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Learning Goal: To identify positive and negative ions. Introduction: Detergents may contain phosphate (PO43-) ions which pollute waterways. Phosphate may be easily tested for because the end result of the test produces a yellow precipitate. If no yellow precipitate forms, the test is negative and the sample does not contain phosphate ions. All ions, not just phosphate, have tests specific to them. We will test for eight ions in this experiment. The tests usually involve the formation of a color or precipitate. First, the test is preformed on a sample that is known to contain the specific ion to observe a positive test. Next, the test is preformed on an unknown sample to determine which tests give the same results as obtained with the knowns. The cations that we are testing for in this experiment are potassium (K+); ammonium (NH4+); calcium (Ca2+); and ferrous (Fe2+). The anions are chloride (Cl-); sulfate (SO42-); phosphate (PO43-); and carbonate (CO32-). Your unknown will contain one cation and one anion which you will identify. CAUTION: All chemicals should be considered hazardous and washed off immediately if spilled on the skin or clothing. One should be especially cautious of the NaOH used in part 2, as well as, the HNO3 and HCl. Procedure: Perform the specific tests for the eight ions using solutions which contain these ions and record the results next to the test procedure. Next, obtain two unknown samples and repeat the tests using solutions that you will make by dissolving some of the unknown in distilled water. Use this unknown solution as a replacement for the ion for which you are testing.
Tests for Ions
1. Potassium Ion (K+) and Calcium Ion (Ca2+): These ions can be detected using a flame test. When K+ compounds are heated in a flame, a lavender flame is obtained. When Ca2+ compounds are heated in a flame, a deep red flame is obtained. Your test solutions for this test are KCl(aq) and CaCl2(aq), in spray bottles. To see what positive results for K+ and Ca2+ look like simply spray each solution, one at a time, directly into the flame. Do not spray too forcefully or the flame may go out. Record your observations on the data sheet.
To test your unknown sample, first clean a spatula by dipping it into a 6.0 M HCl solution and heating it in the flame. Then scoop a small amount of your unknown sample onto the spatula tip, insert it into the flame, and observe.
2. Ammonium Ion (NH4+): The presence of ammonium ions in solution is detected by the release of ammonia (NH3) gas upon adding sodium hydroxide (NaOH) solution. This is illustrated by: NH4+ + NaOH NH3 + H2O + Na+
For a positive test, put two drops of 0.1 M ammonium chloride (NH4Cl) in a well plate. Add two drops of 3.0 M sodium hydroxide. Shortly there after, place a damp piece of pH paper over the mouth of the well. The center section of the paper should turn green or blue. CAUTION – wash any spilled NaOH off of skin and clothes immediately. 3. Calcium Ion (Ca2+): Calcium ions react with oxalate ions (C2O42-) to form a white precipitate of calcium oxalate as shown by: Ca2+ + C2O42CaC2O4
A positive test for Ca2+ is obtained by placing one drop of 0.1 M CaCl2 in a well and adding one drop of 0.1 M ammonium oxalate. Mix. A white precipitate forms. 4. Ferrous Ion (Fe2+): Ferrous ions form a dark blue to green solution and blue precipitate with potassium ferricyanide, K3Fe(CN)6 as shown by: 3Fe2+ + 2Fe(CN)63Fe3[Fe(CN)6]2
Place one drop of 0.1 M ferrous sulfate (FeSO4) in a well, add one drop of 1.0 M HCl. Next add one drop of 0.2 M potassium ferricyanide. Mix and observe. 5. Chloride Ion (Cl-): Chloride ions form a white precipitate (AgCl) with silver ions as shown by: Cl- + Ag+ AgCl
Place one drop of 0.1 M silver nitrate (AgNO3) and one drop 3.0 M HNO3 in a well. Next, add one drop of 0.1 M sodium chloride solution. Mix and observe. CAUTION – wash any spilled HNO3 and silver nitrate off with water, immediately.
6. Phosphate Ion (PO43-): Phosphate ions form a yellow precipitate with ammonium molybdate in acid solution as shown by: 3NH4+ + 24H+ + PO43- + 12MoO42(NH4)3PO4.12MoO3 + 12H2O
Add one drop of 0.1 M sodium phosphate solution and three drops of 6.0 M nitric acid (HNO3) to a well. Mix and add two drops of 0.5 M ammonium molybdate, (NH4)2MoO4. Record the results. CAUTION – Quickly neutralize and wash off any spilled HNO3. 7. Sulfate Ion (SO42-): Sulfate ions form a white precipitate of barium sulfate (BaSO4) with barium ions as shown by: Ba2+ + SO42BaSO4
To carry out the test, add two drops of 0.2 M barium chloride (BaCl2) and one drop of 3.0 M HNO3 to one drop of 0.1 M sodium sulfate (Na2SO4) solution. Mix. A white precipitate indicates a positive test. CAUTION – Neutralize and wash any spilled HNO3 quickly. 8. Carbonate Ion (CO32-): CO2 gas is produced when acid is added to a solution of carbonate ions as shown by: CO32- + 2H+ H2O + CO2
Add two drops of 3.0 M HCl to three drops of 0.1 M Na2CO3 (carbonate solution). Look for gas evolution. You should see bubbles in the liquid, and with higher concentrations of CO32-, the bubbles will rise out of the liquid. CAUTION – Wash any spilled HCl immediately from the skin or clothing.
Identification of an Unknown Ionic Compound
After you have performed the above eight tests using solutions containing the ions specified, obtain your unknown samples. Dissolve about 0.1 g of compound in about 2 mL of deionized water. Record whether the unknown is SOLUBLE or INSOLUBLE in water. Repeat the eight identification tests using the SOLID form of the unknown for the flame test and the SOLUTION form of the unknown for all the other tests. When using the solution form, use two drops of your unknown solution in place of the solutions with the knows in the Tests for Ions Section above. If the known and unknown test results are the same, the unknown sample contains the ion that the test is designed to detect. Your unknown has only one of the four positive ions being tested and only one of the four negative ions being tested. Report the ions found and write the formula for your unknown compound. Do all eight tests with your unknown, even if you think you know the identity of the ions in your unknown before all the tests have been run.
PRE LAB QUESTION 1. What is another name for ferrous ion and ferrous sulfate, referred to in the Tests For Ions section, identification for Ferrous Ion (Fe2+)?
2. List the 16 possible ionic compounds that could form from the 8 ions that you will be testing for. Categorize these compounds as water soluble or water insoluble.
K+ NH4+ Ca2+ Fe2+ ClPO43SO42CO32-
Unknown # Description of a positive result
Is the result positive or negative?
Unknown # Description of a Is the result positive positive result or negative?
Lab Questions: 1. Is your unknown SOLUBLE in water (dissolved clearly) or INSOLUBLE in water (undissolved solid or murky appearance)?
2. Which ions can you eliminate as possibilities for your unknown based JUST on its solubility characteristics in water?
3. FORMULA of your unknown compound: _______________________________ 4. NAME of your unknown compound: ____________________________________ 5. If your identification is not correct, explain the possible error.