ORE RESEARCH & EXPLORATION P/L ABN 28 006 859 856

37A Hosie Street · Bayswater North · VIC 3153 · AUSTRALIA

61 3 9729 0333 61 3 9729 8338
i n f o @o re .c o m.a u w w w.o re .c o m .a u

CERTIFICATE OF ANALYSIS FOR

Li Concentrate
(Spodumene Concentrate, Greenbushes, Western Australia)

CERTIFIED REFERENCE MATERIAL

OREAS 999

Summary Statistics for Key Analytes.

Certified 95% Confidence Limits 95% Tolerance Limits
Constituent 1SD
Value Low High Low High
Peroxide Fusion ICP
Li, Lithium (wt.%) 2.67 0.103 2.63 2.72 2.62 2.73
Li2O, Lithium oxide (wt.%) 5.76 0.222 5.65 5.86 5.63 5.88
4-Acid Digestion
Li, Lithium (wt.%) 2.65 0.057 2.62 2.68 2.59 2.71
Li2O, Lithium oxide (wt.%) 5.70 0.122 5.64 5.76 5.58 5.83
SI unit equivalents: ppm, parts per million ≡ mg/kg ≡ µg/g ≡ 0.0001 wt.% ≡ 1000 ppb, parts per billion.
Note: intervals may appear asymmetric due to rounding.

Document: COA-1422-OREAS999-R1 22-February-2019

(Template:BUP-70-10-01 Rev:2.0)
 TABLE OF CONTENTS

INTRODUCTION ...............................................................................................................6
SOURCE MATERIAL.........................................................................................................6
COMMINUTION AND HOMOGENISATION PROCEDURES ............................................7
ANALYTICAL PROGRAM .................................................................................................7
STATISTICAL ANALYSIS..................................................................................................8
PARTICIPATING LABORATORIES ..................................................................................12
PREPARER AND SUPPLIER ............................................................................................15
METROLOGICAL TRACEABILITY ....................................................................................15
COMMUTABILITY .............................................................................................................15
INTENDED USE ................................................................................................................16
STABILITY AND STORAGE INSTRUCTIONS ..................................................................16
INSTRUCTIONS FOR CORRECT USE ............................................................................16
HANDLING INSTRUCTIONS ............................................................................................16
LEGAL NOTICE .................................................................................................................16
DOCUMENT HISTORY .....................................................................................................16
QMS ACCREDITED ..........................................................................................................17
CERTIFYING OFFICER ....................................................................................................17
REFERENCES ..................................................................................................................17

LIST OF TABLES

Table 1. Certified Values, SDs, 95% Confidence & Tolerance Limits for OREAS 999. ....... 3
Table 2. Indicative Values for OREAS 999. ......................................................................... 6
Table 3. Performance Gates for OREAS 999. ..................................................................... 9

LIST OF FIGURES

Figure 1. Li2O (wt.%) by peroxide fusion ICP in OREAS 999 ............................................ 13

Figure 2. Li2O (wt.%) by 4-acid digestion in OREAS 999................................................... 14

COA-1422-OREAS999-R1 Page: 2 of 17
 Table 1. Certified Values, SDs, 95% Confidence & Tolerance Limits for OREAS 999.
Certified 95% Confidence Limits 95% Tolerance Limits
Constituent SD
Value Low High Low High
Peroxide Fusion ICP
Al, Aluminium (wt.%) 12.23 0.411 12.01 12.46 11.94 12.52
Ba, Barium (ppm) 39.1 2.64 37.5 40.6 35.6 42.5
Be, Beryllium (ppm) 51 2.1 49 52 48 53
Bi, Bismuth (ppm) 2.21 0.185 2.07 2.34 2.06 2.35
Ca, Calcium (wt.%) 0.481 0.059 0.454 0.508 0.458 0.504
Ce, Cerium (ppm) 4.15 0.360 3.75 4.55 3.80 4.50
Co, Cobalt (ppm) 5.24 0.343 4.94 5.54 4.97 5.51
Cr, Chromium (ppm) 112 17 104 120 103 120
Cs, Cesium (ppm) 93 3.6 91 95 91 95
Cu, Copper (ppm) 25.5 3.4 21.6 29.4 22.7 28.2
Dy, Dysprosium (ppm) 0.80 0.050 0.79 0.82 0.76 0.85
Er, Erbium (ppm) 0.27 0.03 0.24 0.30 0.23 0.30
Fe, Iron (wt.%) 1.73 0.067 1.70 1.76 1.69 1.77
Ga, Gallium (ppm) 88 6.4 83 92 85 90
Gd, Gadolinium (ppm) 1.08 0.16 1.02 1.14 0.98 1.17
Ge, Germanium (ppm) 4.31 0.45 4.06 4.56 3.77 4.85
Ho, Holmium (ppm) 0.11 0.011 0.11 0.12 IND IND
K, Potassium (wt.%) 0.522 0.048 0.499 0.544 0.502 0.542
La, Lanthanum (ppm) 1.84 0.25 1.64 2.03 1.69 1.98
Li, Lithium (wt.%) 2.67 0.103 2.63 2.72 2.62 2.73
Li2O, Lithium oxide (wt.%) 5.76 0.222 5.65 5.86 5.63 5.88
Mg, Magnesium (wt.%) 0.473 0.020 0.462 0.484 0.461 0.485
Mn, Manganese (wt.%) 0.147 0.006 0.144 0.150 0.144 0.150
Mo, Molybdenum (ppm) 2.27 0.38 2.06 2.48 IND IND
Nb, Niobium (ppm) 74 6.2 70 78 71 76
Nd, Neodymium (ppm) 1.90 0.22 1.74 2.05 1.66 2.14
Ni, Nickel (ppm) 52 4.2 51 54 47 57
P, Phosphorus (wt.%) 0.016 0.005 0.014 0.019 IND IND
Pr, Praseodymium (ppm) 0.52 0.06 0.46 0.57 0.49 0.55
Rb, Rubidium (ppm) 423 20 411 434 413 432
Sb, Antimony (ppm) 1.02 0.17 0.88 1.16 IND IND
Si, Silicon (wt.%) 30.30 0.680 29.81 30.79 29.63 30.96
Sm, Samarium (ppm) 1.02 0.099 0.97 1.06 IND IND
Sn, Tin (ppm) 84 5.3 80 87 80 87
Sr, Strontium (ppm) 23.0 3.3 20.5 25.4 21.3 24.6
Ta, Tantalum (ppm) 45.5 2.08 44.2 46.8 44.2 46.8
SI unit equivalents: ppm, parts per million ≡ mg/kg ≡ µg/g ≡ 0.0001 wt.% ≡ 1000 ppb, parts per billion.
Note 1: intervals may appear asymmetric due to rounding.
Note 2: the number of decimal places quoted does not imply accuracy of the certified value to this level but are given to
minimise rounding errors when calculating 2SD and 3SD windows.

