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Identification of Unknown Components Using Spectroscopic Techniques
Class: Under Graduate/Post Graduate/Ph.D. Subject: Chemistry
Objective:
Identification of Unknown Components Using Following Spectroscopic Techniques:
1. Mass Spectrometry
2. Infrared Spectroscopy
3. NMR Spectroscopy
Required Material:
1. Mass Spectrometry: 1. Dropper 2. Tube 3. Sample 4. Mass Spectrometer
2 (a). Infrared Spectroscopy (Liquid Sample): 1. Dropper 2. Sample 3. Desiccator 4. Infrared Spectrometer
(b). Infrared Spectroscopy (Solid Sample): 1. Potassium Bromide 2. Sample 3. Mortar & Pestle 4. Ring Set 5. Infrared Spectrometer 6. Spatula
3. NMR Spectroscopy: 1. Dropper 2. Sample 3. Sample Tube 4. NMR Spinner 5. NMR Spectrometer 6. Sample Bottle
Overview:
The aim of this experiment is the identification of unknown compounds through a combination of spectroscopic methods. Used here are Mass spectrometry, Infrared spectroscopy and Nuclear Magnetic Resonance spectroscopy.
Precautions to be taken in the laboratory are as follows: 1. Don't eat or drink anything: Don't forget: You can't eat or drink anything in the lab. That's to make sure that you don't mix up your drink with a chemical, or hold your sandwich with dirty hands. 2. Work tidily and carefully: Make sure to keep your workspace tidy during the experiment. If there's something you don't need any more, just put it away. 3. Move slowly and don't horse around: In the lab, we always move slowly and carefully. After all, we don't want to break anything, because that can be dangerous when working with chemicals. 4. Wear safety glasses and a lab coat: You should wear lab coats and safety glasses while in a lab where chemicals are handled. 5. Listen and read carefully: In the lab, read and listen carefully the instructions given by instructor or written on the manuals.
Step : 1. Click on Lab Coat. Step : 2. Click on Lab Gloves. Step : 3. Click on Lab Shoe Cover. Step : 4. Click on Lab Glasses. Step : 5. Select Technique from given dropdown list.
Using Mass Spectrometry
Step : 1. Click on add button to add tubes. Step : 2. Click on add button to add sample. Step : 3. Click on add button to add dropper. Step : 4. Click on add button to add Mass Spectrometer. Step : 5. Click on the cap of conical flask containing sample to open it. Step : 6. Click on dropper to put sample into the tube. Step : 7. Click on the cap of conical flask containing sample to close it. Step : 8. Click on the cover of mass spectrometer to open it. Step : 9. Click on the tube containing sample to put it in the mass spectrometer. Step : 10. Click on the cover of mass spectrometer to close it. Step : 11. Click on the power button of mass spectrometer. Step : 12. Click on Observe button to observe what is happening inside the Mass Spectrometer.
Step : 13. Click on the Observe button to see the graph on the computer moniter screen.
Observations: Now observe the zoomed in animation of Mass Spectromter. The sample is introduced into the vaporisation chamber which
is instantly vapourised due to high vacuum and heat. Positively charged radical ions are formed by bombardment of beam of high energy
electrons. The positively charged radical ions are accelerated by perforated negative electrodes. The ions are sorted and separated by the
magnetic field according to their mass/charge ratio.
Using Infrared Spectroscopy
Step : 1. Click on add button to add dropper. Step : 2. Click on add button to add sample. Step : 3. Click on add button to add desiccator. Step : 4. Click on add button to add Infrared Spectrometer. Step : 5. Click on the cap of desiccator to open it. Step : 6. Click on the cap of sample to open it. Step : 7. Click on the sample to put it in the desiccator. Step : 8. Click on the cap of desiccator to close it. Step : 9. Again click on the cap of desiccator to open it. Step : 10. Click on the sample to take it out from the desiccator. Step : 11. Again click on the cap of desiccator to close it. Step : 12. Click on the cover of Infrared Spectrometer to open it. Step :13. Click on the handle of Infrared Spectrometer for zoom view. Step : 14. Click on the handle of Infrared Spectrometer to slide it. Step : 15. Click on the dropper to take the sample and put it into the Infrared Spectrometer. Step : 16. Click on the handle of Infrared Spectrometer to slide it back. Step : 17. Click on the cover of Infrared Spectrometer to close it. Step : 18. Click on the cap of sample to close it. Step : 19. Click on Observe button to observe what is happening inside the Infrared Spectrometer.
