Simple Qualitative Analysis

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1 Name Class Date Skills Practice Lab Simple Qualitative Analysis MICROSCALE If an unknown sample is one of a limited number of possible compounds, a simple test often can determine its identity. For example, a flame test can distinguish between KCl and NaNO 3. A drop of potassium hexacyanoferrate(iii) solution can tell you whether FeCl 2 or FeCl 3 is present. There are hundreds of simple qualitative tests such as these to distinguish among a few possibilities. Qualitative tests are important to the forensic chemist, one who is interested in solving crimes, but they have been largely replaced by instrumental analysis, which is fast and requires a very small sample. For example, instrumental analysis can detect as little as g of 9-tetrahydrocannabinol (one of the active ingredients in marijuana) in 1 ml of blood plasma. Unfortunately, this kind of instrumentation (a gas chromatograph connected to a mass spectrograph) is expensive, so simple chemical tests are still often useful. A drop of hydrochloric acid is enough to allow the police department s forensic chemist to distinguish between a bag of cocaine and a bag of baking soda. In this experiment you will identify the contents of a number of vials. The substance in each vial is one of the two compounds listed on the label. To decide which compound is present, you will make a few simple tests. OBJECTIVES Observe qualitative tests using known ionic compounds. Decide which qualitative test to use in identifying an unknown ionic compound. Describe the chemistry of common ionic compounds. MATERIALS beaker, 50 ml Bunsen burner and related equipment cobalt glass plates (2) filter paper, cut into short strips flame-test wire gloves HCl, 1.0 M KMnO 4, 0.1 M lab apron Na 2 CO 3 NaOH, 1.0 M Na 2 SO 3 NH 4 Cl red litmus paper safety goggles sparker spot plate or small test tubes (3) Holt Chemistry 31 Chemical Equations and Reactions

2 Name Class Date Always wear safety goggles and a lab apron to protect your eyes and clothing. If you get a chemical in your eyes, immediately flush the chemical out at the eyewash station while calling to your teacher. Know the location of the emergency lab shower and eyewash station and the procedures for using them. Do not touch any chemicals. If you get a chemical on your skin or clothing, wash the chemical off at the sink while calling to your teacher. Make sure you carefully read the labels and follow the precautions on all containers of chemicals that you use. If there are no precautions stated on the label, ask your teacher what precautions to follow. Do not taste any chemicals or items used in the laboratory. Never return leftovers to their original container take only small amounts to avoid wasting supplies. Call your teacher in the event of a spill. Spills should be cleaned up promptly, according to your teacher s directions. Acids and bases are corrosive. If an acid or base spills onto your skin or clothing, wash the area immediately with running water. Call your teacher in the event of an acid spill. Acid or base spills should be cleaned up promptly. Never put broken glass in a regular waste container. Broken glass should be disposed of separately according to your teacher s instructions. Do not heat glassware that is broken, chipped, or cracked. Use tongs or a hot mitt to handle heated glassware and other equipment because hot glassware does not always look hot. When using a Bunsen burner, confine long hair and loose clothing. If your clothing catches on fire, WALK to the emergency lab shower and use it to put out the fire. Do not heat glassware that is broken, chipped, or cracked. Use tongs or a hot mitt to handle heated glassware and other equipment because hot glassware does not always look hot. Procedure 1. Put on safety goggles, gloves, and a lab apron. 2. Moisten a strip of filter paper with 0.1 M KMnO 4. Place a few crystals of sodium sulfite on a spot plate or in a small test tube, and add 2 drops of 1.0 M HCl. Immediately hold the strip of filter paper over the crystals, as shown in Figure 1. This reaction is characteristic of the sulfite ion, SO 2 3. Record your observations. Holt Chemistry 32 Chemical Equations and Reactions

3 Name Class Date Figure 1 Filter paper KMnO 4 Na 2 SO 3 + HCl 3. Place a few crystals of sodium carbonate on a spot plate or in a small test tube. Add 2 drops of 1.0 M HCl. Immediately hold a strip of filter paper moistened with 0.1 M KMnO 4 over the solution. This reaction is characteristic of the carbonate ion, CO 2 3. Record your observations. 4. Place a few crystals of ammonium chloride on a spot plate or in a small test tube. Add 2 drops of 1.0 M NaOH. Quickly hold a piece of moistened red litmus paper over the solution, as shown in Figure 2. This reaction is characteristic of the ammonium ion, NH 4. Record your observations. Figure 2 Litmus paper NH 4 Cl + NaOH 5. Label a 50 ml beaker Waste and add about 10 ml of HCl to the beaker. Clean the flame-test wire by dipping it in the HCl and then holding it in the colorless flame of the Bunsen burner. Put 10 drops of Na 2 CO 3 into one of the wells. Dip the wire in the Na 2 CO 3 solution, and then hold it in the Bunsen burner flame. Record the color of the flame. 6. You now have a number of simple tests to identify each of the unknowns listed in Table 1. If a solution is needed for a test, dissolve a small amount of the compound in water. Consider all four ions in the two compounds for each unknown. For example, unknown 1 contains K, NO 3, Na, and Cl ions. You should be able to predict the results for each compound before you begin the test. Holt Chemistry 33 Chemical Equations and Reactions

