Calculator 11 Investigating Indicators An indicator solution does what its name suggests – it indicates. In chemistry, a common use of an indicator is to signal the equivalence point of a reaction between an acid and a base. Generally, an indicator is itself a weak organic acid or a blend of weak organic acids. The indicator establishes equilibrium in aqueous solution, which is shifted according to LeChatelier’s principle as the solution changes in pH. The indicator is one color in the presence of a range of concentrations of H+ or OH– ions, and another color when the acidity changes. Knowing when an indicator will change color helps you determine the precise equivalence point of an acid-base reaction. This knowledge is also important as you select the proper indicator for a given reaction. OBJECTIVES In this experiment, you will Conduct strong acid-strong base titrations using solutions of hydrochloric acid and sodium hydroxide, and three different indicator solutions. Select the proper indicator to use with a titration involving a weak acid or a weak base, based on your observations and measurements. Figure 1 CHOOSING A METHOD If you choose Method 1, you will conduct the titration in a conventional manner. You will deliver volumes of NaOH titrant from a buret. You will enter the buret readings manually to store and graph each pH-volume data pair. If you choose Method 2, you will use a Vernier Drop Counter to conduct the titration. NaOH titrant is delivered drop by drop from the reagent reservoir through the Drop Counter slot. After the drop reacts with the reagent in the beaker, the volume of the drop is calculated and a pH-volume data pair is stored. Advanced Chemistry with Vernier 11 - 1 Calculator 11 MATERIALS Materials for both Method 1 (buret) and Method 2 (Drop Counter) LabPro or CBL 2 interface TI graphing calculator Vernier pH Sensor 0.10 M NaOH solution 0.10 M HCl solution 0.10 M HC2H3O2 solution 0.10 M NH3 solution 250 mL beaker 50 mL graduated cylinder magnetic stirrer (if available) stirring bar or Microstirrer wash bottle ring stand utility clamp phenolphthalein indicator solution bromthymol blue indicator solution methyl orange indicator solutions distilled water Materials required only for Method 1 (buret) 50 mL buret 10 mL pipet buret clamp Materials required only for Method 2 (Drop Counter) Vernier Drop Counter reagent reservoir 5 mL pipet 100 mL beaker 10 mL graduated cylinder a second 250 mL beaker METHOD 1: Measuring Volume Using a Buret 1. Obtain and wear goggles. 2. Use a graduated cylinder to measure out 20 mL of 0.10 M HCl solution into a 250 mL beaker. Add exactly two drops of methyl orange indicator solution to the beaker of HCl solution. CAUTION: Handle the hydrochloric acid with care. It can cause painful burns if it comes in contact with the skin. 3. Place the beaker on a magnetic stirrer and add a stirring bar. If no magnetic stirrer is available, stir the reaction mixture with a stirring rod during the titration. Part I Strong Acid – Strong Base Titrations 4. Connect a pH Sensor to Channel 1 of the LabPro or CBL 2 interface. Use the link cable to connect the interface to the TI graphing calculator. 5. Use a utility clamp to suspend the pH Sensor on a ring stand as shown in Figure 1. Position the pH Sensor in the HCl solution and adjust its position so that it is not struck by the stirring bar. 6. Rinse and fill the buret with 0.10 M NaOH solution. CAUTION: Sodium hydroxide solution is caustic. Avoid spilling it on your skin or clothing. 11 - 2 Advanced Chemistry with Vernier Investigating Indicators 7. Set up the calculator and interface for the pH Sensor. a. Turn on the calculator and start the DATAMATE program. Press CLEAR to reset the program. b. Select SETUP from the Main screen. If CH 1 displays PH, proceed directly to Step 8. If it does not, continue with this step to set up your sensor manually. c. Press ENTER to select CH 1. d. Select PH from the SELECT SENSOR menu. 8. Set up the data-collection mode. a. To select MODE, press until the cursor is to the left of MODE and press b. Select EVENTS WITH ENTRY from the SELECT MODE menu. c. Select OK to return to the Main screen. ENTER . 9. Select START to begin data collection. Conduct the titration carefully, as described below. During the titration, make careful note of the color changes in the reaction mixture. Record the volume of NaOH solution added and the pH at which the indicator changed color. a. Before you have added any NaOH solution, press ENTER and type in “0” as the buret volume in mL. Press ENTER to save the first data pair for this experiment. b. Add 1 mL of the NaOH titrant. When the pH stabilizes, press ENTER and type in the current buret reading. You have now saved the second data pair for the experiment. c. Continue adding NaOH solution 1 mL at a time, and enter the buret reading after each increment, until the pH of the mixture is about 5. d. Add NaOH in 0.5 mL increments until the pH is about 10. e. Continue adding NaOH solution until the pH value remains constant. 