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Kalassay Group
Perth - Kalgoorlie - Leonora

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Kalassay Fire Assay

Traditional
and

Fully Robotic!

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Fire Assay
The particular fire assay method we are
discussing here is aimed only at
measuring
Gold and Precious Metals
Variations of Fire Assay can be used for
other metals, however, in most
instances other analytical methods are
favoured

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Fire Assay
- Background
Many methods have been developed and refined over the years,
but Fire Assay remains a favoured method for determining the total gold
content of a sample.
In this method, a pulverised mineral sample is dissolved using heat and fluxing
agents
Precious metals are extracted from the melted material using molten Lead.
The precious metals are then separated from the Lead in a secondary process
called cupellation.

The gold content of the precious metals collected is then determined, using a
variety of analytical techniques.

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Fire Assay
- History
The beginnings of Fire Assay can be traced to finds in Troy II (2600B.C.) where
very pure silver was being produced by cupellation
Biblical references to the use of fire assay techniques can be traced back to the
prophet Moses 31:22,23 (approx 1300B.C.)
2000 years ago, the Romans used an amalgamation and heat process for Gold
recovery
In the middle ages, Agricola wrote De Re Metallica(1550) - the first and foremost
textbook on fire assaying
From that time, fire assay has been used and further refined as an analytical
method
Source: US Geological Survey Bulletin 1445

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Fire Assay Today

Fire Assay is essentially used as a technique for extracting the

gold from a geological sample

The gold is then put into solution, using chemical and heat
digestion methods

Very sensitive, high-tech analytical equipment, is then used to

determine the level of gold in the solution

The amount of gold in the solution is then back-calculated, to

indicate the amount present in the original sample

So ancient technology, centuries of refinement and

modern instrumentation combine to give us a very
powerful analytical tool

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Fire Assay
- Applications

Pictures courtesy Barra Resources

Soil Samples
Exploration Drill Samples
- RAB
- RC
- Diamond Core
Grade Control
Mill Solutions
Tailings

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Traditional Fire Assay Method

(After Sample Preparation)

Sub-sampling & Catch-weigh

Fluxing
Firing
Cooling & Separation
Cupellation
Parting & Dissolution
Analysis

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Fire Assay
- Fluxing
A measured sub-sample (the sample charge) is taken from the
pulverised sample
The charge is mixed with a measured amount of specialised flux,
which contains many components including Lead and Silver.
The flux components are varied to suit the composition of the sample
being treated. This is done to ensure that a successful fusion is
achieved.
The charge and the flux are thoroughly combined by mechanical
agitation
Blanks, repeat samples and standards are introduced into the batch at
this stage

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Fire Assay
- Firing

The flux/charge mixture is loaded into a fire

assay crucible (referred to as a pot), ready
for firing

The pots are loaded into a reducing furnace

and are subjected to a temperature of
1100 C for approximately 50 minutes

This allows the flux and mineral sample to

fuse and form a melt

If a fusion fails in some way, the

assayer must diagnose the problem
and vary the method to overcome the
problem
this demands great skill

During this process, the Lead, Silver and

Gold present in the melt combine

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Fire Assay
- Cooling

The melt is poured out of the pot into

a mould

The Lead / Gold alloy settles to the

bottom of the mould and solidifies as
a metal button as the mass cools

The lighter fractions (i.e. Silica)

solidify on top of this button as a
glassy layer

The solidified mass is removed from

the mould, exposing the button

The button is recovered and the

glassy slag is sent to waste

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Fire Assay
- Cupellation

The Lead/Gold alloy button is placed on a small cup-shaped

receptacle called a Cupel

The Cupel is loaded into a small oxidising furnace and subjected to

1000 C for approximately 50 minutes

During this time the Lead is absorbed into the cupel, leaving behind a
small ball-shaped particle called a Dore Bead

This bead is made up of Silver and precious metals including Gold

Lead Button in
fresh Cupel
awaiting firing

Hot Cupels
removed
from
furnace

Cupel after
firing
showing
Dore Bead

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Fire Assay Digestion

The Dore Bead is put into a test tube and the

Silver is parted from the bead using Nitric
Acid. The Silver is then held in solution.

