Precautions that should be taken during IR spectroscopy include:
1. Avoid crushing the potassium bromide (KBr) to a very fine powder as it can absorb moisture from the environment due to its hygroscopic nature. This can result in the formation of bands in certain IR regions, which can interfere with the analysis.
2. When preparing solid samples, it is important to use salts like NaCl or KBr that are transparent to IR radiation. These salts are commonly used as matrices for mixing the sample.
3. When using the mull technique for preparing solid samples, avoid touching the faces of the salt plates. Touching the plates can introduce contaminants and affect the quality of the spectrum.
4. Be cautious when using solvents for sample preparation, as solvents containing water can dissolve the KBr plates or cause them to fog up. This can obscure important bands in the spectrum. It is recommended to either place a small amount of the compound directly on the plates and add a drop of solvent, or dissolve the compound in a separate test tube and transfer the solution onto the IR plates.
5. Clean the KBr plates thoroughly after each sample preparation to prevent contamination of future samples. Wipe the windows with a tissue, then wash them several times with the appropriate solvent, followed by ethanol. Use a polishing kit to ensure the window surface is clear and free from scratches.
6. When using a laboratory hydraulic press to create KBr pellets, follow the recommended conditions for sample preparation. These conditions include a 100:1 ratio of KBr to sample by weight, a pellet die of 13 mm, and a pressing load of 10 tons. For FTIR applications, 7 mm pellets can be prepared with as little as 2 tons of pressing load.
By following these precautions, one can ensure accurate and reliable results in IR spectroscopy.
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