Test method of the Quality Management System

Determination of Au 30g FA-AAS

ME-AuEF2 Page 1 of 7

GOLD DETERMINATION
FA-AAS

Actlabs Skyline Peru SAC

APPROVAL DATE: 11.02.20

Version ELABORATED REVIEWED APPROVED
Laboratory Head Quality Manager General Manager

01

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Head of Quality
 Test method of the Quality Management System
Determination of Au 30g FA-AAS
ME-AuEF2 Page 2 of 7

1. OBJECTIVE

Determination of the Method for the analysis of Au in geochemical samples and

completion by atomic absorption.

2. SCOPE

This procedure applies to the Fire Testing area for geochemical samples.

3. RESPONSIBLE

3.1 Head of Laboratory: You are responsible for verifying compliance with this test
method
3.2. Analysts: They are responsible for executing the test method in question.

4. 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. Melting pot: Earthenware or porcelain tool similar to a cup in which the material to
be processed by dry means is placed.
4.4. Digestion: Reaction at low temperature, without boiling of the liquid.

5. PRINCIPLES

The gold contained in the exploration samples is collected and concentrated by the
lead from the reduction of litharge, when the sample is melted at a temperature of
approximately 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 cup and the rest is volatilized by temperature, leaving a button of
gold and silver alloy on the surface of the cup (doré ) mainly. After precipitating the
partitioned silver, the gold is solubilized in aqua regia and determined by reading in AAS.

6. RANK AND APPLICATION

The method is applicable to all types of geochemical samples, varying the amount of
sample according to its physical characteristics.
Gold put into solution in this way is determined by atomic absorption reading, in ranges
from 5 ppb to 10,000 ppb.

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Head of Quality
 Test method of the Quality Management System
Determination of Au 30g FA-AAS
ME-AuEF2 Page 3 of 7

7. EQUIPMENT, MATERIALS AND SUPPLIES

7.1. Teams

7.1.1. Natural gas smelting furnace with digital temperature control, reaching a
temperature of 1100 ° C.
7.1.2. Electric cupellation oven with automatic temperature control and internal
ventilation control that reaches a maximum temperature of 1100 ° C.
7.1.3. Analytical balance, precision 0.01 g
7.1.4. Electric iron with a temperature range of 0 ºC to 250 ºC
7.1.5. Gas extractor equipment.

7.2. Materials

7.2.1. Refractory crucibles.

7.2.2. Cups Nº 8, Nº 11
7.2.3. Iron ingot molds listed.
7.2.4. Anvil.
7.2.5. Forceps to manipulate regulus.
7.2.6. Hammer and rope.
7.2.7. Board numbered to place clean regules.
7.2.8. Forceps to manipulate dores (parrot beak).
7.2.9. 5ml test tubes.
7.2.10. Cup loader (48 cups).
7.2.11. Crucible loader.
7.2.12. Heat resistant crayons.
7.2.13. 8x12 plastic bags.
7.2.14. Plastic spoon.
7.2.15. Dispensers.
7.2.16. Bone ash.
7.2.17. Car to load crucibles.
7.2.18. Table to unload crucibles.
7.2.19. Temperature sensor.
7.2.20. Metal and plastic racks.

7.3. Reagents

7.3.1. Geochemical flux (See composition in annex).

7.3.2. Flour.
7.3.3. Potassium nitrate.
7.3.4. Borax.
7.3.5. Nitric Acid 15%
7.3.6. Concentrated Hydrochloric Acid.
7.3.7. Deionized water.

7.4. Security equipments

7.4.1. Mask.
7.4.2. Respirator for metal fumes and vapors.
7.4.3. Aluminized jacket and gloves.
7.4.4. Thermal Wool Gloves.
7.4.5. Safety glasses.

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Head of Quality
 Test method of the Quality Management System
Determination of Au 30g FA-AAS
ME-AuEF2 Page 4 of 7

7.4.6. Face shield against heat and slag.

7.4.7. Ear protector.
7.4.8. Safety shoes.
7.4.9. Long sleeve shirt and pants.

8. DESCRIPTION

8.1. Heavy:

8.1.1. The work order is recorded in the ACT-F-117 Analysis Distribution format by the
sample preparation personnel.
8.1.2. The staff of the area verifies the conformity of the order received with what is
signed 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. The polyethylene bags are listed according to the order to work.
8.1.5. Once satisfied, the samples are weighed in an orderly and ascending
manner, registering it in the LIMS.
8.1.6. Weigh from 10 to 20 grams for our sulphides and from 20 to 30 grams for
oxidized samples (The weight of the sample varies due to the characteristics
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 car.
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 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 a better lead
agglomeration and tapping gently on the discharge table.
8.2.9. Pour the content of the crucible into the numbered mold, clean and
completely dry from front to back.
8.2.10. Let cool for approximately 10 minutes.

