CHEM 1E EXP 5 Spectroscopy and Beers Law Analysis_Revision_Fall18 (1)

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CHEM 1E Experiment 5. S. Crawford Fall 2018. 1 CHEM 1E Experiment 5: Flame Tests and Absorption Spectroscopy Spectroscopy utilizes electromagnetic radiation to determine information about the composition of a chemical system. Spectroscopy can be used to identify elemental or molecular presence, or to determine the concentration of molecular or atomic species in a system of interest. Spectroscopy was largely the contributing source of data that lead to our current understanding of the structure of the atom and how the atoms of different elements vary. Two types of “spectra” most often obtained are emission and adsorption spectra. An emission spectrum is produced when atoms in an “excited” state emit photons characteristic of the element when they return to the lower energy states. Some elements produce very intense spectral lines that can be used to identify the presence of the element. These intense spectral lines are the basis for the flame tests that you will use to identify the presence of the element in a substance. In a flame test, a granule of an ionic solid or a drop of a solution containing the dissolved ionic solid is placed in a hot flame. The flame serves to excite the atom of interest after which a glowing emission of light is observed that is characterized by a wavelength (color) indicative of the element present. In absorption spectroscopy, the wavelengths of light absorbed by a sample can be used to provide information about the presence of a species and the concentration of the species. The primary objective of the absorption spectroscopy portion of this experiment is to determine the concentration of an unknown copper (II) sulfate solution. The CuSO 4 solution used in this experiment has a blue color. You will determine an appropriate wavelength based on the absorbance spectrum of the solution. A higher concentration of the colored solution absorbs more light (and transmits less) than a solution of lower concentration. You will prepare five copper (II) sulfate solutions of known concentration (standard solutions). Each solution is transferred to a small, rectangular cuvette that is placed into the spectrometer. The amount of light that penetrates the solution and strikes the photocell is used to compute the absorbance of each solution. When you graph absorbance vs . concentration for the standard solutions, a direct relationship should result. The direct relationship between absorbance and concentration for a solution is known as Beer’s law . You will determine the concentration of an unknown CuSO 4 solution by measuring its absorbance. By locating the absorbance of the unknown on the vertical axis of the graph, the corresponding concentration can be found on the horizontal axis. The concentration of the unknown can also be found using the slope of the Beer’s law curve. OBJECTIVES In this experiment, you will Conduct flame tests on a variety of cation solutions and record observations Utilize you observations from standard flame test experiments to identify the ion present in an unknown. Prepare and test the absorbance of five standard copper (II) sulfate solutions. Prepare a Beer’s law calibration curve from the test results of the standard solutions. Figure 1
CHEM 1E Experiment 5. S. Crawford Fall 2018. 2 Test the absorbance of a copper (II) sulfate solution of unknown molar concentration. Calculate the molar concentration of the unknown CuSO 4 solution. MATERIALS Nichrome wire 6 M HCl Solutions of known metal ions LabQuest 0.40 M copper (II) sulfate, CuSO 4 , solution copper (II) sulfate, CuSO 4 , unknown solution Vernier Spectrometer one cuvette distilled water five 20 × 150 mm test tubes test tube rack two 10 mL pipets or graduated cylinders stirring rod two 100 mL beakers tissues (preferably lint-free) Here is a site that shows how to use the Vernier labquest spectrometer you will use in this lab. Watch the video on Spectr ometer “tech tips”. Only the absorbance part pertains to this lab, not the fluorescence part. HTTP://WWW.VERNIER.COM/PRODUCTS/SENSORS/SPECTROMETERS/SVIS- PL/
CHEM 1E Experiment 5. S. Crawford Fall 2018. 3 PROCEDURE PART I. FLAME TEST IDENTIFICATION OF IONS. Working in pairs you will observe the emission colors of several aqueous solutions containing certain metal cations. You will record your observations from flame tests and then use your results to identify the metal cations present in an unknown solution. Procedure: Place approximately 0.5 mL of the following solutions into small labeled test tubes: CuCl 2 , KCl, BaCl 2 , SrCl 2 , CaCl 2 Obtain a nichrome wire with a cork holder from the front of the room. Carefully ignite the Bunsen burner. Dip the metal end of your nichrome wire in the 6M HCl solution then into a clean small beaker containing deionized water. Heat the wire in the hottest part of the flame (blue tip). Repeat twice. This will clean off your wire so that any metal contaminates present on the wire will be removed. You will need to repeat this step before examining each different solution. If the HCl solution turns yellow, you will need to replace it with a fresh solution. Perform the flame tests on the known solutions: Dip the wire into your first solution and place it in the hottest part of the Bunsen burner flame. Note the color of the flame and record your observations on your data sheet. You should perform the test a few times for each solution. Clean your wire with the 6M HCl as described. Repeat the tests on the remaining solutions. Record your observations on the data sheet. Make sure to clean the wire between solutions. Once your data sheet is complete, please show it to your lab instructor to obtain your unknown samples. Each student will obtain an unknown from the lab instructor and individually identify the metal cations present. Perform the flame tests on each unknown, record your observations on the data sheet. Don’t forget to record your unknown numbers on the data sheet. PROCEDURE PART II: ABSORBTION SPECTROSC OPY AND BEER’S LAW 1. Obtain and wear goggles. Do this part as a pair. 2. Add 10.0 mL of the 0.40 M CuSO 4 solution to your 50.0 mL graduated cylinder. Add 40.0 mL of deionized water to your graduated cylinder. There should be a total of 50.0 mL of solution in your 50.0 mL graduated cylinder. Your 0.40 M CuSO 4 solution is now diluted to 0.08M CuSO 4 . The concentration of your diluted CuSO 4 solution can be calculated as follows: M i V i = M f V f (0.40M)(10.0mL) = (M f )(50.0mL) M f = 0.08M
