NORANDA INC. - FALCONBRIDGE LTD.

DRILL CORE SAMPLING AND ANALYSIS PROTOCOLS

Version 2.0
July, 2003

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Contributors:
Version 1.0
Analytical Solutions Ltd.

Lynda Bloom Analytical Procedures, Quality Control

Noranda Inc. Lionel Martin Six Sigma: Variation Identification and Analysis, Capability
Analysis (removed), Variable Gage R&R (removed)
Robin Adair Drill Core Procedures
Matt Rees Field Procedures
Reviewed by:

Noranda Exploracion Peru Diane Nicolson

Noranda Pacific PTY. Ltd. Craig MacDougall
Simon Tear
Jock Gilfillan
Noranda Inc.

Rory Kempster

Version 2.0
Charles Beaudry : Theory of Sampling and Sources of Error in Assays, Digestion,
Integrated Variance Studies, Assays as a Measurement System, Measure of Variance in
Assays.

Reviewed by:

B. Mercer, L. Vandamme, C. Moore

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TABLE OF CONTENTS
Preface to Version 2.0............................................................................................................................................... 1
Introduction.............................................................................................................................................................. 1
Terms of Reference................................................................................................................................................... 2
1. Theory of Sampling and Sources of Error in Assays ............................................................................................ 5
1.1. Sampling and Assaying as a Process ............................................................................................................ 6
1.2. Accuracy and Bias....................................................................................................................................... 7
1.3. Precision and Variance ................................................................................................................................ 7
1.4. Sample Switching........................................................................................................................................ 9
2. The QAQC Manager..........................................................................................................................................11
3. Specifying Preparation and Analytical Procedures ..............................................................................................13
3.1. Laboratory Selection ..................................................................................................................................13
3.2. Laboratory Communication and Service Contract .......................................................................................13
3.3. Preparation of Pulp Standards and Round Robin Surveys ............................................................................14
3.4. Sample Preparation ....................................................................................................................................14
3.4.1.
Crushing and Splitting ........................................................................................................................14
3.4.2.
Pulverizing .........................................................................................................................................17
3.4.3.
Digestion ............................................................................................................................................17
3.5. Selecting Geochemical Analyses or Assay Determinations..........................................................................18
3.6. Analysis for Deleterious or Secondary "Pay" Elements ...............................................................................19
3.7. Documentation...........................................................................................................................................20
4. Quality Control at the Sampling Stage................................................................................................................21
4.1. Blanks........................................................................................................................................................21
4.1.1.
Preparation of Blanks..........................................................................................................................21
4.1.1.1.
Materials Required ......................................................................................................................22
4.1.1.2.
Procedure....................................................................................................................................22
4.1.2.
Insertion of Blanks..............................................................................................................................22
4.1.2.1.
Materials Required ......................................................................................................................23
4.1.2.2.
Procedure....................................................................................................................................23
4.2. Pulp Standards ...........................................................................................................................................23
4.2.1.
Purchased or Project Pulp Standards....................................................................................................23
4.2.2.
Purchased Control Standards...............................................................................................................24
4.2.3.
The Advantage of Control Standards Prepared from Project Materials .................................................25
4.2.4.
Limitations of Using Control Standards Prepared from Project Materials.............................................26
4.2.5.
Insertion of Pulp Standards .................................................................................................................26
4.2.5.1.
Materials Required ......................................................................................................................26
4.2.5.2.
Procedure....................................................................................................................................26
4.2.6.
Sample Log ........................................................................................................................................27
5. Stage I, II, III Procedures ...................................................................................................................................29
5.1. Stage I - Grassroots Projects .......................................................................................................................29
5.2. Stage II - Discovery Stage Projects .............................................................................................................30
5.3. Stage III - Advanced Exploration and Evaluation ........................................................................................31
6. Procedures at the Drill and Drill Core Sampling .................................................................................................33
6.1. Communication with the Drill Company and Drill Crew .............................................................................33
6.2. Security......................................................................................................................................................33
6.3. Procedures at the Drill................................................................................................................................33
6.4. Transportation ............................................................................................................................................34
6.5. Chain of Custody Management...................................................................................................................34
6.6. Drill Core Duplicates..................................................................................................................................37
7. Submission of Samples to Primary Laboratory ...................................................................................................39
7.1. Submitting Samples to Primary Laboratory.................................................................................................39
7.1.1.
Materials Required..............................................................................................................................39

7.1.2.
Procedure ...........................................................................................................................................39
7.2. Batch Size..................................................................................................................................................40
7.3. Data Entry and Database Management........................................................................................................40
8. Review of Quality Control Data .........................................................................................................................41
8.1. Control Charts............................................................................................................................................41
8.2. Logic Table of Failures...............................................................................................................................42
8.3. Table of failures .........................................................................................................................................44
9. Quality Control Failure: Request for Repeat Analyses ........................................................................................45
10.
Additional Quality Control Procedures ...........................................................................................................47
10.1.
Coarse Crush Particle Size Analysis........................................................................................................47
10.1.1. Sample Selection ................................................................................................................................47
10.2.
Pulp Check Assays .................................................................................................................................47
10.2.1. Submission of Pulp Replicates to the Secondary Laboratory................................................................47
10.2.2. Analytical Methods.............................................................................................................................48
10.2.3. Sample Selection ................................................................................................................................48
10.2.4. Sample Submission.............................................................................................................................48
10.2.5. Comparison of Results for Checks Assays ...........................................................................................49
10.2.5.1. X-Y Plot and Regression .............................................................................................................49
10.2.5.2. Mean vs. the %Difference Plot ....................................................................................................50
10.2.5.3. Paired t-Test................................................................................................................................51
10.2.6. Corrective Action ...............................................................................................................................51
10.3.
Reject Replicates ....................................................................................................................................52
10.3.1. Submission of Reject Replicates for Check Analyses...........................................................................52
10.3.1.1. Sample Selection.........................................................................................................................52
10.3.1.2. Sample Submission .....................................................................................................................52
10.3.1.3. Analysis of Results......................................................................................................................53
10.4.
Integrated Variance Studies ....................................................................................................................53
11.
Measurement System Analysis .......................................................................................................................55
11.1.
Assays as a Measurement System ...........................................................................................................55
List of References and Selected Bibliography ............................................................................................................57
Appendix I Glossary of Terms ..............................................................................................................................59
Appendix II Guidelines for Preparation of Analytical Service Contract ...................................................................63
Appendix III
Detailed Process Maps ....................................................................................................................65
Appendix IV
List of Pulp Standards Prepared by Noranda and Falconbridge.........................................................83
Appendix V Laboratory Audit Guidelines.............................................................................................................111

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List of Figures
Figure 1 : Typical simplified flow chart of sampling and assaying process. ................................................................. 6
Figure 2 : Rhino Jaw crusher with 10mesh sieve attachment.......................................................................................16
Figure 3 : Process map for homogenization of sample in a Jones splitter.....................................................................16
Figure 4 : Methods for preventing and detecting tampering. ......................................................................................35
Figure 5 : Samples should not cross geological boundaries. .......................................................................................36
Figure 6 : Standard Control Chart .............................................................................................................................41
Figure 7 : X-Y plot of Check Assays (Cu2_pct) vs Original Assays (Cu_pct). Blue line is for X=Y (slope of 1). Black
dashed line is actual regression line for the least squares trend between variables. ...............................................50
Figure 8 : Mean (Cu_pct) vs percent Cu difference plot.............................................................................................50
Figure 9 : Absolute difference vs mean concentration plot. Results indicate a distinc grouping of samples with higher
variance, possibly due to erratic or nuggety copper. ......................................................................................53
Figure 10 : Thompson and Howarth Plot...................................................................................................................54

List of Tables
Table 1 : Definition of accuracy and precision............................................................................................................ 5
Table 2 : Selecting an Analytical Method ..................................................................................................................19
Table 3 : Noranda - Falconbridge, recommended rates of insertion of control materials..............................................21
Table 4 : Example of a Sample Log ..........................................................................................................................27
Table 5 : Example of logic table of failures ................................................................................................................43
Table 6 : Example of table of failures to keep track of what controls failed in which batches and what actions were
taken..................................................................................................................................................................44
Table 7 : Regression analysis of check assays against original assays (X Variable 1). The pertinent outputs are the
coefficients for the intercept (X0) and for the X variable (k) (see bottom second column) to be used in the linear
function Check Assay = k(Original Assay) + X0. The P-value for the intercept is >0.05 and is therefore not
significantly different than 0. The P-value for the X variable and the R-square are meaningless in this case
because of the naturally strong relation between the variables. ............................................................................49
Table 8 : Example of output from paired t-Test calculation in Excell. In this case there is bias between the two datasets
because the P-value for the two-tailed test is less than 0.05. The check assays are on average 5.7% higher than the
original assays. ..................................................................................................................................................51

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Preface to Version 2.0

The following document is a revised version of the Drill Core Sampling and Analysis
Protocols v1.0, published in April 2000 by Lionel Martin with contributions from numerous
collaborators. This publication is a result of a second Six Sigma project that focused on
reducing the sources of variance in Noranda and Falconbridge's diamond drill core
assays and used a centralized QAQC database as a source of data to analyze the
performance of assays from different projects. A number of experiments were undertaken
to study the effects of different equipment and procedures on variance and bias of assays.
Where conclusive the results of these experiments have been included as recommended
equipment or operating procedures that are expected to help to reduce the variance and
prevent bias in assaying procedures.
Introduction
This manual describes the Noranda and Falconbridge protocol for the collection,
sampling and analysis of diamond drill core, and the auditing of analytical results. It is the
responsibility of management and the project manager/geologist to ensure this protocol is
diligently applied to exploration, evaluation and feasibility stage projects.
Diamond drill core sampling is mandated as the sampling method for a mineral body of
potential economic significance where ground quality permits acceptable recoveries.
The project manager is responsible for the quality assurance (QA) of the sampling
procedure, shipping of samples, chemical analyses (including selection of appropriate
analytical method) as well as the quality control (QC) and security of both the core and
analytical samples. Project managers must ensure there is complete documentation (both
hard copy and digital) of all procedures and results at all stages of the project to provide a
clear audit trail for subsequent (and possibly external) reviews.
Implementation of standardized quality control procedures for all of Noranda and
Falconbridge's exploration and development offices is a key objective. Although the
approach to quality control described in this document can be applied to rock samples,
core, RC samples, soil/silt samples and lithogeochemical samples this document pertains
only to drill core and the quality control program consists of:
The submission of blanks to monitor contamination and data accuracy.
The submission of control samples (i.e. pulp standards), of known metal
concentration, to monitor data accuracy.
Acquisition of data for laboratory internal pulp replicates to monitor analytical
precision.
Collection and review of all internal laboratory data for blanks and in-house
control standards to monitor accuracy.
The submission of reject replicates to monitor sample homogeneity and
preparation procedures.

 The submission of pulps to a secondary laboratory (also referred to as

cross-checks) to verify analytical methodology, laboratory bias and data
accuracy.
Submission of coarse crush rejects to a secondary laboratory for coarse
crush particle size analysis to monitor preparation procedures.
Submission of core duplicates to monitor total sampling and analysis
variation.
Management and review of all quality control data.
The purpose of documenting the procedures, and any revisions, is to ensure consistency.
Written protocols ensure that all project employees can reference the protocols if they are
not clearly explained or if forgotten. Jobs are clearly defined and procedures are
consistently applied. The project manager assigns responsibility for different procedures
to specific individuals so that there is accountability for each aspect of the quality control
program. Any changes to the procedures and the date of the change must be recorded.
Protocols exist for all stages of exploration, and are particularly important for projects
where pre-feasibility or feasibility studies are planned. Third party engineering firms,
investment bankers and other individuals from outside the company may request
documentation of the sampling, sample preparation and quality control procedures.
Compliance with these protocols will be monitored and reported to senior management, or
in the case of feasibility studies, third parties. Inclusion of quality control samples such as
blanks, control standards and replicates will allow laboratory errors to be readily identified
and corrected.
This approach provides a high quality database that will improve
confidence in the decisions based on these data.
The procedures documented in this manual are general guidelines. It is envisioned that
the procedures may be modified with experience and new technological developments,
however documentation of all changes is necessary.

Terms of Reference
In response to the Best Practices Guidelines proposed by the Toronto Stock Exchange
and Ontario Securities Commission (TSE/OSC) Mining Standards Task Force, Noranda
and Falconbridge implemented a review of the company's quality control practices with
respect to the submission of samples for analysis.
A series of documents were distributed internally for discussion including notes from a
1998 PDAC short course, "Practical Application of Exploration Geochemistry", written by
Lynda Bloom, Stephen Amor and Peter Ward as well as a paper titled "The Role of
Economic Geologists in Evaluating Data Quality" by L. Bloom (1998). This document
applies to drill core only, however protocols for rock sampling (grab, outcrop, channel,
etc.), lithogeochemistry (whole rock) and sediment sampling (soils, silts, HMC's) can be
adapted from this protocol as many of the procedures will be similar.

The quality control guidelines described in this document are designed to maintain a high
level of confidence in analytical results for Noranda and Falconbridge management and
geologists, joint venture partners, regulatory authorities and the public domain.
Adequate mineralogical and metallurgical testing and geotechnical measurements also
need to be introduced at specific stages to identify negative economic consequences
early in the exploration process. The additional objective of this protocol is to characterize
potential ores early in the process and, where appropriate, testing can be used to
compliment preliminary predictive metallurgy reviews. The results are to be carried to the
advanced metallurgical testing stage with the clear identification of potential negative
impacts of deleterious elements and complex mineralogy early in the process.
The components of a quality control program will vary according to commodities, deposit
type and location. The number of quality control checks will increase as a project
advances and the financial exposure to the risk associated with the project also increases.
This protocol envisions that the exploration process is governed by three principle stages
that reflect increasing success from grassroots through to feasibility. Each stage
represents the progressive addition of quality controls with increased success as well as
the concomitant implementation of metallurgical, mineralogical, and rock physical property
measurements (e.g. RQD).

