To prepare KBr pellets for FTIR analysis, the process involves mixing a small amount of the sample with KBr powder, pressing it into a pellet, and ensuring it is transparent for accurate spectral readings. The typical ratio of KBr to sample is 100:1, and the pellet size should match the specifications of the FTIR equipment, typically ranging from 3 mm to 13 mm in diameter.
Detailed Steps:
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Preparation of KBr Powder:
- Begin by pulverizing KBr powder to a maximum of 200 mesh.
- Dry the pulverized KBr at approximately 110°C for two to three hours to remove moisture. Rapid heating should be avoided to prevent oxidation of KBr to KBrO3, which can cause discoloration.
- After drying, store the KBr powder in a desiccator to maintain its dryness.
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Mixing the Sample with KBr:
- Mix the sample with the KBr powder at a ratio of 100:1 by weight. For FTIR analysis, only a small amount of sample (0.1 to 1.0%) is needed.
- Ensure the mixture is well-mixed and finely pulverized to ensure homogeneity and transparency of the final pellet.
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Forming the Pellet:
- Place the mixture into a pellet-forming die of the appropriate diameter (typically 13 mm for standard FTIR applications).
- Apply a pressing load of approximately 8 tons under a vacuum of several mm Hg for several minutes. This step is crucial to form a transparent pellet and to eliminate air and moisture that could affect the pellet's integrity and the quality of the FTIR spectrum.
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Equipment Needed:
- A pellet press die set that matches the diameter required by the FTIR equipment.
- A pestle and mortar, preferably made of agate for its smooth surface and minimal contamination.
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Final Steps:
- After pressing, the pellet should be transparent, indicating that it is suitable for FTIR analysis.
- The pellet should be handled carefully to avoid breaking, as it needs to be transparent to allow IR radiation to pass through for accurate spectral analysis.
This method ensures that the sample is properly prepared for FTIR analysis, allowing for precise and accurate readings of the sample's infrared spectrum.
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