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AS 1038.10.4-2001 (R2013)
M00004106
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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>
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<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>
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<pageno>4</pageno>
<text>PREFACE</text>
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<pageno>4</pageno>
<text>CONTENTS</text>
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<pageno>5</pageno>
<text>FOREWORD</text>
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<pageno>6</pageno>
<text>1 SCOPE</text>
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<pageno>6</pageno>
<text>2 REFERENCED DOCUMENTS</text>
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<pageno>6</pageno>
<text>3 PRINCIPLE</text>
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<pageno>6</pageno>
<text>4 SAFETY</text>
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<bookmark index='8'>
<pageno>6</pageno>
<text>5 REAGENTS</text>
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<pageno>6</pageno>
<text>5.1 General</text>
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<pageno>7</pageno>
<text>5.2 Silica</text>
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<pageno>7</pageno>
<text>5.3 Solutions for ISE measurement</text>
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<pageno>7</pageno>
<text>5.3.1 Standard fluorine solution (1 g = 200 ug F)</text>
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<pageno>7</pageno>
<text>5.3.2 Absorption solution (0.025 mol/L NaOH)</text>
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<pageno>7</pageno>
<text>5.3.3 Unspiked buffered absorption solution (pH 6.5)</text>
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<pageno>7</pageno>
<text>5.3.4 Buffer added after pyrohydrolysis (pH 6.5)</text>
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<pageno>7</pageno>
<text>5.3.5 Solutions for conditioning fluoride ISE</text>
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</bookmark>
<bookmark index='17'>
<pageno>7</pageno>
<text>5.4 Solutions for IC measurement</text>
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<pageno>7</pageno>
<text>5.4.1 Standard fluorine solution (1 g = 200 ug F)</text>
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<pageno>7</pageno>
<text>5.4.2 Absorption solution</text>
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</bookmark>
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<pageno>7</pageno>
<text>5.5 Oxygen</text>
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<pageno>7</pageno>
<text>6 APPARATUS</text>
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<pageno>7</pageno>
<text>6.1 Vials</text>
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<pageno>8</pageno>
<text>6.2 Polypropylene bottles (or polystyrene vials)</text>
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<pageno>8</pageno>
<text>6.3 Polystyrene vials</text>
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<bookmark index='25'>
<pageno>8</pageno>
<text>6.4 Balances</text>
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<pageno>8</pageno>
<text>6.5 Polyethylene dispensing bottles</text>
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<pageno>8</pageno>
<text>6.6 Micropipette</text>
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<pageno>8</pageno>
<text>6.7 Apparatus for tube furnace pyrohydrolysis (see Figure 1).</text>
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<pageno>8</pageno>
<text>6.7.1 Steam generator</text>
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<pageno>8</pageno>
<text>6.7.2 Silica tube furnace and accessories</text>
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<pageno>9</pageno>
<text>6.7.3 Absorption vessel</text>
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<pageno>9</pageno>
<text>6.7.4 Water jacket</text>
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<pageno>9</pageno>
<text>6.8 ISE measurement apparatus</text>
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<pageno>9</pageno>
<text>6.8.1 Magnetic stirrer</text>
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<pageno>9</pageno>
<text>6.8.2 Electrodes</text>
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<bookmark index='36'>
<pageno>9</pageno>
<text>6.8.3 Multivolt meter</text>
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<pageno>9</pageno>
<text>6.9 IC measurement apparatus</text>
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<pageno>9</pageno>
<text>7 SAMPLE</text>
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<pageno>9</pageno>
<text>7.1 Coal and coke</text>
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<pageno>9</pageno>
<text>7.2 Fly-ash</text>
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<pageno>9</pageno>
<text>8 PROCEDURE</text>
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<pageno>9</pageno>
<text>8.1 Number of determinations</text>
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<pageno>9</pageno>
<text>8.2 Blank tests</text>
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<pageno>11</pageno>
<text>8.3 Test sample preparation</text>
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<bookmark index='45'>
<pageno>11</pageno>
<text>8.4 Pyrohydrolysis</text>
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<pageno>11</pageno>
<text>8.4.1 Apparatus conditioning</text>
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<bookmark index='47'>
<pageno>11</pageno>
<text>8.4.2 Pyrohydrolysis</text>
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<pageno>11</pageno>
<text>8.4.3 Pyrohydrolysate processing</text>
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<pageno>12</pageno>
<text>8.5 Solution measurement</text>
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<pageno>12</pageno>
<text>8.5.1 General</text>
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<bookmark index='51'>
<pageno>12</pageno>
<text>8.5.2 Direct-comparsion ISE method</text>
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<pageno>13</pageno>
<text>8.5.3 Analyte-addition ISE method</text>
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<pageno>13</pageno>
<text>8.5.4 IC method</text>
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<pageno>13</pageno>
<text>9 CALCULATIONS</text>
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<pageno>13</pageno>
<text>9.1 General</text>
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<pageno>14</pageno>
<text>9.2 Direct-comparison ISE method</text>
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<pageno>14</pageno>
<text>9.3 IC method</text>
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<pageno>14</pageno>
<text>9.4 Analyte-addition ISE method</text>
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<pageno>15</pageno>
<text>10 REPORTING OF RESULT</text>
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<pageno>15</pageno>
<text>11 PRECISION OF THE DETERMINATION</text>
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<pageno>16</pageno>
<text>12 TEST REPORT</text>
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<pageno>17</pageno>
<text>APPENDIX A - DETERMINATION OF FLUORIDE ELECTRODE SLOPE, RESPONSE TIME AND RESPONSE CURVE</text>
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<text>A1 SCOPE</text>
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<bookmark index='64'>
<pageno>17</pageno>
<text>A2 SLOPE AND RESPONSE TIME MEASUREMENT</text>
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<pageno>17</pageno>
<text>A3 SLOPE CALCULATION</text>
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<bookmark index='66'>
<pageno>19</pageno>
<text>A4 WORKED EXAMPLE OF BLANK AND SLOPE MEASUREMENT BY DOUBLE ANALYTE ADDITION</text>
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<pageno>20</pageno>
<text>A5 WORKED EXAMPLE OF DETERMINATION OF FLUORINE IN COAL BY ISE MEASUREMENT BY SINGLE ANALYTE ADDITION</text>
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</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 |
|