Standard
AS 1038.10.4-2001
[Withdrawn]Coal and coke — Analysis and testing, Part 10.4: Determination of trace elements — Coal, coke and fly-ash — Determination of fluorine content — Pyrohydrolysis method
Sets out a procedure for the pyrohydrolytic separation of fluorine from coal, coke and fly-ash and for determination of fluorine by gravimetric processing and either ion potentiometry or ion chromatography.
Published: 29/06/2001
Pages: 15
Table of contents
Cited references
Content history
Table of contents
Header
About this publication
Preface
Foreword
1 Scope
2 Referenced documents
3 Principle
4 Safety
5 Reagents
5.1 General
5.2 Silica
5.3 Solutions for ISE measurement
5.3.1 Standard fluorine solution (1 g = 200 μg F)
5.3.2 Absorption solution (0.025 mol/L NaOH)
5.3.3 Unspiked buffered absorption solution (pH 6.5)
5.3.4 Buffer added after pyrohydrolysis (pH 6.5)
5.3.5 Solutions for conditioning fluoride ISE
5.4 Solutions for IC measurement
5.4.1 Standard fluorine solution (1 g = 200 µg F)
5.4.2 Absorption solution
5.5 Oxygen
6 Apparatus
6.1 Vials
6.2 Polypropylene bottles (or polystyrene vials)
6.3 Polystyrene vials
6.4 Balances
6.5 Polyethylene dispensing bottles
6.6 Micropipette
6.7 Apparatus for tube furnace pyrohydrolysis (see Figure 1).
6.7.1 Steam generator
6.7.2 Silica tube furnace and accessories
6.7.3 Absorption vessel
6.7.4 Water jacket
6.8 ISE measurement apparatus
6.8.1 Magnetic stirrer
6.8.2 Electrodes
6.8.3 Millivolt meter
6.9 IC measurement apparatus
7 Sample
7.1 Coal and coke
7.2 Fly‑ash
8 Procedure
8.1 Number of determinations
8.2 Blank tests
8.3 Test sample preparation
8.4 Pyrohydrolysis
8.4.1 Apparatus conditioning
8.4.2 Pyrohydrolysis
8.4.3 Pyrohydrolysate processing
8.5 Solution measurement
8.5.1 General
8.5.2 Direct‑comparison ISE method
8.5.3 Analyte‑addition ISE method
8.5.4 IC method
9 Calculations
9.1 General
9.2 Direct‑comparison ISE method
9.3 IC method
9.4 Analyte‑addition ISE method
10 Reporting of result
11 Precision of the determination
12 Test report
Appendix A
A1 Scope
A2 Slope and response time measurement
A3 Slope calculation
A4 Worked example of blank and slope measurement by double analyte addition
A5 Worked example of determination of fluorine in coal by ISE measurement by single analyte addition
Cited references in this standard
AS 2243
Safety in laboratories (series)
Content history
[Superseded]
[Withdrawn]
AS 1038.10.4-2001 Rec:2013
DR 00052
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