Stage I, Stage II or Stage III are briefly described as follows:

Stage I - Grassroots Exploration: Stage I projects primarily involve drill testing
geophysical, geological and/or surface geochemical targets. These projects may not
encounter mineralized zones and, in the absence of significant mineralization, the focus is
identification of anomalous metal values and alteration patterns. Geochemical multielement ICP analysis may be used to estimate the metal content of drill core as a less
expensive alternative to assaying. Significant mineralization will automatically be assayed
as described for Stage II and III projects, as will any indication of gold, silver or
platinum/palladium.
QC procedures are applied to develop a reasonable baseline confidence level with
respect to chemical analyses. Control standards, blanks and replicates are submitted and
monitored. QC data are verified as each set of analyses is received. With increased
success, Stage I projects evolve into Stages II and III with the addition of further QC
checks as well as the initiation of metallurgical and geotechnical data collection.
Stage II - Discovery-Stage Projects: Stage II projects essentially represents a
transitional stage that is initiated upon first discovery of potentially economic
mineralization. It is directed towards additional QC checks, as well as the beginning of the
characterization of a potential ore body. It is acknowledged there will be initially limited
sample availability.
The discovery of potential economic mineralization automatically implies that assay
methods are to be used for all samples within a mineralized interval in place of
3

geochemical analyses more typically used in Stage I. Geochemical multi-element

analysis can be used to "characterize" mineralization for elements other than base and
precious metals with the objective of identifying deleterious components. Geochemical
and assay analyses are not, however, to be mixed in calculating the composite grade.
QC procedures involve the submission of control standards and blanks on a more
frequent basis than Stage I. Replicate samples (pulp and coarse crush) are incorporated
in the QC procedure. Drill core duplicates are optional. QC data are verified upon return
of each sample batch and monitored in a centralized database.
Characterization studies for deleterious elements, optical predictive metallurgical
characterization studies, and geotechnical data collection are initiated. Microprobe work
can compliment this type of study to locate host minerals of deleterious elements.
Stage III - Advanced Exploration and Evaluation: This stage applies to projects that
have advanced to resource delineation and definition. Thorough QAQC procedures are
designed and implemented for the specific project. Control standards (multiple control
samples specific to the style, type and grade of mineralization) and blanks are submitted
with each sample batch. QC data are verified upon receipt. Pulp cross-checks and
coarse crush replicates are submitted, and drill core duplicates remain optional. Coarse
crush particle size analysis are initiated. Crush and pulverization sizes are optimized.
Chemical analysis must be compared with metallurgical evaluations that may be run on
individual holes, bulk samples composed of combined holes and/or large scale bulk
samples. Analysis of deleterious elements is systematic so results can be incorporated in
bulk composites.
At this stage the objective is to characterize the deposit on the basis of geology
(geometry, host rock composition, etc.), chemistry (distribution of grade and deleterious
elements) and metallurgy (variations in grain size, anticipated recovery and therefore NSR
variation). This leads to a high confidence, comprehensive understanding of the deposit
prior to large capital expenditures. The approach needs to reflect the fact that mineral
deposits are not generally homogeneous.
This manual is primarily designed to define a rigorous program of QAQC procedures for
all exploration and development projects. Exceptions to the procedures recommended
in the manual may apply to specific projects. Changes to the recommended
procedures must be documented and reasons provided for these deviations.
Management approval is required.
In addition, the adaptation of this protocol will provide the basis on which opinions are
developed during the evaluation of projects being reviewed by Noranda and
Falconbridge for potential option or acquisition. This will allow for a quantitative
assessment of data quality needed to determine the relative risk related to the quality of
the data provided in such cases.

1. Theory of Sampling and Sources of Error in Assays

Fundamentally there are two different types of errors in assays, bias related to accuracy
and variance related to precision as shown in table 1.
Table 1 : Definition of accuracy and precision.

Accuracy

The average difference between the

value of an analysis and its true value.
The measure of accuracy is bias and is
usually reported in percent of the true
value. Bias is additive and substractive in
the sampling and assaying process.

Precision

Amount of dispersion of repeated

analyses of a sample. Measure of
precision is standard deviation / mean x
100. Variance is the square of the
standard deviation and is additive at each
step in the sampling and assaying
process.

Assays represent a measurement system. In other words we use assays as a means to

measure something else, usually the grade distribution in a mineral deposit for which we
wish to make a risk-based investment decision. These two issues (i.e. accuracy and
precision) are two of the five criteria for assessing the quality of a measurement system,
the others being resolution, linearity, and stability.
Much has been written about sampling and analysis and the sources of error in the
process. The reader is referred to Riddle (1993) and Merks (1985) along with CIM
Special Volume 7, Numbers 1 and 2 (1998) for excellent treatment of the subject and
voluminous bibliography. The following summary will focus on the issues of pertinence to
the explorationist keeping in mind that drill core assays are inherently imprecise and that,
barring mining the ore itself, we cannot spend a lot of money to make them more precise.
It is the nature of sampling and the fact of assaying variable material that causes this and
that we must, in the final resort, accept relatively low precision in assays. By increasing
the number of assays through additional drilling we gradually reduce the error associated
with the estimation of a resource. However it is inherent that each assay will only
imperfectly reflect the grade and tonnage of the material from which it came from. The
question ultimately becomes: how precise are assays and can we improve the precision at
little or not cost? A related question is whether our assaying process is operating at
entitlement and if not, can it? Fortunately, the answer is that we generally do not attain
entitlement and that we can improve our performance with simple measures that do not
add much cost to our assays. Through an understanding of the sources of error in
sampling and assaying, including appropriate control materials with the sample batches,

and the selection of proper sample preparation equipment it has been shown that
performance can be improved significantly.

1.1.

Sampling and Assaying as a Process

The act of sampling core, preparing the sample, and analysing the resulting material can
be modelled as a series of sequential steps in a process that starts with the core that is
delivered from the drill and ends with the assay result. The process is modelled as a
series of flow charts in appendix III and simplified in figure 1. The sequential nature of the
steps involved in getting to the assay result has important consequences for the
development and propagation of errors in the process. An accuracy error or bias may
occur at each step of the process and is usually caused by contamination in sample
preparation, poor calibration of the analytical instrument, and occasionally from poor
design or improper operation of sample preparation equipment. Bias will be additive and
can be positive of negative in value. The principal focus of QAQC procedures is to detect
and prevent bias even at low levels.

Split Core

Crush

Split &
sub-sample

Pulverize

Sub-sample

Digest

Analyze

Figure 1 : Typical simplified flow chart of sampling and assaying process.

Precision error, called variance, occurs during sampling and sample preparation. It is
caused by sub-sampling of material that is not homogeneous so that the sub-sample is
not perfectly representative of the mass from which the sub-sample was taken. It is the
act of sub-sampling itself that introduces most of the variance and this is an inevitable
consequence of trying to estimate the grade of a volume of rock from sampling and
analysing drill core. For economic reasons we accept that the assay will not be perfectly
representative of the volume of rock it is taken from. Nonetheless, we wish to limit and
control the amount of variance introduced by subsampling. A secondary source of
variance is caused by the measurement errors arising from the weighing of samples, the
measurement of volumes and the error of the instrument. These however are generally
much smaller than the errors introduced by splitting and sampling the core, and subsampling during the preparation phase.
Mathematically, precision is defined as the square root of variance and is stated in the
same units as the measurement (i.e %Cu or gpt Au) and used mainly in descriptive
statistics. Variance is always positive and is additive in a sequential process if each step
is independent. For example, the variance of 2 drill core halves is the sum of all the
sources of variance of sample preparation and analysis. Variance therefore increases
from the instrument, backward through the pulp digestion, the pulverizer, the crusher and
the sampling itself.

1.2.

Accuracy and Bias

Since accuracy is a measure of how close an assay is to its true value we need some
definition of the truth to base our estimate. Although we cannot know the "true" value of
an assay, we can include with the assay a sample for which we know the value. This is
generally a pulp standard and the subject of a detailed treatment in section 3.3. Knowing
the value of a pulp standard with a certain level of precision, it is possible to apply
standard hypothesis testing to the assay results of the same standard inserted in batches
and judge whether results are biased. Moreover it is possible to monitor, from batch to
batch the "randomness" of the error, in other words, that part of the error which is
systematic (true bias) from the part which is random (variance).
An additional method of measuring bias is to submit a second cut of the pulps to the
secondary lab for analysis. A systematic bias between laboratories can be measured
from the slope and intercept of the equation linking the assays from the two labs. A
second approach is to undertake a paired t-test of the duplicate results to test the
hypothesis that the average difference between the assays is different than zero (null
hypothesis).
Contamination in sample preparation (i.e. crushing, splitting and pulverizing) is a common
source of bias and is monitored using blank samples. They will typically have an
elemental concentration that is near the detection limit for the analytical method. Blanks
are submitted with each batch and go through the same processing steps as the normal
samples and therefore can monitor contamination at any step in the sample preparation
process.
Finally, analyzing the second half of the core can provide evidence of "over sampling",
that is, the biased sampling of the core, a common problem with visible mineralization
where the sampler tends to either oversample for mineralization or, conversely,
oversample for waste. Here also, the bias can be measured by the slope and intercept of
the equation linking the assays of the two halves of the core or by a paired t-test.

1.3.

Precision and Variance

As mentioned above, variance is a consequence of sub-sampling and it is additive

through the sampling and assaying process. Information on variance is contained in the
duplicate analyses of core, coarse crush and pulps material and is directly obtainable from
the distribution of assay results of pulp standards.
Under conditions of grade constant variance (only true for narrow grade ranges), the
variance is calculated as followed:

= S (2nd assay - 1st assay)2 / 2N

(1)

Unfortunately variance is also a function of grade and is a second-order polynomial of the

form of equation 2 (Franois-Bongaron, 1998b):
s 2 = (s 2(0) + Beta Grade2) + s 2(s) Grade ,

(2)

where,
s 2 (0) = The variance at a grade of zero or constant analytical variance
s 2 (s) = The sampling variance independent of grade as in 1 above
Beta = The coefficient of proportionality of analytical variance.
The square root of equation 2 becomes:
s (c) = s (0) + k Grade

(3)

This equation is equivalent to equation 1 of Thompson and Howarth (1978) and is used to
estimate parameters Std(0) and k in their equation 2 which translates as follows:
Pc = 2 s (0) / Grade + 2 k

(4)

From this equation we can calculate the precision (Pc) or relative standard deviation
(RSD%) (the two are equivalent) for any grade.
The variance arising specifically from the act of sub-sampling has been analyzed in detail
by Gy (1982) and is summarized by Franois-Bongaron (1998b). In his simplified
equation Gy expresses the variance of sampling error as a function of particle size (dN)
and masses of the sample (Ms) and the lot (Ml) as follows:
s (FSE) 2 = (c l) (f g dN3) * (1/Ms - 1/Ml),

(5)

where,
c = mineralogical factor related to grade of the lot and densities of the mineral of interest
and the rest of the rock,
l = liberation factor related to size distribution and arrangement of mineral grains within
rock fragments,
f = shape factor, g = granulometric factor, and dN = nominal size.
The importance of this equation comes from the fact that certain conditions are required
for it to be applicable. The most important is factor "g" that requires that the PSA be 95%
for it to be constant (Franois-Bongaron, 1998b). For this reason it is essential that PSA
specifications always be defined in terms of the sieve size for which 95% of the material
passes through.

1.4.

Sample Switching

Another possible source of error in assays is sample switching. A study done by C.

Beaudry in 2001 using Noranda's QAQC database concluded that sample switching
occurs in about 5% of all batches (1 in 20). However it was also observed that switching
was more frequent on an advanced project where throughput was much higher and time
schedules much tighter. An FMEA indicates there are at least 20 different failure modes
related to sample switching. It is apparent that switching is more common in the digestion
and analysis steps but also easily detected and corrected, whereas switching is rarer but
more difficult to detect in the pulverizer and crusher and, the latter case impossible to
correct short of analyzing the second half of the core. Finally core sampling is probably a
source of switching but this is almost impossible to detect unless the switched samples
have visibly different metal concentrations.
Fortunately sample switching does not appear to have a large impact on the error of
resource estimation. Permutating two samples within a whole sequence of economic
grade analyses will not change the average grade of the mineralized interval. On the
other hand sample switching can have a profound impact on regional geochemical
surveys where an error in the location of an anomaly can lead to follow-up work in the
wrong location. Fortunately, the probability of switching an anomalous sample in a typical
survey is much less than switching any random sample in a batch.
The risk of sample switching can be reduced by using optical bar code readers as this
eliminates multiple entry of sample numbers. When combined with LIMS-integrated
weighing scale, optical bar codes can eliminate many of the failure modes that lead to
switched samples.

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2. The QAQC Manager

Each drilling project shall have a QAQC manager. In early stage projects this role will
typically be cumulated by the project geologist. On advanced projects and depending on
the situation, a person may be assigned the task and responsibilities of ensuring all quality
procedures are followed. The QAQC Manager must be a "Qualified Person" as per the
definition in NI 43-101.
The QAQC manager is responsible for the following aspects of the drilling program:
Identify adequate pulp standards or, if required, the collection of project
materials to be used to prepare standards, the supervision of the round robin
validation of the standards, and the calculation of the accepted values for
the standards.
The collection and validation of blank material.
The identification and validation of the primary and secondary laboratories.
The planning of the sampling program including the schedule of control
insertion and collection of duplicate samples.
The validation of batches for accuracy using standards and blanks.
The additional validation of the primary lab using check pulp assays at the
secondary lab.
The estimation, as required, of precision of crushing and core sampling from
duplicate samples.
The supervision of the storage of core boxes and pulp and reject materials.
The preparation of the QAQC report to be included in the project drilling
report.
Refer to Appendix III for detailed process maps of the activities necessary to ensure
compliance with the protocol.

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3. Specifying Preparation and Analytical Procedures

Commercial laboratories offer a wide range of preparation and analytical methods. Cost
and availability of services and characteristics of the sample will determine the optimum
methods for a project. Each sample submission must be accompanied by a request
for analysis that indicates the specific analytical procedures, preparation, handling
of pulp and crush rejects and a request for all lab control standards and replicates
associated with the sample batch.
3.1.

Laboratory Selection

A laboratory is selected on the basis of logistics, price, quality, and availability of services.
A laboratory visit is highly recommended, unless impossible, to assess the laboratory's
production and analytical facilities. Refer to Appendix V for a list of details to record
during a laboratory visit. A laboratory visit may also include submission of a series of
control standards to test the laboratory's performance.
Noranda and Falconbridge are required to follow NI-43-101 published by the Canadian
Securities Administrators and adopted by most if not all Canadian provincial securities
commissions. It has been recommended (but not required) that accredited laboratories
are used but the type of accreditation has not been specified. Joint venture partners and
certain regulators may also have specific requirements.
3.2.

Laboratory Communication and Service Contract

It is preferable to negotiate a contract with a commercial laboratory that clearly defines the
services required, reporting formats, quality control parameters, pricing, turnaround time
and penalties in the case turnaround times are not respected.
Laboratories should be asked to report on the following:
Analyses of the second quartz chip sample (i.e. cleaner) to be passed
through the pulverizer equipment prior to each batch of samples being
prepared. Some labs do not routinely analyze the pulverizer blanks.
Laboratory pulp replicate results.
Blank and control standard results. Lab blanks are often solution blanks.
Results of coarse crush particle size analysis performed by the laboratory to
monitor sample preparation quality.
Results of participation in round robins.
The contract should also specify the number of significant digits to be reported. The rule
is that one additional digit should be reported. For example, if results are significant to
two decimal places, three digits should be reported to the right of the decimal place.

13

Although this last digit is not significant, its presence will prevent rounding at the next
higher digit. This will avoid rounding errors and reduce a certain type of defect in the
QAQC database and will contribute to lower overall variance. Refer to Appendix II for a
summary of recommended guidelines for preparing analytical contracts.
3.3.

