To perform a KBr pellet procedure, follow these detailed steps:
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Preparation of Materials: Start by ensuring all materials are at the same temperature. Heat the anvils and the body of the die set to make them as dry as possible. Use dry KBr powder, and ensure that both the anvils, the die set, and the powder are all at the same temperature. This helps in preventing the formation of cloudy wet pellets.
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Mixing the Sample: For a 13mm diameter die, mix approximately 0.1 to 1.0% of the sample with 200 to 250 mg of fine KBr powder. Thoroughly blend the sample with the KBr powder using a mortar and pestle or a grinding mill. This step is crucial for the clarity of the final pellet.
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Pulverization and Drying: Pulverize the mixture to a maximum of 200 mesh and then dry it at approximately 110°C for two to three hours. Be cautious with the drying process to avoid oxidizing the KBr powder to KBrO3, which can cause a brown discoloration.
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Formation of Pellets: Place the dried and pulverized mixture into a pellet-forming die. Apply a force of approximately 8 tons under a vacuum of several mm Hg for several minutes to form transparent pellets. This step involves degassing to eliminate air and moisture from the KBr powder, which is essential for the integrity and clarity of the pellets.
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Analysis and Storage: After forming the pellets, place the collar in a V-shaped sample holder that fits standard 2 × 3 in. slide mounts of any spectrometer for analysis. Post-analysis, the pellet can be rinsed out of the collar with water or ejected and saved for further use.
Throughout the process, maintaining the dryness of the KBr powder and ensuring uniform temperature across all components are critical for the success of the KBr pellet preparation. This method allows for the accurate analysis of samples through infrared spectroscopy by creating a clear and stable pellet.
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