ACIRS-G9-2021

GENERAL COAL REFERENCE MATERIAL

CERTIFICATE of ANALYSIS
Production and certification of this sample was conducted in accordance with ISO 17034.

ASSIGNED PROPERTY VALUES

Certified Standard Standard Expanded
Value1 Deviation2 Uncertainty3a Uncertainty3b
Ash, % d 10.69 0.071 0.013 0.026

Volatile Matter, % d 20.00 0.212 0.040 0.079

Gross Calorific Value, MJ/kg d 32.105 0.064 0.012 0.025

Relative Density, d 1.386 0.016 0.003 0.007

Total Carbon, % d 79.07 0.328 0.075 0.150

Hydrogen, % d 4.31 0.076 0.017 0.035

Nitrogen, % d 1.79 0.029 0.007 0.013

Total Sulfur, % d 0.601 0.007 0.001 0.003

Chlorine, % d 0.056 0.005 0.001 0.003

Phosphorus, % d 0.036 0.001 0.0003 0.001

Mercury, mg/kg d 0.030 0.002 0.0006 0.0011

Fluorine, mg/kg d 100 4.6 1.5 2.9

Carbonate Carbon, % d 0.063 0.006 0.002 0.004

1. Certified values are the best estimate of the true value. They are an unweighted robust mean
value of an accepted dataset obtained from proficiency testing using ISO/IEC 17025 accredited
laboratories each of whom tested three unique samples. The standard test methods used are
detailed in Table 2. Where more than one test method was used, biases between methods were
not observed
2. Standard deviation (s*) 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 standard deviations of the certified value with 95% probability.
3. 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)
a. Standard uncertainty (ua) is a robust value estimated at 1.25 x s*/√n
b. Expanded uncertainty (U) is calculated from ua x a coverage factor k= 2, corresponding to
a level of confidence of about 95%.

Date of Issue: 04 June 2021

Report Number: COA-G9-2021-rev0
Previous ACIRS-G series: This sample supersedes ACIRS-G8-2019

COA-G9-2021-Rev0 Page 1 of 4
 1. Introduction
This report describes the preparation and certification of ACIRS–G9-2021.
This reference material is a higher rank bituminous coal and is intended to be used for
quality control purposes for the analysis of similar coals.

2. Description of the Sample and Preparation

ACIRS–G9-2021 comprises a sealed jar containing approximately 125 g of coal at a
nominal top size of 212 µm. This sample was prepared from 350 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 samples were obtained. Each sample
was then placed into a plastic bag within sealed HDPE jars.
Between-unit homogeneity was quantified by testing ash, gross calorific value and
total sulfur and assessing for sufficient homogeneity in accordance with ISO 17034.

3. Instructions for Use

This reference material is intended to be used as a quality control tool.
Before first use, empty the sample from the inner plastic bag directly into the HDPE jar.
Before each use, the bottle must be thoroughly mixed by end-over-end rotation to re-
homogenise the coal sample.
To minimise the risk of compositional changes due to oxidation, store in a cool, dark
place in the original container 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-G9 is established in accordance with the
standard test methods listed in Table 2. Corrections to dry basis values should be in
accordance with ISO 11722 or equivalent.

4. Characterisation
ACIRS-G9 was characterised in an interlaboratory comparison program conducted
by Proficiency Testing Australia in collaboration with ACIRS. This program was
conducted specifically for characterisation of ACIRS-G9.
Sixteen accredited Australian coal testing laboratories were invited to participate in
the program.
Each participant was provided three unique ACIRS-G9 samples. Additionally, an
ACIRS-G8-2019 sample was provided to participants for quality assurance purposes.
Participant data was accepted in the characterisation dataset when:
• The laboratory was accredited to ISO/IEC 17025 for the specific parameter;
• Testing was conducted by a national or international standard test methods,
and
• When results met technical acceptability along ACIRS guidelines e.g. meeting
standard method precision limits; not identified as an outlier; passed
acceptance testing on ACIRS-G8.

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 The certified values and their associated uncertainties were calculated from an
unweighted mean value of robust means in accordance with the guidelines of:
• ISO/IEC Guide 98-3, Guide to the Expression of Uncertainty in Measurement
(GUM)
• 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 dataset included analyses tested by the standard test methods, where
significant biases were not observed, as detailed in Table 2.
Notes:
• Supplementary testing on an additional three samples was conducted by
ACIRS for certification of mercury.
• This sample has relatively low levels of pyritic sulfur (<0.1%).
Table 1 Methods Used for Certification
n
Parameter Analysis Method(s) Used4
(total)5
Ash ISO 1171* (n=48) 48
Volatile Matte* ISO 562* (n=45) 45
Calorific Value ISO 1928* (n=42) 42
Relative Density AS1038.21.1.1 (n=36) 36
Total Carbon ISO 29541* (n=30) 30
Hydrogen ISO 29541* (n=30) 30
Nitrogen ISO 29541* (n=30) 30
Total Sulfur ISO 19579 (n=27), AS 1038.6.3.3 (n=15) 42
Chlorine ISO 587 (n=6), ISO 18806 (n=6), AS 1038.8.1 (n=6) 18
Phosphorus ISO 622 (n=3), AS 1038.9.3 (n=3), ISO 13605 (n=6), AS 1038.14.3 (n=6) 18
Mercury ASTM D 6722 (n=21) 21
Fluorine ISO 11724* (n=15) 15
Carbonate Carbon AS 1038.23 (n=9), ISO 925*(n=3) 12
4 An * indicates methods used includes the corresponding Australian Standard methods AS
1038.3-2000 (ash, VM), AS 1038.5-1998 (CV), AS 1038.6.4-2005 (C, H, N), AS 1038.10.4 (F).
5 Total number of results (n) is the number of accepted results in the dataset, each being the
average of duplicate results. Three unique samples were tested by each participant for all
parameters except Hg where six unique samples were tested.

5. 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.

6. 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 (February 2025) is provided for oxidation sensitive parameters i.e. for CV, VM, C
and H. All other parameters are considered stable until February 2028.

COA-G9-2021-Rev0 Page 3 of 4
 The stability of this sample will be monitored by ACIRS. It is the responsibility of the user
to obtain the most recent Certificate for this reference material available at
www.acirs.com.au/products/general-coal-reference-material.

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-G9-2021-rev0 Original 04/06/2021

10. Authorisation

Approved by Christine Foster, ACIRS Operations 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]

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