Preparation of Pulp Standards and Round Robin Surveys

Preparation of pulp standards from project materials is a common and very crucial step in
QAQC management. It involves the selection of sample material, usually from core, and
is meant to provide the project with standards to constrain the accuracy of high grade,
average grade and cut-off grade assays. The description of sampling and sample
preparation procedures is beyond the scope of this document. Suffice to say that the
preparation of standards should not be attempted without the supervision of either the
Manager of Geochemistry or an experienced professional and that the laboratory selected
to do the sample preparation must be highly reputable and have the proper equipment.
Once the pulp standards are prepared they are submitted to at least 6 (more if possible)
different laboratories in batches of 8 to 10 samples of each standard and results are
compiled to determine mean values (accepted values). Numerous methods have been
proposed, some of which are summarized in Riddle (1993). The method used by Barry
Smee calculates the accepted value by iteration through the elimination of outliers that are
more than +/-2 standard deviations from the grouped average. If in doubt the project
manager is advised to consult either with the Manager of Geochemistry or an experienced
professional in order to determine accepted values from round robin results.
The round robin survey is also an excellent method to determine the fitness of the
analyses as a measurement system for evaluating mineral deposits. Refer to chapter 11
for a description of the procedure that involves the Gage R&R method of analysis.
The guidelines for sample preparation presented below should be adequate for most
applications but in some instances a custom designed sample preparation flow sheet may
be required. This is commonly the case if coarse particulate gold or other high value
substance is present in the core or if samples need to go through partial size reduction
and sub-sampling in the field prior to transport. In these cases an experienced
professional should be consulted.
3.4.

Sample Preparation

3.4.1. Crushing and Splitting

Samples should be crushed to achieve a minimum of 95% passing a 10 mesh screen
(less than 2 mm). A riffle splitter or, more rarely, a rotary splitter is used to select a sub-

14

sample for pulverising. The amount of sample to be pulverised must be specified to the
laboratory. Variations of crush size may be required on a project basis.
The most important factor for controlling variance in coarse crush sub-sampling is particle
size distribution. The protocol requires that at the start of a project 5% of coarse crush
reject samples be submitted for particle size analysis (PSA) until about 30 samples are
tested and thereafter about 1% of samples.
A variety of crushing equipment is available commercially. The most commonly used is
the Rhino jaw crusher and the roller crusher. The latter has been recommended because
it produces a more reliable PSA measurements. However one of the experiments
performed by C. Beaudry (2001) showed the PSA results to be apparent only and that the
roller crusher tends to produce caking of the samples unless disaggregated with a mortar
and pistle, a procedure that is not done systematically on all samples. Moreover, the
inherent occupational health and safety issues related to the roller crusher argue against
its use for routine assays.
The Rhino crusher, which provides excellent productivity and minimal contamination, has
historically been plagued by poor PSA performance, especially on the first pass where
samples typically achieve about 75% -10mesh. An innovative apparatus being used at
ALS-Bondar in Chile and elsewhere provides a solution to this problem (figure 2). By
welding a 10mesh screen directly to the jaw it is possible to quickly sieve the sample after
crushing and to re-crush the oversize material to any degree of PSA performance.
Typically a second or third pass of the oversized material is required to attain 95% 10mesh. A six sigma experiment has shown that re-homogenizing the samples
afterwards by splitting and recombining three or four times in the Jones riffle splitter using
the flow chart below (figure 3) is sufficient to compensate for the heterogeneity created by
sieving the sample.

15

Figure 2 : Rhino Jaw crusher with 10mesh sieve attachment.

Crushed
Sample

Splitter
50%

75%

50%

25%

62.5%

37.5%

Sample

100%

Figure 3 : Process map for homogenization of sample in a Jones splitter.

16

Some commercial laboratories may be equipped with other types of crushers; however, it
is up to the QAQC manager to ensure that the equipment that is to be used is both
unbiased and introduces acceptable variance. If in doubt consult with the Manager
Geochemistry or an experienced professional.
3.4.2. Pulverizing
Crushed material should be pulverized to achieve a minimum of 95% passing a 150 mesh
screen (106 microns). Optimal particle size, for a particular style of mineralization, is
determined by conducting studies of multiple splits of the coarse crush reject. Both the
size of the sub-sample and the grinding time can be varied. The sample size and grind
characteristics impact on equipment selection. In the event of excess variation these
parameters must be changed.
The laboratory's procedures to clean pulverizer bowls between samples must be
investigated. The use of silica sand cleaners before each sample is recommended to be
specified in cases where samples are high in sulphides or clay content, to avoid sample
cross-contamination.
Commercial laboratories typically use vibratory ring pulverizers. Experiments on the LM1
and LM2 pulverizers used at ALS-Bondar in Chile (see Beaudry QAQC project 2002) have
shown that there is significantly less variance with the small pulverizer (LM1: 250g) than
with the larger one (LM2: 1Kg) in the case of gold analyses but not for copper analyses.
On the other hand gold assays, which use large alliquots of 30 to 50 g, require a larger
split to accommodate possible re-assaying and eventual check assaying and therefore
the LM2 is recommended in spite of its high variance. For base metals both the LM1 and
LM2 can be used according to the requirements of the project.
3.4.3. Digestion

Once a sample has been pulverized to a stated size specification (>95% -150mesh) it is
ready for digestion. Usually about 0.25 to 1.0 g of pulp material is weighed out to three
decimal places and submitted to a digestion prior to analysis by atomic absorption (AA) or
ICP-ES instruments. An experiment showed that there is no improvement in precision
from the use of larger sample weights for digestion. In most cases a pulp weight of
around 0.5 g is sufficient but sometimes as little as 0.1g may be used if the average
grades are very high such as with VMS mineralization but a weight should not exceed 1.0
g except for fire assaying or bulk leaching of samples. Larger weights are generally not
recommended as this increases digestion time and may increase matrix effects leading to
bias.
These recommendations are for the analysis of major components such as bases
metals and do not extend to gold or other "trace" elements. In the case of gold,

17

silver and PGE's a much larger sample is required, typically up to 50g in order to
minimize variance and ensure a statistically representative number of metal-bearing
grains are present in the charge.
Numerous methods have been developed to dissolve constituents of a rock prior to
instrumental analysis and a good summary is presented in Val Loon and Barefoot (1989).
The most common method however is by acid attack, especially for rock samples. In
Canada and other temperate climates hot aqua regia, a combination of heated nitric acid
and hydrochloric acid provides acceptable assay results, particularly when economic
elements form sulfide or carbonate mineral species. In warmer climates such as Australia
and South America and elsewhere it is generally reported that aqua regia digestion under
reports the amount of metal in samples (negative bias). In these tropical environments a
mixture of hot hydrofluoric acid with one or more of nitric, perchloric or hydrochloric acids
are used. In this case glass equipment cannot be used and are usually replaced by
special test tubes made of teflon as it may be heated up to 240C. Such multi-acid
procedures are more expensive however and require special ventilation huts to prevent
the accumulation of explosive gases and precipitates. In addition certain elements such
as As, Sb, and Ge are known to form volatile fluoride complexes which can lead to
negative bias for these elements.
Typical digestion times range from 1 to 3 hours depending on the type of material, the
acid mix, and the size of the sample. The digest is usually heated to dryness or near
dryness in a hot water bath (aqua regia) or directly over a hot plate (multi-acid) before
being re-dissolved to constant volume in beakers (for geochemical analysis) or volumetric
flasks (for assays).
Depending on elements being analysed the digestion parameters can be modified. Lab
personnel should be consulted and possibly some testing carried out before committing to
a particular procedure. Whatever method that is finally selected should be rationalised
and properly documented in the QAQC section of the project report.
3.5.

Selecting Geochemical Analyses or Assay Determinations

The request for analysis should include the method code or quotation number that will
identify a specific analytical procedure.
Analytical methods are selected to achieve
acceptable precision for the anticipated grade range. Cost savings may be achieved by
using multi-element techniques, however detection limits need to be carefully selected in
order not to miss trace concentrations that may be key to further targeting of the
exploration process.
In general, assay determinations for commodity elements provide more precise data than
geochemical determinations for sub-economic or economic ore grades. There is a
continuum of procedures available that may not be clearly identified as being specifically
assay or geochemical determinations.

18

It is recommended that laboratories be asked to specify potentially interfering elements,

elements that are volatilized (i.e. lost) during digestion or fusion, and minerals that might
not be dissolved by the procedure.
Specialised procedures may be required to characterise the ore, such as "acid soluble"
techniques that preferentially dissolve copper present as oxides. The precision of these
techniques is not typically at the same level as "total metal" assays but is used to assess
the metallurgical performance of particular ore types in a deposit.
Some of the technical issues to consider when selecting an analytical method are
summarised in table 2.
Table 2 : Selecting an Analytical Method

Analytical Procedure
Sample Weight
Sample Dissolution
Elements

Dilutions
Upper Limit of Detection
Lower Detection Limit
Instrumentation
Specialized Methods

3.6.

Geochemical Analysis
0.2 0.5 g
Selective extractions
Aqua regia digestion
Compromises used to achieve
maximum no. of reported
elements
Usually
imprecise
and
performed in test tubes
Precision is poor at upper
limits of detection
Generally less than 1 ppm or
0.0001% for major elements
A.A.S. , I.C.P.-O.E.S., I.C.P.M.S., neutron activation
Includes analysis of water,
biogeochemical
samples,
gases, MMI, Enzyme Leach,
etc.

Assay
0.25 1.0 g
HCl+ HNO3+ HClO4 HF
Alkaline fusion
Optimized for single elements

Precise and performed in

volumetric flasks
No upper limit of detection
Usually 0.01% for base metals
A.A.S., I.C.P.-O.E.S., XRF,
fire assay
Colorimetry and gravimetric
techniques may be used for
high grade samples or
concentrates

Analysis for Deleterious or Secondary "Pay" Elements

Minor or trace elements present within a mineral deposit may have positive or negative
impact on the economics of the mining project. They may concentrate with the economic
minerals in the concentrator and lead to either unsellable concentrate or the imposition of
penalties by the smelter or can represent a potential environmental, safety, or health
(ESH) issue during mining, processing, or tailings and waste disposal. Alternatively,
secondary elements may be present in sufficient minor quantities to positively impact the
NSR under favourable metallurgical conditions (secondary pay elements). In any case,

19

the presence of these elements may have a profound positive or negative effect on the
economics of a deposit and must therefore be thoroughly researched early in the project.
In some cases these elements can be present in the bulk rock sample in very low
concentration, perhaps even below the detection limits of many analytical techniques.
However, under certain processing conditions they may be concentrated by a factor of ten
or more in the final concentrate. For example, if selenium was solely present in the
mineral sphalerite and its bulk concentration in the core sample was 0.02%, it could be
concentrated a minimum of six times in the sphalerite concentrate where its concentration
would be 0.12%. This would represent significant increased costs through recovery
problems and treatment charges.
The elements and their threshold concentrations that may impact on the economics of a
mining project vary according to the minerals that contain the elements, the type of
concentrate produced and to which smelter the concentrate is destined. The upper
threshold limits for key elements are usually determined on a project basis by undertaking
preliminary metallurgical tests. Once the elements are identified, a program is formalised
to determine if those elements will be present in concentrates at levels that cause
difficulty. The final assessment of a potential problem must be made through discussions
with a metallurgist or a mineral processor with experience in the specific deposit type.
There is a wide variation of possibilities for the occurrence of deleterious or potential
secondary pay elements in the minerals being concentrated for refining. These elements
may in fact be present only in waste minerals and would therefore report to the tails. As
such the presence of a deleterious element in the bulk chemical analyses may have no
effect on the recovery of a desired element. It is however important to know what is
reporting to the tails for treatment and environmental reasons. Optical mineralogical and
microprobe analyses will determine in which minerals potentially deleterious or secondary
pay elements occur.
3.7.

Documentation

A brief description of the methods is included in a project report and detailed methods
included in appendices. Where possible methods should be specified using the method
codes. Most laboratories will supply detailed method descriptions if requested or they may
be available from some laboratories' web sites. Documentation will be specific to each
project.
It may be necessary to change procedures during the course of a drilling program. The
reasons for these changes and which samples are affected must be documented in detail.

20

4. Quality Control at the Sampling Stage

Quality control starts at the planning stages of a drill program. The project geologist must
acquire suitable materials to be used as blanks and control standards prior to the
commencement of drilling. A procedure must be in place for the submission of these
materials with samples to the laboratory.
The following 2 sections describe the use of blanks and control standards. Additional
quality control procedures including crosscheck analyses on pulps, analysis of coarse
crush replicates, and coarse crush particle size analysis are described in sections 10.1 to
10.3. The recommended rate of insertion of control materials depends on the stage of the
project with more advanced projects requiring more frequent controls (table 3).
Table 3 : Noranda - Falconbridge, recommended rates of insertion of control materials.

Noranda/Falconbridge Protocol
Standards
Blanks

>= 1%
>= 1%

Stage I

Pulp Check Assays

>= 5%

Stage II
>=2%
>=2%
>= 5% of mineralized
samples

Coarse Crush Replicates

Optional

>= 5%

>= 5% initially until 55 samples

collected, afterwards 1%

Core Duplicates

Optional

Optional

>= 5% initially until 55 samples

collected, afterwards 1%

>= 5%

>= 5% initially until about 30

samples show PSA is
aceptable, afterwards 1%

Reject PSA

4.1.

Optional

Stage III
1 per batch or 1:40
1 per batch or 1:40
>= 5% of mineralized samples

Blanks

4.1.1. Preparation of Blanks

"Blank" material is submitted with samples to the laboratory to monitor contamination
caused when crushing or pulverizing equipment is not cleaned properly after mineralized
samples are processed, or due to dust.
Suitable material consists of an unmineralized rock type (barren drill core) where the
metal content does not exceed 100 ppm. The rock type is preferably relatively hard so
that the preparation equipment is thoroughly scoured.
Laboratories are also expected to analyze barren quartz chips or silica sand that is used
to clean sample preparation equipment. Laboratories will routinely include analytical
21

blanks in sample batches. The "blanks" described in this section are submitted without
the knowledge of the laboratory and are designed to monitor contamination throughout
both sample preparation and analysis.
4.1.1.1.

Materials Required

Unmineralized quartzite or sandstone (for example)

20-litre pails
4.1.1.2.

Procedure

A geologist locates a source of suitable material (typically from a quarry or unmineralized

drill core).
Determine how much material to collect by (a) dividing the total of number of samples by
the frequency of blank insertion to determine the total number of blanks for the program
and (b) multiplying by 2 kg (the approximate weight of material submitted).
Store the blank material in pails so that it is ready for routine core sampling.
Record a description of the material and its origin.
Submit five 200-500 gm sub-samples of the "blank" material to the primary laboratory to
confirm low metal values.
Blank material is not processed in advance of its insertion into sample batches. Individual
pieces of rock should be no larger than 5 inches by 5 inches so that they are small
enough to pass the hopper of the crusher.
It is up to the QAQC manager in discussion with the project manager to determine the
defect threshold concentrations for the blanks. This may vary according to project,
mineralization type, and the average grades encountered but should always be less than
1/20th of the anticipated cut-off grade.
4.1.2. Insertion of Blanks
A blank sample is inserted routinely into sample batches. When the sample is analyzed,
the reported analytical values should be near the detection limit of the method. If the
reported values are higher than expected, contamination of the samples during crushing,
pulverizing or analysis may be indicated.
Sample preparation procedures would be reviewed to isolate the cause of contamination
and corrective action taken.

22

4.1.2.1.

Materials Required

Sample bags
Sample tags
"Blank" material

4.1.2.2.

