CR G8 2019 Rev1

GENERAL COAL REFERENCE MATERIAL
ACIRS-G8-2019
CERTIFICATION REPORT
Date of Issue: March, 2019

Report Number: CR-G8-2019-rev01
Previous ACIRS-G series: This is the sixth in the series and supersedes ACIRS-G6-2014-Lot#2
Production and certification of this sample was conducted in accordance with ISO 17034
and ISO Guide 35.
Table 1
ASSIGNED PROPERTY VALUES
Property Standard Expanded Number of
Values1 Deviation2 Uncertainty3 results
Ash, % d 1a 10.14 0.08 0.03 50
Volatile Matter, % d 1b 20.23 0.18 0.06 48
Gross Calorific Value, MJ/kg d 32.357 0.089 0.036 38
Relative Density, d 1.382 0.008 0.004 20
Total Carbon, % d 79.44 0.36 0.19 22
Hydrogen, % d 4.40 0.05 0.03 17
Nitrogen, % d 1.79 0.03 0.02 21
Total Sulfur, % d 0.590 0.013 0.005 41
Chlorine, % d 0.052 0.002 0.001 13
Phosphorus, % d 0.027 0.001 0.001 20
Mercury, mg/kg d 0.02 0.005 0.004 9
Fluorine, mg/kg d 85 5.9 3.8 15
Page 1 of 4
1. Notes
1 Property values are the best estimate of the true value. They are based on the robust
mean of technically valid results from proficiency testing using standard test methods where
biases between methods were not observed. Methods used are detailed in Table 2.
2 Standard deviation (sd) is a robust value used to derive the likely range of results. For
normally distributed data, the value for a measurand from a randomly chosen laboratory
would be expected to lay within 2 standards deviations of the certified value with 95%
probability.
3 The expanded uncertainty provides the user with information on the likely range of the
true (but unknown) value for each parameter and has been estimated in accordance with
the Guide to the Expression of Uncertainty in Measurement (GUM) with a coverage factor k=
2, corresponding to a level of confidence of about 95%. For Hg, a k-factors of 2.2 was chosen
according to the t-distribution for sets of results.
2. Description of the Sample and Preparation

ACIRS–G8-2019 comprises a sealed jar containing approximately 125 g of coal at a nominal
top size of 212 µm. This sample was prepared from 550 kg of a Queensland, Bowen Basin higher
rank bituminous coal at -50 mm top size.
The bulk coal sample was crushed in a swing hammer mill to a nominal top size of 2.36 mm
and stabilised over an extended period. The material was then repeatedly mixed by rotary
sample division (RSD) until lots of approximately 1.4 kg were obtained which were then air dried
and milled to a nominal top size of 212 µm. This pulverised material was further divided by RSD
until representative 125 (± 5) g samples were obtained. Each sample was then placed into a
plastic bag within sealed HDPE jars.
Between-unit homogeneity was quantified by testing ash, calorific value, volatile matter and
total sulfur and assessed in accordance with ISO Guide 35.
3. Instructions for Use

This reference material is intended to be used as a quality control tool.
Before the bottle is opened, it must be thoroughly mixed by end-over-end rotation so that the
material is re-homogenised.
To minimise the risk of compositional changes due to oxidation store in a cool, dark place in
original containers with lids tightly sealed. ACIRS cannot be held responsible for any changes
that occur after the sample bottle has been opened.
The minimum sample intake for ACIRS-G8 is established in accordance with the standard test
methods listed in Table 2.
4. Characterisation
With the exception of fluorine, ACIRS-G8 was characterised through Proficiency Testing
Australia’s (PTA) Round 38 proficiency testing program in which each participant was
provided two samples for testing.
Fluorine was characterised by an independent test program conducted by ACIRS in which
each participant was provided three samples to be tested by ISO 11724 and equivalent test
methods.
Page 2 of 4 Doc No: CR-G8-2019-rev01

