The standard for elemental analysis is X-ray fluorescence (XRF). XRF is a technique that allows for precise analyses with minimal sample preparation. It has become the "gold standard" for elemental composition analysis in many industries. XRF is especially suitable for analyzing solids, powders, slurries, filters, and oils.
XRF is capable of identifying and quantifying the elements present in a bulk material non-destructively. It involves extracting a small sample volume from the uppermost surface layers of the material or taking a fragment of the bulk product and homogenizing it as a fine powder. A benchtop XRF spectrometer is then used to measure the component parts of the sample and develop relative data for the bulk material.
Compared to alternative tools such as optical emission spectrometry (OES) and laser-induced breakdown spectrometry (LIBS), XRF offers more analytical capabilities and does not leave visible marring on workpieces. OES and LIBS can perform elemental analysis of workpieces directly without extensive sample preparation, but they have limited analytical capabilities compared to XRF spectroscopy.
To achieve optimal results with XRF, several pieces of lab equipment are required, including platinum labware, high-performance fusion furnaces, and chemistry-specific molds. This diligent use of lab equipment facilitates the most accurate quantitative and qualitative analysis of samples in a non-destructive manner.
When preparing samples for XRF analysis, pressed pellets are commonly used. These pellets provide better analytical results than loose powders because the grinding and compression create a more homogeneous representation of the sample with no void spaces and little sample dilution. Pressed pellets are excellent for the analysis of elements in the ppm range and are relatively simple and inexpensive to prepare.
In terms of analyzing heavy and light elements, pressed pellets show a higher signal-to-noise ratio compared to loose powders. This allows the lightest elements to be detected easily above the background. Additionally, the absence of thin films in pellets allows the measurement to take place under a vacuum, further improving the detection of light elements.
Particle size is an important factor in producing pellets that provide the best analytical results. The sample should be ground to a particle size of <75µm, with <50µm being ideal. Small particle size ensures that the sample compresses and binds together properly when pressed. Larger or variable particle sizes can lead to heterogeneities in the sample, affecting the accuracy of the analysis.
Overall, XRF with pressed pellets is the standard for elemental analysis due to its non-destructive nature, accurate quantification, and ability to detect both heavy and light elements effectively.
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