Procedure

Two sample tags in each group of 100 tags are reserved for blanks.
Reserved numbers usually end in "-10" and "-60" or, better still, two numbers
chosen at random from each series of 100 sample numbers. The insertion
of blanks randomly is a more robust test of the laboratory but requires
careful training and record keeping.
Prior to moving samples to a sample preparation facility, coarse blank
samples are added as follows:
a) label a plastic sample bag with the sample tag ending in the number "10" or "-60" or the pre-selected random number.
b) insert the sample tag in the sample bag.
c) add an amount of "coarse blank" material to the bag that is similar to
that submitted for samples.
Sort all samples into consecutive numerical order. Submit the "blank"
sample to the sample preparation facility with the samples.
Note: Plastic bags can be filled with blank material in advance, then labeled and the
sample tag added when preparing samples for shipment. Where possible, barren drill core
is submitted so that the laboratory cannot recognize the "blank" material.

4.2.

Pulp Standards

4.2.1. Purchased or Project Pulp Standards

In different circumstances it may be appropriate to purchase control standards or prepare
control standards from materials on the property.

23

4.2.2. Purchased Control Standards

Purchased control standards fall into two main categories: certified reference materials
("CRM") and control samples. Certified reference materials are available for a wide range
of elements and different matrices. The "1994 Compilation of Working Values and
Sample Descriptions for 383 Geostandards" (Geostandards Newsletter, Vol. 18, July
1994) includes a listing of many of the materials which are mostly available from the
geological surveys of different countries. CANMET standards are an example of available
CRMs and cost about $100/100 gram. CRMs are meant to be used for the development
of analytical methods and calibration of laboratory equipment. They are generally too
expensive to use on a routine basis for the quality control programs of mining companies,
which assay thousands of samples, especially when fire assays for precious metals are
required.
A variety of reference materials are also available from several suppliers, most of which
are based in Australia. One such supplier, Geostats, has over 75 gold standards and
another 75 base metals standards (Cu, Pb, Zn, Ni, As, Ag) which are sold for $25/kg.
Control samples (Reference material) have not been treated to the same rigorous
international analytical round robins as the CRMs. However, the Geostats reference
materials have usually been analyzed at a minimum of 20 different laboratories and
"recommended" values are determined using statistical procedures in accordance with
ISO9000 guidelines. Other suppliers offer similar materials thus broadening the
availability of materials with appropriate metal concentrations and matrices. A list of some
commercially certified reference materials is available on the internet at
http://www.crpg.cnrs-nancy.fr/Geostandards/GN_links.html.
Assuming that samples are being submitted for gold assay, it is necessary to include a
minimum of 75 grams of reference material. However, if one sample in 50 is a control
standard, one kilogram of reference material will be used with the submission of
approximately 650 samples.
If samples are being submitted for only base metal analysis, it is necessary to submit only
5 gm. of the reference material. Thus 1 kg of reference material could be used for the
submission of almost 10,000 samples. This translates into a cost of a few cents per
sample if reference materials are purchased.
It is important to carefully review the care and storage instructions for purchased control
standards. In some cases, control standards must be stored under nitrogen or may have
a specified shelf life.
Early stage discoveries will undoubtedly have to rely on purchased control standards, as
there is likely to be insufficient material to prepare control standards from project material.
Alternately, a few pulp standards have been prepared by Noranda and Falconbridge
and may be available in small quatities. Refer to Appendix IV for a current listing of

24

available reference materials. This list will be implemented on the intranet later in 2003
and updated on a regular basis.
4.2.3. The Advantage of Control Standards Prepared from Project Materials
The principal drawback for the use of purchased control standards is that the mineralogy
of the reference material may not match that of the samples which may lead to biased
results. It is preferable in many circumstances to prepare control standards from locally
available materials. This is particularly important for gold projects where the flux used for
the fire assay may have to be adjusted according to concentration of sulphides, oxides,
carbon, etc. Similarly, for copper-oxide, nickel-laterite and other projects, where a variety
of specialized digestions are used to predict metal recovery, it is important to monitor the
effectiveness of the digestions based on reference materials built from sub-economic and
economic ores.
As discussed above, one kilogram of control standard is usually adequate for the
submission of 650 samples for gold assay and almost 10,000 samples for base metal
analyses. Thus for a program of 10,000 samples, it is only necessary to have 1 to 15 kg
of control standards.
A series of control standards at different grade ranges is required and possibly materials
with different characteristics. Where necessary, control standards are recommended to
be prepared that are representative of different ore types, and possibly oxide vs. sulphide
mineralization. Ore types should not be mixed when selecting materials for control
standards. It may be possible to use control standards prepared for other projects in the
same region and geologists are encouraged to coordinate preparation of control
standards with other interested parties.
A total of 3 to 5 control standards are recommended; one for cutoff grade, one for average
grade and one for high grade. Special ore types may also require standards. These
control standards can usually be developed from drill core, outcrop, excess metallurgical
samples or other sources. They must be carefully prepared, well homogenized, split and
then submitted to at least 5 laboratories to determine the range of "acceptable" values.
Pulp standards that are rich in sulphides require special handling. The oxidation of these
materials may alter the analytical results, particularly using hydrochloric and nitric acids for
the determination of base metals. It is preferable to store these materials in vacuumsealed bags in a nitrogen environment to maintain the stability of the sulphides. Control
standards developed for a specific project must be strictly monitored with respect to a
reasonable shelf life and/or the effects of oxidation or degradation over time.

25

4.2.4. Limitations of Using Control Standards Prepared from Project Materials

Once the material for the control standards is received at a laboratory it is likely to take 46 weeks to complete the preparation and analytical stages. An approximate cost to
prepare a 50 kilograms control standard is in the order of four to five thousand dollars per
pulp standard, depending on the number of variables being determined. Typically, half
the cost is related to submission of the material for determination of "acceptable" values
and measurement of homogeneity. This becomes a significant expense and the time
delay is not always manageable.
In certain cases, it may be difficult to prepare a control standard that has sufficient
homogeneity. It can be particularly difficult to prepare a control standard homogeneous
with respect to gold or other metals that are distributed as nuggets or discrete grains. The
insertion of control standards where metal concentrations cannot be anticipated reduces
the effectiveness of a quality control program. It may be preferable to use purchased
control standards in such cases.
4.2.5. Insertion of Pulp Standards

This procedure deals with the insertion of control standards or purchased reference
materials to monitor laboratory performance for Stage III projects.
4.2.5.1.

Materials Required

Fully-prepared (crushed, pulverized, homogeneous and certified) control standards

Small sample bags (approximately 10 x 16 cm)
Sample log (see Note below)
4.2.5.2.

Procedure

Regularly spaced sample numbers ("-25", "-50", "-75" and "-00") are used for control
standards. The number of control standards should reflect the size of the analytical batch
used by the laboratory, which may be in the order of 20 samples for gold fire assay and 40
samples for routine geochemical analysis. For some projects, it may be preferable to
randomly insert control standards. This requires detailed record keeping and careful
organization.
Bags labeled with these numbers are filled with 5 grams of one of the control standards
and the sample tag is inserted in the bag. Approximately 75 grams is suitable to be
submitted if gold fire assays are requested. Care must be taken to ensure that control
standards are not contaminated when handled and, if necessary, packets of the control
standards should be prepared by suppliers or in a laboratory environment.

26

Record which control standard was put in each bag in the sample log or sample cards.
Control standards are inserted in numerical order with the samples prior to shipping.
Ensure that the laboratory analyses the samples in numerical order. In some situations
control standards may be inserted after samples have been pulverized but Noranda and
Falconbridge personnel should supervise insertion of control standards and the
description of the procedures should be included in quality control reports.
The control standards are used on a rotational basis, i.e. the same control standard is not
inserted at "1025" as at "1050".
4.2.6. Sample Log
Complete the internal sample log that records a minimum of the following information:

the sample number,

drill hole number,
meterage/footage,
sample shipment number or batch number,
the date samples were shipped,
the date results were reported and/or laboratory certificate number,
sample numbers assigned for blanks,
sample numbers assigned for control standards and which control standard
was inserted.
sample numbers assigned for drill core duplicates, if used.

Note: Table 4 is an example of the headers for a sample log.

Table 4 : Example of a Sample Log
Sample
Number
1001

Hole-ID

From

To

DH-06

100

101

1002
1003
1004
1005
1006
1007
1008
1009
1010
1011
1012
1013

DH-06
DH-06
DH-06
DH-06
DH-06
DH-06
DH-06
DH-06
DH-06
DH-06
DH-06
DH-06

101
103.4
104.87
105.5
BLANK
107
108
110
113
113.5
114
115.23

103.4
104.87
105.5
107

Shipment
33BH

Shipped
Oct.3

Date
Recd/Cert #
Oct.12
A990343

108
110
111
113.5
114
115.23
115.9

27

1014
1015

DH-06
DH-06

115.9
Control

1016
1017

DH-06
DH-06

116.8
117.33

116.8
STD05
BM&S
117.33
118.75

28

5. Stage I, II, III Procedures

As described, the exploration - discovery - delineation/development process is governed
by three stages that reflect increased success, sample availability and capital risk. While
Stage I encompasses accepted baseline QAQC practices, Stages II and III reflect the
addition of complimentary QAQC procedures, metallurgical testing and analysis for
deleterious and secondary pay elements.

5.1.

Stage I - Grassroots Projects

Stage I projects primarily involve drill testing geophysical, geological and/or surface
geochemical targets. These projects may not encounter mineralized zones and, in the
absence of significant mineralization, the focus is identification of anomalous metal values
and alteration patterns.
Generally, geochemical multi-element ICP analysis is acceptable for Stage I projects to
evaluate the metal content of zones of interest. Analytical technique may vary on a
project basis. Potential economically significant intersections will automatically move the
project to Stage II.
One control standard and one blank sample are submitted with each sample batch with a
minimum of one each per every 100 samples. Coarse reject replicates, coarse crush
particle size analysis, and drill core duplicates are optional. Cross-check analysis of pulps
at a secondary laboratory is recommended for 5% of mineralized samples. Quality control
results are verified upon receipt of analysis and the lab contacted immediately upon failure
at any point.
Under Stage I and specific to ICP analyses and geochemical analysis for gold, the
following guidelines are recommended.
Samples with reported base metal results greater than 10,000 ppm and
silver values greater than 10 ppm are automatically assayed.
Samples analyzed for gold using a geochemical analysis (MIBK-A.A.S. or
fire assay with an instrumental finish) that report gold values greater than
1000 ppb are automatically fire assayed using a gravimetric finish.
Intervals selected for assay, based on the above criteria, shall include lower
grade samples on each end of the interval so that the "cut-off" grade for the
mineralized interval is determined using the same analytical method.

29

5.2.

Stage II - Discovery Stage Projects

Stage II projects essentially represents a transitional stage that is initiated upon first
discovery of potentially economic mineralization. It is directed towards additional QC
checks, as well as the beginning of the characterization of a potential ore body. It is
acknowledged there will be initially limited sample availability.
The discovery of potential economic mineralization automatically implies that assay
methods are to be used for all samples within a mineralized interval. It is very important
not to include geochemical analyses for low grade or barren samples with assays when
calculating grade and width of mineralized intervals.
One control standard and one blank sample are submitted with each sample batch with a
minimum of one each per every 50 samples.
Samples are selected for coarse crush replicates to represent the range of grade and
texture. At least 5% of the mineralized interval(s) samples are submitted.
Coarse crush particle size analysis is conducted as described in Section 10.1. Drill core
duplicates are optional. Cross-check analyses of pulps at a secondary laboratory are
recommended for 5% of mineralized samples.
QC results are verified immediately upon receipt of analyses and the laboratory is
contacted immediately upon failure at any point.
Geochemical multi-element analysis can be used for initial "characterization" of the
chemistry of the mineralization for elements other than base and precious metals with the
objective of identifying deleterious elements. Alternative analytical methods, sometimes
with lower detection limits or use of strong acid digestions may be required to determine
the absolute concentration of deleterious elements and must be employed early in the
process. However care must be taken to ensure the digestion method does not cause
volatilization of the target elements and hence, create bias.
Under Stage II the following guidelines are recommended.
Complete multi-element (deleterious) chemical characterization analyses on
individual representative samples. If practical, characterize all samples that
comprise composite. Do not rely on a standard suite of deleterious
elements for any mining camp to determine characterization of deleterious
elements.
As an indication of a potential resource develops, initiate optical predictive
metallurgical characterization and compare results with chemical analyses.
Microprobe work can compliment this type of study by locating host minerals
of deleterious elements.
Begin collection of geotechnical data.

30

5.3.

Stage III - Advanced Exploration and Evaluation

This stage applies to projects that have advanced to resource delineation and definition.
Chemical analyses lead into, and compliment, metallurgical evaluations that may be run
on individual holes, bulk samples composed of combined holes and/or large scale bulk
samples.
The objective is to characterize the deposit on the basis of chemistry (distribution of
grade, distribution of deleterious elements) and metallurgy, leading to a high confidence,
comprehensive understanding of the deposit prior to large capital expenditures. The
approach needs to reflect the fact that mineral deposits are not generally homogeneous
and that calculations of Net Smelter Return need to reflect variances in metallurgy that
may be predicted from chemical analysis.
One control standard and one blank sample are submitted with each sample batch with a
minimum of one each per every 50 samples. It is required that the laboratory be
consulted for the size of the analytical batch and at least one control standard and one
blank must occur with each analytical batch, normally represented by the the number of
samples in a digestion rack.
Samples are selected for coarse crush replicates to represent the range of grade and
texture. At least 5% of all samples are submitted until about 55 samples are collected. If
precision levels are deemed acceptable (see Howarth-Thompson precision study, section
10.4) afterwards only 1 sample in 100 rejects need be replicated.
Coarse crush particle size analysis is conducted as described in section 10.1.
Cross-check analyses of pulps at a secondary laboratory are recommended for 5% of all
samples.
Each sample is analyzed for deleterious elements until the deposit is reasonably
characterized. Metallurgical analyses will provide a further check on analytical results and
deleterious elemental concentrations.
Under Stage III the following guidelines are recommended.
Assays to be used for all samples.
The selection of deleterious elements may vary for different parts of an ore
body and the analytical requests must reflect a detailed investigation to
document these variations.
Specified sample preparation protocols must be adhered to. Samples
required for metallurgical testing may require different sample preparation
procedures.
Initiate systematic predictive metallurgy prior to advanced metallurgical
analyses and compare results with chemistry. Microprobe work may
31

compliment this type of study by locating host minerals of deleterious

elements.
Assays of metallurgical re-samples (either assays of reject or re-sampling of
drill core) are compared immediately with initial results. Deleterious results
from the metallurgical flow test are compared with geochemical data of the
original samples.
Initiate a statistical review of the spatial (hole to hole) variance of the assay
data.

32

6. Procedures at the Drill and Drill Core Sampling

6.1.

Communication with the Drill Company and Drill Crew

At the foundation of collecting core samples is good communication with the drill company
and crew. Managers and project geologists inform the drill companies of Noranda and
Falconbridge's stringent protocol directed toward collecting quality core samples prior to
awarding of the contract.
Geologists on site must communicate with and monitor the drill crew to ensure attention to
acceptable practices is maintained at all times. This relates not only to the drilling and
sampling, but also to health, safety and environmental issues. Prior to a drill program,
materials that will interfere or contaminate the core (i.e. lubricant contamination of the
samples) must be identified and not used in the program.

6.2.

