M501 R0003 Determination of Gold by Fire Assay and Gravimetric Finish

PERFORMANCE LABORATORIES
Section No.:
METHOD
DETERMINATION OF GOLD BY FIRE ASSAY AND
GRAVIMETRIC FINISH
Compiled by:
S. Marx, Quality Controller
Signature:
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Approved by:
J. Smith, Executive Director
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Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
2009
Determination of gold by fire assay and gravimetric finish

Introduction:
The fire assay is the oldest and, in most circumstances, still the best method for the
determination of gold in ores and metallurgical products.
Estimated to have been practised, in essence, as long ago as the third millennium BC, the
procedure has changed but little since the time of Theophrastus (circa 300 BC). Trial by fire
certainly was performed before the dawn of chemical knowledge and, indeed, it must be
admitted that, in the chemistry of the process, much empiricism remains!
The method enables mining operations to mine only in areas where sufficient gold is indicated,
i.e. to enable economically viable mining.
Scope and application:

This procedure applies to all mining samples requiring the analysis of gold by fire assay and
gravimetric finish.
The practical range of the method is from 0.09 to 3 027g/t gold (Au).
The limit of detection of the method is 0.04g/t gold (Au).
The method-reporting limit is 0.09g/t gold (Au).
Method summary:
Essentially, the method consists of two consecutive pyrochemical separations, followed by a
chemical separation.
Initially, the finely ground sample is fused with a suitable flux under reducing conditions.
The flux combines with the gangue to form a fluid slag, and the litharge in the flux is reduced
to minute globules of lead. The rain of lead globules, falling through the molten mass, collects
the particles of precious metals and coalesces into a button at the bottom of the crucible. As
silver is a better collector of gold than lead and facilitates the easier handling of prills, it is
employed in conjunction with the lead as a co-collector.
Upon cooling, the slag solidifies, and is separated from the lead button containing the gold and
silver.
Subsequently, the lead is removed by oxidising fusion, where the litharge thus formed, wets
the inner surface of the hot, porous cupel and is absorbed (cupellation). The molten precious
metals, are not absorbed because of their high surface tension, and because they do not form
oxides. They remain on the concave bed of the cupel in the form of a bead, called a prill.
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Section No.:
METHOD
GRAVIMETRIC FINISH
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Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
2009
The silver is removed from the prill by acid dissolution (parting). The black, spongy gold thus
obtained is annealed to a coherent, malleable prill of the classical golden yellow colour,
making the gold available for further measurement.
Health and safety:

The toxicity or carcinogenicity of all the compounds or reagents used in this method has not
been precisely determined; however, each chemical compound shall be treated as a potential
health hazard. Exposure to these compounds and to the samples shall be reduced to the
lowest possible level.
A dust mask shall be worn when mixing the samples and flux and transferring the mixture to
the crucibles.
Good hygiene shall be practiced, such as washing hands after working in the furnace area or
coming into contact with flux, and especially before eating and smoking.
Appropriate protective equipment such as a face shield, apron and gloves are supplied and
shall be worn while working at the furnaces.
Overalls and/or lab coats shall be washed on a regular basis. Litharge is a toxin, and is
detrimental to health (lead poisoning).
Appropriate eye protection shall be worn when hammering the slag from the lead buttons.
Care shall be taken when working with silver nitrate, as it is corrosive and stains the skin.
Goggles or safety spectacles shall be worn when working with concentrated solutions of acids
and alkalis.
Latex rubber gloves and goggles or safety spectacles shall be worn when working with
concentrated acids.
Concentrated nitric acid is a strong oxidising agent that may ignite combustible substances.
Avoid cleaning up spills with paper or cotton towelling. Wash away with copious amounts of
water instead.
Nitric oxide fumes that form as a result of the reaction between nitric acid and silver during the
parting process, are extremely toxic. Parting shall be carried out in a fume cupboard.
Avoid vigorous boiling during the parting and drying process.
Asbestos or any other heat resistant gloves, face shields (green tinted) and safety boots shall
be worn when working on fusion or muffle furnaces.
Sample handling:
Handling of samples for testing shall be carried out as described in the section titled: Handling
of test items of the quality manual.
Extreme care shall be taken at all times to ensure integrity of sample identification.
Section No.:
METHOD
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GRAVIMETRIC FINISH
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Technical requirements
conditions:
Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
2009
Approved by:
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for
accommodation
and
environmental
The fire assay area shall be separated from other areas of testing to avoid crosscontamination to and from the area.
The parting area shall be equipped with efficient fume extraction in the form of a fume
cupboard.
The doors of the balance room shall be kept closed and the room temperature maintained at
23 3C.
Interferences:
Interfering elements, in the form of base metals, are removed during the fire assay process.
Sulphur interferes in the fire assay, by forming a mixture of metallic sulphides, known as matte,
above the lead button. Depending on the concentration of sulphide in the ore, the matte may
appear as a layer of considerable thickness, or simply as a crystalline coating on the upper
surface of the button. It always retains some of the gold and silver, with subsequent loss to the
slag when the lead button is cleaned. Sulphur contained in pyrite (fools gold), is removed by
the addition of 10gram Potassium nitrate (KNO3) to a high sulphur content sample, and 5gram
Potassium nitrate (KNO3) to a low sulphur content sample. The presence of pyrite is indicated
by a yellow, shiny metallic appearance, or in the case of pyritic concentrates, by the dark grey
or black colour of the sample.
A mixture of Potassium nitrate (KNO 3) and Sodium carbonate, anhydrous (Na2CO3H2O) can
also be used as a de-sulphurizer, (50% KNO3, 50% Na2CO3H2O), 20gram for high sulphur
content and 10gram for low sulphur content.
Apparatus and equipment:

