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AS 1038.10.4-2001 (R2013)

AS 1038.10.4-2001 (R2013)

Coal and coke - Analysis and testing Determination of trace elements - Coal, coke and fly-ash - Determination of fluorine content - Pyrohydrolysis method

Standards Australia

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Table of Contents

<toc>
<bookmarktable>
<bookmark index=&apos;0&apos;>
<pageno>1</pageno>
<text>AS 1038.10.4-2001 COAL AND COKE-ANALYSIS AND TESTING - DETERMINATION OF TRACE ELEMENTS-COAL, COKE AND FLY-ASH-DETERMINATION O</text>
<bookmark index=&apos;1&apos;>
<pageno>4</pageno>
<text>PREFACE</text>
</bookmark>
<bookmark index=&apos;2&apos;>
<pageno>4</pageno>
<text>CONTENTS</text>
</bookmark>
<bookmark index=&apos;3&apos;>
<pageno>5</pageno>
<text>FOREWORD</text>
</bookmark>
<bookmark index=&apos;4&apos;>
<pageno>6</pageno>
<text>1 SCOPE</text>
</bookmark>
<bookmark index=&apos;5&apos;>
<pageno>6</pageno>
<text>2 REFERENCED DOCUMENTS</text>
</bookmark>
<bookmark index=&apos;6&apos;>
<pageno>6</pageno>
<text>3 PRINCIPLE</text>
</bookmark>
<bookmark index=&apos;7&apos;>
<pageno>6</pageno>
<text>4 SAFETY</text>
</bookmark>
<bookmark index=&apos;8&apos;>
<pageno>6</pageno>
<text>5 REAGENTS</text>
<bookmark index=&apos;9&apos;>
<pageno>6</pageno>
<text>5.1 General</text>
</bookmark>
<bookmark index=&apos;10&apos;>
<pageno>7</pageno>
<text>5.2 Silica</text>
</bookmark>
<bookmark index=&apos;11&apos;>
<pageno>7</pageno>
<text>5.3 Solutions for ISE measurement</text>
<bookmark index=&apos;12&apos;>
<pageno>7</pageno>
<text>5.3.1 Standard fluorine solution (1 g = 200 ug F)</text>
</bookmark>
<bookmark index=&apos;13&apos;>
<pageno>7</pageno>
<text>5.3.2 Absorption solution (0.025 mol/L NaOH)</text>
</bookmark>
<bookmark index=&apos;14&apos;>
<pageno>7</pageno>
<text>5.3.3 Unspiked buffered absorption solution (pH 6.5)</text>
</bookmark>
<bookmark index=&apos;15&apos;>
<pageno>7</pageno>
<text>5.3.4 Buffer added after pyrohydrolysis (pH 6.5)</text>
</bookmark>
<bookmark index=&apos;16&apos;>
<pageno>7</pageno>
<text>5.3.5 Solutions for conditioning fluoride ISE</text>
</bookmark>
</bookmark>
<bookmark index=&apos;17&apos;>
<pageno>7</pageno>
<text>5.4 Solutions for IC measurement</text>
<bookmark index=&apos;18&apos;>
<pageno>7</pageno>
<text>5.4.1 Standard fluorine solution (1 g = 200 ug F)</text>
</bookmark>
<bookmark index=&apos;19&apos;>
<pageno>7</pageno>
<text>5.4.2 Absorption solution</text>
</bookmark>
</bookmark>
<bookmark index=&apos;20&apos;>
<pageno>7</pageno>
<text>5.5 Oxygen</text>
</bookmark>
</bookmark>
<bookmark index=&apos;21&apos;>
<pageno>7</pageno>
<text>6 APPARATUS</text>
<bookmark index=&apos;22&apos;>
<pageno>7</pageno>
<text>6.1 Vials</text>
</bookmark>
<bookmark index=&apos;23&apos;>
<pageno>8</pageno>
<text>6.2 Polypropylene bottles (or polystyrene vials)</text>
</bookmark>
<bookmark index=&apos;24&apos;>
<pageno>8</pageno>
<text>6.3 Polystyrene vials</text>
</bookmark>
<bookmark index=&apos;25&apos;>
<pageno>8</pageno>
<text>6.4 Balances</text>