10. Press STO when you have finished collecting data. 11. When you have completed the titration, dispose of the reaction mixture as directed. Rinse the pH Sensor with distilled water in preparation for the second titration. 12. Print a copy of the graph of pH vs. volume for the first trial. Use the printed graph to show the point or points at which the indicator solution changed color. Describe the color, or colors, as precisely as possible. Make special note of the area around the equivalence point, the region of the graph where the pH increases drastically. It is crucial for the indicator solution to change color at the equivalence point of the titration. 13. Repeat the necessary steps to conduct a second and third titration, using the bromthymol blue and phenolphthalein indicator solutions. Repeat Step 12 to analyze the titration data and indicators for the second and third trials. Part II Selecting an Appropriate Indicator for a Titration 14. Obtain a weak acid or weak base solution from your instructor. If you are testing a weak acid, use the 0.10 M NaOH solution as the titrant. If you are testing a weak base, rinse and fill your buret with the weak base solution, and titrate 20 mL of 0.10 M HCl solution. Use the results of your previous tests to select the appropriate indicator solution for this titration. Conduct the titration as you have in the previous three tests. Print a copy of the graph of pH vs. volume for this final titration. Use the printed graph to show the point or points at which the indicator solution changed color. Describe the color as precisely as possible. Advanced Chemistry with Vernier 11 - 3 Calculator 11 METHOD 2: Measuring Volume Using a Drop Counter 1. Obtain and wear goggles. 2. Add 40 mL of distilled water to a 100 mL beaker. (You can add less, about 20 mL, if you will be using a stirring bar instead of the Microstirrer.) Use a pipet bulb (or pipet pump) to pipet 5.00 mL of the HCl solution into the 100 mL beaker with distilled water. Add exactly one drop of methyl orange indicator solution to the beaker of HCl solution. CAUTION: Handle the hydrochloric acid with care. It can cause painful burns if it comes in contact with the skin. Figure 2 Part I Strong Acid – Strong Base Titrations 3. Connect a pH Sensor to Channel 1 of the LabPro or CBL 2 interface. Lower the Drop Counter onto a ring stand and plug it into the DIG/SONIC 1 port (see Figure 2). Use the link cable to connect the interface to the TI graphing calculator. 4. Obtain the plastic 60 mL reagent reservoir. Close both valves by turning the handles to a horizontal position. Follow the steps below to set up the reagent reservoir for the titration. a. Rinse the reagent reservoir with a few mL of the 0.10 M NaOH solution and pour the NaOH into an empty 250 mL beaker. b. Use a utility clamp to attach the reservoir to the ring stand. c. Fill the reagent reservoir with slightly more than 60 mL of the 0.100 M NaOH solution. d. Place the 250 mL beaker, which contains the rinse NaOH, beneath the tip of the reservoir. e. Drain a small amount of the NaOH solution into the 250 mL beaker so that it fills the reservoir’s tip. To do this, turn both valve handles to the vertical position for a moment, then turn them both back to horizontal. f. Discard the drained NaOH solution in the 250 mL beaker as directed. 11 - 4 Advanced Chemistry with Vernier Investigating Indicators 5. Set up the calculator and interface for the pH Sensor. a. Turn on the calculator and start the DATADROP program. Press CLEAR to reset the program. b. Select SETUP from the Main screen. If CH 1 displays PH, proceed directly to Step 6. If it does not, continue with this step to set up the sensor manually. c. Press ENTER to select CH 1. d. Select PH from the SELECT SENSOR menu. 6. Calibrate the drops that will be delivered from the reagent reservoir. Note: If you are using the stored calibration (20 drops per mL), then skip this step. a. Select CALIBRATE DROPS from the Main screen. If you have done a previous calibration with this particular apparatus, you can choose CALIBRATE DROPS and manually enter the drops/mL ratio. Select OK and proceed to Step 7. If you want to perform a new calibration, continue with this step. b. Fill the reagent reservoir with titrant. c. Select CALIBRATE DROPS from the Main screen. d. Select