The precautions to be taken during x‐ray fluorescence (XRF) analysis of samples containing elemental sulphur were investigated. Elemental sulphur under vacuum (vacuum required for S Kα analysis) undergoes sublimation. As a result, the sulphur intensity signal diminishes in direct relation to the time during which the sample has been under vacuum. The work power accelerates the sublimation of sulphur. A method for obtaining real analytical values is proposed. The risk to the XRF spectrometer constituted due to sublimed sulphur are pointed out.
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