Quality of PGE Fire Assays Using Spark Analysis on Lead Buttons

Traditional fire assay dates back over 3000 years and has changed very little over that time. The only improvement is to replace the gravimetric finish with dissolution of the Precious Metal bead followed by AA or ICP analysis of the solution. The newly developed FIP A (Fast In-line Fire Assay) method allows full automation of the fire assay process from sample preparation to spark analysis of the Pb button. This results in fully quantitative analyses for Pt, Pd, Rh, Ru, lr, Au and Ag in typically less than an hour after a sample is entered into the system. Detection limits are theoretically Pt 0.08 ppm, Pd 0.002 ppm, Rh 0.002 ppm, Au 0.08 ppm and Ag 0.002 ppm but in practice the lower measurable limits are about double these figures. Few opportunities have been available to present data obtained using the FIFA system as all FIFA laboratories have been in the domain of a Pt mining company which prefers to keep all Pt analytical matters confidential. However, IMP has recently participated in the round robin exercise to establish recommended values for a new series of Merensky Reef and UO-2 Layer reference materials produced by African Mineral Standards. The precision of the results was excellent being on average Pt 2.05%, Pd 1.25%, Rh 4.08% and Ru 4.94% being expressed as Relative Standard Deviation. The excellent precision is a reflection of the efficient collection of POEs in the Pb buttons and the homogeneity of the Pb buttons. However, the accuracy was not as good. The poorer accuracy is interpreted as the calibration of the spectrometer not being as good as desired due to the difficulty in acquiring a suitable range of standards with reliable recommended values for the PGEs. The most recent spectrometer was calibrated with the greatest care and produced slightly better results for Pt, Pd and Rh and slightly worse for Ru.