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Analysis Method of the Quality Management System

Determination of Au FA-GRAV
ME-AuEF3 Version: 01 Data: 20/02/2020 Page 1 of 7

DETERMINATION OF GOLD
FA-GRAV

Actlabs Skyline Perú S.A.C.

APPROVAL DATE: 02.20.20


Version ELABORATED REVISED APPROVED
Laboratory Chief Quality Chief General Manager

02

1. OBJECTIVE
This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Quality Chief
Analysis Method of the Quality Management System
Determination of Au FA-GRAV
ME-AuEF3 Version: 01 Data: 20/02/2020 Page 2 of 7

Determination of the method for the analysis of Au in geochemical samples and ores
and completion by gravimetry.

2. SCOPE

This procedure applies to the Fire Assay area for geochemical and ore samples.

3. RESPONSIBLE

3.1. Laboratory Chief / Assistant Laboratory Chief: responsible for verifying compliance
with this test method.

3.2. Analysts: They are responsible for executing the analys method in reference.

1. TERMS AND ABBREVIATIONS

4.1. Foundry: Action and result of melting, turning a solid into a liquid.
4.2. Cupellation: Test discovered by Geber to test Gold with ashes, in this test gold and
silver remain mostly as doré.
4.3. Crucible: of clay or porcelain in a similar way to a cup in which the material to be
processed by fire assay is placed.
4.4. Inquartation: Procedure that consists of obtaining an Ag-Au alloy where the ratio 3: 1
is given, that is, 750 thousandths of silver with 250 thousandths of gold.

4. PRINCIPLES

The gold contained in the samples is collected and concentrated by the lead from the
reduction of litharge, melting the sample at an approximate temperature of 1060 ° C,
with an adequate melt flow. Then the gold is separated from the lead (regulation) by
cupellation, where most of the lead is absorbed in a glass and the rest is volatilized by
temperature, leaving a button of gold and silver alloy (doré) on the surface of the glass
mainly. . After solubilizing and separating the divided silver, the gold is calcined and
determined gravimetrically.

5. RANGE AND APPLICATION

The method is applicable to all types of geochemical samples and ores, varying the
amount of sample according to its physical characteristics. Button gold is determined by
gravimetry, in ranges from 0.4 g / t to 100 g / t.

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Quality Chief
Analysis Method of the Quality Management System
Determination of Au FA-GRAV
ME-AuEF3 Version: 01 Data: 20/02/2020 Page 3 of 7

7. EQUIPMENT, MATERIALS AND SUPPLIES

7.1. Equipment
7.1.1. Natural gas smelting furnace with digital temperature control, reaching a
temperature of 1100 ° C.
7.1.2. Electric cupping oven with automatic temperature control and internal
ventilation control that reaches a maximum temperature of 1100 ° C
7.1.3. Balanza analítica, precisión 0.01 g.
7.1.4. Ultramicrobalance with an accuracy of 0.1 ug
7.1.5. hot plate with a temperature range of 0 ºC to 250 ºC
7.1.6. Gas extractor equipment.

7.2. Reagents
7.2.1. Geochemical Flux
7.2.2. Flour
7.2.3. Potassium nitrate
7.2.4. Borax
7.2.5. Nitric acid 15%
7.2.6. Concentratec nitric acid
7.2.7. Ammonium hydroxide 15%
7.2.8. Deionized water
7.2.9. Silver metal 99.99%
7.2.10. Assay lead foil 99.99%

7.3. Security equipments


7.3.1. Respirator for acid fumes and metal fumes.
7.3.2. Aluminized Jacket
7.3.3. Aluminized Gloves
7.3.4. Wool Thermal gloves
7.3.5. Safety glasses
7.3.6. Face shield
7.3.7. Ear protection
7.3.8. Safety shoes

8. DESCRIPTION

8.1. Weighed:

8.1.1. The work order is recorded in the ACT-F-117 Analysis Distribution by the
sample preparation personnel.
8.1.2. The staff of the area verifies the conformity of the work order received with
what is indicated in the LIMS, in addition to the state in which the samples are
received.
8.1.3. Each work order is coded according to the number of determinations it
presents. Coding is done numerically or alphanumerically, at the discretion of
the analyst.
8.1.4. Plastic bags are listed according to the work order.
8.1.5. Once compliant, the samples are weighed in an orderly and ascending
manner, registering it in the LIMS.