</bookmark>
<bookmark index=&apos;26&apos;>
<pageno>8</pageno>
<text>6.5 Polyethylene dispensing bottles</text>
</bookmark>
<bookmark index=&apos;27&apos;>
<pageno>8</pageno>
<text>6.6 Micropipette</text>
</bookmark>
<bookmark index=&apos;28&apos;>
<pageno>8</pageno>
<text>6.7 Apparatus for tube furnace pyrohydrolysis (see Figure 1).</text>
<bookmark index=&apos;29&apos;>
<pageno>8</pageno>
<text>6.7.1 Steam generator</text>
</bookmark>
<bookmark index=&apos;30&apos;>
<pageno>8</pageno>
<text>6.7.2 Silica tube furnace and accessories</text>
</bookmark>
<bookmark index=&apos;31&apos;>
<pageno>9</pageno>
<text>6.7.3 Absorption vessel</text>
</bookmark>
<bookmark index=&apos;32&apos;>
<pageno>9</pageno>
<text>6.7.4 Water jacket</text>
</bookmark>
</bookmark>
<bookmark index=&apos;33&apos;>
<pageno>9</pageno>
<text>6.8 ISE measurement apparatus</text>
<bookmark index=&apos;34&apos;>
<pageno>9</pageno>
<text>6.8.1 Magnetic stirrer</text>
</bookmark>
<bookmark index=&apos;35&apos;>
<pageno>9</pageno>
<text>6.8.2 Electrodes</text>
</bookmark>
<bookmark index=&apos;36&apos;>
<pageno>9</pageno>
<text>6.8.3 Multivolt meter</text>
</bookmark>
</bookmark>
<bookmark index=&apos;37&apos;>
<pageno>9</pageno>
<text>6.9 IC measurement apparatus</text>
</bookmark>
</bookmark>
<bookmark index=&apos;38&apos;>
<pageno>9</pageno>
<text>7 SAMPLE</text>
<bookmark index=&apos;39&apos;>
<pageno>9</pageno>
<text>7.1 Coal and coke</text>
</bookmark>
<bookmark index=&apos;40&apos;>
<pageno>9</pageno>
<text>7.2 Fly-ash</text>
</bookmark>
</bookmark>
<bookmark index=&apos;41&apos;>
<pageno>9</pageno>
<text>8 PROCEDURE</text>
<bookmark index=&apos;42&apos;>
<pageno>9</pageno>
<text>8.1 Number of determinations</text>
</bookmark>
<bookmark index=&apos;43&apos;>
<pageno>9</pageno>
<text>8.2 Blank tests</text>
</bookmark>
<bookmark index=&apos;44&apos;>
<pageno>11</pageno>
<text>8.3 Test sample preparation</text>
</bookmark>
<bookmark index=&apos;45&apos;>
<pageno>11</pageno>
<text>8.4 Pyrohydrolysis</text>
<bookmark index=&apos;46&apos;>
<pageno>11</pageno>
<text>8.4.1 Apparatus conditioning</text>
</bookmark>
<bookmark index=&apos;47&apos;>
<pageno>11</pageno>
<text>8.4.2 Pyrohydrolysis</text>
</bookmark>
<bookmark index=&apos;48&apos;>
<pageno>11</pageno>
<text>8.4.3 Pyrohydrolysate processing</text>
</bookmark>
</bookmark>
<bookmark index=&apos;49&apos;>
<pageno>12</pageno>
<text>8.5 Solution measurement</text>
<bookmark index=&apos;50&apos;>
<pageno>12</pageno>
<text>8.5.1 General</text>
</bookmark>
<bookmark index=&apos;51&apos;>
<pageno>12</pageno>
<text>8.5.2 Direct-comparsion ISE method</text>
</bookmark>
<bookmark index=&apos;52&apos;>
<pageno>13</pageno>
<text>8.5.3 Analyte-addition ISE method</text>
</bookmark>
<bookmark index=&apos;53&apos;>
<pageno>13</pageno>
<text>8.5.4 IC method</text>
</bookmark>
</bookmark>
</bookmark>
<bookmark index=&apos;54&apos;>
<pageno>13</pageno>
<text>9 CALCULATIONS</text>
<bookmark index=&apos;55&apos;>
<pageno>13</pageno>
<text>9.1 General</text>
</bookmark>
<bookmark index=&apos;56&apos;>