Security

Core must be secured from outside inspection and interference, or accidental internal
interference. Chain of custody must be strictly maintained during transportation, sample
collection, shipping and preparation to avoid tampering or inappropriate release of
privileged information. Assay results must be kept confidential and only released to those
on a need to know basis. Public release of results will only be conducted through a news
release approved by head office. Project staff must be made aware of the need to
maintain the confidentiality of both assay and drill results.

6.3.

Procedures at the Drill

Core boxes are labeled, and arrows drawn so that the core is systematically
laid in the box.
The core box is placed away from any source of contamination.
A wooden or plastic marker is placed in the core box after each run. The
meterage/footage is written on the marker.
Transfer of the core from the core barrel to the box should be done as
carefully as possible. No core is allowed to fall onto the ground. Core is
directly placed in the core box and a plastic mallet is used to loosen core in
the core tube. Breakage of core will produce inaccurate geotechnical
measurements.

33

 Photographs of the core at the drill site will be beneficial for geotechnical
analyses in a number of circumstances where transportation may result in
degradation of the core.
Document intervals of ground core and immediately address inaccuracies in
depth labeling in the core boxes. A rod count must be conducted
immediately to accurately measure the depth of the hole (this is at the drill
company's cost if poor attention to labeling is indicated).
Rod counts should be done at each bit change as a matter of course.
If the core is being orientated, the core is systematically marked to indicate
base of hole.
As soon as a core box is full, a lid is properly secured so that no accidents
occur.
Poor quality or broken core boxes must be discarded.
6.4.

Transportation

Sample collection and transportation procedures may vary between projects. Differences
are commonly related to access, climate, local infrastructure and region.
Sample
collection and transportation procedures must be documented and made available to field
staff. These procedures are recommended to address the following issues where
applicable:
Transportation of core from the drill site to the logging facility must be in a
manner to minimize or eliminate shifting of material in the core boxes.
Transportation and storage of cut or split core must ensure that the
remaining core does not shift and that marked sample intervals remain
intact.
Appropriate measures must be taken to eliminate the possibility of sample
tampering through proper chain of custody management.
6.5.

Chain of Custody Management

It is essential that proof be obtained that the samples were not tampered with between the
time of sampling and arrival at the laboratory. Depending on the project this may be trivial
issue or a very complicated one. All movement of samples from the drill to the lab must
be audited and the chain of custody documented and wherever there is a possibility of
tampering procedures must be implemented to ideally prevent, or at least detect any
tampering.
The chain of custody must be documented before the start of the project and any change
to the protocol, even if only temporary, must be recorded.
The best way to prevent tampering is to have the samples transported by only the most
reliable employees or by reputable transportation services. If samples must be

34

transported in unsecured fashion (eg. on a public bus) use of locked strong boxes is
strongly recommended (figure 4). Reliable transportation can reduce but not prevent
tampering. It is possible however to detect the occurrence by using plastic seals.
Although not completely tamperproof the security seal when combined with the use of
opaque pouches provides a reliable method to transport samples. Contact the Manager
Geochemistry if you require any seals.

Figure 4 : Methods for preventing and detecting tampering.

Core Sampling
The project manager is responsible for the handling of drill core at the core logging and
sampling facility, as well as the sampling process. Accurate sample selection, collection
and documentation are the responsibility of the geologist.
The health, safety and environmental aspects of core cutting must be enforced such as
protection for eyes, ears and hands. As well, in certain circumstances, air filtration
pressure helmets and washable or throwaway paper overalls may be required. Cuttings
that may be high in sulphides, and cutting oils must be disposed of in a proper disposal
facility.
Upon arrival, ensure core boxes are intact. Document all problems.
Organize and open boxes with care.
Measure depth intervals in each box and document any lost core or depth
inaccuracies. Immediately report depth inaccuracies to drill foreman and
initiate a rod count.
Tag boxes with metal tags listing hole name and the interval.
Care should be taken with friable core or poorly indurated core or poorly
bound mineralization (fractures, etc.).
Geotechnical analyses for Stage II and III projects must be conducted before
samples are selected. Photographs may be necessary. Physical property

35

measurements can be conducted at the same time (i.e. magnetic

susceptibility, conductivity).
Align core to be sampled by matching broken pieces.
A geologist is responsible for selecting material and intervals to be sampled.
Intervals are selected on the basis of mineralogy (e.g. oxide vs. hypogene,
pyrite vs. pyrrhotite, including significant grade variations), textures (grain
size, banded vs. massive, disseminated, stringer, folded intervals) and
concentrations of specific minor minerals.
Sample intervals should not cross geological boundaries (figure 5).
High grade

L. grade

Example assay intervals

Waste

1 Meter

Example composite interval

Figure 5 : Samples should not cross geological boundaries.

Intervals should not exceed 2 meters for porphyry deposits in mineralized

zones and 1 meter for massive sulphide deposits.
Intervals should be marked with a grease pencil on the core, and a metal tag
or other permanent tag fixed to the core box in case the pencil mark is lost in
cutting/ splitting.
The geologist marks the core within each interval with a line down the
middle of the core to guide cutting/ splitting. In addition arrows pointing down
core often help to ensure that the core is replaced in the box in the correct
orientation. This line must be selected to reflect the best equal distribution
of grade, mineralogy and texture in both halves of the core.
A diamond saw should be used unless washing action, inherent in the
sawing process, could degrade friable or highly fractured samples.
After cutting, both halves are washed and placed back in the core box and
again aligned. Care must be taken with this according to the nature of the
core and mineralization.
Prior to collecting half core samples, the geologist reviews the sample
intervals with the sampler. It is recommended that the same half of the core
be systematically taken.
Sample numbers to be used for quality control standards are not used for
drill core samples.
The sampler labels plastic bags with the appropriate sample numbers, saws
the core along the marked line and places the drill core for the appropriate
intervals in the sample bags. Every effort is made to select a representative
sample of drill core with poor coherence.
The designated geologist, sampler or quality control manager prepares the
quality control standards to be included with the sample shipment and
completes the sample log.

36

Exceptions to the procedures recommended above and detailed in the procedures may
apply to specific projects. The recommended procedures can be customized for each
project within the context of this document. It may be necessary to establish a detailed
procedure to avoid overselection bias.
However, changes to the recommended
procedures must be documented and reasons provided for these deviations. Management
approval is required.

6.6.

Drill Core Duplicates

The equivalent of field duplicates, at the drilling stage, is the collection of the second half
of the drill core for analysis. Drill core duplicates are recommended for Stage II and III
projects. Generally drill core duplicates are introduced for fewer than one in 100 samples
and they should be carefully selected to represent different ore types, alternation styles
and rock competency.
There is generally considerable reluctance to submit the second half of the drill core for
analysis. Removal of the second half of the drill core eliminates its use as a reference or
library sample, and the intersection cannot be used for metallurgical studies.
The purpose of analyzing the second half of the drill core is to compare the result with that
of the primary sample. This comparison will provide an understanding of variability
introduced by selecting one half of the drill core versus the other. The study of drill core
duplicates may lead to the conclusion that alternative drilling or sampling techniques are
required, such as larger diameter drill core.
It is not effective to sample quarter-core, or one-third of the core, as this does not reflect
the procedures used that are to be tested. If drill core duplicates are not utilized,
management must be provided with a clear explanation of the reasons why the procedure
was not implemented. Management approval is required.

37

38

7. Submission of Samples to Primary Laboratory

All of the work carried out collecting and preparing the sample will be wasted if the
samples are lost in transit. Therefore, it is worthwhile taking special precautions to ensure
that they reach their destination.
Depending on project specifics, strict protocol with respect to chain of custody may be
required for transportation of samples (see section 6.5). In some areas, samples are only
transported in the custody of a Noranda or Falconbridge employee and the samples are
never left unattended. If the sample preparation facility and analytical laboratories are at
different sites, the packaging and transportation procedures of samples must be
approved. The security of storage facilities, both on-site and at the laboratory must be
critically reviewed.
It is also critical that the laboratory performs the same preparation and analytical
procedures for the entire duration of the project. An Analytical Requisition Form that
specifies method codes or refers to a quotation number is recommended to accompany
each sample batch.
Detailed instructions for the retention or disposal of pulps and rejects must be included
with each sample batch or included in a laboratory contract.
7.1.

Submitting Samples to Primary Laboratory

7.1.1. Materials Required

Analytical Requisition Form
Sample log
Re-sealable sample pails, boxes or sacs
7.1.2. Procedure
Insert control standards and blanks per ratio or per batch.
Pack samples tightly into pails, boxes or sacs in numerical order. The containers are
numbered according to the order that they were used.
Complete the Analytical Requisition Form to indicate which samples are included in the
shipment, when samples were shipped, the total number of samples in the shipment and
the analytical procedures. The laboratory should be advised when samples with high
sulphide content or other special characteristics are in the shipment.

39

Enclose a copy of the Analytical Requisition Form in the first container. A second copy of
the form is retained in the files. This form may be submitted in person with the samples
where high security is an issue fax a copy of the Analytical Requisition Form to the
laboratory, where possible.
7.2.

Batch Size

It is important to verify with the lab the number of client samples that go into a full batch.
This is determined by the number of samples in the digestion rack (typically 40) minus the
labs own control samples. The submitted batch size, including control samples (i.e. pulp
standards, blanks and replicates), should be adjusted to this number. This way all the
samples in the batch will be processed in the same digestion rack thus confirming that the
conclusions drawn from the control samples are applicable to the whole batch. This will
also increase the odds of detecting any sample switching that may have occurred.

7.3.

Data Entry and Database Management

Sample locations and the insertion of quality control standards are recorded at the drill
core handling facility but must be transferred to a digital format following these guidelines:
Data is entered or imported (digital) in a timely fashion. All digital data to be
followed by a hard copy and checked and re-checked. The hard copy is
filed with the hole.
All database records are backed-up regularly.
Original hard copy documentation is filed and retained.
Data entry is validated using software validation routines where available,
and also by manual comparison with the original documentation.
For the purpose of internal and centralized auditing, all control standards
and blank results (and replicates) are entered into the Noranda and
Falconbridge QAQC web site database immediately following receipt of the
results.
Results for quality control standards must be verified prior to accepting data
in the database.

Century Systems database software provides a comprehensive environment for the entry
and management of diamond drill data and assay results. The intranet QAQC database
will be replaced by direct access to the Century Systems database to remotely verify the
quality of assay batch results.

40

8. Review of Quality Control Data

Results for control standards and blanks must be monitored as received. Assay batch
data should not be transferred to a database until the results are verified. If the results for
control standards and blanks are not deemed acceptable, immediate corrective action is
required.

8.1.

Control Charts

The results for the blank and each control standard are plotted on control charts in figure
6.

EL Morro Standard # 3

Cu %

(expected value 1.064 % Cu)

1.300

1.250

1.200

1.150

Cu %

1.100

1.050

1.000

0.950

0.900

0.850

0.800
0

20

Data
Linear (Mean -

40
Linear (Mean

2 S.D.)

Linear (Mean +

60
(X bar))
3 S.D.)

80
Linear (Mean +
Linear (Mean -

100

120

2 S.D.)
3 S.D.)

Figure 6 : Standard Control Chart

The results for the blank and each control standard are extracted from the laboratory
results manually or within a database. The results are sorted according to control
standard.

41

The graph is constructed by plotting:

The sample number, batch number or laboratory certificate number on the xaxis.
The analytical value or the difference of the analytical value from the
expected value on the y-axis.
The expected value.
The acceptable range of expected values.
The total number of determinations of the control standard or blank.
The data for the round robin survey of the standard or the lab validation data for the
standard should also be plotted on the diagram in order to visually compare batch results
with the validation data.
The data points should fall within the acceptable range of expected values. If data points
fall outside these limits, it is first verified that the control standard or blank was recorded
properly. If a laboratory error is suspected, repeat analyses are requested (chapter 9).
For multi-element analyses, it may not be necessary to monitor each element. Several
elements of particular economic or exploration significance can be selected.
Laboratories should report results for their internal control standards, analytical blanks and
laboratory replicate analyses. This information is used to assess analytical precision and
laboratory performance. However, it is preferable to base an evaluation of the laboratory's
performance on the basis of hidden or "blind" quality control standards. Having said this it
is evident that unless the sample preparation is performed in a different it is very difficult to
hide the identity of a pulp standard from the lab.
For the purpose of internal and centralized auditing, all control standard and blank results
(and replicates) are entered into the Noranda and Falconbridge QAQC web site
database immediately following receipt of the results.
8.2.

Logic Table of Failures

A logic table of failures is a method to formalize the criteria for approval or rejection of
assay batches (table 5). It is meant to limit the amount of variation in the batch results
and ensure variations remain random (no bias).

42

Table 5 : Example of logic table of failures

Logic for Table of Failures
El Morro Project
1

If one Cu standard fails between 2 and 3 SD, and no other failure occurs in the
batch, the standard is accepted.

If adjacent Cu standards fail between 2 and 3 SD in a single batch, the standards are
classified as failures.

If both a Cu standard and a Field Blank fail in a single batch, both are classified as
failures.

If a Cu standard fails beyond 3 SD, the standard is classified as a failure.

If a Au standard fails between 2 and 3 SD and the Cu standard passes, the standard
is accepted.

If a Au standard fails beyond 3 SD, the standard is classified as a failure (unless

close to the detection limit).

If both Cu and Au fail beyond 2 SD, the standard is classified as a failure.

If a Field Blank fails in Cu in a minor way, the analytical batch is examined for other
QC failures in the same batch. If there are no other failures the laboratory is informed
of potential contamination but no other action is necessary.

If a Field Blank shows a significant failure in Cu, and other QC samples also fail in
the same batch, the most likely cause is sample mis-ordering and appropriate action
is taken to find the extent of the mis-ordering.

10 If a Field Blank alone shows a significant failure in Cu, the surrounding batch is
classified as a failure.
11 No failures will be attributed to Mo, as the concentrations of the standards are too
close to the detection limit to be useful.

A logic table of failures need to be constructed for each project because in detail the table
will change according to the stage of the project and the selection of primary and
secondary elements that are being monitored. The procedure below is general and will be
adapted to each case:
List primary elements (Contribution to NSR >20%).
Standards should plot within Mean+-2Std for primary elements.
Occasionally but not in succession (or for multiple elements) they can plot
between +-2 and 3Std (1 in 20).
Successive standards should plot on either side of Mean line but a few can
plot on same side if less than Mean +-2Std. The more random the better. If
a pattern starts to appear contact lab.
Blanks should not contain more than the limit concentration for any of the
primary elements.
Failures in different elements and/or blanks lead to batch failures.
Standards near detection limit should not lead to batch failures.

43

8.3.

Table of failures

Not all control sample failures lead to batch failures. Moroever sometimes a failures leads
to re-assay of only part of a batch either from the pulps or the rejects for standard and
blank failures, respectively. It is recommended that the failures and the followup actions
be monitored with a table of failures (table 6).