COA-1422-OREAS999-R1 Page: 3 of 17
 Table 1 continued.
Certified 95% Confidence Limits 95% Tolerance Limits
Constituent SD
Value Low High Low High
Peroxide Fusion ICP continued
Tb, Terbium (ppm) 0.18 0.02 0.17 0.19 IND IND
Th, Thorium (ppm) 3.01 0.158 2.92 3.11 2.87 3.15
Ti, Titanium (wt.%) 0.034 0.004 0.032 0.036 0.033 0.036
Tl, Thallium (ppm) 4.26 0.253 4.06 4.46 4.07 4.45
U, Uranium (ppm) 2.51 0.226 2.30 2.72 2.36 2.66
W, Tungsten (ppm) 6.94 0.391 6.78 7.10 6.38 7.51
Y, Yttrium (ppm) 4.19 0.43 3.90 4.48 3.92 4.46
Zn, Zinc (ppm) 77 4.3 75 79 71 83
Zr, Zirconium (ppm) 32.9 3.4 29.6 36.2 31.3 34.5
Borate Fusion XRF
Al2O3, Aluminium(III) oxide (wt.%) 23.39 0.114 23.34 23.44 23.27 23.51
CaO, Calcium oxide (wt.%) 0.670 0.013 0.664 0.676 0.663 0.677
Fe2O3, Iron(III) oxide (wt.%) 2.49 0.033 2.47 2.51 2.47 2.50
K2O, Potassium oxide (wt.%) 0.612 0.009 0.607 0.616 0.602 0.621
MgO, Magnesium oxide (wt.%) 0.796 0.012 0.791 0.801 0.788 0.805
MnO, Manganese oxide (wt.%) 0.192 0.005 0.189 0.194 0.188 0.195
Na2O, Sodium oxide (wt.%) 0.945 0.024 0.933 0.956 0.928 0.961
P2O5, Phosphorus(V) oxide (wt.%) 0.038 0.004 0.035 0.040 0.036 0.040
SiO2, Silicon dioxide (wt.%) 64.23 0.446 64.03 64.43 64.01 64.44
SO3, Sulphur trioxide (wt.%) 0.042 0.006 0.037 0.046 IND IND
TiO2, Titanium dioxide (wt.%) 0.060 0.007 0.057 0.063 0.056 0.065
Thermogravimetry
LOI1000, Loss on ignition @1000°C (wt.%) 0.764 0.114 0.704 0.824 0.720 0.808
4-Acid Digestion
Al, Aluminium (wt.%) 10.77 1.42 10.14 11.40 10.36 11.18
As, Arsenic (ppm) 5.36 1.07 4.82 5.89 4.96 5.75
Ba, Barium (ppm) 39.6 2.34 38.5 40.8 38.2 41.1
Be, Beryllium (ppm) 49.8 3.49 48.3 51.3 48.1 51.5
Bi, Bismuth (ppm) 2.11 0.131 2.05 2.17 1.99 2.23
Ca, Calcium (wt.%) 0.450 0.033 0.437 0.463 0.434 0.466
Co, Cobalt (ppm) 4.95 0.262 4.82 5.08 4.72 5.18
Cr, Chromium (ppm) 81 21 72 89 76 85
Cs, Cesium (ppm) 88 11 83 93 85 91
Cu, Copper (ppm) 25.4 2.34 24.4 26.4 24.3 26.6
Dy, Dysprosium (ppm) 0.67 0.13 0.57 0.78 0.62 0.72
Er, Erbium (ppm) 0.23 0.05 0.19 0.28 IND IND
SI unit equivalents: ppm, parts per million ≡ mg/kg ≡ µg/g ≡ 0.0001 wt.% ≡ 1000 ppb, parts per billion.
Note 1: intervals may appear asymmetric due to rounding.
Note 2: the number of decimal places quoted does not imply accuracy of the certified value to this level but are given to
minimise rounding errors when calculating 2SD and 3SD windows.