Dust extraction.
Large spatula or spoon (approximately the size of a dessert spoon) for weighing samples.
Top pan mass meter of adequate capacity, sensitivity 0.1g.
Analytical mass meter of adequate capacity, sensitivity 0.0001g.
Fire clay fusion crucibles, Economic Fireclay Industries numbers 1, 4 and 5 or similar.
Crucible trays mounted on suitable trolleys.
Flux scoop, size determined by sample mass as in Table M501-1.
Plastic bags (200x300mm)
Compressed air.
Section No.:
METHOD
GRAVIMETRIC FINISH
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Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
2009
Spatula, capacity approximately 50ml or smaller.

Beaker (squat form), capacity, 500ml.
Measuring cylinder, capacity 2 000ml, Class B or better.
Burette, capacity and classification not critical or 2ml Auto drop pipette, 1ml & 2ml Kipps
pipette.
Amber-coloured bottle, glass, capacity at least 5 00ml.
Reagent bottle, glass, capacity approximately 2 000ml.
Furnace, fusion, capable of maintaining a temperature of 1 100 100C.
Manual fork
Crucible tongs.
Slag moulds, cast iron, capacity approximately 50 and 140ml.
Trolleys for slag moulds.
Button trays (clean).
Hammer for shaping lead buttons, medium weight.
Furnace, cupellation (muffle), capable of maintaining a temperature range of 1 000 50C.
Cupels (cleaned by blowing with compressed air), Economic Fireclay Industries codes 7, 8,
and 9 or similar.
Cupel tray.
Muffle door tongs.
Lead button transfer tongs.
Cupel mirror.
Fume hood.
Forceps, 125mm in length, for transferring prills to porcelain cups.
Porcelain cups (clean and dry), capacity approximately 7ml, Haldenwanger 79MF/9 or similar.
Wash bottle, plastic.
Parting trays (clean).
Hammer for silver prills, lightweight.
Anvil (clean).
Fume cupboard.
Separating funnel small
One temp setting for hotplate.
One annealing muffle.
Vacuum pump, equipped with suitable liquid traps.
Micro mass meter of adequate capacity, sensitivity 0.000 001g, Sartorius 4401 or similar.
Goldsoft 2007 veriLIMS system with interface
Computer server loaded with a compatible version of Goldsoft 2007 veriLIMS
Forceps, fine-pointed, for weighing prills on the micro mass meter.
Bullion Roll
Section No.:
METHOD
GRAVIMETRIC FINISH
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Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
2009
46) Bullion parting apparatus
9.
Chemicals and solvents:
1)
2)
3)
Silver nitrate (AgNO3), CP grade or better.

