AS 1038.10.4-2001

This Standard has been reconfirmed. To view or download the Reconfirmation Notice please click here.

1 - AS 1038.10.4-2001 COAL AND COKE-ANALYSIS AND TESTING - DETERMINATION OF TRACE ELEMENTS-COAL, COKE AND FLY-ASH-DETERMINATION O
4 - PREFACE
4 - CONTENTS
5 - FOREWORD
6 - 1 SCOPE
6 - 2 REFERENCED DOCUMENTS
6 - 3 PRINCIPLE
6 - 4 SAFETY
6 - 5 REAGENTS
6 - 5.1 General
7 - 5.2 Silica
7 - 5.3 Solutions for ISE measurement
7 - 5.3.1 Standard fluorine solution (1 g = 200 ug F)
7 - 5.3.2 Absorption solution (0.025 mol/L NaOH)
7 - 5.3.3 Unspiked buffered absorption solution (pH 6.5)
7 - 5.3.4 Buffer added after pyrohydrolysis (pH 6.5)
7 - 5.3.5 Solutions for conditioning fluoride ISE
7 - 5.4 Solutions for IC measurement
7 - 5.4.1 Standard fluorine solution (1 g = 200 ug F)
7 - 5.4.2 Absorption solution
7 - 5.5 Oxygen
7 - 6 APPARATUS
7 - 6.1 Vials
8 - 6.2 Polypropylene bottles (or polystyrene vials)
8 - 6.3 Polystyrene vials
8 - 6.4 Balances
8 - 6.5 Polyethylene dispensing bottles
8 - 6.6 Micropipette
8 - 6.7 Apparatus for tube furnace pyrohydrolysis (see Figure 1).
8 - 6.7.1 Steam generator
8 - 6.7.2 Silica tube furnace and accessories
9 - 6.7.3 Absorption vessel
9 - 6.7.4 Water jacket
9 - 6.8 ISE measurement apparatus
9 - 6.8.1 Magnetic stirrer
9 - 6.8.2 Electrodes
9 - 6.8.3 Multivolt meter
9 - 6.9 IC measurement apparatus
9 - 7 SAMPLE
9 - 7.1 Coal and coke
9 - 7.2 Fly-ash
9 - 8 PROCEDURE
9 - 8.1 Number of determinations
9 - 8.2 Blank tests
11 - 8.3 Test sample preparation
11 - 8.4 Pyrohydrolysis
11 - 8.4.1 Apparatus conditioning
11 - 8.4.2 Pyrohydrolysis
11 - 8.4.3 Pyrohydrolysate processing
12 - 8.5 Solution measurement
12 - 8.5.1 General
12 - 8.5.2 Direct-comparsion ISE method
13 - 8.5.3 Analyte-addition ISE method
13 - 8.5.4 IC method
13 - 9 CALCULATIONS
13 - 9.1 General
14 - 9.2 Direct-comparison ISE method
14 - 9.3 IC method
14 - 9.4 Analyte-addition ISE method
15 - 10 REPORTING OF RESULT
15 - 11 PRECISION OF THE DETERMINATION
16 - 12 TEST REPORT
17 - APPENDIX A - DETERMINATION OF FLUORIDE ELECTRODE SLOPE, RESPONSE TIME AND RESPONSE CURVE
17 - A1 SCOPE
17 - A2 SLOPE AND RESPONSE TIME MEASUREMENT
17 - A3 SLOPE CALCULATION
19 - A4 WORKED EXAMPLE OF BLANK AND SLOPE MEASUREMENT BY DOUBLE ANALYTE ADDITION
20 - A5 WORKED EXAMPLE OF DETERMINATION OF FLUORINE IN COAL BY ISE MEASUREMENT BY SINGLE ANALYTE ADDITION

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.

This Standard 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.

Originated as AS 1038.10.4-1989.
Second edition 2001.