COA-1422-OREAS999-R1 Page: 4 of 17
 Table 1 continued.
Certified 95% Confidence Limits 95% Tolerance Limits
Constituent SD
Value Low High Low High
4-Acid Digestion continued
Fe, Iron (wt.%) 1.62 0.097 1.58 1.66 1.57 1.67
Ga, Gallium (ppm) 82 5.4 80 84 79 85
Hf, Hafnium (ppm) 1.98 0.171 1.91 2.06 1.93 2.04
Ho, Holmium (ppm) 0.090 0.018 0.076 0.103 IND IND
K, Potassium (wt.%) 0.500 0.041 0.482 0.519 0.486 0.514
La, Lanthanum (ppm) 1.68 0.34 1.49 1.87 1.57 1.78
Li, Lithium (wt.%) 2.65 0.057 2.62 2.68 2.59 2.71
Li2O, Lithium oxide (wt.%) 5.70 0.122 5.64 5.76 5.58 5.83
Mg, Magnesium (wt.%) 0.410 0.066 0.380 0.440 0.395 0.425
Mn, Manganese (wt.%) 0.143 0.006 0.141 0.145 0.140 0.146
Mo, Molybdenum (ppm) 2.06 0.140 2.00 2.12 1.92 2.19
Na, Sodium (wt.%) 0.693 0.023 0.682 0.703 0.672 0.713
Nb, Niobium (ppm) 75 4.7 73 77 73 78
Nd, Neodymium (ppm) 1.87 0.28 1.66 2.07 1.74 1.99
Ni, Nickel (ppm) 47.5 1.74 46.8 48.2 46.4 48.6
P, Phosphorus (wt.%) 0.016 0.002 0.015 0.017 0.015 0.017
Pb, Lead (ppm) 5.17 0.304 4.99 5.35 4.78 5.56
S, Sulphur (wt.%) 0.020 0.002 0.019 0.020 0.017 0.022
Sb, Antimony (ppm) 1.11 0.095 1.07 1.15 1.05 1.17
Sc, Scandium (ppm) 1.83 0.37 1.64 2.02 1.74 1.92
Sn, Tin (ppm) 63 5.5 61 66 61 66
Sr, Strontium (ppm) 16.9 2.9 15.5 18.4 16.0 17.9
Ta, Tantalum (ppm) 49.0 4.00 47.3 50.7 47.0 51.0
Tb, Terbium (ppm) 0.15 0.02 0.13 0.17 IND IND
Ti, Titanium (wt.%) 0.034 0.001 0.034 0.035 0.034 0.035
Tl, Thallium (ppm) 4.26 0.188 4.17 4.34 4.09 4.42
U, Uranium (ppm) 2.12 0.37 1.94 2.31 2.01 2.23
V, Vanadium (ppm) 14.8 1.18 14.2 15.3 13.8 15.7
W, Tungsten (ppm) 6.97 0.546 6.71 7.23 6.65 7.29
Yb, Ytterbium (ppm) 0.24 0.022 0.22 0.25 0.21 0.26
Zn, Zinc (ppm) 71 4.1 70 73 69 74
Zr, Zirconium (ppm) 20.0 2.3 18.9 21.1 18.7 21.3
SI unit equivalents: ppm, parts per million ≡ mg/kg ≡ µg/g ≡ 0.0001 wt.% ≡ 1000 ppb, parts per billion.
Note 1: intervals may appear asymmetric due to rounding.
Note 2: the number of decimal places quoted does not imply accuracy of the certified value to this level but are given to
minimise rounding errors when calculating 2SD and 3SD windows.

COA-1422-OREAS999-R1 Page: 5 of 17
 Table 2. Indicative Values for OREAS 999.

Constituent Unit Value Constituent Unit Value Constituent Unit Value

Peroxide Fusion ICP
Ag ppm 3.84 In ppm < 0.2 Sc ppm <5
As ppm 5.68 Lu ppm 0.054 Se ppm 2.64
B ppm < 50 Na wt.% 0.628 Te ppm 0.41
Cd ppm < 0.2 Pb ppm 6.66 Tm ppm 0.037
Eu ppm 0.071 Re ppm < 0.1 V ppm 14.8
Hf ppm 2.09 S wt.% 0.021 Yb ppm 0.26
Borate Fusion XRF
As2O3 ppm < 10 MoO3 ppm < 10 SrO ppm 48.0
BaO ppm 81 Nb2O5 ppm 223 Ta2O5 ppm 70
Cl ppm 325 NiO ppm 61 V2O5 ppm < 100
CoO ppm 17.5 PbO ppm 23.2 WO3 ppm 11.7
Cr2O3 ppm 153 Sb2O3 ppm < 10 ZnO ppm 118
CuO ppm 33.3 SnO2 ppm 90 ZrO2 ppm 77
Thermogravimetry
H2O- wt.% 0.330
4-Acid Digestion
Ag ppm 0.137 Hg ppm <2 Si wt.% 31.71
B ppm 7.43 In ppm 0.022 Sm ppm 0.83
Cd ppm 0.076 Lu ppm 0.028 Te ppm < 0.05
Ce ppm 2.64 Pr ppm 0.46 Th ppm 2.20
Eu ppm 0.060 Rb ppm 338 Tm ppm 0.028
Gd ppm 0.79 Re ppm < 0.002 Y ppm 2.58
Ge ppm 0.12 Se ppm <1
SI unit equivalents: ppm, parts per million ≡ mg/kg ≡ µg/g ≡ 0.0001 wt.% ≡ 1000 ppb, parts per billion.
Note: the number of significant figures reported is not a reflection of the level of certainty of stated values. They are
instead an artefact of ORE’s in-house CRM-specific LIMS.

INTRODUCTION
OREAS reference materials are intended to provide a low cost method of evaluating and
improving the quality of analysis of geological samples. To the geologist they provide a
means of implementing quality control in analytical data sets generated in exploration from
the grass roots level through to prospect evaluation, and in grade control at mining
operations. To the analyst they provide an effective means of calibrating analytical
equipment, assessing new techniques and routinely monitoring in-house procedures.

OREAS reference materials enable users to successfully achieve process control of these
tasks because the observed variance from repeated analysis has its origin almost
exclusively in the analytical process rather than the reference material itself.

SOURCE MATERIAL

OREAS 999 is a spodumene concentrate product derived from the processing of lithium
pegmatite ores sourced from the Eastern Goldfields Region of Western Australia.

COA-1422-OREAS999-R1 Page: 6 of 17
 COMMINUTION AND HOMOGENISATION PROCEDURES

The material constituting OREAS 999 was prepared in the following manner:

 Drying to constant mass at 105°C;

 Milling 100% minus 30 microns;
 Homogenisation;
 Packaging in 10g units in laminated foil pouches and 500g units in plastic wide-mouth jars.

ANALYTICAL PROGRAM
Twenty-four commercial analytical laboratories participated in the program to characterise
the elements reported in Table 1. The following methods were employed:

 Sodium peroxide fusion with full suite elemental package by ICP-OES and/or MS
finish (20 laboratories);
 Lithium borate fusion whole rock analysis package by X-ray fluorescence (19
laboratories);
 Thermogravimetry: Moisture at 105°C (2 laboratories as a part of their fusion
package) and Loss on Ignition (LOI) at 1000°C (8 laboratories used a
thermogravimetric analyser, 4 laboratories used conventional muffle furnace and 9
laboratories included LOI with their fusion package);
 4-acid digestion for full suite elemental package by ICP-OES and MS finish (up to
24 laboratories depending on the element).

