When preparing a sample for FTIR analysis, the ratio of KBr to drug substance is typically 100:1 by weight.
This method involves dispersing the powdered sample in potassium bromide (KBr) and pressing it into a disc.
1. Sample Preparation Technique
The process begins by mixing the drug substance with KBr.
The drug substance is added at a ratio of 1 to 2 percent of the total KBr used.
This means that for every 100 parts of KBr, only 1 to 2 parts of the drug substance are added.
This high dilution ensures that the sample is transparent to infrared light, which is crucial for accurate FTIR analysis.
2. Importance of the Ratio
The 100:1 ratio is chosen to minimize the influence of the drug substance on the FTIR spectrum while ensuring that the sample is detectable.
This dilution helps in reducing scattering losses and absorption band distortions, which are common issues when analyzing solid samples.
The use of KBr as a matrix also helps in maintaining a stable environment for the sample, as KBr is hygroscopic and can absorb moisture, which might otherwise interfere with the FTIR measurements.
3. Procedure Details
After mixing the drug substance with KBr, the mixture is ground to a fine powder.
This step is crucial as it ensures that the sample is uniformly dispersed within the KBr matrix.
The finely ground mixture is then pressed into a disc using a hydraulic press under specific conditions (e.g., 10 ton pressing load for a 13 mm pellet die).
The resulting pellet is then used for FTIR analysis.
4. Environmental Considerations
Since KBr is hygroscopic, it is important to handle the mixture quickly and possibly in a controlled environment such as a glovebox or with a vacuum die to prevent absorption of moisture from the air, which could affect the FTIR measurements.
In summary, the 100:1 KBr to drug substance ratio is a standard method used in FTIR analysis to prepare samples for accurate and reliable spectral readings.
This method ensures that the sample is sufficiently diluted to allow for clear transmission of infrared light while maintaining the integrity of the sample's spectral properties.
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