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Instructors Guide
Sodium carbonate, Na2CO3, 0.2 M, 100 mL* Sodium hydroxide, 6 M, 100 mL* Sodium sulfate, Na2SO4, 0.2 M, 100 mL* Sodium nitrate, NaNO3, 0.2 M, 100 mL* Barium chloride, BaCl2, 0.1 M, 100 mL* Barium hydroxide, Ba(OH)2, 5 g* Potassium thiocynate, KSCN, 0.1 M, 100 mL* Potassium ferrocyanide, K4Fe(CN)6, 0.1 M, 140 mL* Aluminum granules, Al, 50 g* Beral-type pipets, 120*
Unknown No. 1 2 3 4 5 6 7 8 9 10 11
Ag+ X X X X X X X
Cu2+ X X X X X X X
Zn2+ X X X
Fe3+ X X X X X
X X X X X X
Solution of Four Anions Prepare 100 mL of a 0.05 M solution of all the anions to be tested by adding 25 mL of each of the following solutions to a clean 250-mL beaker. 0.2 M sodium chloride, NaCl 0.2 M sodium carbonate, Na2CO3 0.2 M sodium nitrate, NaNO3 0.2 M sodium sulfate, Na2SO4 Mix the solution, dispense in 12 clean 13 X 100 mm test tubes, and stopper the test tubes. Unknown Anion Solutions Prepare the unknown anion solutions for the students to analyze from the four 0.2 M stock solutions of anions. Any combination of these four anions may be prepared. Using a graduated Beral-type pipet, add 2 mL of each ion selected to a 13 X 100 mm test tube. Add distilled water to give a total volume of 8 mL. Stopper the test tube. A matrix of combinations, similar to the cation unknowns, can be generated for the anions. Unknown No. 1 2 3 4 5 6 7 8 9 10 11 ClX X X X X X X CO32X X X X X X X X X X X X X NO3X X X SO42X X X X X
Barium Hydroxide Solution Prepare 100 mL of a saturated barium hydroxide solution by dissolving 5.0 g of barium hydroxide in 100 mL of deionized or distilled water. Transfer the 100 mL of solution to a stoppered or capped bottle and label, Ba(OH) 2 (saturated.)
Safety Precautions
The 0.05 M solutions are very dilute and hazards are greatly reduced. However, dilute silver salts will still stain the skin. Silver nitrate solution is mildly toxic and irritating to body tissue. It also stains skin and clothing. Cupric nitrate solution
is mildly toxic. Zinc nitrate solution is mildly toxic and is irritating to body tissue. Ferric nitrate solution is irritating to body tissue. Barium hydroxide and barium chloride solutions are toxic by ingestion. Potassium thyocyanate solution is slightly toxic by ingestion. Avoid contact with concentrated acids since toxic hydrogen cyanide gas may be liberated. Concentrated ammonia (ammonium hydroxide) solution and hydrochloric acid solutions are toxic by inhalation, ingestion, and are corrosive to all body tissues. Sulfuric acid solution and sodium hydroxide solution are severely corrosive to eyes, skin, and other tissue. Nitric acid solution is severely corrosive, a strong oxidant, and toxic by ingestion and inhalation. Acetic acid solution is a corrosive liquid. Wear chemical splash goggles, chemical-resistant gloves, and a chemical-resistant apron. Have students wash hands thoroughly with soap and water before leaving the laboratory. Please consult current Material Safety Data Sheets for additional safety information.
Dispoal
Provide a separate container for cations and for anions into which the students may empty their waste solutions. Filter the solids from the liquid. Each liquid may be disposed of according to Flinn Suggested Disposal Method #26b. The cation solids may be disposed of according to Flinn Suggestion Disposal Method #26a. For barium solutions and solids from anion steps 2 and 3, place in a separate waste container. This waste may be disposed of according to Flinn Suggested Disposal Method #27h. Please consult your current Flinn Scientific Catalog/Reference Manual for proper disposal procedures.