For the round robin program twelve 300g test units were taken at predetermined intervals
during the bagging stage, immediately following homogenisation and are considered
representative of the entire prepared batch. The six samples received by each laboratory
were obtained by taking two 10g scoop splits from each of three separate 300g test units.
This format enabled nested ANOVA treatment of the results to evaluate homogeneity, i.e.
to ascertain whether between-unit variance is greater than within-unit variance.

Table 1 presents the 101 certified values (including Li in both elemental and oxide form for
peroxide fusion and 4-acid digestion) together with their associated 1SD’s, 95%
confidence and tolerance limits, Table 2 shows 57 indicative values and Table 3 provides
performance gate intervals for the certified values based on their pooled 1SD’s. Tabulated
results of all elements together with uncorrected means, medians, standard deviations,
relative standard deviations and per cent deviation of lab means from the corrected mean
of means (PDM3) are presented in the detailed certification data for this CRM (OREAS 999
DataPack-1.0.190208_104741.xlsx).

Results are also presented in scatter plots for Li2O (wt.%) by peroxide fusion ICP and 4-
acid digestion in Figure 1 and 2 respectively, together with ±3SD (magenta) and ±5%
(yellow) control lines and certified value (green line). Accepted individual results are
coloured blue and individual and dataset outliers are identified in red and violet,
respectively.

COA-1422-OREAS999-R1 Page: 7 of 17
 STATISTICAL ANALYSIS
Certified Values, Standard Deviations, Confidence and Tolerance Limits have been
determined for each analytical method following removal of individual and laboratory
outliers (Table 1). Certified Values are the mean of means after outlier filtering. The 95%
Confidence Limit is a measure of the reliability of the certified value, i.e. the narrower the
Confidence Interval the greater the certainty in the Certified Value. It should not be used
as a control limit for laboratory performance.

95% Confidence Limits are inversely proportional to the number of participating

laboratories and inter-laboratory agreement. It is a measure of the reliability of the certified
value. A 95% confidence interval indicates a 95% probability that the true value of the
analyte under consideration lies between the upper and lower limits. 95% Confidence
Limits should not be used as control limits for laboratory performance.

Indicative (uncertified) values (Table 2) are provided where i) the number of laboratories
reporting a particular analyte is insufficient (< 5) to support certification; ii) interlaboratory
consensus is poor; or iii) a significant proportion of results are outlying or reported as less
than detection limits.

Standard Deviation values (1SDs) are reported in Table 1. They provide an indication of
a level of performance that might reasonably be expected from a laboratory being
monitored by this CRM in a QA/QC program. They take into account errors attributable to
measurement uncertainty and CRM variability. For an effective CRM the contribution of the
latter should be negligible in comparison to measurement errors. The Standard Deviation
values include all sources of measurement uncertainty: between-lab variance, within-run
variance (precision errors) and CRM variability.

The SD for each analyte’s certified value is calculated from the same filtered data set used
to determine the certified value, i.e. after removal of all individual, lab dataset (batch) and
3SD outliers (single iteration). These outliers can only be removed after the absolute
homogeneity of the CRM has been independently established, i.e. the outliers must be
confidently deemed to be analytical rather than arising from inhomogeneity of the CRM.
The standard deviation is then calculated for each analyte from the pooled accepted
analyses generated from the certification program.

In the application of SD’s in monitoring performance it is important to note that not all
laboratories function at the same level of proficiency and that different methods in use at a
particular laboratory have differing levels of precision. Each laboratory has its own inherent
SD (for a specific concentration level and analyte-method pair) based on the analytical
process and this SD is not directly related to the round robin program.

The majority of data generated in the round robin program was produced by a selection of
world class laboratories. The SD’s thus generated are more constrained than those that
would be produced across a randomly selected group of laboratories. To produce more
generally achievable SD’s the ‘pooled’ SD’s provided in this report include inter-lab bias.
This ‘one size fits all’ approach may require revision at the discretion of the QC manager
concerned following careful scrutiny of QC control charts.

Table 3 shows Performance Gates calculated for two and three standard deviations. As a
guide these intervals may be regarded as warning or rejection for multiple 2SD outliers, or
rejection for individual 3SD outliers in QC monitoring, although their precise application
should be at the discretion of the QC manager concerned. A second method utilises a 5%

COA-1422-OREAS999-R1 Page: 8 of 17
window calculated directly from the certified value. Standard deviation is also shown in
relative percent for one, two and three relative standard deviations (1RSD, 2RSD and
3RSD) to facilitate an appreciation of the magnitude of these numbers and a comparison
with the 5% window. Caution should be exercised when concentration levels approach
lower limits of detection of the analytical methods employed as performance gates
calculated from standard deviations tend to be excessively wide whereas those
determined by the 5% method are too narrow. One approach used at commercial
laboratories is to set the acceptance criteria at twice the detection level (DL) ± 10%.

i.e. Certified Value ± 10% ± 2DL (adapted from Govett, 1983)

Table 3. Performance Gates for OREAS 999.

