When it comes to micro XRF, the sample size is crucial for accurate and representative analysis. Typically, samples are prepared in the form of pressed pellets with diameters of either 32 mm or 40 mm. This size is preferred to ensure a large enough sample surface area for precise analysis.
4 Key Steps to Perfect Preparation
1. Grinding the Sample
The first step in preparing a solid sample for micro XRF analysis is grinding. This process is essential to achieve a homogeneous mixture of the sample. Ensuring that the analysis results reflect the characteristics of the entire sample rather than individual grains is crucial. The optimal grain size after grinding should be less than 75 µm. This helps in creating a flat, even surface without voids between the grains when the powder is poured into the cuvette.
2. Forming Pressed Pellets
After grinding, the powder is poured into a cuvette and pressed into pellets using specific dies. The standard sizes for these pellets are 32 mm or 40 mm in diameter. These sizes are chosen to accommodate the requirements of the XRF spectrometers, which are designed to analyze samples of these dimensions. The pressing process is critical as it ensures that the sample is compacted uniformly, minimizing any potential errors in the analysis due to uneven distribution of elements within the sample.
3. Automated vs. Manual Pellet Ejection
For laboratories requiring high sample throughput, automated systems like the APEX 400 press are used. These systems automate the pellet ejection step, which is typically a manual process in standard XRF dies. This automation not only increases efficiency but also reduces the potential for human error in the sample preparation process.
4. Analysis of Liquid Samples
Unlike solid samples, liquid samples can be directly analyzed using XRF without the need for pressing into pellets. This is because the XRF method is not sensitive to the state of aggregation, allowing for direct measurement of liquid samples.
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The importance of sample preparation cannot be overstated. The references highlight that sample preparation is now the most significant source of error in XRF analysis. Therefore, employing high-quality sample preparation techniques is essential for achieving consistent and reliable analytical results. This underscores the importance of understanding and adhering to the specific sample preparation requirements of the XRF spectrometer being used.
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