Ore Research & Exploration Pty LTD: Gold Reference Material Oreas 7ca

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O R E R E S E A R C H & E X P L O R A T I O N P T Y L T D

6-8 Gatwick Road, Bayswater North, Vic 3153 AUSTRALIA


Telephone: 61-(0)3-9729 0333 Facsimile: 61-(0)3-9729 4777












CERTIFICATE OF ANALYSIS FOR


GOLD REFERENCE MATERIAL

OREAS 7Ca



SUMMARY STATISTICS

Recommended value and 95% confidence interval
Constituent Recommended 95% Confidence interval
value Low High
Gold, Au (ppm) 2.54 2.46 2.62


Recommended value and tolerance interval
Constituent Recommended
value
Tolerance interval
1-=0.99, =0.95
Low High
Gold, Au (ppm) 2.54 2.46 2.62



Prepared by:
Ore Research & Exploration Pty Ltd



REPORT 7Ca
Ore Research & Exploration Pty Ltd 1



INTRODUCTION

OREAS reference materials (RM) are intended to provide a low cost method of evaluating
and improving the quality of precious and base metal analysis of geological samples. To
the analyst they provide an effective means of calibrating analytical equipment, assessing
new techniques and routinely monitoring in-house procedures. To the explorationist they
provide an important control in analytical data sets related to exploration from the grass
roots level through to prospect evaluation.

As a rule only source materials exhibiting an exceptional level of homogeneity of the
element(s) of interest are used in the preparation of these materials. This has enabled Ore
Research & Exploration to produce a range of gold RM exhibiting homogeneity that
matches or exceeds that of currently available international reference materials. In many
instances RM produced from a single source are sufficiently homogeneous to produce a
relatively coarse-grained form designed to simulate drill chip samples. These have a grain
size of minus 3mm and are designated with a "C" suffix to the RM identification number.
These standards are packaged in 1kg units following homogenisation and are intended for
submission to analytical laboratories in subsample sizes of as little as 250g. They offer the
added advantages of providing a check on both sample preparation and analytical
procedures while acting as a transparent standard to the assay laboratory. The more
conventional pulped standards have a grain size of minus 75 microns and a higher degree
of homogeneity. These standards are distinguished by a "P" suffix to the standard
identification number. In line with ISO recommendations successive batch numbers are
now designated by the lower case suffixes "a", "b", "c", "d", etc.


SOURCE MATERIALS

The material used to produce gold-bearing standard OREAS 7Ca was taken from a
mineralised shear zone within Ordovician flysch sediments in the Blackwood area of
central Victoria. The sedimentary succession hosting the shear zone consists
predominantly of medium-grained greywackes together with subordinate interbedded
siltstone and slate. Hydrothermal alteration in the vicinity of the mineralisation is indicated
by the development of phyllite. The shear zone, in which gold grades attain a maximum, is
manifested by foliated sericitic and chloritic fault gouge and goethitic quartz veins.

Although no ore mineragraphy or scanning electron microscopy has been undertaken to
determine the nature of occurrence of the gold, the very homogeneous distribution on a
mesoscopic scale and uniform concentration gradient away from the ore zone suggests
the gold is extremely fine-grained and evenly disseminated. Limited percussion drilling
indicates that sulphides are rare to absent in the shear zone.

The approximate major and trace element composition of this oxidised, quartz-veined
metagreywacke comprising gold ore standard OREAS 7Ca is given in Table 1. The
constituents SiO
2
to Total are the means of duplicate XRF analyses determined by the
borate fusion method, while the remaining constituents, As to Zn, are means of twenty-
seven replicate analyses determined via INAA at Becquerel Laboratories.