Nitric acid (HNO3), concentrated, 55% (m/m), CP grade or better.
Chloride-free deionised or distilled water shall be used for all reagents and dilutions, unless
otherwise specified.
4) Lead foil
5) Silver wire / discs
6) Copper metal
10.
1)
2)
3)
4)
5)
Reagents and standards:

Performance Laboratories in house quality check standard (QC). It is imperative that the
procedure titled: Procedure for ensuring the uninterrupted succession of in-house quality
check standards is strictly adhered to in order to assure continuous monitoring of the
assaying process.
General flux prepared as described in the procedure titled: Procedure for the preparation of
fluxes for fire assay.
Silver nitrate solution Weak (0.1M): - Using a top pan mass meter, weigh 34g 0.5g AgNO 3
into a clean, dry, 500ml squat form beaker. Dissolve in approximately 200ml of distilled water.
Transfer quantitatively to a 2 000ml measuring cylinder and make up to the 2 000ml mark with
distilled water. Transfer to an amber-coloured bottle and mix well. Shelf life is six months.
Silver nitrate solution Strong: - Using a top pan mass meter, weigh 130g 0.5g AgNO 3 into a
clean, dry, 500ml squat form beaker. Dissolve in approximately 200ml of distilled water.
Transfer quantitatively to a 1 000ml measuring cylinder and make up to the 1 000ml mark with
distilled water. Transfer to an amber-coloured bottle and mix well. Shelf life is six months.
Nitric acid solution (1:2): - Using a 2 000ml measuring cylinder, measure 1600ml distilled water
into a reagent bottle. Slowly add 800ml concentrated nitric acid using the same measuring
cylinder. The bottle is sealed and the contents gently mixed. Allow to cool to room
temperature. Shelf life is one year.
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METHOD
GRAVIMETRIC FINISH
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Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
2009
Procedure (Fire Assay and gravimetric finish):
1) Prepare the sample to a pulp as described in the procedure titled: Procedure for preparation of
a pulp for fire assay.
At all times, the correct order of samples shall be maintained by following the procedures titled:
Procedure for maintaining the correct order of samples that use No. 1 crucibles and/or
Procedure for maintaining the correct order of samples that use No. 4 or 5 crucibles.
2) Prepare the tray consisting of no more than 36 crucibles by referring to Table M 501-1 for
details regarding the correct combination of crucible size, cupel size, sample mass, flux type,
mass of flux and addition of silver for a particular type of sample. Combinations may be
adapted to suit particular client requirements. In such cases, the Laboratory Manager shall note
the deviations on the jobsheet. For carbon samples prepare lead foil capsules.
3) Each tray of no more than 30 samples shall contain one QC and a minimum of two randomly
selected duplicate sample, chosen either automatically by use of suitable electronic means or
manually by the supervisor. A second QC, and randomly selected duplicate sample may be
included as safeguard, should either the first QC or randomly selected duplicate samples be
lost as a result of a defective crucible.
4)
To counteract the effects of segregation, samples shall be mixed with a spatula, spoon or other
suitable implement immediately before weighing.
5)
All samples shall be checked for dryness by inserting the smooth handle of a spatula or spoon
into the sample and withdrawing it slowly. Any samples showing signs of moisture shall be
dried before weighing.
6)
Place the plastic bags into the marked glass containers, add the appropriate flux using the flux
scoop, as indicated in Table M 501-1. For carbon samples add the required amount of red
lead / litharge, mix well, add required silver wire and enclose capsule. Proceed to point 19
7)
Weigh the appropriate mass of sample as indicated in table M501-1 and transfer to the plastic
bags containing the flux, for carbon sample transfer to the lead capsule.
Section No.:
METHOD
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DETERMINATION OF GOLD BY FIRE ASSAY AND GRAVIMETRIC FINISH

Compiled by:
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Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
Approved by:
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Table M501-1:
Sample type
Crucible
size
Cupel size
Sample mass
(g)
Approx.
flux mass
(g)*
Flux scoop
ID
Flux type
High grade
125
Mine
GO925 or
High Grade
flux
25 ( 2.0)
0.1M
AgNO3
Fusion times
(minutes)
Potassium
Nitrate or
Mixture if
sample is pyritic
(refer to 7.2).
If required,
then 2
35
35
Ag wire in the
ratio 2.5Ag:1Au
Ore
(all mine chip
and boreholes,
grabs & belt
cuts)
ml
5g Maize meal.
5 or 10
or less ( 0.5)
depending on
the sample
size and
estimated
grade
Additional
reagents
required
125
Mine
GO925 or
mine
sample flux
Potassium
Nitrate or
Mixture if
sample is pyritic
(refer to 7.2)
Section No.:
METHOD
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DETERMINATION OF GOLD BY FIRE ASSAY AND GRAVIMETRIC FINISH

