To prepare samples for FTIR analysis, the following steps are typically followed:
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Sample Grinding and Mixing: The sample, usually a powder, is ground with an excess of potassium bromide (KBr) in a 1:100 ratio. This grinding ensures a homogeneous mixture and helps in the formation of a transparent pellet that is suitable for infrared light transmission.
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Pellet Formation: The mixture is then compressed using a hydraulic press in a die chamber. The die, typically with a 13 mm internal diameter but also available in other sizes like 5 mm, 10 mm, and 20 mm, is used to shape the mixture into a solid pellet. The compression process is crucial as it forms a pellet that is primarily transparent to infrared light, allowing for effective analysis.
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Optional Support and Binding: For samples that may not compact easily, a sample support cup made of thin flexible aluminum can be used. This cup is placed inside the die before loading the sample. It supports the sample from the bottom and sides, leaving only the top surface exposed for analysis. Additionally, wax binding additives can be used to help the powder grains adhere to one another, improving the pellet's integrity.
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Cleaning and Preparation of Tools: Before and after the process, it is essential to clean the die set, pestle, and mortar thoroughly with solvents and deionized water, then dry them in a warm oven. This ensures that no contaminants interfere with the sample's analysis.
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Sample Mounting and Analysis: Once the pellet is formed, it is mounted in the path of the IR beam for analysis. The FTIR instrument then uses infrared light to study the properties of the sample, identifying chemical bonds and their vibrations based on the interference pattern created by the light passing through the sample.
This detailed preparation ensures that the sample is suitable for FTIR analysis, providing accurate and reliable data on the molecular structure and composition of the material.
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