Only technically valid data was included for characterisation. Generally, data was excluded
when:
 Reported from in-house/unknown methods;
 Reported from laboratories not accredited to ISO/IEC 17025; or
 When results failed to meet technical acceptability along ACIRS guidelines e.g. failing
to meet standard method precision limits or identified as outliers from the dataset.
Property values and their associated uncertainties were calculated by robust statistical
techniques in accordance with the guidelines of:
 ISO/IEC Guide 98-3, Guide to the Expression of Uncertainty in Measurement (GUM)
 IUPAC, 2006 International Harmonized Protocol for the Proficiency Testing of Analytical
Chemical Laboratories
 ISO 13528-2015, Statistical methods for use in proficiency testing by interlaboratory
comparison, and
 ISO Guide 35 -2017, Reference Materials – Guidance for characterization and
assessment of homogeneity and stability.
The accepted data-set included analyses tested by the standard test methods, where
significant biases were not observed, as detailed in Table 2.
Table 2
Parameter Analysis Methods used in Certification Testing*
Ash ISO 1171 (n=48) AS 1038.3 (n=2)
Volatile Matter ISO 562 (n=48) AS 1038.3 (n=2)
Calorific Value ISO 1928 (n=30) AS 1038.5 (n=6) ASTM D5865 (n=2)
Relative Density AS 1038.21.1.1 (n=24) AS 1038.21.1.2 (n=4)
Total Carbon ISO 29541 (n=12) AS 1038.6.1 (n=4) AS 1038.6.4 (n=2) ASTM D5373 (n=4)
Hydrogen ISO 29541 (n=11) AS 1038.6.1 (n=4) ASTM D5373 (n=2)
Nitrogen ISO 29541 (n=11) AS 1038.6.2 (n=6) AS 1038.6.4 (n=2) ASTM D5373 (n=2)
Total Sulfur AS 1038.6.3.3 (n=20) ISO 19579 (n=17) ASTM D4239 (n=4)
Chlorine AS 1038.8.1 (n=6) ISO/TS 18806 (n=4) ISO 587 (n=1) ASTM D4205 (n=2)
Phosphorus AS 1038.14.3 (n=14) ISO/TS 13865 (n=4) AS 1038.9.3 (n=2)
Mercury ASTM D6722 (n=9)
Fluorine ISO 11724 (n=12) AS 1038.10.4 (n=3)
*Or their technical equivalents
5. Period of Validity
Property values for coal samples are subject to change due to the normal oxidation processes
for coals. For this reason, the minimum shelf-life until the stated period of validity (January 2023)
is provided for oxidation sensitive parameters i.e. for CV, VM, C and H. All other parameters
are considered stable until January 2026. The stability of this sample will be monitored by ACIRS.
It is the responsibility of the user to obtain the most recent Certification Report for this reference
material available at www.acirs.com.au/products/general-coal-reference-material/
6. Metrological Traceability
Property values are operationally defined by methods listed in Table 2. Traceability of the results
is based on traceability of all relevant input factors and was achieved by using only results from
laboratories accredited to ISO/IEC 17025. Certified property values are based on agreement
amongst technically valid results each traceable to the SI through stringent requirements of
accreditation.
Note: Fluorine is traceable to the property value assigned to BCR 460.

7. Health and Safety
Samples shall be handled in accordance with the Safety Data Sheet available from
www.acirs.com.au/products/general-coal-reference-material/
8. Legal Notice
To the extent permitted by law, ACIRS disclaims all warranties whether expressed or implied
with regard to merchantability, non-infringement, or fitness for a particular purpose. In no event
will ACIRS be liable for incidental damage or consequential loss arising from the use of this
product.
Where the product does not conform to assigned property values, giving due consideration
to the stated uncertainties and accepted tolerances, the total liability of ACIRS shall be limited
at ACIRS’ absolute discretion to either replacement of the product or refund of the purchase
price.
9. Revision History
Document Number Summary Date

CR-G8-2019-rev0 Original (rev0) 20/03/2019
CR-G8-2019-rev01 Addition of fluorine, removal of CSN 31/07/2019
10. Authorisation
Approved by: Christine Foster, ACIRS Technical Manager

Australian Coal Industry Reference Samples (ACIRS)
PO Box 2315, DANGAR NSW 2309, AUSTRALIA
Phone +61 (2) 4926 4870
Fax +61 (2) 4926 4902
Email [email protected]

CR G8 2019 Rev1

Uploaded by

Copyright:

Available Formats

CR G8 2019 Rev1

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

CR G8 2019 Rev1

Uploaded by

Copyright:

Available Formats

GENERAL COAL REFERENCE MATERIAL

Date of Issue: March, 2019

2. Description of the Sample and Preparation

3. Instructions for Use

Page 2 of 4 Doc No: CR-G8-2019-rev01

Page 3 of 4 Doc No: CR-G8-2019-rev01

Document Number Summary Date

Approved by: Christine Foster, ACIRS Technical Manager

Page 4 of 4 Doc No: CR-G8-2019-rev01

You might also like