Ore Research & Exploration Pty Ltd 2




COMMINUTION AND HOMOGENISATION PROCEDURES

The gold-bearing greywacke material comprising OREAS 7Ca was prepared in the
following manner:

a) primary crushing in a large (36 x 51cm) jaw crusher
b) drying in a gas-fired rotary drier
c) secondary crushing in a small (10 x 20cm) jaw crusher
d) tertiary crushing in a roller crusher
e) screening to minus 3mm
f) milling of approximately one third in a gamma mill
g) homogenisation in a ribbon blender
h) bagging into 20kg sublots

Throughout the bagging stage twenty-seven 1kg samples were taken at random intervals,
sealed in laminated plastic bags and set aside for analysis. These random sampling
intervals were determined using tables of random numbers.

Prior to bottling in 1kg units each 20kg sublot was further homogenised in a tumble
blender to counter the possibility of unmixing during handling. The resultant material
constitutes the minus 3mm reference material OREAS 7Ca.

For homogeneity testing a 250g scoop split was taken from each of the twenty-seven 1kg
chip samples and pulverised separately for 3 minutes in a vibratory ring mill. One 30g
scoop split was then taken from each of the 250g pulps for gold assay via instrumental
neutron activation analysis on 1g subsamples. The remaining 750g portions of the twenty-
seven chip samples were each pulverised separately for 3 minutes in a vibratory ring mill
and split into 200g subsamples for distribution to the laboratories participating in the round
robin.


ANALYSIS OF OREAS 7Ca

Seventeen laboratories participated in the analytical program and are listed in the section
headed PARTICIPATING LABORATORIES.

To ensure anonymity these laboratories have been randomly designated the letter codes
A through Q. With the exception of Laboratory Q, each laboratory received three 200g
subsamples with instructions to carry out duplicate fire assays for gold (using 50g charges)
on each subsample. Laboratories D, E, F, G, N & L were also instructed to conduct single
gold determinations on each subsample using an aqua regia digest. In all instances a
flame AAS finish was employed. For each laboratory the three 200g subsamples were
selected from different 750g pulps produced from the 1kg random samples taken during
the bagging stage. The results therefore provide an assessment of both the within- and
between-unit homogeneity and are amenable to analysis of variance treatment. Laboratory
Q received twenty-seven 50g subsamples split from the twenty-seven 250g pulps
produced from the 1kg random samples described above. The instructions were to
complete one assay per subsample via instrumental neutron activation analysis on an
analytical subsample weight of 30g.

Ore Research & Exploration Pty Ltd 3



In all instances laboratories were requested to ensure rigorous analytical procedures were
adhered to.

Individual assay results for the fire assay/AAS and INAA methods are presented in Tables
2 and 3 together with the mean, median and standard deviations (absolute and relative)
given for each data set. Interlaboratory agreement of the means of all but four data sets is
good, lying within 8% relative of the raw mean of means of 2.51ppm Au. The exceptions to
this are laboratories B, E, G and N which are 8.4%, 8.1% and 8.3% higher and 14.4%
lower, respectively, than the raw mean of means.

Supplementary aqua regia/flame AAS data from six laboratories are reported in Table 4
and with a mean of means of 2.18 0.32 ppm Au (95% confidence) are, as anticipated, on
average 14% lower than for fire assay determinations. The results obtained by the aqua
regia digest method were not included in the determination of the recommended value.


STATISTICAL EVALUATION OF ANALYTICAL DATA
FOR OREAS 7Ca

Recommended Value and Confidence Limits
The recommended value was determined from the mean of means of accepted replicate
values of accepted laboratory data sets A to Q according to the formulae

x =
1
n
x
i
i
ij
j
n
i
=

1


&& x =
1
p
x
i
i
p
=

1



where

x
n
x is the mean for laboratory i;
x is the mean of means.
ij
i
i
is the jth result reported by laboratory i;
p is the number of participating laboratories;
is the number of results reported by laboratory i;
&&


The confidence limits were obtained by calculation of the variance of the consensus value
(mean of means) and reference to Student's-t distribution with degrees of freedom (p-1)

( )
( )
( )
$
&& && V x x x
p p
i
i
p
=

1
1
2
1


Confidence limits ( ) ( )
( )
=

&&
$
&&
/
/
x t p V x
x 1 2
1
1 2


where t
1-x/2
(p-1) is the 1-x/2 fractile of the t-distribution with (p-1) degrees of freedom.