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CHEM 1E Experiment 5. S. Crawford Fall 2018. 4 3. Label five clean, dry, test tubes 1 5 using a grease pencil. Use your 10mL graduated cylinders to prepare five standard solutions according to the chart below. For example, add 2 mL of 0.08M CuSO 4 and 8 mL of deionized H 2 O to test tube 1 and follow this pattern for test tube 2-5. Thoroughly mix each solution with a stirring rod. Clean and dry the stirring rod between uses. Test Tube 0.08 M CuSO 4 (mL) Deionized Water H 2 O (mL) Concentration (M) 1 2 8 0.016M 2 4 6 0.032M 3 6 4 0.048M 4 8 2 0.064M 5 ~10 0 0.08M 4. Prepare a blank by filling a cuvette 3/4 full with deionized water. To correctly use cuvettes, remember: Wipe the outside of each cuvette with a lint-free tissue. Handle cuvettes only by the top edge of the ribbed sides. Dislodge any bubbles by gently tapping the cuvette. Always position the cuvette so the light passes through the clear sides. 5. Connect the Spectrometer and the power adaptor to LabQuest. Once everything is connected, you may now turn on the LabQuest unit. 6. Calibrate the Spectrometer. a. Choose Calibrate from the Sensors menu. The following message is displayed: “Waiting 90 seconds for lamp to warm up.” After 90 seconds, the message will change to “Warmup complete.” b. Place the blank cuvette filled with deionized water in the Spectrometer. c. Select Finish Calibration . When the message “Calibration completed” appears, select OK . 7. Determine the optimal wavelength for creating the standard Beer’s Law curve and set up the data-collection mode. a. Remove the blank cuvette, and place the 0.08 M standard into the cuvette slot. b. Tap “mode” and under “full spectrum” change the wavelength range to 380 950 nm and select ok. c. Start data collection using the green arrow at the bottom of the screen. A full spectrum graph of the solution will be displayed. Stop data collection with the red square . A graph with a maximum peak will appear on the screen. Use the stylus to tap the top of the peak that appears at the right of the spectrum. This is the wavelength of maximum absorbance ( max). d. Tap the Meter tab. On the Meter screen, tap Mode . Change the mode to Events with Entry. Select OK. e. Select save and save this data to the device.
CHEM 1E Experiment 5. S. Crawford Fall 2018. 5 8. You are now ready to collect absorbance-concentration data for the five standard solutions. a. Using the solution in Test Tube 1, rinse the cuvette twice with ~1 mL amounts and then fill it 3/4 full. Wipe the outside with a tissue and place it in the spectrometer. b. When the value displayed on the screen has stabilized, record the absorbance value for the 0.016 mol/L in your data table. c. Discard the cuvette contents into a waste beaker. Using the solution in Test Tube 2, rinse and fill the cuvette 3/4 full. Wipe the outside and place the cuvette in the spectrometer. Wait for the value displayed on the screen to stabilize, record the absorbance value for the 0.032 mol/L solution in your data table. d. Repeat the procedure for Test Tubes 3 and 4. Trial 5 is the original 0.08 M CuSO 4 solution . Note: Do not test the unknown solution until Step 10. 10. Determine the absorbance and concentration values of the unknown CuSO 4 solution. a. Obtain an unknown CuSO 4 from your lab instructor. Record the number of the unknown in your data table. b. Rinse the cuvette twice with the unknown solution and fill it about 3/4 full. Wipe the outside of the cuvette and place it into the spectrometer. c. Monitor the absorbance value. When this value has stabilized, record it in your data table. PROCEDURE PART III: OBSERVATION OF EMISSION SPECTRA. 1. Go into the balance room and use the SPECTROGRAPH to view the emission lines from one of the atomic vapor lamp provided. Your lab instructor will give you directions. 2. Sketch the emission spectra you observe on your data sheets with wavelengths included.
CHEM 1E Experiment 5. S. Crawford Fall 2018. 6 NAME____________________________ LAB SECTION_________ SCORE________ /20 DATA TABLE. HAND IN WITH YOUR REPORT. DATA TABLE PART I: FLAME TEST OF CATIONS. Solution Observations Cu 2+ K + Ba 2+ Sr 2+ Ca 2+ Unknown # Based on your observations, what is the identity of the cation in your unknown? Unknown #_______ Identity_________________________________ DATA TABLE. PART II: BEER’S LAW Trial Concentration (mol/L) Absorbance 1 0.016M 2 0.032M 3 0.048M 4 0.064M 5 0.08 M 6 Unknown number ____
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CHEM 1E Experiment 5. S. Crawford Fall 2018. 7 DATA ANALYSIS PART II NAME_____________________________ 1. Take your data home and use EXCEL to prepare a Beer’s Law plot of the data from your standards (Trials 1- 5). You should plot Absorbance on the “y” axis and concentration on the “x” axis. Include a print out of your graph with your report. 2. Add a trend line to your graph in the same way that you added the trend line to the graph you prepared in your density experiment (EXP 1). Be sure to show the equation the line on your graph. 3. Utilize your graph to determine the concentration of your unknown copper sulfate solution. Show how you did this on your graph. Unknown Concentration from Graph ____________________M 4. Use the equation of the line on your graph to determine the concentration of your unknown copper sulfate solution. Show your work below. Unknown concentration from linear equation ____________________M DATA FOR PART III: Sketch the emission line spectrum you observed with the spectrograph. Include the wavelengths. ELEMENT IN LAMP________________ SKETCH: