AS 1038 21.1.1-2008 Coal & Coke - Analysis and Testing

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AS 1038.21.1.1-2008 Coal and coke - Analysis and testing - Higher rank coal and
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AS 1038.21.1.1—2008
Australian Standard®
Relative density—Analysis
sample/density bottle method
Coal and coke—Analysis and testing
Part 21.1.1: Higher rank coal and coke—

AS 1038.21.1.1—2008
This Australian Standard® was prepared by Committee MN-001, Coal and Coke. It was
approved on behalf of the Council of Standards Australia on 7 October 2008.
This Standard was published on 30 October 2008.
The following are represented on Committee MN-001:
• Australasian Institute of Mining and Metallurgy

• Australian Coal Association
• Australian Coal Preparation Society
• Australian Institute of Energy
• CSIRO, Energy Technology
• Department of Natural Resources and Mines, Qld
• Institution of Engineers, Australia
• Minerals Council of Australia
• National Generators Forum
• University of Newcastle
• University of New South Wales
• University of Queensland
This Standard was issued in draft form for comment as DR 08161.
Standards Australia wishes to acknowledge the participation of the expert individuals that
contributed to the development of this Standard through their representation on the
Committee and through the public comment period.
Keeping Standards up-to-date

Australian Standards® are living documents that reflect progress in science, technology and
systems. To maintain their currency, all Standards are periodically reviewed, and new editions
are published. Between editions, amendments may be issued.
Standards may also be withdrawn. It is important that readers assure themselves they are
using a current Standard, which should include any amendments that may have been
published since the Standard was published.
Detailed information about Australian Standards, drafts, amendments and new projects can
be found by visiting www.standards.org.au
Standards Australia welcomes suggestions for improvements, and encourages readers to

notify us immediately of any apparent inaccuracies or ambiguities. Contact us via email at
mail@standards.org.au, or write to Standards Australia, GPO Box 476, Sydney, NSW 2001.
AS 1038.21.1.1—2008
Australian Standard®
Part 21.1.1: Higher rank coal and coke—

Relative density—Analysis
Originated as part of AS 1038.21—1983.

Previous edition AS 1038.21.1.1—2002.
Third edition 2008.
COPYRIGHT
© Standards Australia
All rights are reserved. No part of this work may be reproduced or copied in any form or by
any means, electronic or mechanical, including photocopying, without the written
permission of the publisher.
Published by Standards Australia GPO Box 476, Sydney, NSW 2001, Australia
ISBN 0 7337 8945 5
AS 1038.21.1.1—2008 2
PREFACE
This Standard was prepared by the Standards Australia Subcommittee on Coal Evaluation,
under the supervision of the Committee MN-001, Coal and Coke, as a revision of
AS 1038.21.1.1—2002, Coal and coke—Analysis and testing, Part 21.1.1: Higher rank coal
and coke—Relative density—Analysis sample/density bottle method.
The objective of this Standard is to provide those responsible for testing coal and coke with
a standardized method for measuring the relative density using a density bottle, so that
disputes can be minimized.
This revision makes changes to the temperature of the water bath.
The term ‘informative’ has been used in this Standard to define the application of the
appendix to which it applies. An ‘informative’ appendix is for information and guidance
only.
3 AS 1038.21.1.1—2008
CONTENTS
Page
1 SCOPE ........................................................................................................................ 4
2 REFERENCED DOCUMENTS .................................................................................. 4
3 DEFINITIONS............................................................................................................ 4
4 PRINCIPLE ................................................................................................................ 4
5 SAFETY ..................................................................................................................... 4
6 REAGENTS................................................................................................................ 4
7 APPARATUS ............................................................................................................. 5
8 SAMPLE..................................................................................................................... 5
9 CALIBRATION OF DENSITY BOTTLE .................................................................. 5
10 PROCEDURE ............................................................................................................. 6
11 CALCULATION ........................................................................................................ 6
12 REPORTING OF RESULT......................................................................................... 6
13 PRECISION ................................................................................................................ 6
14 TEST REPORT ........................................................................................................... 7
APPENDIX A ALTERNATIVE METHODS FOR DE-AERATING THE ANALYSIS

SAMPLE............................................................................................................ 8
AS 1038.21.1.1—2008 4
STANDARDS AUSTRALIA
Australian Standard
Part 21.1.1: Higher rank coal and coke—Relative density—Analysis