Ore Research & Exploration Pty Ltd 4




Table 1.


Approximate major and trace element of gold-bearing reference
material OREAS 7Ca; SiO2 to Total as weightpercent; rest in
parts per million.

Constituent Concentration Constituent Concentration

SiO2 71.1 As 1917
TiO2 0.68 Ba 683
Al2O3 15.2 Br 5
Fe2O3 4.06 Ce 90
MnO <0.01 Cr 502
MgO 0.72 Cs 10
CaO <0.01 Eu 1.4
Na2O <0.05 Hf 4.4
K2O 4.23 La 50
P2O5 0.08 Rb 168
SO3 0.04 Sb 161
H2O+ 3.44 Sc 14
Total 99.55 Sm 10
Th 16
W 18
Yb 2.8
Zn ~30


Table 2. Analytical results for gold (ppm) in OREAS 7Ca by 50g fire assay/flame AAS (Std. Dev. - one sigma
standard deviation; RSD- one sigma relative standard deviation. Outliers left justified and in bold.

Unit Replicate Lab A Lab B Lab C Lab D Lab E Lab F Lab G Lab H
1 1 2.44 2.69 2.46 2.29 2.90 2.72 2.64 2.67
2 1 2.33 2.69 2.42 2.48 2.52 2.75 2.74 2.42
3 1 2.46 2.69 2.24 2.45 2.65 2.75 2.75 2.42

1 2 2.35 2.84 2.48 2.38 2.83 2.46 2.75 2.64
2 2 2.34 2.75 2.54 2.44 2.54 2.72 2.40
3 2 2.54 2.68 2.40 2.54 2.85 2.75 2.45
Mean: 2.410 2.723 2.423 2.430 2.715 2.692 2.720 2.500
Median: 2.395 2.690 2.440 2.445 2.740 2.735 2.745 2.435
Std. Dev.: 0.084 0.063 0.102 0.086 0.166 0.114 0.054 0.121
RSD: 3.5 2.3 4.2 3.5 6.1 4.3 2.0 4.9


Table 2. Continued.
Unit Replicate Lab I Lab J Lab K Lab L Lab M Lab N Lab O Lab P


1 1 2.43 2.53 2.47 2.56 2.39 1.97 2.65 2.37
2 1 2.43 2.61 2.52 2.64 2.15 2.35 2.69 2.36
3 1 2.45 2.53 2.51 2.69 2.45 2.13 2.65 2.38

1 2 2.48 2.48 2.45 2.80 2.46 2.03 2.68 2.37
2 2 2.44 2.48 2.47 2.59 2.21 2.48 2.71 2.39
3 2 2.46 2.46 2.53 2.73 2.34 1.95 2.68 2.39

Mean: 2.448 2.515 2.492 2.668 2.333 2.152 2.677 2.377
Median: 2.445 2.505 2.490 2.665 2.365 2.080 2.680 2.375
Std. Dev.: 0.019 0.055 0.033 0.090 0.128 0.217 0.023 0.012
RSD: 0.8 2.2 1.3 3.4 5.5 10.1 0.9 0.5

Ore Research & Exploration Pty Ltd 5



Table 3.
Analytical results for gold (ppm) in OREAS 7Ca by instrumental neutron activation
analysis on 30g analytical subsample weights (abbreviations as for Table 2).
Unit No. Lab Q
1 2.416
2 2.452
3 2.414
4 2.451
5 2.462
6 2.496
7 2.482
8 2.492
9 2.451
10 2.456
11 2.426
12 2.413
13 2.401
14 2.514
15 2.401
16 2.428
17 2.446
18 2.423
19 2.410
20 2.479
21 2.424
22 2.410
23 2.410
24 2.384
25 2.487
26 2.487
27 2.442

Mean: 2.443
Median: 2.442
Std. Dev.: 0.035
RSD: 1.4


Table 4. Analytical results for gold (ppm) in OREAS 7Ca by aqua regia digest/flame AAS
on 25-30g analytical subsample weights (abbreviations as for Table 2).