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Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
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Table M501-1 (continued):

Sample mass
(g)
Approx.
flux mass
(g)*
Flux scoop
ID
Flux type
50 ( 5.0)
200
Pulp
50 ( 5.0)
200
Plant residues
125 ( 5.0)
Carbon
N/A
1 2 ( 0.1)
Crucible
size
Cupel size
Sludge, pulps
& cores
Plant feeds
Sample type
AgNO3
GO925 or
Pulp flux
None
45
Pulp
GO925
None
45
375
Residue
GO925 or
Residue
flux
None
50
10 - 20
Red lead /
litharge
Silver wire
35
* Flux mass used is not critical, as long as the flux to sample ratio is 2.5:1.
AgNO3 addition may be increased correspondingly if a higher value result is expected.
ml
Additional
reagents
required
0.1M
Fusion times
(minutes)
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Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
8) Mix the contents under the extraction hood by shaking and then place the sample in its
designated crucible. Mixing of samples shall be carried out under an extraction hood to
prevent cross-contamination by dust.
9) Add metallic tag with same tray no. as tray and use an old cupel to write the information of the
tray on. This metallic tag, info cupel as well as the jobsheet shall accompany the tray
throughout the fire assay procedure until the samples are ready for weighing.
10) Use the colour coded tags accordingly. Black tag for 1st 40 trays, orange colour for 2nd 40 trays
and green colour for Repeat trays.
11) Add any additional reagents that may be required as indicated in Table M 501-1.
12) Add the tip of a spatula (1g) copper sulphate to the appropriate identification crucibles
according to the procedure titled: Procedure for maintaining the correct order of samples.
13) Add 0.1M AgNO3 solution as described in Table M 501-1, using a 50ml burette.
14) Pre-heat a fusion furnace to 1 100 100C. Record the in temperature and time on the
jobsheet and then using a manual fork or crucible tongs, load the crucibles into a fusion
furnace.
15) Fuse the mixture for the time indicated in Table M 501-1. Successful fusion is indicated by the
fluidity of the molten slag.
16) Record the out temperature and time on the jobsheet and then pour the molten charge
steadily and slowly into the apex of a cast iron mould.
17) A lead button will form at the bottom of the mould. After cooling, remove the slag from the
button and transfer the latter to a button tray, while maintaining the correct sample order.
Remove any adhering slag from the button by hammering it into a cube (for easier handling)
and blowing the slag off the anvil using the compressed air jet situated in front of the anvil.
18) Clean a tray of cupels. Load the cupels into a muffle furnace using the correct equipment, for
instance muffle door tongs or a Monckton fork.
19) Preheat the cupels for at least 15 minutes at 1 000 50C. Record the in temperature and
time on the jobsheet and then place the lead buttons on the hot cupels, using the lead button
transfer tongs. The cupels at the back of the furnace should be charged first. Thus, the buttons
are carried over the empty cupels in front, so that, should a button be dropped accidentally, it
will not fall into a cupel that already has been charged. Ensure that the correct order of the
samples is maintained. Record the in time on the jobsheet.
20) Cupel the lead buttons for at least 45 minutes at 1 000 50C or until cupellation is complete.
Use a muffle mirror to check for completeness of cupellation, before unloading the samples.
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Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
21) Record the out temperature and time on the jobsheet and then unload the samples, and
allow to cool on a metal tray under a fume hood.
22) Transfer the prills, using forceps, to the anvil, taking care to maintain the correct sample order.
23) Flatten the prills, using a light hammer.
24) Transfer the prills into porcelain cups, arranged on a parting tray and placed alongside the
anvil, taking care to maintain the correct sample order.
25) Place the tray on the low hot plate in the fume cupboard (identifying metallic tag to remain
with/on tray at all times).
26) Add approximately 3 - 4ml 1:2 HNO3 (about half the porcelain cupful).
27) Allow the reaction to cease completely.
28) Using a separating funnel, add two drops of concentrated nitric acid to the contents of the
porcelain cup.
29) Allow the reaction to proceed until complete. A sufficiently parted prill has a black amorphous
appearance of sponge gold. Ensure that no further reaction takes place. Additional time of
approximately 10 minutes shall be allowed if the reaction is less vigorous than usual.
30) If the reaction is incomplete (visually indicated by a metallic, brassy lustre) due to insufficient
silver having been added initially, the acid is removed as in paragraphs 11.34, and 35 below.
Dry the sample as described in paragraph 11.36 below, and re-inquartate as described in the
procedure titled: Procedure for re-inquartation.
31) Indicate on the jobsheet whether any prills have broken up. If the correct ratio of silver to gold
is maintained at 2.5:1, the prills should not break up. If prills break up regularly, a preventive
action report shall be raised and handed to the relevant Manager without delay (refer to the
section titled: Preventive action of the quality manual).
32) Switch on the vacuum pump or similar and remove the acid mixture by suction.
33) Using distilled water, wash the prill and remove the water by suction, taking care not to suck
the prill up. Repeat once more.
34) Place the tray containing the black, spongy prills on the low temperature hot plate. Allow to dry
for at least 5 minutes.
35) Place the tray in the annealing muffle set at approximately 750 C for at least 30 seconds. This
is the annealing process, where the colour of the prill changes from black to golden yellow.
36) Once the annealing process is complete, remove the tray from the annealing muffle and allow
to cool on an asbestos-cement slab or ceramic tile.
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Document No.:
M501
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Effective date:
1 December 2010
37) The jobsheet shall be attached to the parting tray before sending it - and the identifying tag
and cupel - to the balance room at the end of the fire assay procedure.
38) Upon receipt of the samples to be weighed, the identifying tag and cupel and the number of
samples shall be checked against the jobsheet that accompanies the parting tray. These
actions shall be recorded and duly signed by the analyst responsible for weighing.
39) Using a micro mass meter, determine the mass of each prill to the nearest 0.000 001g (for
operating instructions refer to the logbook for the instrument).
40) Once all the samples have been weighed, the jobsheet signed and the records forwarded to
the analyst/chemist responsible for assuring the quality of test results.
12. Procedure (Bullion):