4 Name Class Date 7. Clean all apparatus and your lab station. Return equipment to its proper place. Dispose of chemicals and solutions in the containers designated by your teacher. Do not pour any chemicals down the drain or in the trash unless your teacher directs you to do so. Wash your hands thoroughly before you leave the lab and after all work is finished. Observations, step 2: Observations, step 3: Observations, step 4: Observations, step 5: Holt Chemistry 34 Chemical Equations and Reactions

5 Name Class Date TABLE 1: TEST RESULTS Unknown Test Used Observations Identity KNO 3 or NaCl NH 4 Cl or MgCO 3 LiNO 3 or Na 2 CO 3 Sr(NO 3 ) 2 or Na 2 SO 3 (NH 4 ) 2 CO 3 or ZnSO 4 BaCl 2 or NaNO 3 Na 2 SO 3 or Na 2 CO 3 Analysis 1. Relating Ideas Explain how to generate ammonia gas in the laboratory. Write and balance the equation for the reaction. 2. Relating Ideas Give the formula and the name of a compound that gives a violet color to a flame and, when HCl is added, produces bubbles of gas that turn potassium permanganate brown. Conclusions 1. Analyzing Results Which salt in the table will react with both HCl and NaOH? Write the equations for the reactions. Holt Chemistry 35 Chemical Equations and Reactions

6 Skills Practice Lab Simple Qualitative Analysis MICROSCALE Teacher Notes TIME REQUIRED One 45-minute lab period SKILLS ACQUIRED Collecting data Experimenting Inferring Predicting Interpreting Organizing and analyzing data RATING Teacher Prep 3 Student Set-Up 2 Concept Level 2 Clean Up 2 Easy Hard THE SCIENTIFIC METHOD Make Observations Students collect qualitative data on chemical reactions. Analyze the Results Conclusions question 1 requires students to analyze their results. Draw Conclusions Students are asked to draw conclusions from their data regarding the identity of the unknown ionic compounds. Communicate the Results Analysis questions 1 and 2, and the Conclusions question MATERIALS Materials for this lab activity can be purchased from WARD S. See the Master Materials List on the One-Stop Planner CD-ROM for ordering instructions. To prepare 200 ml of 1.0 M HCl, observe the required safety precautions. Slowly, and with stirring, add 18 ml of concentrated HCl to enough distilled water to make 200 ml of solution. To prepare 250 ml of 1.0 M NaOH, observe the required safety precautions. Slowly, and with stirring, dissolve 10 g of NaOH in enough distilled water to make 250 ml of solution. To prepare 500 ml of 0.1 M potassium permanganate solution, dissolve 8 g of KMnO 4 in enough distilled water to make 500 ml of solution. To prepare the unknowns, place 15 g of one compound from each of the following pairs into each vial and label the vial with the names of both compounds in the pair: KNO 3 or NaCl, NH 4 Cl or MgCO 3, LiNO 3 or Na 2 CO 3, Sr(NO 3 ) 2 or Na 2 SO 3, (NH 4 ) 2 CO 3 or ZnSO 4, BaCl 2 or NaNO 3, Na 2 SO 3 or Na 2 CO 3. Holt Chemistry 62 Chemical Equations and Reactions

