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    FireAssayLecture CompatibilityMode

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    Waskito Budiawan
    Fire assaying has been used for thousands of years to extract precious metals like gold and silver from ores. The process involves fusing samples with lead oxide and cupelling the resulting lead button to separate precious metals. Key steps include sampling, crucible fusion, producing a lead button, cupellation, and parting. Historically important references include writings from ancient times that describe biblical references to refining silver and gold, as well as important works like De Re Metallica from the 16th century. Modern fire assay still relies on these same fundamental chemical and metallurgical principles.

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    FireAssayLecture CompatibilityMode

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    Fire assaying has been used for thousands of years to extract precious metals like gold and silver from ores. The process involves fusing samples with lead oxide and cupelling the resulting lead button to separate precious metals. Key steps include sampling, crucible fusion, producing a lead button, cupellation, and parting. Historically important references include writings from ancient times that describe biblical references to refining silver and gold, as well as important works like De Re Metallica from the 16th century. Modern fire assay still relies on these same fundamental chemical and metallurgical principles.

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    Fundamentals of Fire Assay

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    Fire assaying has been used for thousands of years to extract precious metals like gold and silver from ores. The process involves fusing samples with lead oxide and cupelling the resulting lead button to separate precious metals. Key steps include sampling, crucible fusion, producing a lead button, cupellation, and parting. Historically important references include writings from ancient times that describe biblical references to refining silver and gold, as well as important works like De Re Metallica from the 16th century. Modern fire assay still relies on these same fundamental chemical and metallurgical principles.

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    © All Rights Reserved
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    97 views71 pages

    FireAssayLecture CompatibilityMode

    Uploaded by

    Waskito Budiawan
    Fire assaying has been used for thousands of years to extract precious metals like gold and silver from ores. The process involves fusing samples with lead oxide and cupelling the resulting lead button to separate precious metals. Key steps include sampling, crucible fusion, producing a lead button, cupellation, and parting. Historically important references include writings from ancient times that describe biblical references to refining silver and gold, as well as important works like De Re Metallica from the 16th century. Modern fire assay still relies on these same fundamental chemical and metallurgical principles.

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    The text discusses the early history of fire assaying dating back to ancient civilizations in Asia Minor in the 3rd millennium BC. It also outlines some of the key process steps involved in fire assaying such as fusion, cupellation, and parting.

    The text mentions that early evidence of fire assaying has been found dating back to 2600 BC in Troy and 2250-1950 BC in Cappadocian tablets, showing very pure silver was produced. It is believed the cupellation process was invented in Asia Minor around this time after the discovery of producing lead from galena.

    Several biblical references to fire assaying techniques are cited such as references to silver being 'purged' or 'refined' like gold, and references to the 'fining pot' or cupel. Passages from books like Jeremiah, Zechariah and Malachi are discussed.

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

    net/publication/327109200

    Fundamentals of Fire Assay

    Presentation · August 2018


    DOI: 10.13140/RG.2.2.22438.78408

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    Corby Anderson
    Colorado School of Mines
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    FIRE ASSAY FUNDAMENTALS
    Dr. Corby G. Anderson
    Harrison Western Professor
    Metallurgical and Materials Engineering
    Room 270 Hill Hall
    Colorado School of Mines
    E: cganders@mines.edu
    T: 303-273-3580
    INTRODUCTION
    The beginnings of fire assaying 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. 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).
    INTRODUCTION
    The first convincing evidence of the
    production of silver from lead ores is
    the cupel buttons found at
    Mahmatlar in the late third millenium
    B.C. and that are now in the Hittite
    Museum in Ankara, Turkey. Biblical
    references to the use of fire-assay
    techniques can be traced to the
    prophet Moses (about 1300 B.C.)
    INTRODUCTION
    "The promises of Yahweh (God) are
    promises unalloyed, silver purged in
    a crucible, of clay refined seven
    times."