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Quality Chief
Analysis Method of the Quality Management System
Determination of Au FA-GRAV
ME-AuEF3 Version: 01 Data: 20/02/2020 Page 4 of 7

8.1.6. Weigh from 10 to 20 grams for sulfur samples and from 20 to 30 grams for
oxidized samples (The weight of the sample varies due to the characteristic
of the sample: color, brightness, density, etc.). The weight of the sample is
added to the properly tared polyethylene bag.
8.1.7. In the weighed sample add flour or potassium nitrate according to
characteristics of the sample and / or experience of the assayer.

8.2. Foundry:

8.2.1. Switch on the EF-03 extractor hood according to EF-IO-003.


8.2.2. Code the crucibles from left to right from back to front according to the work
order and place them in an orderly and ascending order in the sample
carriage.
8.2.3. To each sample add 200 +/- 20 g of geochemical flux mixture and
homogenize the content.
8.2.4. Place the bag with the homogenized sample in the crucible in the
corresponding order, in an ascending order.
8.2.5. Add enough borax to each crucible to cover the sample.
8.2.6. Record the work order that has been prepared in the ACT-F-119 format.
8.2.7. Place the crucibles in the oven from right to left and back to front at an initial
temperature of 880 ° C +/- 50 ° C for a period of approximately 20 to 30
minutes.
Then raise the temperature to 950 ° C +/- 50 ° C for 15 to 20 minutes.
Finally, it is increased to 1060 ° C +/- 50 ° C for 20 to 30 more minutes. The
casting process should take approximately 55 to 80 minutes.
8.2.8. Remove the crucibles from the furnace from left to right and front to back
starting from the first number, using a circular motion for better lead
agglomeration and tapping the discharge in the table gently.
8.2.9. Pour the content of the crucible into the mold listed from front to back,
previously clean and completely dry.
8.2.10. Let cool for approximately 10 minutes.
8.2.11. The mass is removed from the mold, hitting the lead button (regulator) with
the hammer to release the slag. Place the regulators in the regulator holder in
the order in which the casting was unloaded.
8.2.12. Limpiar y martillar en forma cuadrada el botón de plomo de la escoria que
aún haya quedado con ayuda del martillo en forma ordenada, luego
enumerar cada uno de los régulos.

8.3. Copelacion:

8.3.1. Revisar la calidad de los régulos, los cuales deben ser compactos y del
tamaño adecuado. Es necesario repetir el procedimiento cuando no se
cuente con estas características.
8.3.2. El botón de plomo debe tener como mínimo un peso aproximado de 20 g y
como máximo 55 g para copelas número 8. Para pesos mayores se usa la
copela numero 11 teniendo como peso máximo 80g.
8.3.3. Una vez seleccionada las copelas, colocarlas en el horno por un tiempo de
15 a 20 minutos a 950°C +/- 50°C aprox. para su respectivo calentamiento.
8.3.4. Registrar la orden de trabajo en el formato ACT-F-120.
8.3.5. Colocar en las copelas los régulos de atrás hacia delante y de izquierda a
derecha cerrando la puerta al finalizar. (teniendo como referencia la puerta
del horno como delante) y cuando se observe que el regulo se haya
This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Quality Chief
Analysis Method of the Quality Management System
Determination of Au FA-GRAV
ME-AuEF3 Version: 01 Data: 20/02/2020 Page 5 of 7

fundido, abrir el dumper que se encuentra en la parte posterior del horno,


para el escape de los vapores generados.
8.3.6. La copelación dura aproximadamente de 40 a 60 minutos a una
temperatura de 950°C +/- 50°C. El punto final de copelación es notorio y se
identifica al visualizar la formación del dore; proceder a retirar las copelas
del horno y dejar enfriar aproximadamente 10 minutos.

