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AS 1038.14.2-2003 (R2013)
M00003463
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AS 1038.14.2-2003 (R2013)
Coal and coke - Analysis and testing Higher rank coal ash and coke ash - Major and minor elements - Acid digestion/flame atomic absorption spectrometric method
Standards Australia
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Table of Contents
<toc>
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<pageno>1</pageno>
<text>AS 1038.14.2-2003 COAL AND COKE-ANALYSIS AND TESTING - HIGHER RANK COAL ASH AND COKE ASH-MAJOR AND MINOR ELEMENTS-ACID...</text>
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<pageno>4</pageno>
<text>PREFACE</text>
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<pageno>5</pageno>
<text>CONTENTS</text>
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<pageno>6</pageno>
<text>1 SCOPE</text>
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<pageno>7</pageno>
<text>2 REFERENCED DOCUMENTS</text>
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<pageno>7</pageno>
<text>3 DEFINITIONS</text>
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<bookmark index='6'>
<pageno>7</pageno>
<text>4 PRINCIPLE</text>
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<pageno>7</pageno>
<text>5 SAFETY</text>
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<bookmark index='8'>
<pageno>7</pageno>
<text>6 REAGENTS</text>
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<pageno>7</pageno>
<text>6.1 General</text>
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<pageno>8</pageno>
<text>6.2 Boric acid (H3BO3)</text>
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<pageno>8</pageno>
<text>6.3 Solutions</text>
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<pageno>8</pageno>
<text>6.3.1 Hydrochloric acid, rho20 1.16 g/mL to 1.19 g/mL.</text>
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<pageno>8</pageno>
<text>6.3.2 Hydrofluoric acid, rho20 1.20 g/mL, 40% w/V.</text>
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<pageno>8</pageno>
<text>6.3.3 Nitric acid, rho20 1.42 g/mL, diluted 1 + 1.</text>
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<pageno>8</pageno>
<text>6.3.4 Acid matrix base solution</text>
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<pageno>8</pageno>
<text>6.3.5 Caesium chloride solution</text>
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<pageno>8</pageno>
<text>6.3.6 Boric acid solution</text>
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<pageno>8</pageno>
<text>6.4 Standard solutions</text>
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<pageno>8</pageno>
<text>6.4.1 Standard aluminium solution</text>
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<pageno>8</pageno>
<text>6.4.2 Standard calcium solution</text>
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<pageno>8</pageno>
<text>6.4.3 Standard iron solution</text>
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<bookmark index='22'>
<pageno>8</pageno>
<text>6.4.4 Standard magnesium solution</text>
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<pageno>8</pageno>
<text>6.4.5 Standard manganese solution</text>
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<bookmark index='24'>
<pageno>9</pageno>
<text>6.4.6 Standard potassium solution</text>
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<bookmark index='25'>
<pageno>9</pageno>
<text>6.4.7 Standard silicon solutions</text>
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<pageno>9</pageno>
<text>6.4.8 Standard sodium solution</text>
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<pageno>9</pageno>
<text>6.4.9 Standard titanium solution</text>
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<pageno>9</pageno>
<text>6.5 Diluted standard solutions</text>
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<pageno>9</pageno>
<text>6.5.1 Dilute standard manganese solution</text>
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<pageno>9</pageno>
<text>6.5.2 Iron/titanium composite solution</text>
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<pageno>10</pageno>
<text>6.5.3 Calcium/magnesium/sodium/potassium composite solution</text>
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<pageno>10</pageno>
<text>6.6 Calibration solutions</text>
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<pageno>10</pageno>
<text>7 APPARATUS</text>
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<pageno>10</pageno>
<text>7.1 General</text>
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<pageno>10</pageno>
<text>7.2 Atomic absorption spectrometer</text>
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<pageno>11</pageno>
<text>7.3 Polytetrafluoroethylene (PTFE) decomposition vessel</text>
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<pageno>11</pageno>
<text>7.4 Polypropylene digestion bottles</text>
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<pageno>11</pageno>
<text>7.5 Plastic bottles</text>
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<pageno>11</pageno>
<text>7.6 Oven</text>
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<pageno>11</pageno>
<text>7.7 Sand bath</text>
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<pageno>11</pageno>
<text>7.8 Boiling-water bath or ultrasonic bath</text>
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<pageno>11</pageno>
<text>7.9 Weighing device</text>
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<pageno>12</pageno>
<text>8 SAMPLE PREPARATION</text>
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<pageno>12</pageno>
<text>9 DETERMINATION OF ALUMINIUM, CALCIUM, IRON, MAGNESIUM, MANGANESE, POTASSIUM, SILICON, SODIUM AND TITANIUM</text>
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<pageno>12</pageno>
<text>9.1 Number of determinations</text>
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<pageno>12</pageno>
<text>9.2 Blank test</text>
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<bookmark index='47'>
<pageno>12</pageno>
<text>9.3 Check test</text>
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<pageno>13</pageno>
<text>9.4 Determination</text>
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<pageno>13</pageno>
<text>9.4.1 Decomposition of the test portion using PTFE bomb</text>
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<pageno>13</pageno>
<text>9.4.2 Decomposition of test portion using polypropylene bottles</text>
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<bookmark index='51'>
<pageno>14</pageno>
<text>9.4.3 Test solutions</text>
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<bookmark index='52'>
<pageno>14</pageno>
<text>9.5 Measurement</text>
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<pageno>14</pageno>
<text>9.5.1 General</text>
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<pageno>15</pageno>
<text>9.5.2 Calibration graphs</text>
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<pageno>15</pageno>
<text>9.5.3 Graph linearity</text>
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<pageno>15</pageno>
<text>9.5.4 Background correction</text>
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<pageno>15</pageno>
<text>10 CALCULATION</text>
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<pageno>15</pageno>
<text>11 REPORTING OF RESULTS</text>
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<pageno>16</pageno>
<text>12 PRECISION</text>
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<pageno>16</pageno>
<text>13 TEST REPORT</text>
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<pageno>17</pageno>
<text>APPENDIX A - PRECISION DATA FOR ELEMENTAL ANALYSIS OF COAL ASH AND COKE ASH</text>
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</toc>
Abstract
Sets out methods for the determination of nine elements in higher rank coal ash and coke ash by flame atomic absorption spectrometry after acid digestion. Methods for the determination of a further two elements are also referenced.
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 methods for the determination of silicon, aluminium, iron, calcium, magnesium, sodium, potassium, titanium and manganese in higher rank coal ash and coke ash by flame atomic absorption spectrometry after acid digestion.
NOTE: Although a volumetric approach has been specified for solution preparation, a gravimetric alternative may be used.
A spectrophotometric method for the determination of phosphorus and a method for the determination of sulfur are also referenced.
This method is applicable to the determination of the elements listed above (expressed as oxides), in the concentration ranges specified in Table 1.
Table 1 has been devised to accommodate any type of ash that is likely to arise from Australian higher rank coals or cokes.
NOTE: The results in Appendix A have been obtained from test work carried out on the available samples. Although testing was not carried out with a comprehensive range of likely coal compositions, the method is expected to apply over the wider ranges covered by the calibration standards and indicated in Table 1.
General Product Information
| Document Type | Standard |
| Status | Current |
| Publisher | Standards Australia |
| ProductNote | Reconfirmed 06-08-2013 |
| Committee | MN-001 |
| Supersedes |
|