Standard
AS 1038.11-2002
[Withdrawn]Coal and coke — Analysis and testing, Part 11: Coal — Forms of sulfur
Sets out methods for the determination of sulfate sulfur, pyritic sulfur and organic sulfur in coal.
Published: 13/11/2002
Pages: 16
Table of contents
Cited references
Content history
Table of contents
Header
About this publication
PREFACE
FOREWORD
1 SCOPE AND GENERAL
1.1 SCOPE
1.2 REFERENCED DOCUMENTS
1.3 DEFINITIONS
1.4 PRINCIPLE
1.5 SAFETY
1.6 SAMPLE
1.6.1 General
1.6.2 Equilibration
1.7 REPORTING OF RESULTS
1.8 PRECISION
1.9 TEST REPORT
2 DETERMINATION OF SULFATE SULFUR
2.1 PRINCIPLE
2.2 REAGENTS
2.2.1 General
2.2.2 Hydrochloric acid (ρ20 1.18 g/mL)
2.2.3 Hydrochloric acid (ρ20 1.18 g/mL) diluted 1 + 1
2.2.4 Ammonia solution (ρ20 0.88 g/mL) diluted 1 + 2
2.2.5 Barium chloride solution (100 g/L)
2.2.6 Potassium sulfate solution (2 g/L)
2.2.7 Methyl red indicator solution (0.2 g/L)
2.2.8 Wetting agent
2.3 APPARATUS
2.3.1 General
2.3.2 Weighing device
2.3.3 Extraction flask
2.3.4 Condenser
2.3.5 Muffle furnace
2.3.6 Plate
2.3.7 Silica crucible
2.4 PROCEDURE
2.4.1 Number of determinations
2.4.2 Blank test
2.4.3 Determination
2.5 CALCULATION
3 DETERMINATION OF PYRITIC SULFUR
3.1 PRINCIPLE
3.2 EXTRACTION OF THE PYRITIC IRON
3.2.1 Reagents
3.2.1.1 General
3.2.1.2 Hydrochloric acid (ρ20 1.18 g/mL) diluted 1 + 1
3.2.1.3 Nitric acid (ρ20 1.42 g/mL) diluted 2 + 13
3.2.1.4 Hydrogen peroxide solution (300 g/L)
3.2.1.5 Wetting agent
3.2.2 Apparatus
3.2.2.1 General
3.2.2.2 Weighing device
3.2.2.3 Extraction flask
3.2.2.4 Condenser
3.2.3 Procedure
3.2.3.1 Number of determinations
3.2.3.2 Blank test
3.2.3.3 Extraction
3.3 DETERMINATION OF PYRITIC IRON—TITRIMETRIC METHOD
3.3.1 Reagents
3.3.1.1 General
3.3.1.2 Ammonia solution (ρ20 0.88 g/mL)
3.3.1.3 Tin(II) chloride solution (5 g/L)
3.3.1.4 Mercury(II) chloride solution
3.3.1.5 Sulfuric acid/phosphoric acid mixture
3.3.1.6 Potassium dichromate solution (about 0.0033 mol/L)
3.3.1.7 Methyl red indicator solution (0.2 g/L)
3.3.1.8 Sodium diphenylamine sulfonate indicator solution (2 g/L)
3.3.2 Apparatus
3.3.2.1 General
3.3.2.2 Cold water bath
3.3.3 Determination
3.3.4 Calculation of result
3.4 DETERMINATION OF PYRITIC IRON—SPECTROPHOTOMETRIC METHOD
3.4.1 Reagents
3.4.1.1 General
3.4.1.2 Hydroxylamine hydrochloride solution (100 g/L)
3.4.1.3 Sodium acetate solution (328 g/L)
3.4.1.4 Stock iron solution (1 mL ≡ 100 μg Fe)
3.4.1.5 1,10-Phenanthroline solution (2.5 g/L)
3.4.1.6 Congo red paper
3.4.2 Apparatus
3.4.2.1 General
3.4.2.2 Spectrophotometer
3.4.3 Procedure
3.4.4 Preparation of calibration graph
3.4.5 Calculation of result
3.5 DETERMINATION OF PYRITIC IRON—ATOMIC ABSORPTION SPECTROMETRIC METHOD
3.5.1 Reagents
3.5.1.1 General
3.5.1.2 Ammonia solution (ρ20 0.88 g/mL) diluted 1 + 2
3.5.1.3 Stock iron solution (1 mL ≡ 100 μg Fe)
3.5.1.4 Nitric acid (ρ20 1.4 g/mL) diluted 2 + 13
3.5.2 Apparatus
3.5.2.1 General
3.5.2.2 Atomic absorption spectrometer
3.5.3 Procedure
3.5.4 Calibration graph
3.5.5 Calculation of result
4 ORGANIC SULFUR
APPENDIX A
A1 GENERAL
A2 SULFATE SULFUR (see Clause 2.5)
A3 PYRITIC SULFUR-TITRIMETRIC (see Clause 3.3.4)
A4 PYRITIC SULFUR-SPECTROPHOTOMETRIC (see Clause 3.4.5)
A5 PYRITIC SULFUR-ATOMIC ABSORPTION (see Clause 3.5.5)
Cited references in this standard
[Current]
Recommended practice for chemical analysis by atomic absorption spectrometry, Part 1: Flame atomic absorption spectrometry
[Withdrawn]
Coal and coke — Analysis and testing, Part 3: Proximate analysis of higher rank coal
AS 1038.6.3
Coal and coke—Analysis and testing, Part 6.3: Ultimate analysis of higher rank coal—Total sulfur (series)
Content history
[Current]
[Superseded]
DR 02073
AS 1038.11-2002 Rec:2013
ISO 157-1996
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