Separation and Identification of Metal Ions
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1 Vivek Kumar, Ph.D. OBJECTIVES: In this experiment, you will analyze an aqueous solution for the presence of Ag +, Pb 2+ and Hg2 2+ ions LEARNING GOALS 1. To understand and apply chemistry of metal ions especially precipitation reactions. 2. To learn experimental techniques such as selective precipitation and centrifugation. INTRODUCTION Metals such as iron, zinc, and copper are useful in small amounts, most other metals such as mercury and lead are considered potentially dangerous for living beings. Various chemical techniques are available for identification and isolation of these metals. In this experiment you will test an aqueous solution for the presence of Ag +, Pb 2+ and Hg2 2+ ions. The tests are based on their precipitation reactions you learnt in lecture. Separation of Ag +, Pb 2+ and Hg2 2+ ions The chlorides of these three ions are insoluble in water. When a soluble compound or a solution containing chloride ions is added to the sample, they are selectively precipitated. The solid formed is white (dirty white when mixture) in color. 1. Ag + (aq)+ Cl - (aq) AgCl (s, white) 2. Pb 2+ (aq) + Cl - (aq) PbCl 2 (s, white) 3. Hg 2 2+ (aq) + Cl - (aq) Hg 2Cl 2 (s, white) Separation and confirmation of Pb 2+ PbCl2 is soluble in hot water, whereas other two metal chlorides are not. Thus, when a small amount of water is added to the mixture containing three insoluble metal chlorides and heated, PbCl2 dissolves back in water. This helps in selectively removing lead from the mixture. 4. PbCl 2 (s) PbCl 2 (aq) Cold Hot Lead chromate is an insoluble yellow solid. Formation of a yellow precipitate on addition of potassium chromate confirms presence of Pb 2+ ions. CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 1
2 5. PbCl 2 (aq) + K 2CrO 4 (aq) 2 KCl (aq) + PbCrO 4 (s) Separation and confirmation of Ag + Both AgCl and Hg2Cl2 react with ammonia, however silver forms a soluble compound, whereas mercury forms an insoluble mixture. This is used to separate the two ions. When solution is made acidic silver chloride is precipitated back. 6. AgCl(s) + 2 NH 3 Ag(NH 3) 2Cl (aq) 7. Ag(NH 3) 2Cl (aq) + 2 HNO 3 (aq) AgCl (s, white) + 2 NH 4NO 3 (aq) Separation and confirmation of Hg2 2+ Elemental mercury and a mercury (II) compounds are formed on reaction with ammonia. The reaction is a redox reaction, not among the types of reactions you learnt in the lecture. The mixture is an insoluble black solid and confirms the presence of mercury (I) ions. 8. Hg 2Cl 2(s) + 2 NH 3(aq) Hg(s) + HgNH 2Cl(s) + NH 4Cl(aq) Black MATERIALS Known solutions, unknown solution, 6 M HCl, 0.1 M K2CrO4, 6 M acetic acid, 6 M NH3, 6 M HNO3, deionized water, 400 ml beaker, 5 test tubes (Note: You will use the unknown test tube as your unknown test tube # 1), test tube rack, 2 test tube wire holders, stirring rod, watch glass, blue litmus paper, red litmus paper, and centrifuge. CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 2
3 PROCEDURE Safety: Wear gloves and safety goggles throughout. STEP PROCEDURE ILLUSTRATION REACTION 1 Place three clean test tubes in a test tube rack and label as 1, 2, and To T# 1, add 40 drops of known solution To T # 1, add 10 drops of 6 M HCl. On addition, you will observe liquid turning cloudy white Add water to another test tube to about the same height as in T#1. This will be used for balancing T#1 during centrifugation Place T#1 and test tube with about equal amount of water into two diametrically opposite holes in the centrifuge. Centrifuge for 2 minutes. 2 minutes CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 3
4 6. T#1 has a white solid separated from liquid. Decant liquid to a waste beaker. Wast SEPARATION OF Pb Add 6 ml deionized water to T# 1 and heat in boiling water bath for about 5 min. Use two test tube wire holders to hold the test tube in water bath Centrifuge T#1 by balancing with another test tube having about equal amount of water for about 30 sec. 9. Quickly decant the liquid in T#1 to T#2 and save T# seconds 2 CONFIRMATION FOR Pb 2+ CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 4
5 10. To T#2 add 1 drops of 6 M acetic acid and 3 drops of 0.1 M K2CrO4.. A yellow precipitate (cloudy yellow) confirms Pb Add 10 drops of 6 M NH3 solution and 1 ml deionized water to T#1. 2 drops 6 drops SEPARATION OF Ag+ and Hg2 2+ 6, Centrifuge T#1 with another test tube with about equal amount of water for 2 min. 40 drops 2 min CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 5
6 13. A black residue in T#1 confirms mercury. CONFIRMATION OF Hg CONFIRMATION OF Ag Decant liquid in T#1 to T# To the liquid in T#3 add 6M HNO3 drop wise until solution turns acidic (blue litmus red). 7 NOTE: If you add too much HNO3 you may not be able to see the positive test for Ag Formation of a white precipitate confirms Ag Take your unknown sample and record unknown number. Use the test tube containing unknown sample as unknown test tube #1. Repeat steps 1-16 for unknown. Note: Your instructor may ask you to test unknown and known mixtures simultaneously. In that case, you will not need a blank test tube for balancing during centrifugation. The unknown and known test tubes can balance each other. CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 6
7 Cleanups: 1. All waste including the waste collected in waste beaker must go to the designated labeled waste container kept in hood. Mercury waste (T#1 in end) goes in a separate waste container. 2. Wash all glassware and return them to their respective places. CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 7
8 Known or Unknown (40 Drops) Add 68 ml of deionized water to T#1 and heat in hot water for 5 min with stirring. Centrifuge for 15 sec. Quickly decant liquid to #2. Add 1 drop of 6 M acetic acid and 3 drops of 0.1 M K 2CrO 4 to T#2 Add 10 drops of 6 M NH 3 and 1 ml deionized water to T#1. WEAR GLOVES AND SAFETY GOGGLES THROUGHOUT CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 8
9 NAME: DATE: OBSERVATION SHEET Unknown Sample Number: Metal Ion Ag + Present (Yes/No) Evidence Balanced Chemical Equation* Pb 2+ Hg2 2+ * Write balanced chemical equation for the metal ions your unknown sample tested positive for. CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 9
10 POST LABORATORY EXERCISE 1. Can NaCl solution be used in the place of HCl in step # 3? Explain. 2. Write a balanced chemical equation for the reaction between: (i) Aqueous solutions of AgNO 3 and NaCl. (ii) Aqueous solutions of Pb(NO 3) 2 and NaCl. 3. What would happen if you centrifuged the test tube containing lead and mercury solids with hot water too long and let the mixture cool? 4. How does ammonia help in separation of silver and mercury ions? Explain with balanced chemical equations. CHEM 100, Lab Manual, Suffolk County Community College, Michael J. Grant Campus Page 10
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