BS ISO 13605:2018 pdf free.Solid mineral fuels – Major and minor elements in coal ash and coke ash – Wavelength dispersive x-ray fluorescence spectrometric method.
Discs may be prepared by the casting or press-quenching technique. Both methods will produce glass discs of adequate quality. If the casting technique is used, the sample may be fused with the flux in a crucible and then poured into a separate mould; if an appropriately shaped crucible is used, the fusion may be carried out and the glass allowed to cool in the same crucible.
A conventional electric furnace, high-frequency furnace, or gas burner may be used for heating.
Disc-making machines are available commercially, and these may be used to fuse and cast the discs.
Prior to measurement, discs shall be inspected visually, paying particular attention to the analytical surface. The discs shall not contain undissolved material, and shall be whole and free from crystallization and bubbles. Defective discs shall be re-fused or discarded and substitute discs prepared.
Laboratory-prepared ashes for XRF analysis should be freshly prepared; if not, It will be necessary to reheat these to the ashing temperature and hold for 15 mm at this temperature prior to preparation of the XRF disc.
Fluxes are in general hygroscopic and hence shall be dried prior to use, or a loss on fusion (LOF) determination shall be carried out and the mass of flux used corrected to an anhydrous basis. Since it is difficult to maintain flux in an anhydrous state, it is recommended that, for work requiring high accuracy, the latter practice be adopted.
It may be necessary to determine the LOF for boiler ash samples. This is done by allowing the fused material to cool (in a covered crucible) prior to pouring into the mould and reweighing the cooled crucible and fused contents. LOF is equal to the mass of the crucible and its contents prior to fusion minus the mass of the crucible and its contents after fusion. After weighing, the crucible contents is remelted and swirled (to ensure homogeneity). then cast or press-quenched in the normal manner. If loss-eliminated alphas are used, then LOF need not be determined (see Reference [j]).
NOTE Loss of sulfur can occur at the high temperatures (>1 050 °C) used in the preparation of fused discs.
8.5.2 Disc storage
As soon as possible after preparation, the discs shall be transferred to a desiccator so that adsorption of moisture and the possibility of contamination are minimized.
To avoid contamination of the analytical surface, discs shall be handled by their edges. Care shall be exercised to avoid touching the analytical surface with hands or fingers.
8.5.3 Fused disc quality
The quality of disc preparation shall be checked in accordance with Annex C. as follows:
a) prior to each new operator commencing analysis of test samples;
b) by each operator annually.BS ISO 13605 pdf download.
Tags: Solid mineral fuels
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