Experiment 25 Qualitative Analysis II
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- Wilfrid Jordan McDaniel
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1 Experiment 25 Qualitative Analysis II GOAL: This week you develop strategies to use the reactions that you observed in lab last week to identify unknown solutions. You will also learn to use flowcharts to track your results. While it is important to learn the reactions, it is far more important to work on the logic required to solve these unknowns. Especially as the unknowns become more complicated, good logic and thorough record-keeping in flowcharts will be vital. INTRODUCTION: Last week you observed some reactions of seven cations, Na 1+, Mg 2+, Cr 3+, Ni 2+, Zn 2+, Ag 1+, and Pb 2+, and four anions, NO 3 1-, SO 4 2+, Cl 1-, and I 1-. You noted the formation and colors of precipitates and complex ions. These observations will allow you to separate and identify unknown mixtures of the ions. Whenever a precipitate forms, the mixture can be centrifuged and separated into the precipitate and solution portions. This week you will develop strategies for using last weeks tests to separate and identify unknown solutions. Prior to lab, you will be working on a computer to let you focus all of your attention on thinking about the samples rather than manipulating the solutions in the tests. In lab, you will work with real solutions. What tests do we have to choose from? Last week you saw: addition of 1 drop of OH 1-, addition of excess OH 1-, addition of NH 3, addition of Cl 1-, addition of I 1-, sodium flame test, and nitrate brown ring test. These tests can be done individually or combined. The order of tests can matter a great deal. Recall the stability sequences from last week For Ag + : Ag 2 O(s) < AgCl(s) < Ag(NH 3 ) 2 + (aq) < AgI(s) For Pb 2+ : PbCl 2 (s) < PbSO 4 (s) < PbI 2 (s) < Pb(OH) 2 (s) < Pb(OH) 4 2- (aq) in xs OH 1- For Zn 2+ : Zn(OH) 2 (s) < Zn(NH 3 ) 4 2+ (aq) < Zn(OH) 4 2- (aq) in xs OH 1- For Ni 2+ : Ni(OH) 2 (s) < Ni(NH 3 ) 4 2+ (aq) < Ni(OH) 2 (s) in xs OH 1- For Cr 3+ : Cr(OH) 3 (s) < Cr(OH) 4 1- (aq) in xs OH 1- Remember that you can proceed only to the right in each series. So, for example, if you start with Ag 1+ (aq) and add OH 1- (aq), you will get Ag 2 O(s). If you add Cl 1- (aq) to this, you can convert it to AgCl(s). On the other hand, if you add the Cl 1- first, adding OH 1- later cannot take you back to the left to Ag 2 O(s). Since the stability sequences are a little bit different for each cation, they can be used to effect some tricky separations. 1
2 Simple unknowns may be identified with a single test. More complex mixtures require multiple steps. You need a good understanding of the reactions and a good record of your tests and results to identify these unknowns. Flow charts are a useful way to organize this information. Let s say that you are given an unknown that contains only one of the cations from last week. The particular solution you get (Unknown #3) is colorless, so you write Unknown #3, only 1 cation, colorless Could be Na 1+ (aq), Mg 2+ (aq), Zn 2+ (aq), Ag 1+ (aq) or Pb 2+ (aq) You have already eliminated Ni 2+ and Cr 3+ based upon color, so there is no reason to include them in your flowchart. Now which test do you run? Several good choices are available; let s say you choose to add excess OH 1-. When you do this, you get a brown precipitate. How do you record this in a flowchart? Show the precipitate to the left, with a double drop line, and the remaining solution to the right, with a single drop line. You should record this as Unknown #3, only 1 cation, colorless Could be Na 1+ (aq), Mg 2+ (aq), Zn 2+ (aq), Ag 1+ (aq) or Pb 2+ (aq) XS OH 1- Brown ppt, Ag 2 O so unknown was Ag 1+ Colorless You ve identified your unknown in one step. Do you really need to record the color of the solution, or can you just write nothing under the single drop line? It is probably safer to write colorless. That way, when you come back to this later, your observations will be clear. Will just adding excess OH 1- always work so well? That depends on the unknown. Let s give you another clear, colorless unknown that contains only one of the seven cations (Unknown #4). This time when you add excess OH 1- you get no precipitate and a colorless supernatant solution. You would write Unknown #4, only 1 cation, colorless Could be Na 1+ (aq), Mg 2+ (aq), Zn 2+ (aq), Ag 1+ (aq) or Pb 2+ (aq) XS OH 1- No ppt colorless soln Remember that Ni 2+ and Cr 3+ are eliminated as possibilities off the top since your unknown is colorless. What does the lack of precipitate tell you? You must not have Ag 1+ because that would have given a brown precipitate, and you must not have Mg 2+ because that would have given a white precipitate. So your unknown must have been Na 1+, Zn 2+, or Pb 2+. Let s be careful how we write this, however, because we will have some complex ions after adding OH 1-. 2