8.4. Partición:

8.4.1. Extraer él dore y laminarlo con un martillo, luego colocarlo en un crisol de


porcelana debidamente codificado.
8.4.2. Agregar al crisol 10 ml HNO3 al 15% y llevarlo a plancha a una temperatura
inicial de 120 +/-10 °C.
8.4.3. Luego de la disolución de la plata (no hay burbujeo en el botón de oro),
agregar 20 gotas de HNO3 concentrado al crisol y subir la temperatura a
150°C por 30 minutos aproximadamente.
8.4.4. Retirar el crisol de la plancha y separar la solución de nitrato de plata del
botón de Oro.
8.4.5. Hacer el lavado del oro con agua desionizada 2 veces, luego agregar 10
gotas de Hidróxido de amonio Concentrado y llevar a plancha a una
temperatura de 120°C por 5 minutos aproximado, desechar y dar una
lavada más con agua desionizada. Dejar secar en plancha.
8.4.6. Luego calcinar en el horno a una temperatura de 950°C por espacio de 2
minutos aproximado, observando su brillo dorado característico y dejarlo
enfriar.
8.4.7. Pesar el oro en la ultra-microbalanza.

8.5. Cálculos:

Where:

Ley = Sample law expressed in g / tm


WAu = Weight of gold in mg.
Wmuestra = Weight of the sample expressed in gr.

9. OBSERVATIONS

9.1. Cuando el dore no reacciona con el HNO3 probablemente la relación de


Ag/Au (3:1) no es la correcta entonces se procede a encuartar el dore con
plata metálica y envolverlo con plomo laminado con un peso aprox. de 15 a 20
g.
9.2. Cupels No. 8 will be used when the weight of the regulus is 20 to 55 g and cupels
No. 11 from 56 to 80 g.
9.3. Fluxes composition for exploration and ore samples:

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Quality Chief
Analysis Method of the Quality Management System
Determination of Au FA-GRAV
ME-AuEF3 Version: 01 Data: 20/02/2020 Page 6 of 7

Note: 0.2 g of Silver Nitrate per kg of flux

9.4. El mayor problema en ensayos al fuego es cuando en la muestra hay presencia


de altos contenidos de Cu, Fe en los óxidos y sulfuros de Cu, Fe, As, Sb, etc., por
lo que es necesario bajar la cantidad de muestra.
9.5. Es necesario que las copelas se calienten antes de cargar los régulos en el
proceso de copelación para evitar proyecciones u otros inconvenientes.

10. BIBLIOGRAPHIC REFERENCES

JIS M8111: 1967 (Review 98)


Method for the determination of gold and silver in minerals

FIRE ASSAYING por SHEPPARD AND DIETRICH

A TEXTBOOK OF FIRE ASSAYING por EDWARD E. BUGBEE

Annexed 1

WEIGHED
(30 g sample)

Flour or KNO3.
200 +/- 20g fundente

HOMOGENIZED

Borax
T1 = 880 + 50 ºC 30 min.
T2 = 950 + 50ºC 15 min. FOUNDRY
T3= 1060 + 50ºC 30 min.
Escoria
This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Quality Chief
Analysis Method of the Quality Management System
Determination of Au FA-GRAV
ME-AuEF3 Version: 01 Data: 20/02/2020 Page 7 of 7

T = 950 + 50°C 40 min COPELACION


min.

10 ml HNO3 15% PARTICION T = 120 + 10°C y 150 + 10°C


20 gotas HNO3cc
Solución de Nitrato de
Plata
2 veces agua Desionizada
WASH 10 gotas NH4OH Cc
1 vez, Agua Desionizada

T = 150°C 2 min
CALCINATED

PESADO DE ORO
(mg)

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Quality Chief

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