Fundamentals of Fire Assay

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Fundamentals of Fire Assay
Presentation · November 2020
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FUNDAMENTALS OF FIRE
ASSAY
By
Dr. Corby G. Anderson

Kroll Institute for Extractive Metallurgy
FIRE ASSAY COURSE
On Line Fire Assay Course
Montana Tech
December 3 & 4, 2020
Drop me an e mail
cganders@mines.edu
FIRE ASSAY
The beginnings of fire assaying and analysis can
be traced to the finds in Troy II (about 2600
B.C.) and in the Cappadocian Tablets (2250 -
1950 B.C.).
These finds prove that very pure silver was

made in the twenty-fifth century B.C.

Fundamentals of Fire Assay Lecture
FIRE ASSAY
From this evidence we must conclude that the
cupellation process, and therefore fire assaying,
was invented in Asia Minor in the first half of the
third millennium B.C. shortly after the discovery
of the manufacture of lead from galena (Forbes,
1950).

FIRE ASSAY
"From Jeremiah
"The bellows blow fiercely, but the lead comes
whole from the fire. It's useless to go on refining,
the wicked are not removed."
Zechariah states:
“ And I will bring the third part through the fire, and
will refine them as silver is refined, and will try
them as gold is tried:

FIRE ASSAY
With the fall of the Roman Empire by the invasions
and conquests of the barbarian hordes, intellectual
life stagnated for about 500 years.
With the revival of learning in the latter centuries of

the Middle Ages, the art of fire assaying was
renewed vigorously.

FIRE ASSAY
One man stands out above all in this period -
Agricola (1494-1555).
In about 1529 he began to write "De Re Metallica"

(1556), which he completed in 1550 but did not
send to the publishers until 1553.
Preparation of the woodcuts delayed publication

until a year after the death of Agricola.

De Re Metallica
Georgius Agricola (24 March 1494 – 21 November 1555) was a German

scholar and scientist. Known as "the father of mineralogy", he was born at
Glauchau in Saxony. His real name was Georg Pawer; Agricola is the
Latinised version of his name, Pawer/(Bauer) meaning farmer. He is best
known for his book De Re Metallica.

De Re Metallica

De Re Metallica Woodcuts

FIRE ASSAY AUTHORS
• “De La Pirotechnia”, 1540 Vannoccio
Biringuccio
• “De Re Metallica”, 1556 Georgius Agricola
• “Treatise on Ores and Assaying”, 1574
Lazarus Ercker

MODERN FIRE ASSAY
AUTHORS
• ‘The Metallurgy of Gold’, 1906, T.K. Rose
• A Manual of Practical Assaying’, 1908, Furman
and Pardoe
• ‘Modern Assaying’, 1910, J.R Smith
• ‘A Textbook of Assaying’, 1910, C. and J.
Beringer
• “Textbook of Fire Assaying’, 1915, E.E. Bugbee

MODERN FIRE ASSAY
AUTHORS
• ‘A Manual of Fire Assaying’, 1929, C. H. Fulton
• ‘Fire Assaying’, 1940, O. Shepard and W.
Dietrich
• The Sampling and Assay of the Precious Metals,
1947, E. A.Smith
• Assay and Analytical Practice in the South
African Mining Industry, 1986, W. Lenahan and
R. Murray-Smith
• Recovery and Refining of Precious Metals,
1997, C. W. Ammen
FIRE ASSAY
• In summation, the use of lead oxide for
fire assay and analysis dates back to the
finds in Troy II and the Cappadocian
Tablets about 3000 B.C.
• Now used for Au, Ag, and PGM’s
• Historically used for Pb, Cu, Bi, Sn, Sb, Hg
and Fe.

De Re Metallica
written in 1556 by Agricola
• “It is necessary that the assayer who is
testing ore or metals should be prepared
and instructed in all things necessary in
assaying, and that he should close the
doors of the room in which the assay
furnace stands, lest anyone coming at an
inopportune moment might disturb his
thoughts when they are intent on work.”