3 Unknown #4, only 1 cation, colorless Could be Na 1+ (aq), Mg 2+ (aq), Zn 2+ (aq), Ag 1+ (aq) or Pb 2+ (aq) XS OH 1- No ppt colorless soln unknown Na 1+ or Zn(OH) or Pb(OH) 4 can t be Ag 1+ or Mg 2+ Why is it important to remember that we now have the complex ions? It will affect the next step we do to identify this unknown. We need to do another test and we can choose to test either some more of the original unknown solution, or the solution left after the addition of excess OH 1-. How about trying a sodium flame test now? That is a fine choice, but make sure that you test the original solution! The OH 1- solution we added in our first test is actually NaOH(aq). Once this has been added, later solutions will test positive for Na 1+ even if it wasn t in our original unknown. What about adding I 1- to see if we get that yellow PbI 2 precipitate? This is also a fine choice. Which solution should we test? Again, we need to test the original solution. Look at the stability sequence for lead. What happens if you add I 1- to Pb(OH) 4 2-? Nothing, because PbI 2 if left of Pb(OH) 4 2- in the stability sequence. OK, let s say that we take some more of our original sample, we do a sodium flame test and see no yellow color. We take some more of the original sample, add I 1-, and get no precipitate. What do we know? How do we record this? Just keep adding to the flowchart. Unknown #4, only 1 cation, colorless Could be Na 1+ (aq), Mg 2+ (aq), Zn 2+ (aq), Ag 1+ (aq) or Pb 2+ (aq) XS OH 1- flame test I 1- colorless No ppt colorless soln Not Na 1+ no ppt colorless unknown can t be Ag 1+ or Mg 2+ Not Pb 2+ Zn 2+ only possible We ruled out everything but Zn 2+, so by process of elimination, Unknown #4 must be Zn 2+. Do you always want to go back and do subsequent tests on the original solution? Definitely not, especially if the unknown could contain multiple ions. Let s illustrate this by giving you a more complicated unknown this time to help illustrate how and why. Your unknown #5 is a pale green solution known to contain three of the seven cations. What does the green color tell you? It probably contains Ni 2+, but we need to be careful since occasionally Cr 3+ can take on a green color (though usually a darker green). In fact, it s possible that both colored ions are present, so we can keep our hunch in mind as we choose tests, but still be open to several possibilities. We can t rule out any of the seven cations until we do some tests. Let s try adding NH 3 this time. When we do this, we get a violet solution and some precipitate that turns out to be white after we centrifuge and decant. 3
4 Unknown #5, 3 ions, green Likely Ni 2+, could include Cr 3+ (aq), Na 1+ (aq), Mg 2+ (aq), Zn 2+ (aq), Ag 1+ (aq) or Pb 2+ (aq) NH 3 white ppt violet soln. We need to think carefully about where each of our possible ions would end up and whether we have ruled any ions in or out. Ni 2+ gives a violet solution with NH 3, so we have confirmed its presence. Cr 3+ should have formed a green/grey precipitate, so we ve ruled that out. Na 1+ would stay in solution. Zn 2+ reacts to form Zn(NH 3 ) 4 2+ and Ag 1+ forms Ag(NH 3 ) Both are complex ions, so they will be in the solution if they are present. The white precipitate could be Mg(OH) 2 (s) and/or Pb(OH) 2 (s). Put all this information in your flowchart as Unknown #5, 3 ions, green Likely Ni 2+, could include Cr 3+ (aq), Na 1+ (aq), Mg 2+ (aq), Zn 2+ (aq), Ag 1+ (aq) or Pb 2+ (aq) NH 3 white ppt violet soln. could be Pb(OH) 2 or Mg(OH) 2 definitely contains Ni(NH 3 ) violet unknown definitely doesn t have Cr 3+ could contain Na 1+, Zn(NH 3 ) , Ag(NH 3 ) 2 With the precipitate separate from the violet solution, we can now test these separately since we already know something about what they may contain. How could we decide if the precipitate contains lead or magnesium or both? Would adding Cl 1- or I 1- work? Nope! Check the stability sequence for lead to see why. We could add excess OH 1-. If Pb(OH) 2 is present, it will dissolve to form Pb(OH) 4 2-, but Mg(OH) 2 (s) would remain unchanged. In lab, we add excess OH 1- and the precipitate dissolves except for the tiniest speck. We definitely had Pb 2+. Does this test mean we also had Mg 2+? Probably not, since we should expect about half of the precipitate to remain. For now, we ll rule out Mg 2+, but still record that lingering speck in case our later results are troublesome. Unknown #5, 3 ions, green Likely Ni 2+, could include Cr 3+ (aq), Na 1+ (aq), Mg 2+ (aq), Zn 2+ (aq), Ag 1+ (aq) or Pb 2+ (aq) NH 3 white ppt violet soln. could be Pb(OH) 2 or Mg(OH) 2 definitely contains Ni(NH 3 ) violet unknown definitely doesn t have Cr 3+ could contain Na 1+, Zn(NH 3 ) , Ag(NH 3 ) 2 XS OH 1- no ppt (tiny speck) colorless soln too little for Mg(OH) 2 2+ must be Pb(OH) 4 OK, we ve got Ni 2+ and Pb 2+ confirmed. We ve ruled out Cr 3+ and Mg 2+. How do we decide among the remaining three ions? Let s think through the options. We could do a sodium flame test. Should we test 4
5 the original solution or the violet one? Actually it doesn t matter. The NH 3 we added won t affect that test. What could we do to tell Zn(NH 3 ) 4 2+ from Ag(NH 3 ) 2 1+? How about adding excess OH 1-? Look carefully at the stability sequences. Nope, that won t help. Zn(NH 3 ) 4 2+ will react to form Zn(OH) 4 2- but both are clear and colorless and won t let us distinguish between zinc and silver. How about adding Cl 1-? That won t work either since AgCl is to the left of Ag(NH 3 ) 2 1+ in the stability sequence. Adding I 1-? Yes! If Ag(NH 3 ) 2 1+ is present, it will react to form AgI. Should we go back and add I 1- to the original solution or the violet one? In either case AgI will precipitate if Ag 1+ was in the unknown. But wait, we know that Pb 2+ was also in the original unknown and it will precipitate with I 1-. We want to use the violet solution to avoid this complication. In lab when we add I 1- to the violet solution, we get a light yellow precipitate, confirming Ag 1+. Unknown #5, 3 ions, green Likely Ni 2+, could include Cr 3+ (aq), Na 1+ (aq), Mg 2+ (aq), Zn 2+ (aq), Ag 1+ (aq) or Pb 2+ (aq) NH 3 white ppt violet soln. could be Pb(OH) 2 or Mg(OH) 2 definitely contains Ni(NH 3 ) violet unknown definitely doesn t have Cr 3+ could contain Na 1+, Zn(NH 3 ) , Ag(NH 3 ) 2 XS OH 1- I 1- no ppt (tiny speck) colorless soln cream ppt, AgI violet soln too little for Mg(OH) 2 must be Pb(OH) 4 Ni(NH 3 ) 4 So our Unknown #5 contained Ni 2+, Pb 2+, and Ag 1+. Did we actually rule out Zn 2+ and Na 1+? Yes, but only because we knew our unknown had three ions present. If any number of ions could be present then we would have needed to do even more tests! Could we have started work with this unknown in other ways? Sure. Some people might prefer to start with excess OH 1-, others like to start by adding I 1-. Some routes give quicker and cleaner identifications than others, but that can vary with the unknown. Don t be afraid to try different combinations. Don t be afraid to start over if your first attempt leads you to a messy, unhelpful dead end. The unknowns we have worked through in this Introduction are meant to give you a sense of the logic and decision-making processes that you should use to identify your own unknowns. Flowcharts are an important way of showing your logic and tracking your results. None of the unknowns we have worked required us to identify the anions Cl 1-, I 1-, SO 4 2-, and NO When working these solutions, you use the brown ring test and reactions with Ag 1+ and Pb 2+. When you need to identify both the cation and the anion in a sample, you can include the tests all on one large flowchart, or do two separate flowcharts. General advice for solving unknowns: 1. Take advantage of what you know about the total number of ions present. 2. Pay attention to colors of solutions and precipitates to rule in or rule out ions. 3. Start with a test that will let you learn something specific about the sample. 4. When a precipitate forms, centrifuge and separate it from the supernatant solution. 5. Use a flow chart to track what you have done 5
6 6. Label your samples so that you know which is which. For example, the colorless solution left after adding I 1- might be labeled I 1- soln. or you might call it soln B and then write that identifying label into your flowchart record. 7. Never use all of your original sample. Use a small amount for your first test and save the rest in case you need to start over. 8. Don t try to lay out one master plan to apply to all unknowns. You must think and re-evaluate with each step. PRE-LAB ASSIGNMENT: Complete the Pre-Lab section below to turn in at the beginning of lab. The pre-lab is designed to give you practice using flowcharts to think about the logic involved in determining the identities of the unknown ions in solution. The software for the pre-lab experiment is called WinQual. You can either download it to your own PC or use it on the RC computer network. WinQual will allow you to see reactions using the same chemicals you had in lab last week and to identify unknown solutions with these reactions. To download WinQual to your PC: 1. Download WinQual from 2. Install WinQual in default directory: C:\Program Files\WinQual 3. Run the WinQual shortcut on the desktop 4. Choose Enter Registration Code Now: Name: Roanoke College Reg. Code: F2 To use WinQual in a computer lab, log on to the network and then choose the Start, RC lab software, Chemistry, then WinQual. Take a few moments to learn about the software. You will save time and frustration in the long run. See the appendix at the end of this handout about using WinQual. Choose the top pop-up Experiment menu. Note that here you can explore reactions or solve several types of unknowns. Our main use of the software will be to give you practice identifying unknowns. From the Experiment menu, choose the type of unknown that you need to do. To get acquainted with the program, choose the One Positive Ion option. When you choose a One Positive Ion experiment, you will see a picture of a solid: your unknown cation with a nitrate anion. You will also see the result of putting this solid into water. To save this treated sample, click on one of the seven Saved Samples slots in the upper right. Note that you could click on the Trash Can to discard the treated sample. Make one of the Saved Samples your Active Sample by clicking on it. [If you have trouble working the program or get unexpected results, it is often because you have forgotten to click on the sample you want to be your active sample.] You can now do a Na 1+ flame test, do a NO 3 1- test, or add any of the chemicals used in lab to your sample. Only complete compounds can be added, so for example, if you want to add XS OH 1- to the active sample, you must click on Na 1+, XSOH 1-, and then ADD. The User Notes field on the screen provides much helpful information on using the program. 6
7 Right click on any saved sample to review its history. When you think you know the identity of the cation in the unknown, go to the Experiment dropdown menu and choose Answer. Note that all of the positive ion unknowns have nitrate as the anion. When you select the answers for these positive ion unknowns, also select nitrate ion. Be sure that you print your results to include in your report. PRE-LAB ASSIGNMENT In the WinQual software, do One Positive Ion unknowns until you have gotten three of these correct. Note that the anion is always nitrate in these unknowns. Be sure to print your results for inclusion in your report. Use your summary table from last week, the three flowcharts you wrote for Question 2 in Experiment 24, the general advice for solving unknowns on Pages 5and 6 of this handout, and the information elsewhere in the Introduction to guide your test choices. As you work on each unknown, keep track of your tests and logic using a flowchart. After printing out your results for an unknown, handwrite your flowchart directly onto the printout. These flowcharts should be fairly simple, something like those shown in the Introduction for Unknowns 3 and 4. In the WinQual software, do Two Positive Ions unknowns until you have gotten two of these correct. Note that the anion is always nitrate in these unknowns. Be sure to print your results for inclusion in your report. As you work on each of the unknowns, record what you do and see in flowchart format. After you get your computer printout for each unknown, copy a clean version of your flowchart directly onto the printout. What did you learn about identifying unknowns from solving these One and Two Positive Ion unknowns? Address this in several well-organized paragraphs. Include a discussion of the merits of starting your identification attempt with several different tests, e.g. starting by adding excess OH 1- vs. adding NH 3, or I 1-, etc. Support your statements using your results from doing the