Table 6 : Example of table of failures to keep track of what controls failed in which batches and what actions
were taken.
EL Morro Project Quality Assurance/Quality Control
Table of Failures
Batch Number

February 6, 2003
Sample Number

Sample Type

Feb-09-2002

306675

Blank Pulp
Std EM-1

Nor-020203-01
BC302-46177.0

Feb-09-2002

306706

Field Blank

Nor-020203-04
BC302-46175.0

Feb-09-2002

305800

Std EM-2
Leached Zone

Nor-020205-03
BC302-464400

Feb-13-2002

305821

Blank Pulp
Std EM-1

Nor-020218-01

Mar-08-2002

306040

Blank Pulp
Std EM-1

Nor-020303-01
BC302-461400

Mar-09-2002

307677

Std EM-3
Enriched Zone

Nor-020203-01
BC302-46177.0

Date

Cause of Failure
Cu value 0.007 is >
3S.D above expected
value
Ag = 0.63 ppm
exp. value <50 ppm.
ond

2 sample from blank

was 2.02ppm Ag.

Subsequent Action
Subsequent control standard & field
blank were in spec for Cu
Batch accepted .
Cu, Mo, & Au values in Field Blank
were in range. Re-run Ag on 306706 &
306708. Batch accepted.

Cu & Au values in field blank and

Cu value 0.012 between
blank pulp within specs.
2SD & 3SD
Batch accepted.
Cu value of 0.005 is > 3 Cu for adjacent standard & Au in both
S.D. below expected
standard & blank pulp & field blank
within specs. Batch accepted.
value
Au = 0.02 ppm is > 3
Cu for adjacent standard & Au in both
S.D. below expected
standard & blank pulp & field blank
within specs. Batch accepted.
value
Cu for adjacent standard & Au in both
Cu value of 1.147 is < 3 standard & blank pulp within specs.
S.D. >2 S.D. over
Blank pulp 0.03 in Cu. Possible
expected value
contamination. Batch not accepted It
should be???

This table when used with the Logic Table of Failures provides a very high level of control
on batch results and ensures the highest quality of assays.

44

9. Quality Control Failure: Request for Repeat Analyses

If results for blanks or control standards are outside predetermined acceptable limits, it is
necessary to determine the appropriate action. The following items should be checked
prior to contacting the laboratory:
If the values for blanks are unacceptably high, determine if the previous
samples are high grade as this may explain sample carry-over in preparation
or analysis. Further discussion with the laboratory is required to isolate the
cause.
If all the values for a control standard are outside the acceptable limits check
that the control standard was recorded correctly.
To determine if a sample mix-up is likely, review the data for several
samples before and after the questionable quality control sample to see if
any results are similar to the expected values. If a sample mix-up is
identified, request re-analysis of the suspect samples.
If the value for a control standard is nominally outside the acceptable limits
and all other quality control data for the sample batch are acceptable, no
further action is necessary.
If the values for several quality control standards are similarly biased high or
low, even though close to acceptable values, repeat analyses are requested
for all the samples (and control standards) bracketed by the questionable
control standard results.
If it is determined that there is no immediate explanation for unacceptable
quality control results, the following guidelines apply:
If a sample mix-up is suspected or there is no explanation for
unacceptable quality control results, request re-analysis of sample pulps
that incorporate the suspect quality control sample(s). Repeat analyses
should be requested for approximately 10 samples before and 10
samples after the suspect quality control sample(s). It is preferable to
request return of the pulps for the samples that are subsequently renumbered and submitted with different quality control samples.
If sample contamination is suspected based on poor results for the blank,
request that a new pulp is prepared from the reject and re-analyzed.
Sample cross-contamination is more likely at the pulverization stage than
the crushing stage of sample preparation, but is also possible during
analysis.
When re-analyses are reported, compare these values against the original
results. If results are similar no further action is required and it is acceptable
to retain the original results in the database. The repeat analyses should be
retained in a separate table. The Century Systems database will store all
values but will automatically use the most recently entered value by default.
If repeat values are different than the original results, the laboratory must
provide an explanation and state changes to their internal procedures that

45

will prevent another occurrence. The original values are replaced with the
corrected data.
If quality control results are consistently unacceptable for a sample
submission, the entire sample batch must be re-analyzed.
It is preferable to discuss the quality control requirements of a program with the laboratory
providing services prior to the start of a program. Most major laboratories will provide
repeat analyses, based on a quality control program, free of charge. A laboratory contract
is a useful business tool which can define the conditions under which repeats are free of
charge or when charges may apply.
Invoices for analytical services should not be paid until quality control data has been
verified and any necessary repeat analyses completed.

46

10.

Additional Quality Control Procedures

10.1. Coarse Crush Particle Size Analysis

A sample set comprising remaining coarse crush material samples (reject) is regularly
submitted to a secondary laboratory. The secondary laboratory is requested to sieve the
complete sample. The procedure is used to verify that the primary laboratory has
prepared samples according to the requested specifications. For example the primary
laboratory may be requested to crush the rock samples to 95% passes 2 mm (-10 mesh)
as the operating procedure deemed necessary to obtain acceptable homogeneity and
sample representation. The secondary laboratory will re-sieve the reject material and
verify whether 95% of the crushed material passes a 10-mesh screen.
If a 10mesh sieve attachment is available on the crusher the project manager may prefer
to request a PSA determination from the primary lab on each sample and provide
instructions that an average of >95% is required for a batch and that in no case will an
individual PSA <93% be acceptable. However the requirement of PSA determinations in
the secondary laboratory remain for Stage II and III projects.

10.1.1.

Sample Selection

Approximately 5% of the sample rejects should be submitted for re-sieving at the

beginning of a project. If all the samples meet specifications after approximately 30 check
samples have been processed, it is acceptable to reduce the number of rejects for resieving to one in 100.
The optimum approach is to randomly select samples such as selecting every 10th or
20th sample.

10.2. Pulp Check Assays

10.2.1.

Submission of Pulp Replicates to the Secondary Laboratory

Pulps prepared at the primary laboratory are regularly submitted to a secondary laboratory
for cross-checks. This procedure is generally used to verify the accuracy and analytical
procedures of the primary laboratory in which case it is important to request that the same
analytical procedures be used at both laboratories.

47

Inter-laboratory bias may account for differences between results for two laboratories,
which influences the extent to which the accuracy of the primary laboratory can be tested.

10.2.2.

Analytical Methods

In some circumstances, it is preferable to request check assays using different

procedures. For example, there may be a logistical reason for using a local laboratory
that does not offer x-ray fluorescence analysis but has used a supposedly "total
digestion". To determine if the "total digestion" is appropriate for the mineralogy of the
samples, it may be preferable to submit samples to a secondary laboratory that offers xray fluorescence analysis that determines total metal values.
10.2.3.

Sample Selection

Approximately 5 to 10% of the sample pulps should be submitted for cross-checks

especially at the beginning of a Stage III project. If the accuracy of the primary laboratory
is confirmed (and other aspects of the quality control program are acceptable), it may be
possible to reduce the number of checks to 2 to 5% of the total number of samples.
The optimum approach is to randomly select samples for cross-checks such as selecting
every 10th or 20th sample. It is useful to ensure that a selection of high-grade samples,
typical of different types of ore, are also submitted for cross-checks.
Cross-checks are performed less often for a Stage II project and may only be randomly
performed for a Stage I project.

10.2.4.

Sample Submission

Control standards should be included with the submission of cross-checks to ensure that
the secondary laboratory has performed properly.
The "Best Practice Guidelines" of the Toronto Stock Exchange are somewhat unclear
about the whether it is necessary to use an accredited laboratory. If an accredited
laboratory has not been used as a primary laboratory, it is strongly suggested that the
secondary laboratory be at least ISO9002 accredited (and preferably Guide 25
accredited).

48

10.2.5.

Comparison of Results for Checks Assays

When results from the secondary laboratory are reported, it is necessary to systematically
compare these results against the original results. Standard x-y graphs or log-log x-y
plots can be used to quickly assess whether there are significant differences between the
data sets.
10.2.5.1. X-Y Plot and Regression
The advantage of X-Y plots is that the relationship between the original and check
analyses can sometimes be quantified by means of the regression equation (table 7 and
figure 7). However keep in mind that a bias relationship can be complex and not reducible
to a simple regression. Moreover the regression function, although easy to understand
and available on virtually all statistic packages, even in Excell (see data analysis tool
pack), the regression itself assumes one dependant and one independent variable and
that all the variance is taken up by one of the dependant variable. This is not strictly
correct because both analyses are independent. Nonetheless the method is simple and
can help to identify a major bias relationship between the two datasets.

Table 7 : Regression analysis of check assays against original assays (X Variable 1). The pertinent outputs are
the coefficients for the intercept (X0) and for the X variable (k) (see bottom second column) to be used in the
linear function Check Assay = k(Original Assay) + X0. The P-value for the intercept is >0.05 and is therefore
not significantly different than 0. The P-value for the X variable and the R-square are meaningless in this case
because of the naturally strong relation between the variables.

SUMMARY OUTPUT
Regression Statistics
Multiple R
0.9772
R Square
0.9549
Adjusted R Square
0.9542
Standard Error
0.1033
Observations
63
ANOVA
df
Regression
Residual
Total

Intercept
X Variable 1

1
61
62

SS
13.7832
0.6510
14.4342

Coefficients
0.0370
0.9158

Standard
Error
0.0389
0.0255

MS
13.7832
0.0107

t Stat
0.9520
35.9366

F
Significance F
1291.4419
0.0000

P-value
0.3449
0.0000

Lower 95%
-0.0408
0.8648

Upper 95%
0.1149
0.9667

49

3
2.5
2
Cu
2_
pct

1.5
1
0.5
0
0

0.5

1.5

2.5

3.5

Cu_pct

Figure 7 : X-Y plot of Check Assays (Cu2_pct) vs Original Assays (Cu_pct). Blue line is for X=Y (slope of 1).
Black dashed line is actual regression line for the least squares trend between variables.

10.2.5.2. Mean vs. the %Difference Plot

It is possible to document more subtle variations in the data by using a "mean vs %
difference plot". In this case, the mean (or average) of two values is calculated as well as
the percent difference between the two values, calculated as the difference divided by the
mean multiplied by 100. The mean is then plotted against the difference for each sample
(figure 8).

Original Assays > Check Assays

Check Assays > Original Assays

3.5
3
Mean_Cu_pct

2.5
2
1.5
1
0.5
0
-50

-30

-10

10

30

50

%Cu_Difference

Figure 8 : Mean (Cu_pct) vs percent Cu difference plot.

50

This plot allows the direct estimation of the bias that is present in each grade range and
shows any sub-groups that could have special causes of bias.

10.2.5.3. Paired t-Test

Another very good test that can be used to quantify the average bias between the original
and check assays is the paired t-Test (table 7). Although it can be neutralized when
opposite biases are present in different parts of the grade distribution the test, when
appropriate, allows us to unequivocally determine that bias is present and the amount of
the bias.

Table 8 : Example of output from paired t-Test calculation in Excell. In this case there is bias between the two
datasets because the P-value for the two-tailed test is less than 0.05. The check assays are on average 5.7%
higher than the original assays.

t-Test: Paired Two Sample for Means

Mean
Variance
Observations
Pearson Correlation
Hypothesized Mean
Difference
df
t Stat
P(T<=t) one-tail
t Critical one-tail
P(T<=t) two-tail
t Critical two-tail

10.2.6.

Original Assays Check Assays % Difference

0.042
0.044
5.7%
0.0020
0.0023
60
60
0.994
0
59
-3.193
0.001
1.671
0.002
2.001

Corrective Action

If it is determined that a bias exists, it is necessary to determine what the cause of the
bias might be and if the primary laboratory needs to take corrective action. Segregation of
samples during transport, oxidation of samples and different analytical methods should be
considered as possible explanations. In extreme cases, it may be necessary to find an
alternative primary laboratory if the secondary laboratory results are reliable. It is then
necessary to determine if all the project samples need to be re-analyzed.

51

10.3. Reject Replicates

10.3.1.

Submission of Reject Replicates for Check Analyses

A second split of the reject material (the -2 mm or -10 mesh left over crushed sample) is
prepared in a similar manner to the original pulp. A second split is prepared in order to (a)
measure sampling errors introduced by selection of a split for pulverizing , (b) check for
sample mix-ups in sample preparation and (c) determine if sample preparation procedures
should be changed to improve representivity of the analysis.

10.3.1.1. Sample Selection

Approximately 5 to 10% of the sample rejects should be submitted for replicate analysis at
the beginning of a project for Stage III projects. Rejects should be returned and renumbered. In general, 30 replicate pairs should be accumulated prior to assessing the
reproducibility of the results. If analytical reproducibility is determined to be adequate, the
number of checks can be increased until about 55 pairs are collected and then the rate of
submittal should be decreased to 1 to 2% of the total number of samples. The renumbered rejects are returned to the primary laboratory for preparation and analysis so
that methods are duplicated as closely as possible.
For Stage II projects, less than 5% of the sample rejects can be submitted for replicate
analysis. Replicate analysis is generally only carried out for a Stage I project if significant
mineralization has been intersected.
The optimum approach is to randomly select samples such as selecting every 10th or
20th sample.
10.3.1.2. Sample Submission
In many cases, a laboratory both crushes and pulverizes samples. Preparation of two
splits at the same time is advantageous since the -2 mm material is probably relatively
homogeneous after crushing. The disadvantage of requesting that two splits be prepared
at the same time is that the second split is not submitted to the laboratory "blind". The
laboratory may "optimize" results for the second split, by comparing results with those for
the first split, prior to reporting results.
In some cases, particularly in remote locations, crushing but not pulverizing may be
carried out on-site. Usually a split of the crushed material is prepared for shipment to a
laboratory for pulverizing and analysis. In this case, a second split of the crushed material
should be prepared for submission to the laboratory, but numbered differently than the
primary sample.

52

10.3.1.3. Analysis of Results

Results of paired assays can be analysed using the absolut difference vs mean grade plot
to identify sub-groups of samples that may have greater variance (figure 9).
In addition the paired results can be used to estimate the variance of sub-sampling the
coarse crush material through the Thompson & Howarth (1978) method shown in the next
section.

Figure 9 : Absolute difference vs mean concentration plot. Results indicate a distinc grouping of samples with
higher variance, possibly due to erratic or nuggety copper.

10.4. Integrated Variance Studies

Variance or precision error occurs at each step of the sampling and assaying process and
is additive. As a result the observed variance of duplicate samples increases from the
instrument backwards through the pulverizer, crusher and core sampling. With at least 55
duplicates from each of core and coarse crush rejects it is possible to map out the

53

contribution to variance of the core sampling and coarse crush splitting steps and uncover
potential problems (figure 10).

Figure 10 : Thompson and Howarth Plot.

The method proposed here is taken from Thompson and Howarth (1978) and is
reproduced verbatim:
From the (N>=55) pairs of results ai, bi (i=1, 2,..., N), form list of pair means
(ai - bi)/2 and the corresponding absolute differences |ai - bi| (do not
logtransform the data).
Sort the of the means into increasing order and the differences into the
corresponding order.
Select the first nine results and calculate the mean of the pair means and
the median (i.e. the central value, not the average) of the differences.
Repeat this procedure for successive groups of eleven results, and obtain
corresponding lists of means and medians. Ignore any terminal group of
less than eleven results.
Either: plot the medians as a function of the means and obtain the intercept
and slope of the line graphically by eye; or: obtain the same parameters by
regression. These parameters correspond respectively with s (0) and k in
equation 4 of the section on Precision above.
Plot equation 4 for each control sample set to determine the precision for a
given grade range for each of core, coarse crush and pulp duplicates and
standards. The curves should not intersect.

