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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