unknowns and the flowcharts you wrote for Question 2 in Experiment 24. Which ions seem easiest or most difficult to identify? Which is easier, colored or colorless unknowns? Why? Your Pre-Lab results are due at the beginning of your lab period. IN-LAB PROCEDURE: In lab, you will be given a set of 7 unknowns that you must identify using the tests available in the experiment. These will be done with real solutions, not using WinQual. You will have TWO unknown solutions that contain ONE unidentified cation. Identify these cations. (Each solution also contains NO 3 -, which will not interfere with your tests.) You will have TWO unknown solutions that contains ONE unidentified anion (as well as Na + ). Identify these anions. You will have TWO unknown solutions that will contain TWO unidentified cations. Identify these cations. 7
8 The final unknown will be a solid that contains TWO unidentified cations and TWO unidentified anions. Identify these four ions. As noted in the General Procedures, you start a solid unknown by adding a small amount of the solid to some distilled water. Adding 0.1 g of solid to 5 milliliters of water is about right. You may get a precipitate at this point if two of the ions present react to form one. Consult your Reaction table to consider what that precipitate may be. Do not attempt to keep adding water to get it to dissolve. Be sure that you a. Record all of the unknown numbers! b. Think before you work. Decide which tests will be helpful and run those. Do NOT run every test on every unknown. This shows poor understanding of the principles. c. Use the general procedures listed on Page 9. d. Use your unknown carefully since it is all you have. e. Don t contaminate your unknown. f. Carefully record everything you do and observe. g. Label test tubes with a marker so that you don t mix them up! h. Record the conclusions that you can draw from each test, both about what might and what cannot be present based on your observations. i. Collect all used solutions and leftover unknowns in your waste container. After you have identified all of your unknowns, discard your wastes in the designated container in the hood. In all cases, the logic you use as described in your flowcharts is FAR more important than getting an unknown correctly identified. It will count heavily in your report grade. Do not just guess at unknowns. See your instructor if you are having trouble with the logic. RESULTS: For each unknown you analyzed this week, the unknown number a clean copy of the flow chart showing the logic you used to reach your conclusion, colors and formulas for all precipitates and solutions your final conclusion about the content of that sample The results should be recorded neatly in your lab notebook. You will turn in your results before leaving lab this week or by the date noted by your lab instructor. There will be no additional report to turn in following lab. 8
9 Appendix 1: General Procedures for Exploring Reactions in Lab Your unknown solutions will be supplied in test tubes. If your unknown is a liquid, begin any of the tests below by putting about 10 drops of the solution to be tested in a CLEAN test tube. (After cleaning your test tubes with soap and brush, rinse with distilled water and allow the excess water to drain.) Never do tests directly in the original test tube of unknown. If your unknown is a solid, add a small amount of solid to several milliliters of water (about 0.1 grams in 5 ml of water) to prepare a solution that you can then test. Record colors of precipitates and solutions throughout. Test for reaction with OH - Add just one drop of OH - solution to your test solution. Observe for the formation of a precipitate. Tests for reaction with excess OH - or NH 3 Add one drop of OH - or NH 3 solution and observe. Now continue adding drops until you have 10 drops added. Observe as you go to determine if a precipitate initially formed, and if so, whether it redissolves in excess. Test for reaction with other ions Add 5-15 drops, observing as you go. Sodium flame test Dip a clean cotton swab into the solution to be tested and then heat the tip of the swab in a Bunsen burner flame. A very intense yellow flame is observed when Na + is present. Douse the swab in water to extinguish the flame and dispose of it in the container provided. Nitrate brown ring test Put 20 drops of the solution to be tested into a test tube, and then, carefully and slowly, add 20 drops of concentrated H 2 SO 4. (The test tube will get hot, and may splatter if the acid is added too quickly.) If necessary, cool this mixture by allowing cold tap water to run over the outside of the test tube. In a second test tube, dissolve about 0.1 g FeSO 4. 