AP Chemistry Standards
This lab fulfills the requirements for the College Board recommended AP Experiment #14: Separation and Qualitative Analysis of Cations and Anions.
Lab Hints
Four to five 50-minute lab periods are needed to analyze the known and unknown solutions for both cations and anions. One hour of prep time will be needed to prepare the known and unknown solutions. Students should have a set of reagents available to them in small (15-39 mL) dropping bottles. To simplify preparation of the sets of dropper bottles, have each student group clean and label a set of dropper bottles for the reagents. Dispense the reagents from the stock solutions. Use great caution in dispensing the strong, concentrated acids and bases from the stock solutions. Wear chemical splash goggles and chemical-resistant gloves. If a complete set of dropper bottles is not available for each student group, a set may be shared between groups. Check centrifuges to make sure that they are balanced and spin quietly while empty. It may be necessary to weigh the centrifuge tubes and place those with the closest weights opposite on another. The test tubes should not drop so far into the centrifuge tubes that they cannot be easily removed. If necessary, place a small cork in the bottom of each centrifuge tube so that the test tubes extend just a little above the centrifuge tubes. It is not necessary to stopper the test tube when centrifuging the solution. A test tube must be counterbalanced by placing a similar tube with an equal volume of water opposite it. Caution students not to stop the centrifuge while it is spinning. Water baths can be shared. Enough solution is provided for each lab group to perform multiple tests. Encourage students to run tests until they get clear and reproducible results.
Teaching Tip
The solution that is analyzed has a small total solution volume. Great care is needed in adding reagents, mixing solutions, precipitating the substances, separating the liquids from solids, washing precipitates, adjusting pH, and following the laboratory procedures. It is essential to maintain a good record of the results of each step because the procedure will be carried out over a number of laboratory periods. Students should be able to demonstrate an understanding of the chemistry involved in the steps as well as the procedures used.
Cu2+ present
Fe3+ present
CO32- present
SO42- present
3. When Fe3+ and Cu2+ react with NH3 solution they form two different types of products. One is a precipitate and one a complex ion in solution. Write equations for these two reactions. Fe3+(aq) + 3NH3(aq) + 3H2O(l) Fe(OH)3(s) + 3NH4+(aq) Cu2+(aq) + 4NH3(aq) Cu(NH3)42+(aq) 4. The confirmatory test for chloride ion with silver ion is the same chemical reaction used to confirm silver in the cation analysis scheme. Explain what the reaction is and how the initial precipitate is dissolved and reprecipitated. Use equations in your explanation. Precipitation: Ag+(aq) + Cl-(aq) AgCl(s) Dissolution: AgCl(aq) + 2NH3(aq) Ag(NH3)2+(aq) + Cl-(aq) Reprecipitation: Ag(NH3)2+(aq) + Cl-(aq) + 2H+(aq) AgCl(s) + 2NH4+(aq) 5. Write separate oxidation and reduction half-reactions for the procedure used in the test for nitrate ions. NO3-(aq) + 6H2O(l) + 8e- NH3(aq) + Al(OH)4-(aq) Al(s) + 4OH-(aq) Al(OH)4-(aw + 8ereduction oxidation
NO3-(aq) + Al(s) + 5OH-(aq) + 6H2O(l) NH3(aq) + Al(OH)4-(aq) overall 6. In the nitrate test, why must care be taken to keep the moist litmus from coming in contact with the cotton or the solution? The solution being tested is basic. If the litmus comes in contact with the solution or cotton moist from the solution, it will turn blue from the solution contact, not from the evolving ammonia. 7. In step 4, Ba2+ is added to the solution containing all four of the anions and precipitates BaSO 4, but not BaCO3. However, in step 3, the precipitation of BaCO3, is the confirmatory test for carbonate ion. Why doesnt BaCO 3 precipitate in step 4 but does in step 3? BaSO4 will precipitate in acidic solution, but in acidic solution BaCo3 will decompose to form CO2 gas, H2O, and Ba2+(aq).