Making KBr pellets is a crucial step in various analytical applications, especially in spectroscopy.
Here’s a detailed guide to help you prepare clear and effective KBr pellets.
How do you make KBr pellets? 4 Essential Steps to Clear and Effective Pellets
1. Preparation of Equipment and Materials
Heat the Anvils and Die Set: Before making the pellet, ensure that the anvils and the body of the die set are heated. This helps in keeping them as dry as possible, which is crucial for the clarity of the final pellet.
Use Dry KBr Powder: It is essential to use dry KBr powder. If the powder is not dry, it can lead to cloudy pellets. Heating the KBr powder in a dry environment or grinding fresh powder from KBr cuttings can help maintain dryness.
Temperature Consistency: Ensure that the anvils, die set, and powder are all at the same temperature. A mismatch in temperature can result in a wet, cloudy pellet.
2. KBr Pellet Technique
Mixing and Loading: Mix the sample with KBr powder in the appropriate ratio (typically 0.2 to 1 percent sample). The mixture should be well-mixed to prevent moisture absorption.
Pressing the Pellet:
- Pour the KBr powder/sample matrix into the hole in the stainless steel (SS) collar with one anvil inserted.
- Insert the second anvil and place the assembly in the press handle.
- Apply pressure by squeezing the handle. The recommended pressure for a 13 mm diameter pellet is about 10 tonnes.
Removal and Analysis:
- Remove the anvils from the collar, leaving the KBr pellet inside.
- Place the collar in a V-shaped sample holder compatible with the spectrometer.
- After analysis, remove the pellet from the collar either by rinsing with water or ejecting it.
3. Special Considerations for Different Analyses
FT-IR Analysis: Ensure the KBr and sample are well-mixed without excess moisture. A standard pressure of 10 tonnes is typically sufficient.
XRF Analysis: Use larger pellet diameters (32 mm or 40 mm) to accommodate the X-ray beam.
4. Preparation of KBr Powder
Pulverization and Drying: Pulverize the KBr powder to a maximum of 200 mesh and dry it at about 110°C for two to three hours. Rapid heating can oxidize KBr to KBrO3, causing discoloration.
Storage: After drying, store the powder in a desiccator to maintain its dryness.
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By adhering to these detailed steps and precautions, you can successfully prepare clear and effective KBr pellets for various analytical applications.
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