Unit Lab D Lab E Lab F Lab G Lab L Lab N

1 1.97 2.24 2.13 2.22 2.72 2.00
2 1.97 1.94 2.05 2.43 2.68 1.98
3 1.98 1.80 2.07 2.25 2.82 1.98
Mean: 1.973 1.993 2.083 2.300 2.740 1.987
Median: 1.970 1.940 2.070 2.250 2.720 1.980
Std. Dev.: 0.006 0.225 0.042 0.114 0.072 0.012
RSD: 0.3 11.3 2.0 4.9 2.6 0.6

Ore Research & Exploration Pty Ltd 6



The distributions of the values are assumed to be symmetrical about the mean in the
calculation of the confidence limits.

The test for rejection of individual outliers was based on the test criterion, T, and reference
to tables of critical values of T at the 1% level of significance (ASTM E 178-94) as follows:

( )
T x x s
ij ij i i
= /

where
T
ij
is the test criterion for the jth result of laboratory i;
s
i
is the standard deviation of laboratory i.

The same principles were applied in testing for outlying laboratory means. Individual and
mean outliers are shown in bold type in Table 2 and 3 and have been omitted in the
determination of recommended values.





Table 5. Recommended value and 95% confidence interval
Constituent Recommended
value
95% Confidence interval
Low High
Gold, Au (ppm) 2.54 2.46 2.62


Statement of Homogeneity
The variability of replicate assays from each laboratory is a result of both measurement
and subsampling errors. In the determination of tolerance limits it is desirable to eliminate,
or at least substantially minimise, those errors attributable to measurement. One way of
achieving this is by substantially reducing the analytical subsample weight to a point where
most of the variability in replicate assays is due to sampling error and measurement error
becomes negligible. This approach has been adopted for pulp reference materials where
no additional processing is involved prior to taking the analytical subsample. In the case of
chip RM's, however, this method is inappropriate as two stages of subsampling and an
intervening pulverisation stage are involved. Instead homogeneity has been determined by
taking a 30g subsample from each of the twenty-seven 250g pulps prepared from the 1kg
random chip samples described earlier and assaying via INAA. From these results (Table
3) an estimated tolerance interval of 0.08ppm, calculated for an analytical subsample
weight of 50g (from the sampling constant relationship of Ingamells and Switzer, 1973),
was obtained using tables of factors for two-sided tolerance limits for normal distributions
(ISO Guide 3207) in which

( ) Lower limit is && , , x k n p s
2
1
( ) Upper limi x k n p s t is && , , +
2
1
where
Ore Research & Exploration Pty Ltd 7




n is the number of results reported by laboratory Q;
1- is the confidence level;
p is the proportion of results expected within the tolerance limits;
is the factor for two- sided tolerance limits (m, unknown);

k
2


and s is computed according to the formula

( )
s
x x
n
j
j
n
=

2
1
1 2
1
/


No individual outliers were removed from the results prior to the calculation of
tolerance intervals.

The meaning of these tolerance limits may be illustrated for gold (refer Table 6), where
99% of the time at least 95% of 250g-sized subsamples will have concentrations lying
between 2.46 and 2.62ppm. 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%
of the tolerance intervals would cover less than 95% of the total population (IS0 Guide 35).
Obviously, if OREAS 7Ca is subsampled in weights less than or greater than 250g, the
anticipated tolerance interval will be greater than or less than, respectively, that of
0.08ppm.