Nuclear Magnetic Resonance (NMR) Spectroscopy
Step : 1. Click on add button to add dropper. Step : 2. Click on add button to add sample. Step : 3. Click on add button to add sample bottle. Step : 4. Click on add button to add sample tube. Step : 5. Click on add button to add NMR spinner. Step : 6. Click on add button to add cloth. Step : 7. Click on the cap of conical flask containing sample to open it. Step : 8. Click on the cap of sample bottle to open it. Step : 9. Click on the dropper to take sample and pour it into the sample bottle. Step : 10. Click on the cap of sample bottle to close it. Step : 11. Click on the cap of conical flask containing sample to close it. Step : 12. Click on the sample bottle containing sample to shake it. Step : 13. Click on the cap of sample tube to open it. Step : 14. Click on the cap of sample bottle to open it. Step : 15. Click on the dropper to take sample from the sample bottle and pour it into the sample tube. Step : 16. Click on the cap of sample tube to close it. Step : 17. Click on the cap of sample bottle to close it. Step : 18. Click on the sample tube to take it out from the beaker. Step : 19. Click on the NMR spinner to fix it on the sample tube. Step : 20. Click on the cloth to wipe the sample tube containing sample.
Step : 21. Click on NMR Spectrometer for zoom view. Step : 22. Click on the sample tube to put it into the NMR Spectrometer. Step : 23. Click on Observe button to observe what is happening inside the NMR Spectrometer.
Step : 24. Click on the Observe button to see the graph on the computer moniter screen.
Observations: Now observe the zoomed in animation of the NMR Spectrometer. It can be seen that the NMR Tube is rotated between
Radio Frequency Generator and Radio Frequency Receiver while the Magnetic Field passes through it.
Step : 1. Click on add button to add mortar & pestle. (Make sure mortar & pestle should be clean) Step : 2. Click on add button to add potassium bromide (KBr). Step : 3. Click on add button to add sample. Step : 4. Click on add button to add ring set. Step : 5. Click on add button to add spatula. Step : 6. Click on add button to add Infrared Spectometer. Step : 7. Click on the cap of bottle containing potassium bromide to open it. Step : 8. Click on the spatula to take potassium bromide from the bottle and put it in the mortar. Step : 9. Click on the cap of potassium bromide to close it. Step : 10. Click on the cap of bottle containing sample to open it. Step : 11. Click on the spatula to take sample from the bottle and put it in the mortar. Step : 12. Click on the cap of sample to close it. Step : 13. Click on the pestle to grind potassium bromide and sample. Step :14. Click on ring for zoom view. Step : 15. Click on the cap of ring to open it. Step : 16. Click on the spatula to take mixture of potassium bromide and sample and put it in the ring. Step : 17. Click on the stick of ring to fix the mixture well, in the ring. Step : 18. Click on the cover of Infrared Spectrometer to open it. Step : 19. Click on the handle of Infrared Spectrometer for zoom view. Step : 20. Click on the handle of Infrared Spectrometer to slide it. Step : 21. Click on the ring containing mixture to put it in the Infrared Spectrometer. Step : 22. Click on the handle of Infrared Spectrometer to slide it back. Step : 23. Click on the cover of Infrared Spectrometer to close it. Step : 24. Click on Observe button to observe what is happening inside the Infrared Spectrometer.
Step : 20. Click on the Observe button to see the graph on the computer moniter screen.
Observations: Now observe the zoomed in animation of the Desiccator. The ray goes from the IR Source to the Beam Splitter, from where
it further proceeds to the Fixed and Movable Mirrors. The reflected rays are merged at the Beam Splitter and proceed towards the Detector
for detection.
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