Absolute Standard Deviations Relative Standard Deviations 5% window
Certified
Constituent
Value 2SD 2SD 3SD 3SD
1SD 1RSD 2RSD 3RSD Low High
Low High Low High
Peroxide Fusion ICP
Al, wt.% 12.23 0.411 11.41 13.06 11.00 13.47 3.36% 6.72% 10.08% 11.62 12.84
Ba, ppm 39.1 2.64 33.8 44.3 31.2 47.0 6.75% 13.49% 20.24% 37.1 41.0
Be, ppm 51 2.1 46 55 44 57 4.12% 8.24% 12.36% 48 53
Bi, ppm 2.21 0.185 1.84 2.58 1.65 2.76 8.40% 16.81% 25.21% 2.10 2.32
Ca, wt.% 0.481 0.059 0.363 0.599 0.304 0.658 12.25% 24.51% 36.76% 0.457 0.505
Ce, ppm 4.15 0.360 3.43 4.87 3.07 5.23 8.66% 17.32% 25.99% 3.94 4.36
Co, ppm 5.24 0.343 4.56 5.93 4.21 6.27 6.54% 13.08% 19.63% 4.98 5.50
Cr, ppm 112 17 78 145 62 162 14.90% 29.79% 44.69% 106 117
Cs, ppm 93 3.6 86 100 82 104 3.90% 7.80% 11.70% 89 98
Cu, ppm 25.5 3.4 18.7 32.3 15.3 35.7 13.29% 26.58% 39.87% 24.2 26.8
Dy, ppm 0.80 0.050 0.71 0.90 0.66 0.95 6.17% 12.34% 18.51% 0.76 0.84
Er, ppm 0.27 0.03 0.20 0.33 0.17 0.36 11.86% 23.72% 35.58% 0.25 0.28
Fe, wt.% 1.73 0.067 1.60 1.87 1.53 1.93 3.85% 7.69% 11.54% 1.65 1.82
Ga, ppm 88 6.4 75 101 68 107 7.32% 14.63% 21.95% 83 92
Gd, ppm 1.08 0.16 0.77 1.39 0.61 1.55 14.55% 29.10% 43.65% 1.03 1.13
Ge, ppm 4.31 0.45 3.41 5.22 2.95 5.68 10.52% 21.04% 31.56% 4.10 4.53
Ho, ppm 0.11 0.011 0.09 0.14 0.08 0.15 9.95% 19.89% 29.84% 0.11 0.12
K, wt.% 0.522 0.048 0.426 0.617 0.378 0.665 9.16% 18.32% 27.49% 0.496 0.548
La, ppm 1.84 0.25 1.35 2.33 1.10 2.57 13.35% 26.70% 40.05% 1.74 1.93
Li, wt.% 2.67 0.103 2.47 2.88 2.36 2.98 3.86% 7.73% 11.59% 2.54 2.81
Li2O, wt.% 5.76 0.222 5.31 6.20 5.09 6.42 3.86% 7.73% 11.59% 5.47 6.05
Mg, wt.% 0.473 0.020 0.432 0.514 0.412 0.534 4.32% 8.64% 12.96% 0.449 0.497
Mn, wt.% 0.147 0.006 0.136 0.158 0.130 0.163 3.79% 7.59% 11.38% 0.139 0.154
Mo, ppm 2.27 0.38 1.51 3.02 1.13 3.40 16.68% 33.35% 50.03% 2.15 2.38
Nb, ppm 74 6.2 61 86 55 92 8.42% 16.84% 25.25% 70 77
Nd, ppm 1.90 0.22 1.46 2.34 1.24 2.55 11.54% 23.09% 34.63% 1.80 1.99
Ni, ppm 52 4.2 44 61 40 65 7.99% 15.97% 23.96% 50 55
P, wt.% 0.016 0.005 0.006 0.026 0.001 0.031 31.10% 62.20% 93.30% 0.015 0.017
Pr, ppm 0.52 0.06 0.39 0.65 0.32 0.71 12.40% 24.79% 37.19% 0.49 0.54
Rb, ppm 423 20 383 462 364 482 4.66% 9.31% 13.97% 402 444
SI unit equivalents: ppm, parts per million ≡ mg/kg ≡ µg/g ≡ 0.0001 wt.% ≡ 1000 ppb, parts per billion.
Note 1: intervals may appear asymmetric due to rounding.
Note 2: the number of decimal places quoted does not imply accuracy of the certified value to this level but are given to
minimise rounding errors when calculating 2SD and 3SD windows.

