Lynda Bloom, Analytical Solutions Ltd.

Craig Hamlyn, ORE Research & Exploration P/L.

Papers
Why dont
round-robin
statistics apply
in real-life?

2
ISO Guide 35: Reference
Materials General and
statistical principles for
certification
Homogeneity study (between bottle
variation)
Stability study (lifetime and shelf life)
Characterization study

3
Characterization Study
Collaborative study/trial (round robin)
Standardized methods including
transformation
When using multiple laboratories include
some kind of standard substance,
mixture or solutionto verify accuracy
Assumes there exists a population of
laboratoriesequally capableto
provide results with acceptable
accuracy

4
Characterization Study (2)
If every result can be assumed technically
valid = six to eight participants
If there can be statistically and technically
invalid results = at least 10 and preferably
15 participants
2 units per participants but 6 replicates
over (at least) 2 days
To determine homogeneity, minimum 3 -4
units

5
Statistical Analysis
Assumes normal distribution; for small
numbers of determinations assumption
may be invalid
Assigning a single property value is
only useful when there is agreement
among methods and/or laboratoriesif
there is no agreement between the
laboratories..then the characterization
data are unsuitable for establishing
property values

6
OREAS 6Pc
17 international laboratories
6 replicates from randomized sub-samples
during packaging
Mean = 1.52 g/t Au
Std. Dev. within lab = 0.01 to 0.06 g/t Au
(or 0.65 to 4.25% RSD)
Performance Gate (Pooled Std. Dev.) =
0.07 g/t Au (4.26% RSD)

7
6Pc: Round Robin Assays
OREAS 6Pc

1.9

1.8

1.7
+2 Std. Dev.

1.6
Gold (g/t)

Mean
1.5

1.4 -2 Std. Dev.

1.3
0.5 gm by INAA

1.2

1.1
0 1 2 3 4 5 6 7

8
6Pc: 5 vs 17 Laboratories
OREAS 6Pc

1.8

1.7
+2 Std. Dev.
5 Highest Labs (Mean = 1.60 g/t)
1.6
Pooled
Mean
Gold (g/t)

1.5

5 Lowest Labs (Mean = 1,44 g/t)

1.4
-2 Std. Dev.

1.3

1.2

1.1
0 1 2 3 4 5 6 7

9
10
 Canadian Laboratory Example
OREAS 6Pc (N = 338)

1.8

+3 Std. Dev.

1.7 +10%

+2 Std. Dev.
1.6
Gold (g/t)

1.5

1.4 -2 Std. Dev.

-10%

1.3
-3 Std. Dev.

1.2
15/05/2009 04/06/2009 24/06/2009 14/07/2009 03/08/2009 23/08/2009 12/09/2009 02/10/2009 22/10/2009

Date Received

11
 Overseas Laboratory Example
6Pc

1.8
+3 Std. Dev.

1.7 +10%

+2 Std. Dev.
1.6
Gold (g/t)

1.5

1.4 -2 Std. Dev.

-10%
1.3
-3 Std. Dev.

1.2
0 50 100 150 200 250 300

Date Received

12
Dilemma?
Require a large number of laboratories for
confidence in the accepted value (>15)
Pooled better reflects real-time
performance
Pooled is dependent on accuracy of
participating laboratories

13
Suggestions
Only use accredited laboratories
Standardized analytical methods
Submitted blind and with CRMs
Well-blended, fine particles (100% 30)
2-stage nested design of subsample selection

Multiple submissions over time

Homogeneity testing
Treatment of outliers
Large batches (>150 kg)

14
 Submissions over time
Fig. 1. Results for CuT in LS11 Control Lines
Green = Certified Value
1.18
Yellow = 5% Control
Orange = 3SD (within-lab)
1.16 Red = 3SD (between-lab)

1.14

1.12
CuT (wt.%)

1.10

1.08

1.06

1.04

1.02

1.00 Low bias

No batch variation High batch variation

15
 Homogeneity Testing: < 1
gram
22000

21600
Au ppb

21200

20800

20400
0.2 gm Replicates - INAA
20000 1 gm Replicates - INAA

19600
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21

16
Homogeneity Testing: 30 gm
1550

1500

1450

Au 1400
ppb
1350

1300

INTERNATIONAL STD.
1250
ORE 6P
1200
1 2 3 4 5 6 7 8 9 10

17
Outlier vs.
Straggler/ Maverick/ Aberrant Value

Grubbs or Dixon Test (~ > 2.5 )

ASTM E178: statistical tests are used to
identify outliers, not to reject them from
the data set
Difficult to identify outliers in small data
sets (n < 5)
If outliers are included, will be larger

18
CONCLUSIO
NS
Industry needs to agree on
statistical parameters and
methodologies

Additional test work will lead

to higher costs unless larger
batches are produced

An international research
program has been proposed
to compare laboratory
performance vs CRM quality
19