7H 2 O in 1 ml of water. Now, hold the test tube containing the H 2 SO 4 solution at a 45 o angle while you allow 5 drops of the FeSO 4 solution to run slowly down the inside of the tube. Do NOT mix. The aqueous FeSO 4 should form a layer above the acid. If nitrate ion is present, a smoky brown ring will form at the solution interface. This ring may take several minutes to form, and will disappear eventually. Look at the interface between the two layers from several angles. If you were doing this test on a real unknown sample, and there were a chance that the sample also contained I 1-, this would interfere with the test. To remove I -, add several drops of saturated Ag 2 SO 4 solution until no more AgI precipitates. Centrifuging The centrifuge allows you to separate a solid precipitate from its supernatant liquid. Choose two test tubes that are as similar as possible. You precipitate and its solution will be in one test tube. Add water to the second test tube to approximate the amount in the first one. Place your test tubes directly across from each other in the centrifuge. Close the lid. Centrifuge for 1-2 minutes. Allow the centrifuge to come to a complete stop before removing the tubes. More tubes can be centrifuged at one time, but you must keep the centrifuge balanced. If you do more than one sample at a time, use a marker to label them. 9
10 Appendix 2: General Procedures for Exploring Reactions with WinQual Choose the top pop-up Experiment menu. Note that here you can explore reactions or solve several types of unknowns. We will use this program to Explore reactions. From the Experiment menu, choose Explore Reactions. A picture of a test tube with only water will appear. To begin, click one cation, such as Na +, and one anion, such as OH -. The name of this compound should appear in the Compound to be added box. Click on Add to add this compound to the test tube. You should now have another picture of a test tube in the Treated sample window. If you right click on this window, a box will pop up detailing what species, liquids and solids, are present in this solution. In our example, Na + and OH - should be listed under liquid composition. We will use this as our base solution to test the reaction of OH - with other cations and the reaction of Na + with other cations. Click in box 2 in the Saved Samples window. You can right click on this picture as well to see what is present in the solution. At this point, box 1 should have a solution with only water and box 2 should have a solution with Na + and OH -. We now want to test what happens when we add other compounds to this solution of NaOH(aq). We must make this the active solution. To do so, click in box 2. The Active Sample (previously just water) will be replaced with our NaOH(aq) solution. You can always check the composition of a given solution by right clicking on the picture. We will start by testing OH - with other cations. To the active sample add Mg(NO 3 ) 2. Record your observations and the formula of any solid that forms in the appropriate square of your table. When you are finished, discard your sample by clicking on the trashcan. Repeat this test with Ni(NO 3 ) 2, Cr(NO 3 ) 3, Zn(NO 3 ) 2, AgNO 3, and Pb(NO 3 ) 2. You must discard your sample between each test. If nothing is observed (the result is a clear, colorless solution and all ions are in the liquid composition column of the sample composition box), write NR for no reaction in the appropriate box of your table. We want to fill in the rest of the table using a similar procedure. Next, make an active sample of NaOH using excess OH - (select the XS OH - button for the anion). Test the reaction of this salt solution with the nitrate salt solutions (Mg(NO 3 ) 2, Ni(NO 3 ) 2, Cr(NO 3 ) 3, Zn(NO 3 ) 2, AgNO 3, and Pb(NO 3 ) 2 ). Do the same starting with NaCl, NaI, and NaSO 4. Also fill in the column for reactions with NH 3. Finally, perform do a Na + flame test and a NO 3 - brown ring test on a sample of NaNO 3. Prepare this solution and make it the active sample. To perform the Na + test, click on Na +? Record the result. To test for NO 3 -, click on NO 3 -? Record the result. 10
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