COA-1422-OREAS999-R1 Page: 9 of 17
 Table 3. Performance Gates continued.
Absolute Standard Deviations Relative Standard Deviations 5% window
Certified
Constituent
Value 2SD 2SD 3SD 3SD
1SD 1RSD 2RSD 3RSD Low High
Low High Low High
Peroxide Fusion ICP continued
Sb, ppm 1.02 0.17 0.69 1.36 0.53 1.52 16.22% 32.43% 48.65% 0.97 1.08
Si, wt.% 30.30 0.680 28.94 31.66 28.26 32.34 2.24% 4.49% 6.73% 28.78 31.81
Sm, ppm 1.02 0.099 0.82 1.21 0.72 1.31 9.75% 19.50% 29.25% 0.96 1.07
Sn, ppm 84 5.3 73 94 68 99 6.30% 12.61% 18.91% 79 88
Sr, ppm 23.0 3.3 16.3 29.7 13.0 33.0 14.54% 29.09% 43.63% 21.8 24.1
Ta, ppm 45.5 2.08 41.4 49.7 39.3 51.8 4.56% 9.12% 13.68% 43.3 47.8
Tb, ppm 0.18 0.02 0.14 0.22 0.12 0.24 11.11% 22.22% 33.33% 0.17 0.19
Th, ppm 3.01 0.158 2.70 3.33 2.54 3.48 5.24% 10.47% 15.71% 2.86 3.16
Ti, wt.% 0.034 0.004 0.026 0.043 0.022 0.047 11.99% 23.98% 35.97% 0.033 0.036
Tl, ppm 4.26 0.253 3.76 4.77 3.50 5.02 5.94% 11.88% 17.83% 4.05 4.48
U, ppm 2.51 0.226 2.06 2.96 1.83 3.19 9.02% 18.04% 27.07% 2.38 2.64
W, ppm 6.94 0.391 6.16 7.73 5.77 8.12 5.63% 11.27% 16.90% 6.60 7.29
Y, ppm 4.19 0.43 3.33 5.05 2.90 5.48 10.25% 20.50% 30.75% 3.98 4.40
Zn, ppm 77 4.3 68 85 64 90 5.58% 11.15% 16.73% 73 81
Zr, ppm 32.9 3.4 26.1 39.7 22.8 43.0 10.27% 20.54% 30.81% 31.3 34.5
Borate Fusion XRF
Al2O3, wt.% 23.39 0.114 23.16 23.62 23.05 23.74 0.49% 0.98% 1.47% 22.22 24.56
CaO, wt.% 0.670 0.013 0.643 0.696 0.630 0.709 1.98% 3.96% 5.93% 0.636 0.703
Fe2O3, wt.% 2.49 0.033 2.42 2.55 2.39 2.59 1.31% 2.62% 3.94% 2.37 2.61
K2O, wt.% 0.612 0.009 0.593 0.630 0.583 0.640 1.55% 3.09% 4.64% 0.581 0.642
MgO, wt.% 0.796 0.012 0.772 0.820 0.760 0.832 1.50% 2.99% 4.49% 0.756 0.836
MnO, wt.% 0.192 0.005 0.182 0.201 0.177 0.206 2.50% 5.01% 7.51% 0.182 0.201
Na2O, wt.% 0.945 0.024 0.897 0.993 0.873 1.017 2.54% 5.08% 7.62% 0.897 0.992
P2O5, wt.% 0.038 0.004 0.031 0.045 0.027 0.049 9.65% 19.30% 28.95% 0.036 0.040
SiO2, wt.% 64.23 0.446 63.34 65.12 62.89 65.56 0.69% 1.39% 2.08% 61.02 67.44
SO3, wt.% 0.042 0.006 0.029 0.054 0.023 0.060 14.63% 29.26% 43.89% 0.040 0.044
TiO2, wt.% 0.060 0.007 0.047 0.073 0.041 0.080 10.81% 21.63% 32.44% 0.057 0.063
Thermogravimetry
LOI1000, wt.% 0.764 0.114 0.536 0.993 0.421 1.107 14.96% 29.91% 44.87% 0.726 0.802
4-Acid Digestion
Al, wt.% 10.77 1.42 7.92 13.62 6.50 15.04 13.22% 26.44% 39.66% 10.23 11.31
As, ppm 5.36 1.07 3.22 7.49 2.15 8.56 19.94% 39.89% 59.83% 5.09 5.62
Ba, ppm 39.6 2.34 34.9 44.3 32.6 46.6 5.90% 11.81% 17.71% 37.6 41.6
Be, ppm 49.8 3.49 42.8 56.8 39.3 60.2 7.01% 14.01% 21.02% 47.3 52.3
Bi, ppm 2.11 0.131 1.85 2.37 1.72 2.51 6.18% 12.36% 18.55% 2.01 2.22
Ca, wt.% 0.450 0.033 0.384 0.516 0.351 0.548 7.31% 14.63% 21.94% 0.427 0.472
Co, ppm 4.95 0.262 4.43 5.48 4.17 5.74 5.29% 10.58% 15.88% 4.71 5.20
Cr, ppm 81 21 40 122 19 142 25.49% 50.97% 76.46% 77 85
Cs, ppm 88 11 66 110 56 121 12.31% 24.61% 36.92% 84 93
Cu, ppm 25.4 2.34 20.8 30.1 18.4 32.5 9.19% 18.38% 27.56% 24.2 26.7
Dy, ppm 0.67 0.13 0.42 0.93 0.30 1.05 18.72% 37.45% 56.17% 0.64 0.71
SI unit equivalents: ppm, parts per million ≡ mg/kg ≡ µg/g ≡ 0.0001 wt.% ≡ 1000 ppb, parts per billion.
Note 1: intervals may appear asymmetric due to rounding.
Note 2: the number of decimal places quoted does not imply accuracy of the certified value to this level but are given to
minimise rounding errors when calculating 2SD and 3SD windows.