<pageno>14</pageno>
<text>9.2 Direct-comparison ISE method</text>
</bookmark>
<bookmark index=&apos;57&apos;>
<pageno>14</pageno>
<text>9.3 IC method</text>
</bookmark>
<bookmark index=&apos;58&apos;>
<pageno>14</pageno>
<text>9.4 Analyte-addition ISE method</text>
</bookmark>
</bookmark>
<bookmark index=&apos;59&apos;>
<pageno>15</pageno>
<text>10 REPORTING OF RESULT</text>
</bookmark>
<bookmark index=&apos;60&apos;>
<pageno>15</pageno>
<text>11 PRECISION OF THE DETERMINATION</text>
</bookmark>
<bookmark index=&apos;61&apos;>
<pageno>16</pageno>
<text>12 TEST REPORT</text>
</bookmark>
<bookmark index=&apos;62&apos;>
<pageno>17</pageno>
<text>APPENDIX A - DETERMINATION OF FLUORIDE ELECTRODE SLOPE, RESPONSE TIME AND RESPONSE CURVE</text>
<bookmark index=&apos;63&apos;>
<pageno>17</pageno>
<text>A1 SCOPE</text>
</bookmark>
<bookmark index=&apos;64&apos;>
<pageno>17</pageno>
<text>A2 SLOPE AND RESPONSE TIME MEASUREMENT</text>
</bookmark>
<bookmark index=&apos;65&apos;>
<pageno>17</pageno>
<text>A3 SLOPE CALCULATION</text>
</bookmark>
<bookmark index=&apos;66&apos;>
<pageno>19</pageno>
<text>A4 WORKED EXAMPLE OF BLANK AND SLOPE MEASUREMENT BY DOUBLE ANALYTE ADDITION</text>
</bookmark>
<bookmark index=&apos;67&apos;>
<pageno>20</pageno>
<text>A5 WORKED EXAMPLE OF DETERMINATION OF FLUORINE IN COAL BY ISE MEASUREMENT BY SINGLE ANALYTE ADDITION</text>
</bookmark>
</bookmark>
</bookmark>
</bookmarktable>
</toc>

Abstract

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.

RECONFIRMATION NOTICE
Technical Committee MN-001 has reviewed the content of this publication and in accordance with Standards Australia procedures for reconfirmation, it has been determined that the publication is still valid and does not require change.
Certain documents referenced in the publication may have been amended since the original date of publication. Users are advised to ensure that they are using the latest versions of such documents as appropriate, unless advised otherwise in this Reconfirmation Notice.
Approved for reconfirmation in accordance with Standards Australia procedures for reconfirmation on 15 July 2013.
The following are represented on Technical Committee MN-001:

Australasian Institute of Mining and Metallurgy
Australian Coal Association
Australian Coal Industry Reference Samples
Australian Coal Preparation Society
Bureau of Steel Manufacturers of Australia
Coalfield Geology Council of NSW
CSIRO Energy Technology
National Association of Testing Authorities Australia
National Generators Forum
The University of New South Wales
The University of Queensland
University of Newcastle


To view or download a copy of the reconfirmation notice please go to the reconfirmation link near the top of this page.

Scope

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.

General Product Information

Document Type Standard
Status Current
Publisher Standards Australia
ProductNote Reconfirmed 06-08-2013
Committee MN-001
Supersedes
  • DR 00052
  • AS 1038.10.4-1989

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