ANALYTICAL CHEMISTRY & TESTING SERVICES

Indicator Mineral Chemistry

Quality Control Discussion

Mary Doherty
ALS Chemex
ANALYTICAL CHEMISTRY & TESTING SERVICES

Quality Control Discussion

Value of Quality
Define Sources of Error
Measurement of Error
Systems to minimize and control error
NI 43-101, ISO 9001, 17025, reporting
requirements
 Value of a Gold Company is directly related to Au Assay

ANALYTICAL CHEMISTRY & TESTING SERVICES

(Pitard, 2005)

Corporate Wealth is directly tied to quality

ANALYTICAL CHEMISTRY & TESTING SERVICES

Field Define Sources of Error

Variability

Field
Collection
Sampling Error

Sample
Preparation

Mineral ID
Analytical
ANALYTICAL CHEMISTRY & TESTING SERVICES

Field Variability

Stream Sediment Sample

Weight: 10 Kg Size Fraction: -2 mm
 Gys Safety Curve
ANALYTICAL CHEMISTRY & TESTING SERVICES
10kg

1kg Assume:
Homogeneous sample
Initial sample size
Sample
100g
Weight

te
Safe
Was

10g

1g
10um 100um 1mm 10mm
400 100 60 35 18 10 6 # Mesh
200
Maximum Particle Size
ANALYTICAL CHEMISTRY & TESTING SERVICES

Sample Heterogeneity

A. 3,0,1,1,1,0,0,0,1
Answer: <1
B. 9,4,3,2,4,3,3,4,5
Answer : 5

(Pitard)
ANALYTICAL CHEMISTRY & TESTING SERVICES

Field
Variability Define Sources of Error

Field
Collection
Sampling Error

Sample
Processing

Mineral ID
Analytical
 ANALYTICAL CHEMISTRY & TESTING SERVICES

Sample Processing

Sieve
Gravity Density
Separation

Liquid Density Magnetic

Separation Separation Mineral Picking
ANALYTICAL CHEMISTRY & TESTING SERVICES

Define Sources of Error, Processing

Sample processing is complicated by
mineral chemistry variations, chemistry
varies magnetic susceptibility and
density.
Loss sample
Sample switches
Grain losses
Sample contamination/carry-over
Splitting error
ANALYTICAL CHEMISTRY & TESTING SERVICES

Split Error

Taking a representative split from a large

sample is not as simple as many people believe.
(Rocklabs)
ANALYTICAL CHEMISTRY & TESTING SERVICES

Split Error
Split all sample
Even split
No density separation
No loss of fines or size segregation
Error Comparison
Cone and Quarter 13.6%
Scoop Sample 10.3%
Riffle Split 2%
Rotary 0.25%
(Allen and Kahn, 1970)
Riffle may be as good if operator
careful, less likely for larger
samples requiring multiple splits.
Rotary not too fast to segregate
fines, more cones preferable.
ANALYTICAL CHEMISTRY & TESTING SERVICES

Field
Variability Define Sources of Error

Field
Collection
Sampling Error

Sample
Processing EMP
LA-ICPMS

Mineral ID
Analytical
 ANALYTICAL CHEMISTRY & TESTING SERVICES

Analytical Batch errors

Batch Problems INAA
22

18 Baseline Shifts Instrumental Drift

14

10
Co ppm

Baseline Shifts
2
12701 12759 12812 12869 12925 12980 13038 13095 14906
ANALYTICAL CHEMISTRY & TESTING SERVICES

I want a motorcycle
ANALYTICAL CHEMISTRY & TESTING SERVICES

Quality Control Discussion

Value of Quality
Define Sources of Error
Measurement of Error
Systems to minimize and control error
ANALYTICAL CHEMISTRY & TESTING SERVICES

Measure and Monitor Quality Control

Field duplicates
Two samples in field
Are they useful for indicator mineral
sampling?

Probability of field recovery

5%
Probability of lab recovery
92.99%

Suggest 5%
ANALYTICAL CHEMISTRY & TESTING SERVICES

Measure and Monitor Quality Control

Blanks:

Ceramic grade coarse sand

Detects process sample carry-over
or sample switches
First sample of batch to prevent
carry-over from previous work.
 ANALYTICAL CHEMISTRY & TESTING SERVICES

Measure and Monitor Quality Control

Standards:

Multiple site duplicates, Site

standards
Set of samples taken from a known
valuable field site
Spike samples
Known number of distinct grains
Unique color diamonds
 ANALYTICAL CHEMISTRY & TESTING SERVICES

Measure and Monitor Quality Control

Standards:

Spike samples
Known number of distinct grains
Laser Etching

(photos from Whiteford)

 ANALYTICAL CHEMISTRY & TESTING SERVICES

Quality Control for Grain Analysis

Kalamazoo Ore Indicator
Lac de Gras Cr Diopside Minerals in Till F3 = Fe and Mg
240 F6 = U, Th, Eu
24%

220 3

200
2
19%
180

160 1
Cr-Diopside
140
0
Low Cr-Diopside 12% High Cr-Diopside
120
No of obs

100 -1

80
7% 7% 7% -2
60 6%

40
4%
-3
3%
3%
2%
20
None
None
None
None

1% 1%
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
Propyl
1% 1% 0%
0% 0% 0% 0%