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Head of Quality
 Test method of the Quality Management System
Determination of Au 30g FA-AAS
ME-AuEF2 Page 5 of 7

8.2.11. The mass is removed from the mold, hitting with the hammer to free the lead
button (regulus) from the slag. Place the regulators in the regulator holder in the
order in which the casting was unloaded.
8.2.12. Clean and cube the lead button from the slag that is still left with the help of
the rope in an orderly manner, then list each of the regules.

8.3. Cupellation:

8.3.1. Check the quality of the regulums, which must be compact and of the
appropriate size. It is necessary to repeat the procedure when these
characteristics are not available.
8.3.2. The lead button must have a minimum weight of approximately 20 g and a
maximum of 55 g for cups number 8. For larger weights, use cup number 11
with a maximum weight of 80g.
8.3.3. Once the cups have been selected, place them in the oven for 15 to 20
minutes at 950 ° C +/- 50 ° C approx. for their respective warm-up.
8.3.4. Record the work order in the ACT-F-120 format.
8.3.5. Place the rules from back to front and from left to right in the cups, closing
the door at the end. (with reference to the oven door as in front) and when it
is observed that the regulator has melted, open the dumper located at the
back of the oven to escape the vapors generated.
8.3.6. Cupellation takes approximately 40 to 60 minutes at a temperature of 950 ° C
+/- 50 ° C. The final cupellation point is noticeable and is identified by
visualizing the browning; proceed to remove the cups from the oven and
allow to cool for approximately 10 minutes.

8.4. Partition:

8.4.1. Code the 5 ml tubes in an orderly manner according to work orders and
place them in the metal rack.
8.4.2. Extract the bead (product of the cupellation) and place it in the coded 5 ml
tubes as appropriate in an orderly manner.
8.4.3. Turn on the iron at a temperature of 150 ° C +/- 10 ° C and turn on the
extractor.
8.4.4. Record the work order in ACT-F-121 format.
8.4.5. Add 1 ml of 15% HNO3 to each tube containing the bead.
8.4.6. Place the metal rack with the tubes on the heating plate, the attack ends
until the complete dissolution of the silver and releasing the gold identified by
visualizing a brown point. This process takes approximately 20 to 30 minutes
8.4.7. After dissolving the silver, add 1.2 ml of concentrated hydrochloric acid,
observing a total dissolution of the gold and precipitation of silver with
elimination of nitrous vapors. This process takes approximately 20 to 30
minutes.
8.4.8. Remove the rack from the plate and allow the solution in the tubes to cool
completely.
8.4.9. Make up to 5 ml with deionized water, cover the tube with parafilm, shake.
8.4.10. Check the order of the tubes according to the work order.
8.4.11. Once you are satisfied with the order, register the order submission in the
ACT-F-041 format and send it to the atomic absorption area.

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Head of Quality
 Test method of the Quality Management System
Determination of Au 30g FA-AAS
ME-AuEF2 Page 6 of 7

8.5. Calculations:

Where:
Law = Law of the sample expressed in ppb.
AAS reading = Reading concentration expressed in mg / L.
BK = Target reading concentration expressed in mg / L.
V = Volume of capacity.
W = Weight of the sample expressed in grams.

9. OBSERVATIONS

9.1. Flux composition for geochemical and / or ore samples.

9.2. The biggest problem in fire tests is when the sample contains high contents of Cu,
Fe in the oxides and sulphides of Cu, Fe, As, Sb, etc., so it is necessary to vary the
flux or lower the quantity of sample, the analyst will decide what action to take
taking into account the detection limit of Au.
9.3. During the process, maintain good laboratory practices.
9.4. It is necessary for the cups to be heated prior to loading the regulums in the
cupping process to avoid splashing or other inconveniences.
9.5. When the flux is received, the respective analysis is carried out to determine its
degree of contamination as a quality control to verify the conformity of the
product, registering it in the ACT-F-110 format.
9.6. The use of safety equipment is mandatory.

10. BIBLIOGRAPHIC REFERENCES

 ASTM E400
Standard for the method of analysis for ores, minerals and rocks by pre
concentration FIRE ASSAY - AAS (Revision 97)
 FIRE ASSAYING by SHEPPARD AND DIETRICH
 A TEXTBOOK OF FIRE ASSAYING by EDWARD E. BUGBEE
 GOLD METALLURGY by Fidel Sergio Misari Ch. (Pages 90 - 92)
 GCH
Course-workshop on gold and silver assays in FireAssay

11. RECORDS

 ACT-F-041 Analysis distribution

 ACT-F-119 Foundry
 ACT-F-120 Cupellation
 ACT-F-121 Partition

This document is CONFIDENTIAL, it should not be photocopied except with the permission of the General
Management and / or Head of Quality
 Test method of the Quality Management System
Determination of Au 30g FA-AAS
ME-AuEF2 Page 7 of 7

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