54

11.

Measurement System Analysis

11.1. Assays as a Measurement System

Assays form the basis of mineral resource estimates and as such represent a
measurement system. Resource estimates then form the basis of investment decisions
about mining projects. At Noranda and Falconbridge all mining projects must be
advanced and evaluated using a formal methodology called the Mining Stage Gate
Procedure (MSGP) which is based on methodologies developed for DFSS or Design for
Six Sigma. All Six Sigma projects require that measurement systems be validated using
five distinct criteria, namely resolution, accuracy, linearity, stability, and precision with the
final criterion divided into two components, repeatability and reproducibility. The round
robin survey provides a convenient model for a measurement system analysis (Beaudry,
2003) because it is usually performed for mutiple standards (parts) and submitted to
several laboratories (operators).
Resolution is determined by the "ten bucket" rule. Since assays are always reported to at
least 2 decimal places and the precision of assays are typically in the 30 to 50% range,
the % of tolerance is calculated as 100 * 0.01/0.4 = 2.5%. This value must be less than
10%.
Accuracy is measured primarily using pulp standards and to lesser extent, blanks and the
populations of repeat analyses. Noranda and Falconbridge QAQC protocol requires
that a table of logic be applied to results of pulp standards. This procedure can detect
early signs of bias that may appear in the digestion and instrumental measurements and
ensures that variations in results from batch to batch remain random. The protocol also
requires the plotting of repeat analyses on difference vs average plots and these graphs,
although not as sensitive, allow the identification of potential bias in the sample
preparation or sampling steps of the process. Noranda and Falconbridge's protocol
does not permit any bias in assay results and in practice procedures are in place to detect
and correct any situation of bias.
Linearity is a measure of the variation of accuracy over the range of measurements of the
process. Assays range in grade from 0 (approximation of the lower detection limit) to
more than 30% and although no bias is acceptable in practice our capacity to detect bias
is a function of the precision of measurements, which is known to vary with grade.
Therefore it is somewhat more difficult to detect bias at high grade than at low grade.
Over the grade range of assays in a porphyry deposit this should not cause a problem but
in VMS or SEDEX deposits, or high grade gold deposits the issue can be important.
Stability is the measure of the change in accuracy over time and can be caused by
changes in laboratory performance or denaturing of pulp standards through oxidation.
This may be important for projects that are drilled off over several years using the same
standards. Packaging pulps standard in a nitrogen atmosphere mitigates this problem

55

although the cost may be prohibitive. Otherwise, running yearly round robin surveys on
existing pulp standards can help to detect and quantify the effects of oxidation.
The most important issue regarding assays as a measurement system is precision
because this impacts on our our capacity to detect bias. This measure is divided into the
components of repeatability and reproducibility. The former defined as the variance of
repeat measurement by the same lab on the same sample whereas the latter is the
variance of measurement on the same sample between labs. It follows from this that the
round robin survey with its requirement of different operators (labs) and parts (pulp
standards) can be analyzed using the Gage R&R procedure found in Minitab software.
Six Sigma methodology requires that the Gage R&R procedure pass three critical tests.
The first is %Tolerance or P/T ratio which measures the percentage of the process
tolerance taken up by the measurement system and is divided between repeatability and
reproducibility. In assays the process variation is taken as the allowable error in sample
preparation and analysis and averages about +/- 40% as measured by duplicate analyses
of core.
A measurement system must have a %Tolerance less than 30 and ideally less than 10. In
the case of base metal assays the within lab variance is typically better than between lab
variance. Since the assays for a project are done primarily in a single lab the %Tolerance
for repeatability is more important and should definitely be less than 30%. Values greater
than 30 should be investigated thoroughly as the problem may reside with an individual
standard, especially low grade ones.
The second index is the Gage R&R itself that measures the proportion of the process
consumed by the measurement system. As with %Tolerance, Six Sigma methodology
requires that this index be less than 30% and ideally less than 10%.
Finally the last criterion of the Gage R&R the discrimination index (DI) which provides the
number of divisions or categories that the measurement system can accurately measure
across the process variation. A minimum value of 5 is required and ideally this index
should be greater than 10.

56

List of References and Selected Bibliography

AMOR, S., BLOOM, L., WARD, P., 1998.
Practical Application of Exploration Geochemistry. Proceedings of a short course
presented by the Prospectors and Developers Association of Canada, Toronto.
BEAUDRY, C., 2002. Quality in diamond drill assaying : reducing the variation. Six sigma
Brown Belt project.
BEAUDRY, C., 2003. The Round Robin as a model of a measurement system analysis for
assays. Explore, Number 119, April 2003, pp. 12-29.

BLOOM. L., 1999.

Third Party Vetting of Geochemical Programs or Return on Quality. In Quality Control in
Mineral Exploration: A short course presented during the 19th International Geochemical
Exploration Symposium, April, 11, 1999.
BLOOM, L., 1998.
The Role of Economic Geologists in Evaluating Assay Data Quality. Proceedings of Short
Course Presented by the GAC and PDAC, November, 1998.
FRANOIS-BONGARON, F., 1998a.
Error variance information from paired data: Applications to sampling theory. In Valle,
M. and Sinclair, A. (eds.), Quality assurance, continuous quality improvement and
standards in mineral resource estimation : Exploration and Mining Geology, Journal of the
Geological Society of CIM, Vol. 7, Numbers 1 and 2, pp. 161-165.
FRANOIS-BONGARON, F., 1998b.
Extensions to the demonstration of Gy's formula. In Valle, M. and Sinclair, A. (eds.),
Quality assurance, continuous quality improvement and standards in mineral resource
estimation : Exploration and Mining Geology, Journal of the Geological Society of CIM,
Vol. 7, Numbers 1 and 2, pp. 149-154.
GY, P. M., 1982.
Sampling of particulate materials, theory and practice. Elsevier, Amsterdam, 431 p.
HOWARTH, R.S., THOMPSON, M., 1976.
Duplicate analysis in geochemical practice, Part II: Analyst 101 (1206), 699-709.
MERKS, J. W., 1985.
Sampling and weighing of bulk solids. Series on Bulk Material Handling Vol. 4. Trans
Tech Publications, 410 p.
RIDDLE, CHRIS, 1993.
Analysis of geological materials. Marcel Dekker Inc. 463 p.

57

THOMPSON, M., 1992,

Data quality in applied geochemistry: the requirements and how to achieve them: Jour
Geochem Expl, 44, 3-22.
THOMPSON, M., HOWARTH, R.J., 1978.
A new approach to the estimation of analytical precision: Jour Geochem. Explor., 9, 2330.
SMEE, B., 1999.
Laboratory Audit II - The Geochemist's Point of View. In: Quality Control in Mineral
Exploration, A Short Course Presented During the 19th International Geochemical
Exploration Symposium, April, 1999.
VALLE, M. AND SINCLAIR, A., 1998.
Quality assurance, continuous quality improvement and standards in mineral resource
estimation : Exploration and Mining Geology, Journal of the Geological Society of CIM,
Vol. 7, Numbers 1 and 2. 180 p.

58

Appendix I

Glossary of Terms

ANALYSES
A.A.S.: Atomic absorption spectroscopy is a single element, solution based technique.
Geological samples must be dissolved prior to A.A.S. analysis. Sample solutions are
compared against the quantity of light adsorbed for calibration solutions at a specific
wavelength to determine elemental concentrations.
Accuracy: The degree to which an analysis, or the mean of a set of analyses, approaches
the "true concentration".
Assays: Assays are distinguished from geochemical analysis by being more precise and
designed for higher-grade material. In general, assays are assumed to represent "total"
metal. Assays are used to quantify metal contents for ore reserve definition. The
precision of assays is not dependent on the type of instrumentation used for the analysis.
The precision of the method is dependent on the amount of sample used, the digestion (or
fusion) technique used to dissolve the sample, dilution procedures, spectral interference
and optimization of the instrumentation for specific grade ranges.
Deleterious Elements: Smelters will reduce payments for concentrates if there are
elements present that negatively impact metal recovery or create environmental concern.
Fire Assay: Fire assay is a traditional assay method for precious metals, specifically gold,
silver, platinum and palladium. There are four steps consisting of fusion, cupellation,
parting and weighing of the precious metal bead. A gravimetric finish includes weighing of
the precious metal bead. To achieve lower detection limits and to determine platinum and
palladium, the bead is dissolved and the solution analyzed by A.A.S. The traditional fire
assay method includes collection of the precious metals by lead during the fusion. A
nickel sulphide fusion can be used for collection and determination of the entire suite of
platinum group elements but the procedure generally costs 15 times more than the
standard lead collection procedure.
Geochemical Analyses: Geochemical analyses generally cost less than assays. The
laboratory uses partial digestions and lower sample weights for geochemical analyses
than for assays. In general, geochemical analyses are less precise than assays and have
a lower upper detection limit. Geochemical analyses often
provide multi-element data and compromises are made in order to report a wide range of
elements.
I.C.P.-O.E.S.: Inductively coupled plasma - optical emission spectroscopy is primarily
used as a multi-element, solution based technique. Quantification is achieved with
reference to multi-element aqueous solutions. Matrix effects can be more significant than
for A.A.S. determinations but mathematical corrections can usually be applied to correct
for interference and spectral overlap. I.C.P. has a greater dynamic range than A.A.S.
59

meaning that a broader range of concentrations can be determined without requiring

dilutions or calibration changes for higher concentration samples.
I.C.P.-M.S.: Inductively coupled plasma - mass spectrometry is a multi-element, solution
based technique. Mass spectra are measured, as opposed to emission spectra I.C.P.O.E.S., which are less complicated so that there is less potential interference. I.C.P.M.S. is primarily used for the determination of rare earth elements, low level elemental
concentrations (in the ppb-range) and some isotopes.
MIBK (or DIBK)-A.A.S.: An analytical procedure used in some regions to determine gold.
A 10 to 20 gram sample is digested in aqua regia and the digest solution is extracted.
The digest solution is then shaken with an organic solvent (methyl isobutyl ketone or an
alternative) and the gold is extracted into the organic solvent. The organic solvent is then
analyzed for gold using an instrumental method such as A.A.S. The method is usually
restricted to use with geochemical surface samples and may underestimate gold content.
Precision: Precision is the difference or range of differences between similar estimates or
measurements. In mineral exploration, precision is usually defined as the percent relative
variation at the two standard deviation (95%) confidence level.
QUALITY CONTROL
Blanks: A material with negligible metal values that is used to monitor contamination
during sample preparation or analysis.
Certified Reference Materials ("CRM"): Certified reference materials ("CRM") are a special
classification of control samples that are high quality materials. CRM's have been
subjected to rigorous international testing. CRM's are seeing wider use in exploration and
development circles, however they are typically used in routine testing to develop
analytical methods and calibrate equipment.

Coarse Crush Reject: In most circumstances, an entire drill core interval or rock sample is
crushed. The crushed material is referred to as the "coarse crush". A sub-sample is
usually removed for pulverizing. Any coarse crush material remaining is referred to as the
coarse crush reject. The reject is stored for future reference and coarse crush particle size
analyses.
Control Samples: Control samples are materials of a known metal concentration, which
are usually fine-grained and homogeneous. Control samples, "controls" or standard
reference materials ("SRM") are used to monitor the accuracy of laboratory results.
Control samples are sometimes referred to as "reference materials". Controls samples
can be prepared from project materials and "recommended" values are determined from a
process of submitting sub-samples to various laboratories to measure the homogeneity
and metal content. (a round robin). Alternatively, these materials can be purchased.
Certified reference materials ("CRM") are a special classification of control samples that

60

are high quality materials that have been subjected to rigorous international testing (see
CRMs).
Drill Core Duplicate: The second half of the drill core may be submitted for preparation
and analysis, which is referred to as a drill core, duplicate.
Field Duplicates: A second sample collected at the same time, using the same sampling
protocol as the primary sample, to measure sample representivity. Field duplicates are
collected for rock samples, stream sediments, soils and other sample media. An
analogous procedure for drill core programs is submission of the second half of the drill
core for analysis.
Particle Size Analysis (PSA): Measurement of the percentage of material passing a
specified mesh size. Experimental work by Gy (1982) and Franois-Bongaron (1998a)
show that this measure should be stated as the mesh size that is required for 95% of the
sample to pass. Noranda and Falconbridge's protocol requires that 95% of coarse
crush sample pass a 10mesh (2mm) sieve screen and that 95% of pulps pass a 150 mesh
(0.1mm) screen.
Primary Laboratory: The primary or principal laboratory where samples are originally
submitted for analysis.
Primary Samples: The first sample collected at any stage of sample collection or sample
preparation is arbitrarily referred to as the "primary" sample.
Pulp: A finely-ground rock sample or fine-fraction of a soil or stream sediment that is
usually only a portion of the original sample collected. In most cases, analysis is done on
the pulp.
Pulp Replicate: A sample pulp may be analyzed a second time to measure analytical
precision. A sub-sample is removed from the original pulp for analysis that typically
weighs 0.5 to 2.0 g for base metal determinations. Most commercial laboratories routinely
perform pulp replicate determinations and these are also referred to as "laboratory
duplicates". Alternatively, the pulp may be submitted to a secondary laboratory for
analysis, which is referred to as a "cross-check" analysis.
QA (Quality Assurance): Quality assurance has a broad definition outside the mining
industry and has been defined as "All those planned or systematic actions necessary to
provide adequate confidence that a product or service will satisfy given needs".
QC (Quality Control): Quality control is one aspect of quality assurance. The difference
between the two concepts is described as; "Assurance in the quality context is the relief of
concern about the quality of a product. Sampling plans and audits, the quality control
devices, are designed to supply part of this assurance".

61

Reject Replicate: A second split of the reject may be submitted for pulverization and
analysis, which is referred to as a reject replicate. The same preparation and analytical
procedures are performed on the reject replicate as the primary sample.
Secondary Laboratory: A laboratory selected for analysis of a selection of sample pulps in
order to check the accuracy or bias of the primary laboratory's results.
OTHER TERMS
Capability Analysis: A procedure completed annually to define the excess variance due to
sampling procedure plus sample preparation. The Capability Analysis monitors year-toyear improvements compared against initial 1999 results from Six Sigma experimentation.
Geotechnical Data: Rock property data and physical property measurements such as rock
quality description (RQD), fracture frequency, hardness (mineralization, gangue and host
rock) and alteration on fracture surfaces. As well these data may include analyses of the
acid generating capability of waste rock, self heating analyses (oxidation rates) of any
sulphides present, magnetic susceptibility and radioactivity among others.
Predictive Metallurgical Analyses: Predictive metallurgical analyses allow for an early
stage characterization of the metallurgy of significant mineralization with the objective of
an early stage characterization of a potential ore body. Predictive metallurgy evolves into
more advanced bulk and bench scale testing. Both stages rely on good sampling
techniques, abundant sample availability and most importantly, a uniform drill density and
spacing that is representative of the variable nature of most deposits. Samples are
subjected to optical, chemical, microprobe and, with increased sample availability, bench
testing. Optical analyses investigate the mineralogical features (minerals present, oxides
vs. sulphides, etc.) and textures (grain size, grain to grain relationships, intergrowths, etc.)
including the nature of the gangue (hardness, etc.) and host rock (dilution). Chemical
analyses determine the presence of potentially deleterious elements. In combination with
the optical investigations, the microprobe analyses determines the distribution of these
elements in the minerals present and will give a good indication of where, if at all, the
deleterious elements will report. Bench testing subjects a larger quantity of material to the
milling and recovery process.