COA-1422-OREAS999-R1 Page: 10 of 17
 Table 3. Performance Gates continued.
Absolute Standard Deviations Relative Standard Deviations 5% window
Certified
Constituent
Value 2SD 2SD 3SD 3SD
1SD 1RSD 2RSD 3RSD Low High
Low High Low High
4-Acid Digestion continued
Er, ppm 0.23 0.05 0.14 0.33 0.10 0.37 19.56% 39.12% 58.68% 0.22 0.25
Fe, wt.% 1.62 0.097 1.42 1.81 1.33 1.91 5.99% 11.99% 17.98% 1.54 1.70
Ga, ppm 82 5.4 71 93 66 98 6.58% 13.16% 19.74% 78 86
Hf, ppm 1.98 0.171 1.64 2.33 1.47 2.50 8.62% 17.23% 25.85% 1.89 2.08
Ho, ppm 0.090 0.018 0.055 0.125 0.037 0.142 19.54% 39.07% 58.61% 0.085 0.094
K, wt.% 0.500 0.041 0.418 0.582 0.377 0.623 8.20% 16.40% 24.60% 0.475 0.525
La, ppm 1.68 0.34 1.00 2.36 0.66 2.69 20.24% 40.48% 60.71% 1.59 1.76
Li, wt.% 2.65 0.057 2.54 2.76 2.48 2.82 2.14% 4.27% 6.41% 2.52 2.78
Li2O, wt.% 5.70 0.122 5.46 5.95 5.34 6.07 2.14% 4.27% 6.41% 5.42 5.99
Mg, wt.% 0.410 0.066 0.277 0.543 0.211 0.609 16.20% 32.41% 48.61% 0.389 0.430
Mn, wt.% 0.143 0.006 0.132 0.154 0.126 0.160 3.96% 7.92% 11.89% 0.136 0.150
Mo, ppm 2.06 0.140 1.78 2.34 1.64 2.48 6.81% 13.63% 20.44% 1.95 2.16
Na, wt.% 0.693 0.023 0.646 0.739 0.622 0.763 3.38% 6.76% 10.14% 0.658 0.727
Nb, ppm 75 4.7 66 85 61 89 6.20% 12.39% 18.59% 72 79
Nd, ppm 1.87 0.28 1.31 2.42 1.03 2.70 14.85% 29.70% 44.55% 1.77 1.96
Ni, ppm 47.5 1.74 44.0 51.0 42.3 52.7 3.65% 7.31% 10.96% 45.1 49.9
P, wt.% 0.016 0.002 0.013 0.019 0.011 0.021 10.59% 21.18% 31.76% 0.015 0.017
Pb, ppm 5.17 0.304 4.56 5.78 4.26 6.08 5.88% 11.76% 17.65% 4.91 5.43
S, wt.% 0.020 0.002 0.016 0.023 0.015 0.024 8.00% 16.00% 24.00% 0.019 0.021
Sb, ppm 1.11 0.095 0.92 1.30 0.83 1.39 8.51% 17.03% 25.54% 1.05 1.17
Sc, ppm 1.83 0.37 1.09 2.57 0.72 2.94 20.19% 40.37% 60.56% 1.74 1.92
Sn, ppm 63 5.5 52 74 47 80 8.62% 17.23% 25.85% 60 67
Sr, ppm 16.9 2.9 11.2 22.7 8.3 25.6 16.97% 33.93% 50.90% 16.1 17.8
Ta, ppm 49.0 4.00 41.0 57.0 37.0 61.0 8.17% 16.33% 24.50% 46.6 51.5
Tb, ppm 0.15 0.02 0.10 0.20 0.08 0.23 16.31% 32.62% 48.94% 0.14 0.16
Ti, wt.% 0.034 0.001 0.031 0.037 0.030 0.039 4.31% 8.63% 12.94% 0.033 0.036
Tl, ppm 4.26 0.188 3.88 4.63 3.69 4.82 4.43% 8.86% 13.29% 4.04 4.47
U, ppm 2.12 0.37 1.38 2.86 1.01 3.23 17.43% 34.87% 52.30% 2.02 2.23
V, ppm 14.8 1.18 12.4 17.1 11.2 18.3 7.97% 15.94% 23.91% 14.0 15.5
W, ppm 6.97 0.546 5.88 8.07 5.34 8.61 7.83% 15.66% 23.49% 6.62 7.32
Yb, ppm 0.24 0.022 0.19 0.28 0.17 0.30 9.50% 19.00% 28.50% 0.22 0.25
Zn, ppm 71 4.1 63 80 59 84 5.72% 11.45% 17.17% 68 75
Zr, ppm 20.0 2.3 15.5 24.6 13.2 26.9 11.39% 22.79% 34.18% 19.0 21.0
SI unit equivalents: ppm, parts per million ≡ mg/kg ≡ µg/g ≡ 0.0001 wt.% ≡ 1000 ppb, parts per billion.
Note 1: intervals may appear asymmetric due to rounding.
Note 2: the number of decimal places quoted does not imply accuracy of the certified value to this level but are given to
minimise rounding errors when calculating 2SD and 3SD windows.

Tolerance Limits (ISO Guide 3207) were determined using an analysis of precision errors
method and are considered a conservative estimate of true homogeneity. The meaning of
tolerance limits may be illustrated for lithium oxide (Li2O) by peroxide fusion ICP, where
99% of the time (1-α=0.99) at least 95% of subsamples (ρ=0.95) will have concentrations
lying between 5.63 and 5.88 wt.%. Put more precisely, this means that if the same number
of subsamples were taken and analysed in the same manner repeatedly, 99% of the
tolerance intervals so constructed would cover at least 95% of the total population, and 1%

COA-1422-OREAS999-R1 Page: 11 of 17
of the tolerance intervals would cover less than 95% of the total population (ISO Guide
35). Please note that tolerance limits pertain to the homogeneity of the CRM only and
should not be used as control limits for laboratory performance.

ANOVA Study
The homogeneity of OREAS 999 has also been evaluated in an ANOVA study for all
certified analytes occurring at least 20 times the lower limit of detection. No significant p-
values were found indicating that no evidence exists that between-unit variance is greater
than within-unit variance.

It is important to note that ANOVA is not an absolute measure of homogeneity. Rather, it

establishes whether or not the analytes are distributed in a similar manner throughout the
packaging run of OREAS 999 and whether the variance between two subsamples from the
same unit is statistically distinguishable to the variance from two subsamples taken from any
two separate units. A reference material therefore, can possess poor absolute homogeneity
yet still pass a relative homogeneity test if the within-unit heterogeneity is large and similar
across all units.

Based on the statistical analysis of the results of the inter-laboratory certification program it
can be concluded that OREAS 999 is sufficiently homogenous and is fit-for-purpose as a
certified reference material (see ‘Intended Use’ below).

PARTICIPATING LABORATORIES

1. AGAT Laboratories, Mississauga, Ontario, Canada

2. Alex Stewart International, Mendoza, Argentina
3. ALS, Brisbane, QLD, Australia
4. ALS, Lima, Peru
5. ALS, Loughrea, Galway, Ireland
6. ALS, Perth, WA, Australia
7. ALS, Vancouver, BC, Canada
8. American Assay Laboratories, Sparks, Nevada, USA
9. Bureau Veritas Commodities Canada Ltd, Vancouver, BC, Canada
10. Bureau Veritas Geoanalytical, Adelaide, SA, Australia
11. Bureau Veritas Geoanalytical, Perth, WA, Australia
12. Inspectorate (BV), Lima, Peru
13. Intertek Genalysis, Perth, WA, Australia
14. Intertek Testing Services Philippines, Cupang, Muntinlupa, Philippines
15. Nagrom, Perth, WA, Australia
16. Ontario Geological Survey, Sudbury, Ontario, Canada
17. PT Geoservices Ltd, Cikarang, Jakarta Raya, Indonesia
18. Reminex Centre de Recherche, Marrakesh, Marrakesh-Safi, Morocco
19. Saskatchewan Research Council, Saskatoon, Saskatchewan, Canada
20. SGS, Randfontein, Gauteng, South Africa
21. SGS Australia Mineral Services, Perth, WA, Australia
22. SGS Canada Inc., Vancouver, BC, Canada
23. SGS Lakefield Research Ltd, Lakefield, Ontario, Canada
24. UIS Analytical Services, Centurion , South Africa

