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Specialty Assay Procedure

Sulphur Analysis Methods


S- IR08, S- IR07, S- GRA06, S- GRA06a, S- CAL06, S-
CAL06a, S- GRA08

Sample Decomposition
Various

Analytical Method
Leco sulphur analyzer, Gravimetric

Total Sulphur - Method Code: S- IR08


The sample is analyzed for Total Sulphur using a Leco sulphur analyzer. The sample (0.01 to 0.1 g) is heated to
approximately 1350 C in an induction furnace while passing a stream of oxygen through the sample. Sulphur dioxide
released from the sample is measured by an IR detection system and the Total Sulphur result is provided.

Sulphide Sulphur - Method Code: S- IR07


A prepared sample is selectively leached in warm sodium carbonate solution to convert the metal sulphate into
insoluble carbonates and soluble sulphate. The resulting residue is removed by filtration and the sulphide residue
is washed free of carbonate solution and analyzed by a Leco sulphur analyzer.

Sulphate Sulphur Carbonate Leach - Method Code: S- GRA06


A prepared sample is boiled with a sodium carbonate solution for 30 minutes. Any insoluble materials are
removed by filtration and ferric iron is reduced to ferrous iron by the addition of hydroxylamine hydrochloride.
The sulphate in the resulting filtrate is then precipitated with barium chloride in a dilute hydrochloric acid
medium. The barium sulphate precipitate is filtered, ignited, weighed and calculated as %S (of total sulphate)
in the original sample.

Sulphate Sulphur HCl Leachable - Method Code: S- GRA06a


A prepared sample (0.2 to 1.0 g) is heated with dilute hydrochloric acid for 30 minutes. Silica and any acid-
insoluble materials are removed by filtration and ferric iron is reduced to ferrous iron by the addition of
hydroxylamine hydrochloride. The sulphate in the resulting filtrate is then precipitated with barium chloride in a
dilute hydrochloric acid medium. The barium sulphate precipitate is filtered, ignited, weighed and calculated as
%S (of the HCl-leachable sulphate) in the original sample.

Revision 01.02 | Apr 14, 2009 www.alsglobal.com


Sulphur Analysis Methods
Sulphide Sulphur - Method Code: S- CAL06
Sulphide Sulphur (%S) is calculated by subtracting the Carbonate Leach Sulphate (%S) from the Total Sulphur
(%S) obtained from the Leco analyzer.

Sulphide Sulphur - Method Code: S- CAL06a


Sulphide Sulphur (%S) is calculated by subtracting the HCl Leach Sulphate (%S) from the Total Sulphur (%S)
obtained from the Leco analyzer.

Total Sulphur - Method Code: S- GRA08


The ore sample is digested with nitric acid and potassium chlorate and bromine is added to assist oxidation.
After complete dehydration of the silica and complete removal of the nitric acid and silica, the iron in solution
is reduced with hydroxylamine hydrochloride. The sulphate is then precipitated by the addition of barium
chloride solution and is filtered and weighed as barium sulphate.

Lower Upper
Method Code Description Symbol Units
Limit Limit

S-IR08 Total Sulphur (Leco) S % 0.01 50

S-IR07 Sulphide Sulphur (Leco) S % 0.01 50

S-GRA06 Sulphate Sulphur (carbonate leach) S % 0.01 50

S-GRA06a Sulphate Sulphur (HCl leach) S % 0.01 50

S-CAL06 Sulphide Sulphur (calculated) S % 0.01 50

S-CAL06a Sulphide Sulphur (calculated) S % 0.01 50

S-GRA08 Total Sulphur (Gravimetric) S % 0.01 100

Revision 01.02 | Apr 14, 2009 www.alsglobal.com

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