1)
Weigh a representative portion ~500mg of bullion and place in a pre folded lead envelope. A
sample of proof plate is also weighed to allow for the correction of the retained silver in the
final calculation (surcharge). The proof plate is treated as a sample from this point forward.
2)
Add approximately 2.5- 3X the bullion mass of silver wire/discs. (generally this mass equates
to 1 silver disc)
3)
Add approximately 15 mg of copper in the form of a piece of metallic copper.
4)
Seal lead envelope.
5)
Clean a tray of No 7 cupels. Load the cupels into a muffle furnace using the correct
equipment, for instance muffle door tongs or a Monckton fork.
6)
Preheat the cupels for at least 15 minutes at 1 000 50C. Ensure that the correct order of the
samples is maintained.
7)
Cupel the lead envelopes for at least 20 minutes at 1 000 50C or until cupellation is
complete. Use a muffle mirror to check for completeness of cupellation, before unloading the
samples.
8)
Care must be taken when offloading samples as rapid cooling will cause spitting. Samples
must thus be removed gradually from the furnace. Allow to cool on a metal tray under a fume
hood.
9)
Transfer the prills, one at a time, using forceps, to the anvil, and hammer it on its side. Hold
with a pair of long nose pliers and clean with a wire brush to remove adhering cupel material.
Place the base prill on one side for later weighing. Place the remaining flattened prills in the
annealing furnace for 30 seconds
10) Using the bullion rolls, roll the flattened prill into a ribbon like shape. Anneal the ribbon in the
annealing furnace and roll into a cornet using the tweezers.
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Document No.:
M501
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Effective date:
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11) Place the rolled cornets into the parting apparatus.