FIRE ASSAY ANALOGY
• Pyrometallurgical lead smelting.
• Controlled or incomplete reduction.

FIRE ASSAY ANALOGY
• Pyrometallurgical solvent extraction.
• Utilizes ‘selective extractant’ for Au, Ag or
PGM’s.
• Requires proper ‘lixiviant’ slag.
• The ‘selective extractant’ is ‘strippable’
producing a pure, concentrated precious
metal.

GENERAL FIRE ASSAY
METHODOLOGY
• Accurate and representative, well
characterized sample.
• Determine reducing or oxidizing power of
material.
• Appropriate precious metals collector.
• Correct slag and fusion formulation.
• Correct lab skills.

FUNDAMENTAL CHEMISTRY
OF FIRE ASSAY
Fusion
12PbO + C6H10O5  12Pb + 5 H2O + 6CO2
162 2,486
Cupellation
Pb + ½ O2 PbO

BASIC OPERATIONS OF
FUSION

CRUCIBLE FUSION SAMPLES

BASIC OPERATIONS OF
FUSION

FUSION

FUSION LAYERS
Lead Button
Boundary
Slag

CUPELLATION
• Oxidizing the lead button from fusion back
to litharge.
Pb + ½ O2  PbO
• Cupel, either magnesia or ‘bone ash’
absorbs litharge and base metals.
• Precious metals are left in a dore ‘bead’.

CUPELLATION

CUPELLATION

CUPELLATION

DORE BEADS

THE BEAD SILVER PARTING
PROCESS
• Used to separate silver from gold in final
bead.
• Must have 3 to 1 ratio of silver to gold.
‘Inquartation’ with silver used to ensure
this ratio. (Herman inquarts/AgNO3)
• Use 1 part nitric acid and 7 parts water.
• Heat flattened/rolled bead in nitric acid
solution.

PROCESS
• Weigh the cupelled bead and then flatten or roll
it.
• Use chloride free nitric acid one part to seven
parts distilled water.
• Heat solution to hot but not boiling in a porcelain
parting cup.
• After silver is dissolved, wash the gold sponge
several times using a swirling action.

PROCESS
• Dry the gold sponge by heating it to a red
heat to anneal it.
• Weigh the gold.
• The gold sponge weight subtracted from
the original bead weight is the silver
content.

FIRE ASSAY
• In summation, the use of lead oxide for
fire assay and analysis dates back to the
finds in Troy II and the Cappadocian
Tablets about 3000 B.C.
• Now used for Au, Ag, and PGM’s
• Historically used for Pb, Cu, Bi, Sn, Sb, Hg
and Fe.

De Re Metallica
written in 1556 by Agricola
• “It is necessary that the assayer who is
testing ore or metals should be prepared
and instructed in all things necessary in
assaying, and that he should close the
doors of the room in which the assay
furnace stands, lest anyone coming at an
inopportune moment might disturb his
thoughts when they are intent on work.”

FIRE ASSAY COURSE
On Line Fire Assay Course
Montana Tech
December 3 & 4, 2020
Drop me an e mail
cganders@mines.edu
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ASSAY
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Kroll Institute for Extractive Metallurgy

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See discussions, stats, and author profiles for this publication at: https://www.researchgate.

Fundamentals of Fire Assay

Presentation · November 2020

Alkaline Digestion of Monazite and Xenotime View project

The user has requested enhancement of the downloaded file.

Dr. Corby G. Anderson

These finds prove that very pure silver was

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

With the revival of learning in the latter centuries of

Dr. Corby G. Anderson

In about 1529 he began to write "De Re Metallica"

Preparation of the woodcuts delayed publication

Dr. Corby G. Anderson

Georgius Agricola (24 March 1494 – 21 November 1555) was a German

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

Dr. Corby G. Anderson

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