7 SAFETY CAUTIONS Safety goggles, gloves, and a lab apron must be worn at all times. All flame tests must be performed in the hood. Wear goggles, face shield, impermeable gloves, and a lab apron when you prepare the HCl solution. Work in a hood known to be in operating condition, with another person present nearby to call for help in case of an emergency. Be sure you are a 30 s walk from a safety shower and eyewash station known to be in operating condition. Remind students of the following safety precautions: Always wear safety goggles and a lab apron to protect your eyes and clothing. If you get a chemical in your eyes, immediately flush the chemical out at the eyewash station while calling to your teacher. Know the location of the emergency lab shower and the eyewash stations and procedures for using them. Do not touch any chemicals. If you get a chemical on your skin or clothing, wash the chemical off at the sink while calling to your teacher. Make sure you carefully read the labels and follow the precautions on all containers of chemicals that you use. If there are no precautions stated on the label, ask your teacher what precautions you should follow. Do not taste any chemicals or items used in the laboratory. Never return leftovers to their original containers take only small amounts to avoid wasting supplies. Call your teacher in the event of a spill. Spills should be cleaned up promptly, according to your teacher s directions. When using a Bunsen burner, confine long hair and loose clothing. If your clothing catches on fire, walk to the emergency lab shower, and use it to put out the fire. Do not heat glassware that is broken, chipped, or cracked. Use tongs or a hot mitt to handle heated glassware and other equipment because hot glassware does not look hot. Never put broken glass in a regular waste container. Broken glass should be disposed of properly. DISPOSAL Provide labeled waste containers for the various solids. These can be saved for reuse. Carry out the following procedures in the order stated. a. Combine all solutions containing Na 2 SO 3, and, in a hood known to be operating properly, slowly add 1.0 M HCl while stirring until no more SO 2 is evolved. b. Combine all solutions containing NH 4, and, in a hood known to be operating properly, add an equal volume of 1.0 M NaOH solution. Then heat to boiling and continue to heat until all NH 3 is driven off. c. Combine all solutions containing KMnO 4, and add 1 ml of 1.0 M HCl. Then, while stirring slowly, add 1.0 M Na 2 S 2 O 3 until the mixture is decolorized. d. Combine all Zn 2 solutions. Add 1.0 M NaOH slowly with stirring until all zinc has precipitated as the hydroxide. Holt Chemistry 63 Chemical Equations and Reactions

8 TECHNIQUES TO DEMONSTRATE Show the students the proper method for using the filter paper strips. Review proper safety precautions required when dealing with chemicals. Review proper disposal and clean up procedures. TIPS AND TRICKS Emphasize that each of these tests requires only a few crystals of sample. Caution students about not contaminating the unknown samples. Holt Chemistry 64 Chemical Equations and Reactions

9 Name Class Date Skills Practice Lab Simple Qualitative Analysis MICROSCALE If an unknown sample is one of a limited number of possible compounds, a simple test often can determine its identity. For example, a flame test can distinguish between KCl and NaNO 3. A drop of potassium hexacyanoferrate(iii) solution can tell you whether FeCl 2 or FeCl 3 is present. There are hundreds of simple qualitative tests such as these to distinguish among a few possibilities. Qualitative tests are important to the forensic chemist, one who is interested in solving crimes, but they have been largely replaced by instrumental analysis, which is fast and requires a very small sample. For example, instrumental analysis can detect as little as g of 9-tetrahydrocannabinol (one of the active ingredients in marijuana) in 1 ml of blood plasma. Unfortunately, this kind of instrumentation (a gas chromatograph connected to a mass spectrograph) is expensive, so simple chemical tests are still often useful. A drop of hydrochloric acid is enough to allow the police department s forensic chemist to distinguish between a bag of cocaine and a bag of baking soda. In this experiment you will identify the contents of a number of vials. The substance in each vial is one of the two compounds listed on the label. To decide which compound is present, you will make a few simple tests. OBJECTIVES Observe qualitative tests using known ionic compounds. Decide which qualitative test to use in identifying an unknown ionic compound. Describe the chemistry of common ionic compounds. MATERIALS beaker, 50 ml Bunsen burner and related equipment cobalt glass plates (2) filter paper, cut into short strips flame-test wire gloves HCl, 1.0 M KMnO 4, 0.1 M lab apron Na 2 CO 3 NaOH, 1.0 M Na 2 SO 3 NH 4 Cl red litmus paper safety goggles sparker spot plate or small test tubes (3) Holt Chemistry Chemical Equations and Reactions

10 Name Class Date Always wear safety goggles and a lab apron to protect your eyes and clothing. If you get a chemical in your eyes, immediately flush the chemical out at the eyewash station while calling to your teacher. Know the location of the emergency lab shower and eyewash station and the procedures for using them. Do not touch any chemicals. If you get a chemical on your skin or clothing, wash the chemical off at the sink while calling to your teacher. Make sure you carefully read the labels and follow the precautions on all containers of chemicals that you use. If there are no precautions stated on the label, ask your teacher what precautions to follow. Do not taste any chemicals or items used in the laboratory. Never return leftovers to their original container take only small amounts to avoid wasting supplies. Call your teacher in the event of a spill. Spills should be cleaned up promptly, according to your teacher s directions. Acids and bases are corrosive. If an acid or base spills onto your skin or clothing, wash the area immediately with running water. Call your teacher in the event of an acid spill. Acid or base spills should be cleaned up promptly. Never put broken glass in a regular waste container. Broken glass should be disposed of separately according to your teacher s instructions. Do not heat glassware that is broken, chipped, or cracked. Use tongs or a hot mitt to handle heated glassware and other equipment because hot glassware does not always look hot. When using a Bunsen burner, confine long hair and loose clothing. If your clothing catches on fire, WALK to the emergency lab shower and use it to put out the fire. Do not heat glassware that is broken, chipped, or cracked. Use tongs or a hot mitt to handle heated glassware and other equipment because hot glassware does not always look hot. Procedure 1. Put on safety goggles, gloves, and a lab apron. 2. Moisten a strip of filter paper with 0.1 M KMnO 4. Place a few crystals of sodium sulfite on a spot plate or in a small test tube, and add 2 drops of 1.0 M HCl. Immediately hold the strip of filter paper over the crystals, as shown in Figure 1. This reaction is characteristic of the sulfite ion, SO 2 3. Record your observations. Holt Chemistry Chemical Equations and Reactions

