Fire Assay
FA Fusion
The appropriate amount of a sample is weighed on an analytical balance, mixed
with lead collection flux to a homogeneous state (uniform colour) and loaded
into a fusion furnace at 1150°C for 50 minutes. The reducing conditions will
convert litharge(lead oxide) to metallic lead that will form a lead and three of the
PGMs(Pt, Pd, Rh) and Au complex.
Cupellation
The lead button, after being hammered into a form of a cube, is loaded into a
cupellation furnace at 1 000°C for an hour. The lead will be absorbed by the
cupel and some is oxidized because of the presence of atmospheric oxygen in the
furnace. When the cupellation is complete the PGMs & Au and Ag (added as
silver nitrate) prill will be left on a hollow surface of the cupel.
Total Au
Fusion and Cupellation stages are as described above. After the cupellation
stage, the silver, PGMs and Au prill, is flattened and transferred into a parting
porcelain crucible, 30% HNO3 added to remove silver, dried and analyzed by
weighing on the analytical balance and a simple calculation done to determine
the PGM concentrations. The detection limit is 0.08 g/t.
PGM+Au
Fusion and Cupellation stages are as described above. After the cupellation
stage, the silver, PGMs and Au is transferred into a multi-hole cupel and loaded
into a higher temperature furnace for 1,5 hours. It is then removed, left to cool
and weighed on the analytical balance and a simple calculation done to
determine the PGM concentrations. The detection limit is 0.28 g/t.
3E
The prill is transferred into a SOmI beaker and dissolved with aqua-regia on a
hotplate. When the dissolution is complete, the solution is transferred into a
25m volumetric flask containing an appropriate amount of HCI and internal
standard,, made up to volume with de-ionized water and assayed on the ICP-
OES or ICP-MS, depending on the grade and required detection levels.
4E
The PGMs and Au held by the silver prill is transferred by the forceps into a
borosilicate glass tube and aqua regia added. The tube is then sealed and
transferred into a metal housing and placed into a dissolution oven. The tube
with aqua regia solution and PGMs and Au will be left to dissolve in an oven at
220°C for eight (8) hours. The tube is popped and the solution of PGM and Au
transferred into a volumetric flask, internal standard added, made up to volume
and assayed on the ICP-OES or ICP-MS, depending on the grade and required
detection levels.
6EThe fusion stage is as described above except the type of flux at 1020°C. The
Nis button is crushed to fine pieces on the hydraulic press and transferred into a
600ml beaker containing an appropriate amount of reagents, e.g. HCI. The
dissolution is carried out on a steam bath for about 16 hours under the fume
cupboard to ensure complete dissolution of the PGM’s. The next step is to
carefully filter the solution through a Buchner funnel under vacuum, through a
0.45 microns Durapore membrane filter. The PGM’s which remain on the filter
paper are dissolved by gently heating the residue in acid on a hot plate. The
solution is then transferred into a 2Sml volumetric flask with the correct ratio of
acid and internal standard, made up to volume and assayed on the ICP-OES or
ICP-MS, depending on the grade and desired detection levels.