AS 4030.3-2002

1 - AS 4030.3-2002 LEAD SULFIDE CONCENTRATES-CHEMICAL ANALYSIS - DETERMINATION OF SILVER AND GOLD CONTENTS-FIRE ASSAY AND FLAME A
4 - PREFACE
5 - CONTENTS
7 - 1 Scope
7 - 2 Normative references
7 - 3 Principle
7 - 3.1 Scorification
8 - 3.2 Cupellation
8 - 4 Reagents
8 - 4.1 Sodium carbonate
8 - 4.2 Litharge
8 - 4.3 Silica
8 - 4.4 Potassium nitrate or sodium nitrate
8 - 4.5 Flour
8 - 4.6 Nitric acid
8 - 4.7 Nitric acid wash solution
8 - 4.8 Nitric acid
8 - 4.9 Hydrochloric acid
8 - 4.10 Borax
8 - 4.11 Silver metal
8 - 4.12 Gold metal
8 - 4.13 Aqua regia
8 - 4.14 Ammonia solution
8 - 4.15 Sodium chloride
8 - 4.16 Standard solutions
9 - 4.16.1 Silver standard solutions
9 - 4.16.2 Gold standard solutions
9 - 4.17 Calibration solutions
9 - 4.17.1 Silver calibration solutions
10 - 4.17.2 Gold calibration solutions
10 - 5 Apparatus
10 - 5.1 Volumetric glassware,
10 - 5.2 Conventional fire assay equipment
10 - 5.2.1 Assay crucible furnace
10 - 5.2.2 Muffle furnace
10 - 5.2.3 Crucibles
10 - 5.2.4 Scorifiers
10 - 5.2.5 Cupels
10 - 5.2.6 Conical mould
10 - 5.2.7 Pulverizer
10 - 5.3 Balances
10 - 5.3.1 Top loading
10 - 5.3.2 Precision analytical
10 - 5.4 Atomic absorption spectrometer (AAS)
10 - 5.5 Filtration equipment
10 - 5.5.1 Membrane filter - cellulose nitrate/cellulose acetate
10 - 5.5.2 Vacuum flask
10 - 5.5.3 Membrane filter funnel
10 - 5.6 Burette
11 - 6 Sample
11 - 6.1 Test sample
11 - 6.2 Test portion
11 - 7 Procedure
11 - 7.1 Number of determinations
11 - 7.2 Trial fusion
11 - 7.3 Blank tests
11 - 7.4 Charge preparation
12 - 7.5 Primary fusion
12 - 7.6 Selection of recovery procedure
13 - 7.7 Scorification
13 - 7.7.1 General
13 - 7.7.2 Retreatment fusion
13 - 7.7.3 Scorification
13 - 7.8 Cupellation
13 - 7.8.1 General
14 - 7.8.2 Retreatment fusion
14 - 7.8.3 Cupellation
14 - 7.9 Treatment of the lead buttons or silver/gold beads
14 - 7.10 Determination of silver in the test solution by flame atomic absorption spectrometry
15 - 7.11 Determination of gold in the test solution by flame atomic absorption spectrometry
16 - 8 Expression of results
16 - 8.1 Silver content
16 - 8.2 Gold content
16 - 9 Precision
16 - 9.1 Expression of precision
17 - 9.2 Method for obtaining the final result
17 - 9.3 Precision between laboratories
18 - 9.4 Check of trueness
19 - 10 Test report
20 - Annex A - Procedure for the preparation and determination of the mass of a predried test portion
20 - A.1 Scope
20 - A.2 Principle
20 - A.3 Reagents
20 - A.4 Apparatus
20 - A.5 Procedure
20 - A.5.1 Preparation of the weighing vessel
20 - A.5.2 Test portion
21 - A.5.3 Determination of the test portion dry mass
21 - A.6 Calculation of the test portion dry mass
22 - Annex B - Trial fusion
22 - B.1 Introduction
22 - B.2 Procedure
23 - Annex C - Blank determination
23 - C.1 Introduction
23 - C.2 Procedure
24 - Annex D - Flowsheet of the procedure for the acceptance of analytical values for the test samples
25 - Annex E - Derivation of precision equations
25 - E.1 Introduction
25 - E.2 Design of test programme
25 - E.3 Test samples
25 - E.4 Statistical evaluation
32 - Annex F - Bibliography

Sets out a fire assay flame AAS method for determining the silver and gold contents of lead sulfide concentrates. This Standard is identical with and has been reproduced from ISO 12740:1998.

This International Standard specifies a fire assay and flame atomic absorption spectrometric procedure for the determination of silver and gold contents of lead sulfide concentrates.The method is applicable to the determination of silver and gold in lead sulfide concentrates containing 10 % (m/m) to 80 % (m/m) lead.The method is applicable to silver contents from 200 g/t to 2 000 g/t and gold contents from 0,1 g/t to 25 g/t.

First published as AS 4030.3-2002.