Preparing KBr pellets for FTIR analysis is a crucial step to ensure accurate spectral readings. This process involves mixing a small amount of the sample with KBr powder, pressing it into a pellet, and ensuring it is transparent for precise analysis. 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.
5 Steps to Perfect KBr Pellets for FTIR Analysis
1. 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.
2. 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.
3. 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.
4. 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.
5. 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.
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