    “ The fining pot [cupel] is for silver


    and the furnace for gold: but the
    Lord trieth the hearts."
    INTRODUCTION
    "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:
    INTRODUCTION
    More reference is made to the "fining
    pot" (cupel) in Malachi;
    "And he shall sit as a refiner and
    purifier of silver: and he shall purify
    the sons of Levi, and purge them as
    gold and silver, that they may offer
    unto the Lord an offering in
    righteousness."
    INTRODUCTION
    These references are but a few that
    demonstrate the extent to which fire-
    assay techniques permeated Asia Minor
    in ancient times. The Romans were able
    to desilver lead down to 0.01 percent or
    even to 0.002 percent in some cases
    and marked their cupelled desilvered
    lead "EX ARG." Roman lead pipe was
    found to be desilvered almost
    completely. In addition to the
    employment of fire-assay techniques
    for refining lead and silver, the Romans
    were the first to make extensive use of
    the amalgamation process.
    INTRODUCTION
    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. 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
    Written in 1556 by Agricola

    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
    Written in 1556 by Agricola
    Woodcuts
    De Re Metallica
    Written in 1556 by Agricola
    Woodcuts
    INTRODUCTION
     In summation, the use of lead oxide
    for the fire assay process 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.
    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
    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 ‘diluent’ 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.


    DISCUSSION
    OF SAMPLING
     A key to a successful fire assay.
     Particulate sampling paper on Blackboard.
     Three key aspects of particulate sampling;
    – 1). Each particle must have an equal
    opportunity to be sampled.
    – 2). The correct amount of representative
    sample related to the top size of the particle
    distribution must be taken.
    – 3). Take as many sub samples as reasonable
    to create the correct amount of required
    representative sample.
    FUNDAMENTAL ASSAY UNITS
     An assay ton (AT) is 29.166 grams.
     There are 14.583 Troy ounces of
    precious metals in one pound.
     In the USA Precious Metals content is
    expressed in Troy Ounces per Short
    Ton. A short ton is 200 lbs.
     One troy ounce is 31.1035 grams.

     A metric tonne is 2204.62 lbs.

     So, 34.2857 grams per tonne is one


    Troy Ounce.
    FUNDAMENTAL CHEMISTRY
    OF FIRE ASSAY

    Fusion
    12PbO + C6H10O5  12Pb + 6CO2 +5H2O
    162 2,48
    Cupellation
    Pb + ½ O2 PbO
    ESSENTIAL REAGENTS USED
    IN FIRE ASSAYING
     Basic Reagents
    Litharge – PbO
    Sodium Carbonate – Na2CO3
     Neutral Reagents
    Fluorspar – CaF2
    Cryolite – AlNa2F6
     Acid Reagents
    Silica, quartz, glass – SiO2
    ESSENTIAL REAGENTS USED
    IN FIRE ASAYING
     Acid Reagents
    Borax – NaB4O7:10H2O
    Borax Glass - NaB4O7
     Reducing Reagents
    Flour, carbon,metallic iron
     Oxidizing Reagents
    Niter – potassium nitrate – KNO3
    Litharge – PbO
    BASIC OPERATIONS OF
    FIRE ASSAY
     Sampling, weighing and combining the
    material to be assayed with an
    appropriate flux.
     Fusing the mixture in the crucible.
     Pouring the reduced button.
     Separating slag from button.
     Cupeling the button.
     Parting the bead.
     Scorification if necessary.
    FIRE ASSAY REDUCING
    POWER TEST
    FUNDAMENTAL CHEMISTRY
    OF FIRE ASSAY

