This document provides step-by-step instructions for running a Fourier-transform infrared spectrophotometer (FTIR) to obtain infrared spectroscopy (IR) spectra. The FTIR allows you to collect an IR spectrum of a sample in one step without any sample preparation. The document walks through collecting a background spectrum, loading and analyzing a sample of acetone, and printing and annotating the resulting IR spectrum to identify functional groups present. Safety precautions for using the FTIR and identifying samples are also outlined.
This document provides step-by-step instructions for running a Fourier-transform infrared spectrophotometer (FTIR) to obtain infrared spectroscopy (IR) spectra. The FTIR allows you to collect an IR spectrum of a sample in one step without any sample preparation. The document walks through collecting a background spectrum, loading and analyzing a sample of acetone, and printing and annotating the resulting IR spectrum to identify functional groups present. Safety precautions for using the FTIR and identifying samples are also outlined.
This document provides step-by-step instructions for running a Fourier-transform infrared spectrophotometer (FTIR) to obtain infrared spectroscopy (IR) spectra. The FTIR allows you to collect an IR spectrum of a sample in one step without any sample preparation. The document walks through collecting a background spectrum, loading and analyzing a sample of acetone, and printing and annotating the resulting IR spectrum to identify functional groups present. Safety precautions for using the FTIR and identifying samples are also outlined.
This document provides step-by-step instructions for running a Fourier-transform infrared spectrophotometer (FTIR) to obtain infrared spectroscopy (IR) spectra. The FTIR allows you to collect an IR spectrum of a sample in one step without any sample preparation. The document walks through collecting a background spectrum, loading and analyzing a sample of acetone, and printing and annotating the resulting IR spectrum to identify functional groups present. Safety precautions for using the FTIR and identifying samples are also outlined.
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How to run a Fourier Transform infrared
Spectrophotometer Raad Bassam A Mulla Introduction As part of studying sciences and engineering curriculums in Penn State, you will be required to take CHEM213, a course in which you will be asked to identify the final product of most, if not all, of your experiments. Hence, you will be asked to run an infrared spectroscopy (IR) for your final product. IR helps you prove the identity of your final product by identifying common functional groups. Currently, the chemistry department uses the FTIR instrument. In Fourier Transform infrared Spectrophotometer (FTIR), unlike other IR spectrometers, the whole spectrum is obtained at once with no sample preparation. Fourier transform is a mathematical algorithm used to convert the information obtained by the detector into a conventional spectrum. You will be placing your sample directly on the instrument. The FTIR is located in the instrument room. So, before you leave the lab, put ~30 mg of your sample in a shorty vial, label it, and place it in your TAs basket. As a beginner, you will probably take 20 minutes to get the IR spectra. With practice, you will master it in about half the time. This document will walk through a general example of collecting a background spectrum first, then, using Acetone as a sample. Pictures were taken under the supervision of Dr. Rummel, who is a faculty member of the chemistry department and chairman of undergraduate courses. Note: This guide is specific to FTIR manufactured by THERMO SCIENTIFIC, model iS10, which is compatible with OMNIC software. Safety information Caution should be used when looking inside the instrument when the cover is off, since an FTIR instrument includes a laser. Because it emits light at a known and constant frequency, the laser acts as the internal calibrator, controls the moving mirrors position, and triggers the capture of data. Wear your gloves when conducting an IR operation, in case the final product (your sample) is hazardous. When inside the lab, follow the safety rules concerning labs such as wearing long shorts, wearing glasses, wearing covered-up shoes etc. Materials needed Acetone Shorty vial Spatula Gloves Kim wipes P a g e 2 | 6
Running FTIR software
Step 1 This is the Diamond ATR Accessory. The Diamond plate is where the sample goes.
Step 2 Locate the OMNIC Software on the Computer
Step 3 Acquire a Background Spectrum, Part 1 Screw the black knob CLOCKWISE so the metal tip descends and hits the shiny metal plate. You cant over-tighten the knob-once the tip hits the plate it turns indefinitely
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Step 4 Acquire a Background Spectrum, Part 2 In the OMNIC software on the computer, click on the second button in from the left (ColBkg).
Step 5 The Background Spectrum When the 32 scans are done (in the bottom- left of the screen), the spectrum will appear as well as a message window, click NO in the response.
Step 6 Loading your Sample, Part1 Screw the black knob COUNTER CLOCKWISE so that the metal tip ascends and is no longer in contact with the shiny metal plate. Swing the arm to the right to leave room for you to load your sample
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Step 7 Loading your Sample, Part 2 With a spatula, place a small amount of your sample in the middle of the metal plate on top of the diamond chip.
Step 8 Loading your Sample, Part 3 Swing the arm back over top of the sample and turn the knob CLOCKWISE so that the metal tip squashes your sample into the diamond groove.
Step 9 Collecting the Sample IR Spectrum Click on the third button in from the left (ColSmp).
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In the pop-up window, click OK to scan your sample You can monitor the progress of the process by looking at the 32 scan bar in the bottom- left of the screen
Step 10 The IR Spectrum of your Sample! When the scans are all done, a window will appear on the screen. Type in your name, the sample name, and the date then click OK.
In the next pop-up, click YES.
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Step 11 Annotation of Peaks Click on the button with the green arrows to pick peaks (FindPks). The programs will auto- label any major peaks BELOW the black horizontal line (can be moved by clicking on the spectrum).
Step 12 Print your Spectrum and Clean up Click on the printer icon to print. Finally, wipe the metal tip and the metal plate with a clean and dry Kim wipe. Dispose of all trash in the proper container.
Conclusion Congratulations! You got your IR spectrum. Hopefully, you are able to prove the identity of your final product; otherwise, you will have to redo your whole experiment. Final note, have one of the attending TA sign your printed spectrum.
Synthesis of Ketobemidone Precursors Via Phase-Transfer Catalysis - T Cammack, PC Reeves - J Het Chem, 1986, 23 (1), 73-75 - DOI 10.1002/jhet.5570230115