1 SCOPE
This Standard sets out a method for the determination of the relative density of higher rank
coal and coke by a relative density bottle.
2 REFERENCED DOCUMENTS
The following documents are referred to in this Standard:
AS
1038 Coal and coke—Analysis and testing
1038.3 Part 3: Proximate analysis of higher rank coal
1038.4 Part 4: Coke—Proximate analysis
1038.16 Part 16: Assessment and reporting of results
2378 Density bottles
2418 Coal and coke—Glossary of terms
2706 Numerical values—Rounding and interpretation of limiting values
4264 Coal and coke—Sampling
4264.1 Part 1: Higher rank coal—Sampling procedures
4264.2 Part 2: Coke—Sampling procedures
AS/NZS
2243 Safety in laboratories (series)
3 DEFINITIONS
For the purpose of this Standard, the definitions given in AS 2418 apply.
4 PRINCIPLE
The mass of water displaced by a known mass of air-dry coal or coke is determined in a
density bottle.
5 SAFETY
For information on laboratory safety, reference should be made to the relevant parts of
AS/NZS 2243.
6 REAGENTS
6.1 Distilled water
Distilled water or water of equivalent purity.
© Standards Australia www.standards.org.au

5 AS 1038.21.1.1—2008
6.2 Wetting agent solution

A solution of non-ionic liquid wetting agent prepared in either distilled or deionized water
with a concentration of between 10 mL/L and 15 mL/L.
7 APPARATUS
7.1 Density bottle
A density bottle of 50 mL capacity, and conforming to AS 2378 (see Figure 1).
7.2 Water bath
A water bath with stirrer, thermostatically controlled to maintain a bath temperature
of 30 ±1°C.
NOTE: The water temperature should be kept constant throughout both stages of the procedure
described in Clauses 9 and 10. The actual temperature need not be reported with the result, as
differences within this range are not significant.
7.3 Vacuum desiccator
7.4 Vacuum pump
Capable of evacuating the desiccator to 8 kPa.
7.5 Weighing device
A balance having a minimum capacity of 100 g and readable to the nearest 0.001 g.
8 SAMPLE
8.1 General
The sample shall be the analysis sample prepared to a nominal top size of 212 µm. Sample
preparation procedures are described in AS 4264.1 and AS 4264.2.
8.2 Equilibration
The moisture content of the sample shall be equilibrated with the laboratory atmosphere by
exposure in a thin layer on a tray.
The sample shall be thoroughly mixed immediately before analysis.
9 CALIBRATION OF DENSITY BOTTLE

The density bottle shall be calibrated regularly as follows:
(a) Fill the density bottle (7.1) to within 5 mm of the top with wetting agent solution
(6.2).
(b) Place the bottle in the water bath (7.2), maintain the temperature as specified in
Clause 7.2, and allow to stand for at least 30 min or until air bubbles cease to rise
through the liquid. Tap the bottle gently to help to disperse any trapped air bubbles.
(c) When the surface of the liquid is free from air bubbles, fill the density bottle with
wetting agent solution.
NOTE: A beaker of wetting agent solution should be kept in the water bath.
Carefully insert the density bottle stopper, ensuring that no air bubbles remain
trapped beneath the stopper. Remove the drop of water from the top of the stopper
with a piece of filter paper. (This should be done only once.) Remove the density
bottle and contents from the bath, and carefully wipe the bottle with a clean, dry
cloth.
(d) Weigh, and record the mass (m1) of the density bottle with stopper and wetting agent
solution.
www.standards.org.au © Standards Australia

AS 1038.21.1.1—2008 6
NOTE: To avoid losses due to evaporation, this weighing should be carried out within 5 min
of removal from the water bath.
The initial calibration should be carried out in triplicate. The spread of the triplicate values
shall be not greater than 0.005 g; otherwise, the entire calibration shall be repeated. Regular
verification of this calibration should be carried out. If there has been no change to the
apparatus or concentration of the wetting agent, the initial calibration mass (m1) should
continue to be used.
10 PROCEDURE
The procedure shall be as follows:
(a) Weigh, to the nearest milligram, approximately 2 g of the sample and transfer it to the
clean density bottle. Record the mass (m) of the sample. Concurrently, weigh out a
sample for moisture determination by the method of AS 1038.3 or AS 1038.4.
(b) Add 10 mL to 15 mL of wetting agent to the density bottle and mix to ensure that the
sample is wet. Continue to add wetting agent to wash down the sides of the bottle
(approximately 20 mL).
(c) Transfer the bottle and contents to the vacuum desiccator (7.3). Connect the
desiccator to the vacuum pump (7.4) and reduce the pressure in the desiccator to
about 8 kPa, absolute. Do not evacuate to below 7 kPa, as boiling and violent frothing
may occur.
NOTE: Other methods of de-aerating, such as boiling or vibrating with ultrasonic waves, may
be used. These methods are described in Appendix A.
(d) Remove the density bottle and contents from the desiccator and repeat Steps 9(b)
and 9(c).
(e) Weigh and record the mass (m2) of the density bottle with stopper, wetting agent
solution, and sample.
11 CALCULATION
The result for relative density shall be calculated using the following equation:
m
R elative density = . . . (1)
m + m1 − m2
where
m = mass of sample, in grams
m1 = mass of stoppered density bottle, completely filled with wetting agent
solution, in grams (mean of triplicate results determined during calibration)
m2 = mass of stoppered density bottle, plus wetting agent solution, plus sample,
in grams
12 REPORTING OF RESULT
The result, the mean of duplicate determinations, for relative density, shall be reported to
the nearest 0.01, rounded in accordance with AS 2706.
13 PRECISION
The values of repeatability and reproducibility should not exceed those give in Table 1.
Otherwise reference shall be made to AS 1038.16.