12) The parting apparatus is placed in a beaker containing weak hot Nitric Acid. The acid must be
stirred prior to the parting apparatus being inserted.
13) The samples are allowed to react for 20 minutes after the evolution of brown fumes.
14) The samples are then transferred to a beaker containing boiling strong acid and allowed to
react for 20 minutes. The acid must be stirred prior to the parting apparatus being inserted.
15) Once complete the samples and annealing apparatus are rinsed twice in hot, distilled water.
Excess moisture is removed with clean paper and then placed on the hotplate to dry.
16) Once dry the entire apparatus is placed in an annealing muffle for 30 seconds.
17) Samples are allowed to cool and transferred into a porcelain crucible.
18) Using a micro mass meter, determine the mass of each prill to the nearest 0.000 001g (for
operating instructions refer to the logbook for the instrument).
19) Once all the samples have been weighed, the jobsheet signed and the records forwarded to
the analyst/chemist responsible for assuring the quality of test results.
13. Calculations:
1)
Calculation of the gold concentration:

Mass of prill (mg) X 1 000
Gold concentration =
Sample mass (g)
grams/tonne (g/t Au)
For the calculation of bullion the following example explains and must be applied:
ALIQ
(mg)
1) 501,11
2) 501,61
3) 502,22
BASE
506,24
PROOF
516,28
2)
PARTED
PARTED SURCHARGE
440,08
440,68
441,13
439,69
440,29
440,74
490,11
968,1
SURCHARGE
+ 0,39
516,67
FINENESS
PARTED x
1000 / ALIQ
877,4
877,8
877,6
Notes:
AVE
877,6
BASE
GOLD
SILVER
968,1
877,6
90,5
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Effective date:
1 December 2010
a) For Goldsoft 2007 veriLimms generated work, data from the micro mass meter is
captured simultaneously on the Pc and the Goldsoft veriLims server system. When
weighing of the gold prills on the tray has been completed, the prill masses are imported
to the Goldsoft veriLims sample sheet. The prill masses are automatically inserted next
to the sample when pressing interface button, this will also zero the balance again
before weighing another sample on the computer system (Goldsoft 2007 veriLIMS), this
will then immediately work out the final gold concentration. The Goldsoft verilims
system will also show repeats on replictate / duplicate samples or on QC samples failing
the parameters.
b) When the link between the micro mass meter and the Goldsoft veriLims server is
interrupted, the gold prills are weighed as above, but the prill masses are noted down on
the job sheet manually. A manual data entry shall then be performed to insert the prill
masses in the Goldsoft veriLims computer file for the respective job. The data is then
converted by the system to obtain the final gold concentration.
Calculation of the magnitude of limits to be used for duplicates/repeats:
Residue samples:
Maximum allowable difference (g/t Au) = 14.4136 X (Mean [Au] of the duplicates in g/t)
-0.5251
Mine & Head samples

-0.5394
Carbon samples
14.
1)
-0.2846
Quality control:
All sample trays shall be subjected to the evaluation procedures described in paragraphs 13.2
to 13.7, and only once the requirements for both QCs and duplicate samples have been met,
may results be forwarded for reporting.
2) Each tray of no more than 30 samples shall contain one QC and two randomly selected
duplicate samples, chosen either automatically by use of suitable electronic means or manually
by the supervisor. A second QC and randomly selected duplicate sample may be included as
safeguard, should either the first QC or randomly selected duplicate sample be lost as a result
of a defective crucible.
3)
When assessing the performance of the QC(s), the following rules shall apply:
a) If the tray contains only one QC, the value of the QC shall be recorded and compared to
current working limits and/or control charts to determine its validity (refer to the section
Section No.:
METHOD
GRAVIMETRIC FINISH
Compiled by:
Signature:
Approved by:
Signature:
Page 14 (of 18)

Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
titled: Assuring the quality of test results of the quality manual). Failure of the QC shall
render all results for the tray in which it is contained invalid.
b) If the tray contains two QCs, the values of the QCs shall be recorded and compared to
current working limits and/or control charts to determine their validity (refer to the section
titled: Assuring the quality of test results of the quality manual). Failure of either of the
QCs shall render all results for the tray in which it is contained invalid irrespective of
whether the other QC conforms to control limits unless the failure can be attributed to
a defective crucible. By implication, failure of both QCs (for whatever reason) shall
render all results for the tray in which they are contained invalid.
4)
New QC values, with the exception of gross outliers, shall be transferred to a chart pertaining
to the relevant QC. If any sign of loss of control becomes apparent, a preventive action report
shall be raised and handed to the Laboratory Manager without delay (refer to the sections
titled: Assuring the quality of test results and Preventive action of the quality manual).
5)
When assessing the performance of the duplicate(s), the following rules shall apply:
a) If the tray contains only one set of duplicates, failure of the duplicates to comply with the
limit as defined in paragraph 12.3 shall render all results for the tray in which they are
contained invalid.
b) If the tray contains two sets of duplicates, at least one set of the duplicates shall conform
to the limit as defined in paragraph 12.3. However, unless the failure can be attributed to
a defective crucible, a replicate of the failed duplicate shall be reanalysed to establish
conformance to the limit as defined in paragraph 12.3. Failure of the replicate to comply
with this limit, shall render all results for the tray of which it originally formed part, invalid.
c) If the tray contains two sets of duplicates, and both fail to comply with the limit as
defined in paragraph 12.3, the entire tray shall be repeated, as the possibility that
samples may have been swapped around during the fluxing procedure is very real.
6)
Additional repeats may also be done at the discretion of the Laboratory Manager. These
additional repeats shall be selected by looking for samples differing from the norm or chosen
randomly.
15.
Rounding off and reporting of results:
1)
Manual rounding off of results:

When truncating results manually as indicated in Table M 501-2, the following rules shall
apply:
Section No.:
METHOD
Page 15 (of 18)

GRAVIMETRIC FINISH
Compiled by:
Signature:
Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
Approved by:
Signature:
a) As a practical operating rule, the results of a calculation whereby several numbers are
multiplied or divided, are rounded off to as few significant figures that are present in the
factor.
b) Assuming the following calculation must be made to obtain the result
56 x 0.003 462 x 43.22
1.684
A ten place calculator yields an answer of 4.975 740 998. Round off this number to
5.0 because one of the measurements that entered into the calculation, 56 has only
two significant figures. It was unnecessary to measure the other three factors to four
significant figures because the 56 is the weakest link in the chain and limits the
accuracy of the answer.
2) Applying the above principle to a typical analysis situation in a fire assay laboratory.
Table M 501-2:
A
Calculation g/t
Sample mass
grams
Au prill
mass
milligrams
Mg Au X 1000
Sample mass
Decimal places
Weakest link in
chain
Number of
Allowed when
significant
Significant figures
figures
grams
Are applied to
Reported value
g/t Au
calculation
150.0
0.025
0.167
150.0
Four
Three
0.167
125.0
0.029
0.232
125.0
Four
Three
0.232
100.0
0.034
0.340
100.0
Four
Three
0.340
50.0
0.084
1.680
50.0
Three
Two
1.68
25.0
0.198
7.920
25.0
Three
Two
7.92
10.0
0.229
22.900
10.0
Three
One
22.9
5.0
1.256
251.2
5.0
Two
None
251
The gram masses obtained in column A are based on one decimal place balances currently
being used.
3) The mg values obtained as indicated in column B are based on readings obtained on a
microbalance with a readability of 1 microgram.
4) Practical tables 002 and 003 as indicated in Reporting of results shall be used as
references to indicate decimal places allowed, taking sample masses and value range into
account.
Section No.:
METHOD
GRAVIMETRIC FINISH
Compiled by:
Signature:
Approved by:
Signature:
Page 16 (of 18)

Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
5) Rounding off of results by means of Microsoft Excel or Goldsoft 2007 veriLIMS:

In the raw state, both software packages employ the same rules as outlined in paragraph
14.1. It is possible to adapt the functionality of the software by applying additional formulas
and/or conditions. Due caution shall be exercised to ensure that alterations to the processing
properties of the software would not allow the rules given in paragraph 14.1 to be breached.
6)
The Quality Controller shall run regular monthly checks to establish the integrity of rounding off
and/or truncating procedures for both Microsoft Excel and Goldsoft 2007 veriLIMS at points of
reporting and keep a log of the investigation.
16.
Reporting of results:
1)
All results shall be signed and dated by the analyst performing the test.
2)
Results shall be reported as indicated in Tables M 501-3 and M 501-4.
3) Table M 501-3:
For sample masses of 100-150g
Au value range g/t
0.09 1
1 10
10 100
>100
Decimal places allowed

3
2
1
0
4) With reference to range 0.09-1g/t, certain clients only require results to be reported to 2
decimal places
5) The most likely values to be encountered in the 100 150g sample range are between 0.09
and 1g/t.
Table M 501-4:
For sample masses of 10 100g
Section No.:
METHOD
GRAVIMETRIC FINISH
Compiled by:
Signature:
Au value range g/t