11 Name Class Date Figure 1 Filter paper KMnO 4 Na 2 SO 3 + HCl 3. Place a few crystals of sodium carbonate on a spot plate or in a small test tube. Add 2 drops of 1.0 M HCl. Immediately hold a strip of filter paper moistened with 0.1 M KMnO 4 over the solution. This reaction is characteristic of the carbonate ion, CO 2 3. Record your observations. 4. Place a few crystals of ammonium chloride on a spot plate or in a small test tube. Add 2 drops of 1.0 M NaOH. Quickly hold a piece of moistened red litmus paper over the solution, as shown in Figure 2. This reaction is characteristic of the ammonium ion, NH 4. Record your observations. Figure 2 Litmus paper NH 4 Cl + NaOH 5. Label a 50 ml beaker Waste and add about 10 ml of HCl to the beaker. Clean the flame-test wire by dipping it in the HCl and then holding it in the colorless flame of the Bunsen burner. Put 10 drops of Na 2 CO 3 into one of the wells. Dip the wire in the Na 2 CO 3 solution, and then hold it in the Bunsen burner flame. Record the color of the flame. 6. You now have a number of simple tests to identify each of the unknowns listed in Table 1. If a solution is needed for a test, dissolve a small amount of the compound in water. Consider all four ions in the two compounds for each unknown. For example, unknown 1 contains K, NO 3, Na, and Cl ions. You should be able to predict the results for each compound before you begin the test. Holt Chemistry Chemical Equations and Reactions

12 Name Class Date 7. Clean all apparatus and your lab station. Return equipment to its proper place. Dispose of chemicals and solutions in the containers designated by your teacher. Do not pour any chemicals down the drain or in the trash unless your teacher directs you to do so. Wash your hands thoroughly before you leave the lab and after all work is finished. Observations, step 2: When acid is added to a sulfite, bubbles appear. These bubbles change the purple permanganate solution to a brown color. Observations, step 3: When acid is added to a carbonate, bubbles appear. These bubbles do not affect the color of KMnO 4 solution. Observations, step 4: The color of red litmus paper turns blue. Observations, step 5: The color of the flame is yellow orange. Holt Chemistry Chemical Equations and Reactions

13 Name Class Date TABLE 1: TEST RESULTS Unknown Test Used Observations Identity KNO 3 or NaCl NH 4 Cl or MgCO 3 LiNO 3 or Na 2 CO 3 Sr(NO 3 ) 2 or Na 2 SO 3 (NH 4 ) 2 CO 3 or ZnSO 4 BaCl 2 or NaNO 3 Na 2 SO 3 or Na 2 CO 3 Flame test Yellow-orange flame NaCl Step 3 Litmus paper turned blue NH 4 Cl Step 2 and Nothing for step 2 Na 2 CO 3 flame test flame was yellow-orange Step 1 Filter paper turned Na 2 SO 3 brown Steps 2 Nothing for step 2 (NH 4 ) 2 CO 3 and 3 litmus paper turned blue Flame test Flame was green BaCl 2 Step 1 Filter paper turned Na 2 SO 3 brown Analysis 1. Relating Ideas Explain how to generate ammonia gas in the laboratory. Write and balance the equation for the reaction. Add sodium hydroxide to an ammonium salt, such as ammonium chloride. NH 4 Cl(s) NaOH(aq) NaCl(aq) NH 3 (g) H 2 O(l) 2. Relating Ideas Give the formula and the name of a compound that gives a violet color to a flame and, when HCl is added, produces bubbles of gas that turn potassium permanganate brown. Answer should be a compound composed of sulfite ion, such as K 2 SO 3, potassium sulfite. Conclusions 1. Analyzing Results Which salt in the table will react with both HCl and NaOH? Write the equations for the reactions. Ammonium carbonate reacts with both HCl and NaOH. (NH 4 ) 2 CO 3 (s) 2HCl(aq) 2NH 4 Cl(aq) H 2 O(l) CO 2 (g) (NH 4 ) 2 CO 3 (s) 2NaOH(aq) 2NH 3 (g) 2H 2 O(l) Na 2 CO 3 (aq) Holt Chemistry Chemical Equations and Reactions

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