Assayers Canada Services Explained
Gold and Precious Metal Analysis by Fire Assay
Fire Assaying, a technique that has been around for centuries, is still the most generally accepted method of analysis for gold, and platinum group elements.
Though a number of variations are available (depending on the size of sample assayed and the method of final reading of the metal concentration), the basic technique in Fire Assaying for gold involves adding flux (which includes lead) and silver to the pulverised sample and fusing (melting) it. The extra silver acts as a collector of the gold, and, in very low-grade samples, ensures that at the end of the fusing there is enough precious metal to be easily handled.
At the end of the fusion process, the resultant molten material is poured into a metal mould
and allowed to cool into a lead button (which contains the precious metals) at the bottom,
overlain by silica glass slag. The slag is chipped off and discarded, and the lead button is
subjected to a second process called cupellation, in which the precious metals are separated
from the lead.
In cupellation the lead button (containing the gold) is placed into a small porous
crucible called a cupel, and heated. The lead then becomes oxidised and is absorbed
into the cupel, leaving a small silver/gold bead remaining in the cupel.
It now remains only to separate the silver from the gold. To do this, the bead is placed in a test tube and nitric acid is added, which, when the test tube is put in a hot water bath, dissolves the silver, leaving a small particle of pure gold.
If the particle of gold is large enough, it is usually weighed to determine the original grade of the sample. This is called a gravimetric finish to the fire assay. For lower grade samples with very small and difficult to handle gold particles the gold is dissolved in hydrochloric acid and the gold concentration is measured using AAS.
While Fire Assaying is normally done on a 1 Assay Tonne (roughly 30 gram) split of the
pulverised material, a slight cost saving is to be found in selecting a smaller (15-gram) sample
size. On the other hand, high-grade samples, for which there must be a gravimetric finish, are
slightly more expensive than those that are read on the AAS.
In the analysis of platinum group elements, roughly the same procedure is followed, but the final element readings are normally done using ICP.