. Add about 2 - 3 mL of water. 3. Add a few drops of 0.3 M NaOH and observe. 4. If a white precipitate (cloudy solution) forms the solid is MgSO4. If the solution remains clear, the solid is either Sucrose or Fructose - go to step G. Copper Sulfate Test (Done with NEW test tube and samples. Increase sample size to ~1/4 tsp) 1. Add about 2-3 mL of copper sulfate solution. 2. Add approximately 10 drops of 0.3 M NaOH. 3. Warm the test tube in a hot water bath and observe. Be patient - this reaction could take several minutes. It is helpful to run a sample of fructose at the same time as your unknown. 4. If the solid is fructose a green color will initially be observed followed by the formation of a red precipitate. If the solid is sucrose, the solution will remain light blue. Sample Data Table (Indicate results of tests here.) Unk # Solubility Iodine Vinegar 1 Acid/Base Indicator NaOH Vinegar 2 Copper Reduction Product Identity • Adapted from: Journal of Chemical Education, Volume 68' Number 4, April 1991, pp. 328-324. 3 Household Product Qualitative Analysis Scheme Sucrose, Fructose, CaCO3, NaOH, MgSO4, CaSO4, Na2CO3, Cornstarch Insoluble Soluble Water CaCO3, CaSO4, Cornstarch Blue Sucrose, Fructose, NaOH, MgSO4, Na2CO3 Brown Pink Iodine Cornstarch Phenolphthalein Colorless CaCO3, CaSO4 NaOH, Na2CO3 Bubbles Sucrose, Fructose, MgSO4 No Bubbles Vinegar CaCO3 CaSO4 Bubbles No Bubbles Vinegar Na2CO3 NaOH Sodium Hydroxide NaOH MgSO4 Sucrose, Fructose Red precipitate Copper Sulfate Fructose Sucrose 4 White precipitate