Phyl Int
Phyl Int
Phyl Int
Phyl Int
Phyl Int
0% 0% 0% 0% 0% 0% 0% 0%

Phyl Mid
Phyl Mid
Phyl Mid

Potassic
Potassic
Potassic
Potassic
Potassic
Potassic
Potassic
Potassic
Potassic
0

Phyl Top

Phyl Low
Phyl Low
Phyl Low
0.0 0.4 0.8 1.2 1.6 2.0 2.4 2.8 3.2 3.6 4.0 5.0 6.0 7.0
Cr2O3

Quantitative QC especially in research development

 1-Sep-97
10-Aug-97
1-Aug-97
1-Mar-97
20-Aug-97
10-Aug-97
1-Aug-97
1Jul97
20-Sep-97
15-Sep-97
1-Sep-97
20-Aug-97
10-Aug-97
Comparison of Replicates for Ce

1-Aug-97
EMP vs. Laser Determinations

1-Jul-97
1-Mar-97

0
7000

6000

5000

4000

3000

2000

1000
CE
ANALYTICAL CHEMISTRY & TESTING SERVICES

Standard 3

1-Sep-97
10-Aug-97
1-Aug-97
1-Mar-97
Standard 2
20-Aug-97
10-Aug-97
1-Aug-97
1Jul97
20-Sep-97
15-Sep-97
1-Sep-97
20-Aug-97
10-Aug-97
1-Aug-97

Standard 1
1-Jul-97

Standard
1-Mar-97

EMP
1.2

1.0

0.8

0.6

0.4

0.2

0.0
CE2O3
ANALYTICAL CHEMISTRY & TESTING SERVICES

Precision - Replication of a value with no regard to its

reflection of absolute truth

Accuracy - Comparison of a value to absolute truth.

Precise, Not Precise, Not Precise, Precise,

Not Accurate Accurate Not Accurate Accurate
ANALYTICAL CHEMISTRY & TESTING SERVICES

Measure and Monitor Quality Control

Grain Analysis, EMP and LA-ICPMS

Known grains
Randomize
Duplicate grains
Batch repeats
Duplicate samples to second lab
ANALYTICAL CHEMISTRY & TESTING SERVICES

Quality Control Discussion

Value of Quality
Define Sources of Error
Measurement of Error
Systems to minimize and control error
NI 43-101, ISO 9001, 17025, reporting
requirements
ANALYTICAL CHEMISTRY & TESTING SERVICES

NI 43-101
Canadian regulation governing disclosure of technical
information by exploration/mining companies listed on
stock exchanges
Widely adopted as a general guideline for best practices
by international companies
Delegates responsibility for technical information to a
Qualified Person
Requires regular reporting according to industry-
standard guidelines
A response to the scandal to re-instill confidence in
Canadian traded companies
ANALYTICAL CHEMISTRY & TESTING SERVICES

Implications of NI 43-101

Requires Disclosure of all Relevant Technical Information

Defines the Role of Qualified Person
Requires the Qualified Person to Verify all Technical
Information Reported
Requires the Qualified Person to Set Up and Maintain a
Quality Control Program on Projects
Recommends the Use of Accredited Laboratories and Industry
Standard Practices
 ANALYTICAL CHEMISTRY & TESTING SERVICES

What is ISO 9001:2000?

ISO 9001:2000 is a term for a set of international

quality standards developed by the International
Organization of Standards in Geneva,
Switzerland.
This organization has a membership of standards groups
representing 110 countries. The American National
Standards Institute (ANSI) is the United States
representative.
Over 140 countries recognize the standard.
Over 8,500 companies are certified in the United States
ANALYTICAL CHEMISTRY & TESTING SERVICES

Certification - ISO 9001:2000

Requires evidence of a quality
management system covering all aspects
of an organisation.
Reviews what the organization does to
fulfill:
the customer's quality requirements and
applicable regulatory requirements,
achieve continual improvement of its
performance in pursuit of these objectives.
Registration requires an audit by an
external agency accredited by ISO
Requires annual renewal
ISO 9001:2000 is a model/standard that lists requirements for
a system
ANALYTICALto manage
CHEMISTRY quality
& TESTING assurance; not a strict set of rules
SERVICES

but a series of common sense guidelines

Key: Say what you do; Do

what you say.
A common sense standard.
ANALYTICAL CHEMISTRY & TESTING SERVICES

Initial registration
Annual renewal
ANALYTICAL CHEMISTRY & TESTING SERVICES

Quality Control Recommendations

Visit the lab and review the project.

Define potential sources of error.
Find out what the lab is doing to control quality
ANALYTICAL CHEMISTRY & TESTING SERVICES

Quality Control Recommendations

Insert 10% quality control samples in both

processing and grain analytical batches.
Field Duplicates Site Variability: 1 in 20-30
Blanks carry-over contamination: 1 in 20
Analytical Control Samples Accuracy: 1 in 20
Lab Replicates Precision: 1 in 20
Confirm Data with Follow-up Sampling (5%)
Check with a second lab (10%)
ANALYTICAL CHEMISTRY & TESTING SERVICES

Hit the mark, with a well designed system

which will recognize error, measure the error,
minimize error.
The wealth of your Corporation is dependent upon the
quality of the exploration and reserve data.