Please Note: Above numbered alphabetical list of participating laboratories does

not reflect the Lab ID numbering on the scatter plots below

COA-1422-OREAS999-R1 Page: 12 of 17
 Figure 1. Li2O (wt.%) by peroxide fusion ICP in OREAS 999

COA-1422-OREAS999-R1 Page: 13 of 17
 Figure 2. Li2O (wt.%) by 4-acid digestion in OREAS 999

COA-1422-OREAS999-R1 Page: 14 of 17
 PREPARER AND SUPPLIER
Certified reference material OREAS 999 was prepared, certified and supplied by:

ORE Research & Exploration Pty Ltd Tel: +613-9729 0333

37A Hosie Street Fax: +613-9729 8338
Bayswater North VIC 3153 Web: www.ore.com.au
AUSTRALIA Email: [email protected]

It is packaged in 10g units in laminated foil packets and in 500g units in wide-mouth plastic jars.

METROLOGICAL TRACEABILITY
The analytical samples were selected in a manner to represent the entire batch of
prepared CRM. This ‘representivity’ was maintained in each submitted laboratory sample
batch and ensures the user that the data is traceable from sample selection through to the
analytical results that underlie the consensus values. Each analytical data set has been
validated by its assayer through the inclusion of internal reference materials and QC
checks during analysis.

The laboratories were chosen on the basis of their competence (from past performance in
inter-laboratory programs undertaken by ORE Pty Ltd) for a particular analytical method,
analyte or analyte suite, and sample matrix. Most of these laboratories have and maintain
ISO 17025 accreditation. The certified values presented in this report are calculated from
the means of accepted data following robust statistical treatment as detailed in this report.

Guide ISO/TR 16476:2016, section 5.3.1 describes metrological traceability in reference

materials as it pertains to the transformation of the measurand. In this section it states,
“Although the determination of the property value itself can be made traceable to
appropriate units through, for example, calibration of the measurement equipment used,
steps like the transformation of the sample from one physical (chemical) state to another
cannot. Such transformations may only be compared with a reference (when available), or
among themselves. For some transformations, reference methods have been defined and
may be used in certification projects to evaluate the uncertainty associated with such a
transformation. In other cases, only a comparison among different laboratories using
the same method is possible. In this case, certification takes place on the basis of
agreement among independent measurement results (see ISO Guide 35:2006, Clause 10).”

COMMUTABILITY
The measurements of the results that underlie the certified values contained in this report
were undertaken by methods involving pre-treatment (digestion/fusion) of the sample. This
served to reduce the sample to a simple and well understood form permitting calibration
using simple solutions of the CRM. Due to these methods being well understood and
highly effective, commutability is not an issue for this CRM. All OREAS CRMs are sourced
from natural ore minerals meaning they will display similar behaviour as routine ‘field’
samples in the relevant measurement process. Care should be taken to ensure ‘matrix
matching’ as close as practically achievable. The matrix and mineralisation style of the
CRM is described in the ‘Source Material’ section and users should select appropriate
CRMs matching these attributes to their field samples.

COA-1422-OREAS999-R1 Page: 15 of 17
 INTENDED USE
OREAS 999 is intended to cover all activities needed to produce a measurement result.
This includes extraction, possible separation steps and the actual measurement process
(the signal producing step). OREAS 999 may be used to calibrate the entire procedure by
producing a pure substance CRM transformed into a calibration solution.

OREAS 999 is intended for the following uses:

 For the monitoring of laboratory performance in the analysis of analytes reported
in Table 1 in geological samples;
 For the verification of analytical methods for analytes reported in Table 1;
 For the calibration of instruments used in the determination of the concentration
of analytes reported in Table 1.

STABILITY AND STORAGE INSTRUCTIONS

OREAS 999 was sourced from Li concentrate (spodumene) and is low in reactive
sulphides. In its unopened state and under normal conditions of storage it has a shelf life
beyond ten years. Its stability will be monitored at regular intervals and purchasers notified
if any changes are observed.

INSTRUCTIONS FOR CORRECT USE

The certified values for lithium borate fusion XRF and for LOI are on a ‘dry sample’ basis
whilst all other certified values are reported on a ‘sample as received’ basis.

HANDLING INSTRUCTIONS
Fine powders pose a risk to eyes and lungs and therefore standard precautions such as
the use of safety glasses and dust masks are advised.

LEGAL NOTICE
Ore Research & Exploration Pty Ltd has prepared and statistically evaluated the property
values of this reference material to the best of its ability. The Purchaser by receipt hereof
releases and indemnifies Ore Research & Exploration Pty Ltd from and against all liability
and costs arising from the use of this material and information.

DOCUMENT HISTORY

Revision No. Date Changes applied

nd Updated ‘SOURCE MATERIAL’ section.
1 22 February 2019
Table of content got ‘QMS ACCREDITED’ link added.
th
0 11 February 2019 First publication.

COA-1422-OREAS999-R1 Page: 16 of 17
 QMS ACCREDITED
ORE Pty Ltd is accredited to ISO 9001:2015 by Lloyd’s Register Quality Assurance Ltd for
its quality management system including development, manufacturing, certification and
supply of CRMs.

CERTIFYING OFFICER

22nd February, 2019

Craig Hamlyn (B.Sc. Hons - Geology), Technical Manager - ORE P/L

REFERENCES
Govett, G.J.S. (1983), ed. Handbook of Exploration Geochemistry, Volume 2: Statistics and
Data Analysis in Geochemical Prospecting (Variations of accuracy and precision).
ISO Guide 30 (2015), Terms and definitions used in connection with reference materials.
ISO Guide 31 (2015), Reference materials – Contents of certificates and labels.
ISO Guide 3207 (1975), Statistical interpretation of data - Determination of a statistical
tolerance interval.
ISO Guide 35 (2017), Certification of reference materials - General and statistical
principals.

COA-1422-OREAS999-R1 Page: 17 of 17