0.09 1
1 10
10 100
>100
Approved by:
Signature:
Page 17 (of 18)

Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
Decimal places allowed

2
2
1
0
6) With reference to ranges 0.09 1 and 1 10 g/t certain clients require results to be reported
to only 1 decimal place.
7) For sample masses of below 10g no decimal place.
All values obtained in calculation will be rounded up! And all values <0.09g/t to be reported
As <0.09 g/t or the actual value reported as a non accredited value.
17.
1)
Range, limit of detection, uncertainty, bias and precision:

The range, limit of detection, uncertainty, bias and precision of this method is documented in
the validation record titled: Validation - Determination of gold by fire assay and gravimetric
finish: Method M 501.
References:
Lenahan, W.C. and Murray-Smith, R. de L. 1986. Assay and Analytical Practice in the South
African Mining Industry. The South African Institute of Mining and Metallurgy Monograph
Series M6, Johannesburg.
Olivier, R.P. 2003-09-22. Acceptance criteria for duplicate analyses (Internal record). Performance
Laboratories, Randfontein.
Appendix:
APPENDIX M 501-000
REVISION LIST OF METHOD
Section No.:
METHOD
GRAVIMETRIC FINISH
Compiled by:
Signature:
Approved by:
Signature:
END OF DOCUMENT
Page 18 (of 18)

Document No.:
M501
Revision No.
0003
Effective date:
1 December 2010
Section No.:
PROCEDURE
GRAVIMETRIC FINISH
REVISION LIST OF METHOD
Compiled by:
Signature:
REVISION No.
Approved by:
Signature:
EFFECTIVE DATE
0001
1 May 2008
0002
1 October 2009
0003
1 December 2010
Page 1 (of 1)
Document No.:
M 501-001
Revision No.
0003
Effective date:
1 December 2010
NATURE OF REVISION
Major revisions refer to revision 0000 for changes. These
major changes includes the methods for carbon & bullion
analyses.
Tabel M501-1; Inserting sample aliquot mass limits for each
type of sample.
11.6 Introduction of plastic bags. 11.7 Transfer sample to
plastic bags.11.9 Removed. 11.13 Add Silver Nitrate using a
burette.
0004
0005
0006
0007
0008
0009
0010
END OF DOCUMENT

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Page 1 (of 18)

Determination of gold by fire assay and gravimetric finish

Scope and application:

Page 2 (of 18)

Health and safety:

DETERMINATION OF GOLD BY FIRE ASSAY AND

Apparatus and equipment:

Page 4 (of 18)

Spatula, capacity approximately 50ml or smaller.

Page 5 (of 18)

46) Bullion parting apparatus

Chemicals and solvents:

Silver nitrate (AgNO3), CP grade or better.

Reagents and standards:

Page 6 (of 18)

Procedure (Fire Assay and gravimetric finish):

DETERMINATION OF GOLD BY FIRE ASSAY AND GRAVIMETRIC FINISH

DETERMINATION OF GOLD BY FIRE ASSAY AND GRAVIMETRIC FINISH

Table M501-1 (continued):

AgNO3 addition may be increased correspondingly if a higher value result is expected.

Page 9 (of 18)

Page 10 (of 18)

Page 11 (of 18)

12. Procedure (Bullion):

Add approximately 15 mg of copper in the form of a piece of metallic copper.

Seal lead envelope.

Page 12 (of 18)

11) Place the rolled cornets into the parting apparatus.

Calculation of the gold concentration:

Sample mass (g)

grams/tonne (g/t Au)

Page 13 (of 18)

Mine & Head samples

Page 14 (of 18)

Rounding off and reporting of results:

Manual rounding off of results:

DETERMINATION OF GOLD BY FIRE ASSAY AND

Page 16 (of 18)

5) Rounding off of results by means of Microsoft Excel or Goldsoft 2007 veriLIMS:

Results shall be reported as indicated in Tables M 501-3 and M 501-4.

Decimal places allowed

Au value range g/t

Page 17 (of 18)

Decimal places allowed

Range, limit of detection, uncertainty, bias and precision:

REVISION LIST OF METHOD

Page 18 (of 18)

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