CALIBRATE NOW. e. Open the bottom 2-way (on-off) valve to begin releasing drops from the vessel through the Drop Counter (the top valve finely adjusts the drop rate). f. Continue to release drops until there are between 9 and 10 mL of liquid in the graduated cylinder. g. Close the bottom valve on the vessel to stop the drops. h. Press ENTER . i. Type the precise volume of liquid in the graduated cylinder in milliliters and press ENTER . j. The number of drops/mL will be displayed. It may be helpful to record the value for that particular reagent reservoir for future titrations. k. Select OK to return to the Main screen. l. Discard the NaOH solution in the graduated cylinder as indicated by your instructor and set the graduated cylinder aside. 7. Assemble the apparatus. a. Place the magnetic stirrer on the base of the ring stand. b. Insert the pH Sensor through the large hole in the Drop Counter. c. Attach the Microstirrer to the bottom of the pH Sensor. Rotate the paddle wheel of the Microstirrer, and make sure that it does not touch the bulb of the pH Sensor. d. Adjust the positions of the Drop Counter and reagent reservoir so they are both lined up with the center of the magnetic stirrer. e. Lift up the pH Sensor, and slide the beaker containing the HCl solution onto the magnetic stirrer. Lower the pH Sensor into the beaker. f. Adjust the position of the Drop Counter so that the Microstirrer on the pH Sensor is just touching the bottom of the beaker. g. Adjust the reagent reservoir so its tip is just above the Drop Counter slot. h. Turn on the magnetic stirrer so that the Microstirrer is stirring at a fast rate. Advanced Chemistry with Vernier 11 - 5 Calculator 11 8. You are now ready to perform the titration. a. Select START. No data will be collected until the first drop goes through the Drop Counter slot. b. Fully open the bottom valve—the top valve should still be adjusted so drops are released at a rate of about 1 drop every 2 seconds. When the first drop passes through the Drop Counter slot, check the data table to see that the first data pair was recorded. 9. Continue watching your graph to see when a large increase in pH takes place—this will be the equivalence point of the reaction. When this jump in pH occurs, let the titration proceed for several more milliliters of titrant, then press STO . Turn the bottom valve of the reagent reservoir to a closed (horizontal) position. 10. When you have completed the titration, dispose of the reaction mixture as directed. Rinse the pH Sensor with distilled water in preparation for the second titration. 11. Print a copy of the graph of pH vs. volume for the first trial. Use the printed graph to show the point or points at which the indicator solution changed color. Describe the color, or colors, as precisely as possible. Make special note of the area around the equivalence point, the region of the graph where the pH increases drastically. It is crucial for the indicator solution to change color at the equivalence point of the titration. 12. Repeat the necessary steps to conduct a second and third titration, using the bromthymol blue and phenolphthalein indicator solutions. Repeat Step 11 to analyze the titration data and indicators for the second and third trials. Part II Selecting an Appropriate Indicator for a Titration 13. Obtain a weak acid or weak base solution from your instructor. If you are testing a weak acid, use the 0.10 M NaOH solution as the titrant. If you are testing a weak base, rinse and fill your buret with the weak base solution, and titrate 5 mL of 0.10 M HCl solution. Use the results of your previous tests to select the appropriate indicator solution for this titration. Conduct the titration as you have in the previous three tests. Print a copy of the graph of pH vs. volume for this final titration. Use the printed graph to show the point or points at which the indicator solution changed color. Describe the color as precisely as possible. DATA ANALYSIS 1. Describe how the three indicator solutions worked in the titrations. Which indicator solution is the best for a strong acid-strong base titration? Specify the color changes and the pH readings where the color changes occurred. 2. For which type of acid-base titrations would the other two indicator solutions be best suited? Explain. 11 - 6 Advanced Chemistry with Vernier Investigating Indicators 3. Use the graphs to compare how accurately the indicator solutions “indicated” the equivalence point of the titrations that you conducted. In your judgment, can an indicator alone accurately determine the equivalence point of an acid-base reaction? Explain. Advanced Chemistry with Vernier 11 - 7