Hydrochloric Acid is added to solution, forming

Aqua Regia This very powerful acid mixture
dissolves the Gold into solution

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Fire Assay
Instrumental Analysis - AAS

Acid digest solution is subjected to AAS analysis

Level of Gold determined by measurement of

atomic absorption in the Gold wavelength

Detection level Gold by Fire Assay / AAS method

= 0.01ppm

Results captured and collated on LIMS

Results analysed by use of QA/QC controls:

Duplicates
Blanks
Standards

for
for
for

Authorised data sent to client

Reproducibility
Contamination
Bias

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Fire Assay
Instrumental Analysis ICP-OES

Acid digest solution is diluted by computercontrolled dilutors and then subjected to analysis
by ICP-OES instruments

ICP-OES has the advantage of being able to

analyse
Gold and other elements such as PGEs in one
reading

Results compared to known and verified

standards

Results captured and collated on LIMS

Detection level Gold by Fire Assay / ICP-OES

method = 0.01ppm

Lower detection limits, down to sub-ppb

available by other methods / instruments

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Fire Assay

Low - Level Gold

Agilent 7500 ICP-MS

at Kalassays
Perth Assay Laboratory

Fire assay is also a very useful technique for ppb-level

analysis. Fire assay allows us to produce very good
values for Gold and PGEs

The process followed is the same as standard fire assay,

but after the bead digest stage, the solution is subjected
to analysis by Inductively Coupled Plasma Mass
Spectometry (ICP-MS)

ICP-MS is a very sensitive, very sophisticated instrument.

Three of the latest generation of these instruments are
located in the Perth Assay Laboratory.

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Robotic Fire Assay

Kalassay is investing heavily in automated systems

for Sample Preparation and Analysis.
The Fully Robotic Integrated Sample Preparation and Fire Assay System in
Kalgoorlie is a prime example.
This system takes a
4kg sample and
through a series of
processes first
produces a pulped
sample and then a
fire assay result
without human
physical
involvement!

Robotics offer superb consistency and maximum control over all aspects of the entire
process from sample preparation to final analytical result.

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Robotic Fire Assay 2

This first of Kalassays robotic systems is a fully robotic

integrated Sample Preparation and Fire Assay Facility, at
the Kalgoorlie Assay Laboratory
This system will be capable of taking a large, coarse
sample and taking it through all stages of preparation and
analysis to the production of final results without being
touched by human hands
Robots are used to transport the sample from one
automated stage to another
The whole process is controlled and monitored by highly
sophisticated computer systems under the control of highly
experienced, qualified analysts.
All standard Kalassay Q.A./Q.C. protocols are incorporated
into the process

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Results Reporting

Results captured and collated on LIMS

Results analysed by routine utilisation of control samples:
Duplicates
for
Reproducibility
Blanks
for
Contamination
Standards
for
Bias
Authorised data sent to client Results of analytical work are normally
reported by e-mail to a list of recipients authorised by the client
Various report formats are available, but the overwhelming favourite is .csv
as this is readily imported into most databases
Our Laboratory Information System (LIMS) is able to publish QA / QC data
at the same time as the job results, allowing real-time data verification.
Results are also available in hard copy on request

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Customer Focus

The Kalassay Group operates solely within the mining industry, offering
analytical services to mining exploration companies from all over the world

Our future is inextricably connected to the mining industry and we participate

in many industry organisations and initiatives

Our aim is to meet and exceed our clients expectations at all times

We tailor our service to match client needs

We are always looking for ways to extend and improve our services

Got a challenge?
Got a problem?

Come to us!
Come to us!

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on the web!
On-line Sample Submission
Analytical Batch Information
Useful Industry Links
and The Latest Kalassay News !

www.assay.com.au

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.at your service !

Perth

Kalgoorlie

Leonora

Assay Laboratory

Assay Laboratory

Assay Laboratory

Tony White

Kevin Bride

Wayne Turner

Ph: (08) 9250 6122

Ph: (08) 9091 7227

Ph: (08) 9037 6160

Fx: (08) 9250 6133

Fx: (08) 9091 7228

Fx: (08) 9037 6270

Em: perth@assay.com.au

Em: kalgoorlie@assay.com.au

Em: leonora@assay.com.au

www.assay.com.au