7 AS 1038.21.1.1—2008
14 TEST REPORT
The test report shall contain the following information:
(a) Complete identification of the sample tested.
(b) Reference to this Australian Standard, i.e. AS 1038.21.1.1.

(c) The result of the determination including the basis of reporting, i.e. air-dry.
(d) The moisture content of the sample.
TABLE 1
PRECISION DATA FOR RELATIVE
DENSITY DETERMINATION
Repeatability Reproducibility
Relative density
r R
<1.6 0.03 0.08
≥1.6 0.03 0.08
FIGURE 1 TYPICAL DENSITY BOTTLE
www.standards.org.au © Standards Australia

AS 1038.21.1.1—2008 8
APPENDIX A
ALTERNATIVE METHODS FOR DE-AERATING THE ANALYSIS SAMPLE
(Informative)
A1 METHOD 1—BOILING
A1.1 Apparatus
The following apparatus is required:
(a) Glycerine bath—A suitable vessel in which sufficient glycerine can be heated for the
lower two-thirds of the density bottle to be immersed.
(b) Air condenser—A glass tube of approximate length 1 m which may be attached to the
top of the density bottle.
A1.2 Procedure
The procedure is as follows:
(a) Attach the air condenser (A1.1(b)) to the neck of the bottle with rubber tubing, and
immerse the bottle in a glycerine bath (A1.1(a)).
(b) Heat the bath so that the water in the bottle begins to boil vigorously.
(c) Wash down any scum with a few millilitres of the hot, air-free water.
(d) After 30 min boiling, remove the bottle from the glycerine bath, detach the air
condenser and allow the bottle to cool.
A2 METHOD 2—ULTRASONIC VIBRATING

A2.1 Apparatus
An ultrasonic bath with timer.
A2.2 Procedure
The procedure is as follows:
(a) Add sufficient water to the ultrasonic bath to immerse the density bottle to the bottom
of its neck.
(b) Place the density bottles in the bath, and vibrate until free of air bubbles.
(c) Remove the density bottles and allow to cool.

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also supports excellence in design and innovation through the Australian Design Awards.
For further information visit www.standards.org.au
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Committees of experts from industry, governments, consumers and other relevant sectors prepare Australian
Standards. The requirements or recommendations contained in published Standards are a consensus of the views
of representative interests and also take account of comments received from other sources. They reflect the latest
scientific and industry experience. Australian Standards are kept under continuous review after publication and are
updated regularly to take account of changing technology.
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vital in assisting local industry to compete in international markets. Standards Australia represents Australia at both
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ISBN 0 7337 8945 5

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LICENCE

Licensee: David Brown

Date: Thursday, February 19, 2009 1:53 PM

1. Definitions and Interpretations

Australian Standards means Australian Standards and includes Joint ISO/Australian

ISO Standards means Standards

Licence means the right to access and use the Product.

Part 21.1.1: Higher rank coal and coke—

The following are represented on Committee MN-001:

• Australasian Institute of Mining and Metallurgy

This Standard was issued in draft form for comment as DR 08161.

Keeping Standards up-to-date

Standards Australia welcomes suggestions for improvements, and encourages readers to

Coal and coke—Analysis and testing

Part 21.1.1: Higher rank coal and coke—

Originated as part of AS 1038.21—1983.

APPENDIX A ALTERNATIVE METHODS FOR DE-AERATING THE ANALYSIS

Coal and coke—Analysis and testing

Part 21.1.1: Higher rank coal and coke—Relative density—Analysis

© Standards Australia www.standards.org.au

6.2 Wetting agent solution

9 CALIBRATION OF DENSITY BOTTLE

www.standards.org.au © Standards Australia

© Standards Australia www.standards.org.au

(b) Reference to this Australian Standard, i.e. AS 1038.21.1.1.

FIGURE 1 TYPICAL DENSITY BOTTLE

www.standards.org.au © Standards Australia

A2 METHOD 2—ULTRASONIC VIBRATING

© Standards Australia www.standards.org.au

For further information visit www.standards.org.au

Sales and Distribution

For information regarding the development of Standards contact:

For information regarding the sale and distribution of Standards contact:

ISBN 0 7337 8945 5

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