Table 6. Recommended values and tolerance limits
Constituent Recommended
value
Tolerance limits
1-=0.99, =0.95
Low High
Gold, Au (ppm) 2.54 2.46 2.62

It should be noted that these tolerance intervals are based on the assumption that all of the
observed variablilty is attributable to sampling error. Given that this variability in OREAS
2Ca is of similar magnitude to the measurement error associated with INAA, the estimate
of homogeneity should be regarded as conservative.


PARTICIPATING LABORATORIES

Amdel Laboratories Ltd, Thebarton, SA, Australia
Amdel Laboratories Ltd, Wangara, WA, Australia
Ammtec Limited, Balcatta, WA, Australia
Analabs Pty Ltd, Cooee, TAS, Australia
Analabs Pty Ltd, East Brisbane, QLD, Australia
Analabs Pty Ltd, Townsville, QLD, Australia
Analabs Pty Ltd, Welshpool, WA, Australia
Anglo American Research Laboratories Pty Ltd, Johannesburg, South Africa
Ore Research & Exploration Pty Ltd 8



Assaycorp Pty Ltd, Pine Creek, NT, Australia
Australian Assay Laboratories Pty Ltd, Balcatta, WA, Australia
Australian Laboratory Services Pty Ltd, Bendigo, VIC, Australia
Australian Laboratory Services Pty Ltd, Malaga, WA, Australia
Becquerel Laboratories, Lucas Heights, NSW, Australia
Genalysis Laboratory Services Pty Ltd, Maddington, WA, Australia
Minlab, Malaga, WA, Australia
SGS Australia Pty Ltd, Queens Park, WA, Australia
Western Mining Corporation Ltd, Kalgoorlie, WA, Australia


PREPARER AND SUPPLIER OF THE REFERENCE MATERIAL

The gold ore reference material, OREAS 7Ca has been prepared and certified and is
supplied by:
Ore Research & Exploration Pty Ltd
6-8 Gatwick Road
Bayswater North VIC 3153
AUSTRALIA

Telephone (03) 9729 0333 International 613-9729 0333
Facsimile (03) 9729 4777 International 613-9729 4777

It is available in unit sizes of 1kg.


INTENDED USE

OREAS 7Ca is a reference material intended for the verification of sample preparation
and analytical methods for gold.


STABILITY AND STORAGE INSTRUCTIONS

OREAS 7Ca has been prepared from gold-bearing metasediments within the oxidised
zone of a mineralised shear zone. It is therefore considered to have long-term stability
under normal storage conditions.


INSTRUCTIONS FOR THE CORRECT USE OF THE REFERENCE
MATERIAL

The recommended value for OREAS 7Ca refers to the concentration level of gold after
removal of hygroscopic moisture by drying in air to constant mass at 105
0
C. In its undried
state a hygroscopic moisture content of 0.56% has been established. If the reference
material is not dried by the user prior to analysis, the recommended value should be
corrected to the moisture-bearing basis.



Ore Research & Exploration Pty Ltd 9



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.


CERTIFYING OFFICER: Dr Paul Hamlyn


ACKNOWLEDGMENTS

The costs of development of this reference material were sponsored in part by the
Australian Minerals Industry Research Association Limited (AMIRA Project 388) through
funds contributed by Acacia Resources Limited, BHP Minerals, MIM Exploration Pty Ltd
and Western Mining Corporation Limited. Continent Resources Pty Ltd provided access to
lease areas. The assistance of these organisations and the cooperation of all participating
laboratories is warmly acknowledged.




REFERENCES

ASTM E178-94 (1994), Standard practice for dealing with outlying observations.

Ingamells, C. O. and Switzer, P. (1973), Talanta 20, 547-568.

ISO Guide 35 (1985), Certification of reference materials - General and statistical
principals.

ISO Guide 3207 (1975), Statistical interpretation of data - Determination of a statistical
tolerance interval.

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