    Fusion
    12PbO + C6H10O5  12Pb + 6CO2 +5H2O
    162 2,486
    Cupellation
    Pb + ½ O2 PbO
    REDUCING AND OXIDIZING POWER
    FLUX AND SLAG CHARACTERISTICS
    EXAMPLE FLUX MIXTURES.
    EXAMPLE FLUX MIXTURES.
    EXAMPLE FLUX MIXTURES.
    CRUCIBLE FUSION
    CRUCIBLE FUSION
    CRUCIBLE FUSION
    CRUCIBLE FUSION
    CRUCIBLE FUSION
    FIRE ASSAY MOLDS AND TRAYS
    CRUCIBLE FUSION
    CRUCIBLE FUSION
    CRUCIBLE FUSION
    CRUCIBLE FUSION
    Pb BUTTONS
    The lead button is separated from the
    slag using a hammer. It can then be
    pounded into a cube to be placed in a
    cupel
    Pb BUTTONS
    FLUXES AND SLAGS
     Slag components classified according
    to acidity or basicity.
     Classified according to the silicate
    degree which is the ratio of oxygen
    in the acids to oxygen in the bases.
     Metal oxides tend to be soluble in
    metallurgical slags.
    FLUXES AND SLAGS
    ASSAY SLAG COLORS
     Green slags indicate ferrous silicates
    or copper.
     Brick red slags indicate copper and
    the absence of iron. Color from
    cuprous silicate or cuprous borate.
     White to gray white (opaque) slags
    indicate calcium, magnesium,
    aluminum or zinc.
    ASSAY SLAG COLORS
     Antimony gives a greenish-yellow
    color.
     Iron bearing slags are yellow-brown
    or black. An acid slag bearing iron
    will be pale green and transparent.
    ASSAY SLAG COLORS
    ASSAY SLAG COLORS
     Cobalt blue slags indicate cobalt.
     Purple to light pink slags indicate
    manganese.
     Slags should always be examined for
    ‘shotting’ of entrained particles of
    lead.
    IMPURITIES IN THE SLAG
     Shotting – metals entrained in slag.
    Modify slag viscosity.
     Speiss - As, Sb - Heavier than matte
    but lighter than lead. Usually only
    found when copper present. Use
    more litharge.
     Matte - iron and copper sulfides.
    IMPURITIES IN THE LEAD
    BUTTON
     Most base metal impurities cause
    problems in cupellation.
     Bismuth is special case.

     Electomotive series shows that


    besides PM’s only Sb, Bi, As, Cu,Te,
    and Hg are below Pb. Thus, they
    may be reduced with Pb.
    IMPURITIES IN THE LEAD
    BUTTON
    IMPURITIES OF THE LEAD
    BUTTON
     Bismuth – acts like lead – bead
    ‘sweating’.
     Antimony, Arsenic, Telleriurm and
    Copper – easy to oxidize with excess
    litharge.
     When in doubt use excess litharge.

     Scorification used at times.


    IMPURITIES IN THE LEAD
    BUTTON
    IMPURITIES IN THE LEAD
    BUTTON
    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

     Heat furnace to 850O C.


     Place cupels in furnace with
    ‘deadheads’ for 15 minutes to
    850O C.
     Hammer lead buttons into cubes.

     Place button in cupel.

     When cupel button ‘opens’ lower


    temperature.
    CUPELLATION

     When lead is nearly gone, raise


    temperature up to ‘drive’ the lead
    out.
     Be careful with high silver buttons
    because of ‘spitting’.
     Take cupels from furnace and
    remove precious metal ‘beads’.
    CUPELLATION
    CUPELLATION
    CUPELLATION
    CUPELLATION
    CUPELLATION
    CUPELLATION
    Feathering
    CUPELLATION
    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.
     Use 1 part nitric acid and 7 parts
    water.
     Heat bead in nitric solution.
    FIRE ASSAY TOOLS
    FIRE ASSAY TOOLS
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    FIRE ASSAY FUNDAMENTALS


    Dr. Corby G. Anderson
    Harrison Western Professor
    Metallurgical and Materials Engineering
    Room 270 Hill Hall
    Colorado School of Mines
    E: cganders@mines.edu
    T: 303-273-3580

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