To make a KBr disc, follow these steps:
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Preparation of KBr Mixture: Start by mixing KBr powder with the sample. The typical ratio is 1 part sample to 100 parts KBr. Ensure the mixture is well-blended, either by using a mortar and pestle or a grinding mill. Over-grinding should be avoided as it increases moisture absorption. The amount of KBr required depends on the disc size; for a ½ inch (12.7 mm) diameter disc, about 200-250 mg of KBr is sufficient.
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Use of Pellet Press: Place the pellet press die sleeve onto the base plate and add the mixed KBr and sample. Place the plunger on top. It's crucial to ensure that all components (anvils, die set, and powder) are at the same temperature to prevent the formation of a cloudy pellet. Heating the anvils and the die set before use can help in maintaining a dry environment.
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Compression: Compress the mixture using a hydraulic press. The uniform force will produce a solid, transparent pellet suitable for infrared spectroscopy. The clarity of the disc depends on the quantity and type of sample used. For a 13mm diameter die, using 200-300 mg of KBr and 1 mg of sample with a load of 8 tons is a good starting point.
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Post-Preparation Care: After making the KBr disc, ensure that the equipment is thoroughly cleaned to prevent contamination of future samples. This includes cleaning the anvils and die set with appropriate solvents and polishing the surfaces to ensure clarity and absence of scratches.
By following these detailed steps, you can effectively prepare a KBr disc for use in infrared spectroscopy, ensuring accurate and clear spectral readings.
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