62

Appendix II

Guidelines for Preparation of Analytical Service Contract

The objective of an analytical service agreement is to clearly articulate sample processing

and analytical specifications and the required level of quality in analytical results in
addition to price and turn around times. The agreement should include the following :

Lab code for each analysis package.

The maximum weight of samples before crushing overcharges are applied.
The make and model of crushers to be used for the crushing of samples.
Unless special sample preparation procedures are required all samples will
be crushed to minimum 95% -10mesh.
If a 10mesh sieve is attached to the crusher, for each sample determine the
percentage of material passing 10mesh and the procedure for rehomogenizing the coarse crush material. Otherwise the lab should provide
one 10mesh sieve test per 40 samples.
The coarse crush splitting procedure and type of splitter to be used.
The size of coarse split.
The make and model of pulverizers to be used for pulverization of samples.
Unless special sample preparation procedures are required all samples will
be pulverized to minimum 95% -150mesh.
The pulverization procedure (i.e. time and additives).
Frequency of pulverizer 150 mesh sieve tests.
Frequency of laboratory preparation blanks.
Size of aliquots for digestion and fire assays.
Types and quantities of reagents used in digestion.
Source and quantity of litharge and inquart used in fire assay fusion.
Description of digestion and/or fusion procedures.
Number of client samples and number and description of control samples in
digestion and fusion rack.
Make and model of analytical instruments.
Source of calibration solutions.
Frequency of solution blanks.
Certified reference materials and in-house standards to be used with each
lab package and the tolerances the lab uses for those standards.
Units for each element in package and number of significant digits to be
reported.
The detection limits for each element.
All analytical results for control samples should be reported in
assay/analysis certificate and in digital copies of lab reports.
The sample preparation and analytical specifications should be summarized
in a flow chart (one for each principal lab package) to be included as part of
the laboratory service agreement.
The logic table of failures should be discussed with the lab and the lab agree
with the tolerances placed on Noranda and Falconbridge standards and
blanks.
63

Cost for each lab package and for other services.

Maximum turn-around time and penalties for delays.
Method of delivery of results.
Instructions regarding return of pulps and rejects.

64

Appendix III

Detailed Process Maps

1: Project Pre Drilling Process Map

2: Laboratory Validation Process Map
3: Pulp Standard Preparation Process Map
4: Round Robin Validation Process Map
5: Blank Validation Process Map
6: Sampling Process Map
7: Sample Preparation Process Map
8: Sample Analysis Process Map
9: Au Fire Assay Process Map
10: Batch QAQC Results Analysis Process Map
11: Standard Failure Process Map
12: Blank Failure Analysis Process Map
13: Pulp Check Assay Analysis Process Map
14: Coarse Crush Replicate Analyses
15: Particle Size Analysis Evaluation Process Map
16: Deliterious ESH Sampling Process Map
17: Post Drilling Process Map

65

PROJECT PRE-DRILLING
PROCESS MAP
Establish
objectives of
analytical program

Obtain sufficient
pulp standard
material

Determine type of
sampling to be
performed (i.e.
core size)

Obtain sufficient
blank material

Determine
average sample
size

Secure laboratory
service contract

Estimate number
of analyses
required

Prepare logic
table of failures

Estimate number
of pulp standard
analyses required

Prepare sampling
instructions

Estimate number
of blank analyses
required

Carry out training

Estimate number
of pulp check
analyses required

Proceed with
Sampling

Estimate number
of coarse crush
duplicate analyses
required

Estimate number
of core duplicates
required

Establish
analytical
requirements

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

66

LABORATORY
VALIDATION PROCESS
MAP
Number and
Quantity of
pulp standard
required

INPUT

Validate Project
Standards

CRM
Standards
preferred?

No

Criteria:
- Quantity required
- Stage of project
- Availability of materials
- Time

Yes
Purchase
sufficient quantity
of CRM standards
Primary and
secondary labs
part of round
robin?

No

Submit 10
samples of each
standard to
primary and
secondary lab for
estimation of
accuracy
precision

Laboratory
performances
acceptable?

Yes

Criteria:
- Price
- Location
- Turn around time
- Reputation
- Other

Select primary
and secondary
laboratory

No

Criteria:
- Mean of lab within +-2Std of
global mean.
- Distribution normal.

Yes

Store pulp
standards

OUTPUT

Pulp
Standards

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

67

PULP STANDARD
PREPARATION PROCESS MAP

INPUT

Decision to
prepare
pulp
standards

Identify laboratory
capable of
preparing pulp
standard

Send standards to
lab for sample
preparation.

Estimate
approximate cutoff grade, average
grade and high
grade for project

Analyze 20
samples of each
standard

Determine number
(min 3) of
standards and
quantity of each
standard required
for project

Identify source of
materials for pulp
standards

Collect material
for each pulp
standard

RSD%
acceptable?

Criteria:
- For base metals and other
major components RSD% < 4.0
- For gold and other precious
metals RSD% < 7.0
No
Contact lab to
discuss
homogeneity of
standard(s)

Yes

Divide into 200 g

packets and seal

Material
for Round
Robin

OUTPUT

Ship samples to
laboratory

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

68

ROUND ROBIN
STANDARD VALIDATION
PROCESS MAP
INPUT

Packets of
pulp
standards

Select laboratories for

round robin (at least 6)
(include primary and
secondary labs)

Send 8-10
samples of each
standard to each
lab

Criteria:
- For base metals RSD% < 5.0%
- For gold and precious metals
RSD% < 8.0%

Split results and

recombine by
standard

Send 8-10
samples of each
standard to
replacement lab(s)

Interpret results

Remove lab(s)
from list and
select
replacement lab(s)

Data
Acceptable?

No

Problem is with
one or more lab(s)
(homogeneity was
tested previously)

No

Select new
primary or
secondary labs
and repeat.

Yes
Criteria:
- Primary lab mean passes Ftest and t-test compared to
accepted values.

Primary and
secondary labs
acceptable?
Yes
Publish Accepted
value and Std for
standard

Valid
Standards

OUTPUT

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

69

PROJECT BLANK
VALIDATION PROCESS
MAP

Quantity of
Blank
material
required

INPUT

Determine source
of blank material

Carry out
collection of blank
material

No

Submit 10
samples of blank
to primary
laboratory for
analysis of
required elements

Blanks are
acceptable

Criteria:
- Blanks should be near
detection limit for analytical
method.

Yes

Store blank
material for project

Blanks

OUTPUT

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

70

INPUT

Core intervals
marked for
splitting/
sawing

DRILL CORE SAMPLING

PROCESS MAP
Core split or
sawed

Allways same side

collected

Criteria:
- Stage II: 1:50 or batch until
about 55 duplicates
- Stage III: 1:50 or batch until
about 55 duplicates for each
major drilling program.

Core duplicate
required?

Yes
Collect 2nd half of
core and identify
with nonsequential number

No

Place sample in
bag and label

Criteria:
- Stage I: 1:100 or batch
- Stage II: 1:50 or batch
- Stage III: 1:50 or batch

Criteria:
- Stage I: 1:100 or batch
- Stage II: 1:50 or batch
- Stage III: 1:50 or batch
(If grades are variable include
sample of cut-off, average, and
high grade standards in each
batch)

Blank insertion
required?

Yes

Insert Blank

Yes

Insert appropriate
standard

No

Standard
insertion
required?

Assemble batch
and prepare
manifest and lab
instructions

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

Samples
ready for
shipment

OUTPUT

71

Sample crushed
to >95% -2 mm
(10mesh)

Samples
arrive at lab

INPUT

DRILL CORE SAMPLE

PREPARATION
PROCESS MAP

Samples sorted
and checked for
dammage

10mesh sieve
attachment
present?

Yes

Job definition file

created in LIMS

Homogenize
sample

No

Sample Numbers
recorded in LIMS
Criteria:
- Evidence of tampering
- Evidence of contamination
- Insufficient sample
Yes

PSA
measurement
required?
Any samples
unsuitable?

No

Yes

Sieve with 2mm

(10 mesh) screen
and report %
passing mesh to
customer.

No

No

Contact Customer

Weigh oversize
and report to
customer along
with initial weight

Determine weight
of sample to be
pulverized

Sample listing
matches
manifest?
Yes

Split required
weight of subsample

Sample weighed

Clean pulverizer
with quartz sand
Sample
already a pulp?

No

Pulverize sample
Yes

Samples dried
Store pulverized
sample in kraft
envelope
Crusher cleaned
with quartz sand
Batch
ready for
analysis

OUTPUT

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

72

INPUT

SAMPLE ANALYSIS
PROCESS MAP

Batch of
pulverized
samples

Retrieve samples
from storage

Weight between
0.1 to 1.0 g of pulp

Criteria:
- Aqua regia digestion is
prefered in temperate climates
and where sulfides are fresh.
- Multi-acid digestion is prefered
in tropical climates and where
oxidation of sulfides significant.

Multi-acid
digestion
required?

Yes

Add multi-acids to
sample
in teflon tube

No
Add aqua regia to
sample in boron
glass tube

Heat on hot plate

until near dryness

Pour into
volumetric flask
and complete to
fixed volume

Analyze with AA
or ICP-ES

Results of
analyses

OUTPUT

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

73

SAMPLE GOLD/SILVER
FIRE ASSAY PROCESS
MAP

INPUT

Samples
retrieved
from
storage

Weigh appropriate
amount (<= 50 g)
Cuppel the lead to
Ag-Au bead

Add flux
Gravimetric
finish?

Add Litharge
(PbO)

No

Dissolve Au and
Ag in aqua regia

Criteria:
- Samples with >1,000 ppb Au
should be re-assayed with
gravimetric finish.

Yes

Dissolve Ag in
HNO3

Analyze with
dedicated AAS
instrument

Weigh Au bead in
micro balance

Assay
Result

Add inquart
(AgNO3)

OUTPUT

Homogenize
sample

Fuse in
temperature
controlled furnace

Pour into moulds

and break out lead
button

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

74

Assay
results from
lab

INPUT

BATCH QAQC RESULTS

INTERPRETATION
PROCESS MAP

Compare lab
results to request
sheet

Contact lab and

obtain clarification

Criteria:
- Missing samples
- Extra samples
- Analytical schedule correct
- Reported decimals correct
- Lab QAQC data included

Results
consistent with
request?

No

Yes
Extract QAQC
control samples

Merge with
previous
standards

Merge with
previous blanks

Merge with core

duplicates

Plot control charts

Plot control charts

Plot X1 vs X2 and
calculate
regression, plot
diff vs mean

Criteria:
- Logic table of failures.
No

Criteria:
- Logic table of failures.
Data
acceptable?

Data
acceptable?

Yes

Obvious bias
present?

Criteria:
- If duplicates are
consitently lower or
higher in grade than
original assays.

Yes
No

Yes
Go to standard
failure flow chart

Go to blank failure
flow chart

Potential sampling
problem. Discuss
with drill geologist
and sampler

Do HowarthThompson
precision study

No

Total No.
duplicates >
50?

Yes

No

OUTPUT

Validated
Batch

Batch Accepted.
Merge data in
DDH assay
database

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

Criteria:
- Look for excessive RSD% near
cut-off grade.
- RSD% curve for core should
be higher than rejects and pulps.
Overall
precision poor?

Yes

Possible subsampling issues.

Contact Manager
Geochemistry

No

75

STANDARDS FAILURE
INTERPRETATION
PROCESS MAP

INPUT

Standard
failed

Criteria:
- Logic table of failures.
Blanks are
good?

Criteria:
- Logic table of failures.
No

Criteria:
- Logic table of failures.
Previous batch
failed on same
No
secondary
element?

Yes

No

Possible
contamination.
contact lab. Reanalyze coarse
reject

Criteria:
- Logic table of failures.

Primary
element
failure?

New results
good?

Yes

Contamination
probably from
pulverizer. Pass
re-analyzed batch.
Discuss with lab.

Yes
Contact lab. Reanalyze pulps

No

Contamination
probably from
crusher. Contact
Manager
Geochemistry

Yes

Pass batch

Contact lab. Reanalyze pulps

Problem
persists?

No

Pass re-analyzed
batch

Yes

Contact Manager
Geochemistry

Yes
Contact lab. Reanalyze coarse
rejects.

Problem
persists?

No

Pass re-analyzed
batch

Validated
Batch

OUTPUT

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

76

BLANK FAILURE
INTERPRETATION
PROCESS MAP

INPUT

Possible
contamination.
Contact Manager
Geochemistry

Blank
failure

No

Standards in
batch are
good?

Criteria:
- Logic table of failures.

Yes

Contact lab. Reanalyze pulps

Problem
persists?

Yes
Contact lab. Reanalyze coarse
rejects
No
Problem
persists?

Yes

Contact Manager
Geochemistry

No
Pass re-analyzed
batch. Discuss
failure with lab.

Validated
Batch

OUTPUT

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

77

Selection of sample
numbers from
previous batches

INPUT

PULP CHECK ASSAY

PROCESS MAP

Retrieve pulps

Assemble batch
with blanks and
standards

Ship to secondary
laboratory

Upon receipt of
results validate
QAQC data

Plot X1 vs X2
charts and
calculate
regression

Calculate paired
T-test on results

Compare bias with

results of predrilling laboratory
validation
Criteria:
- If observed bias near
standards values >> than bias
observed during lab testing.
Contact Manager
Geochemistry

Yes

Bias of pulps
>> validation
bias?

No

Yes

Any detectable
bias?

No

Plot Difference vs
Mean chart

Total No. of
pulp replicates
> 50?
Yes

OUTPUT

Verification
of check
assays

No action required

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

Criteria:
- If null hypothesis rejected.
- If break in slope present on on
X1 vs X2 plot.

Do HowarthThompson
precision study
Yes

Criteria:
- Look for excessive RSD% near
cut-off grade.
- RSD% curves for core and
rejects should be higher than
pulps.
Precision
acceptable?
No

Contact Manager
Geochemistry

78

COARSE CRUSH
REPLICATE STUDY
PROCESS MAP

Selection of
samples from
previous batches

INPUT

Retrieve coarse
rejects

Assemble batch
with blanks and
standards

Ship to primary
lab

Upon receipt of
results Validate
QAQC data

Plot Difference vs
Mean charts

Complete about 55
repeat analyses of
coarse crush rejects

No

Total No. of
coarse crush
replicates > 50
Yes
Undertake
HowarthThompson
precision study

Contact Manager
Geochemistry

No

Precision
acceptable?

Criteria:
- Look for excessive RSD% near
cut-off grade.
- RSD% curve for rejects should
be higher than pulp checks and
lower than core duplicates.

Yes
No more coarse
crush replicates
required

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

Precision of
crushing and
sub-sampling

OUTPUT

79

CRUSHER PARTICLE
SIZE ANALYSIS
EVALUATION PROCESS
MAP
Selection of sample
numbers from
previous batches

INPUT

Retrieve coarse
rejects

Submit to
secondary
laboratory for PSA
analysis

Upon receipt of data

plot %passing
10mesh vs date of
original analysis

Discuss crushing
history with
laboratory

Yes

Any changes
over time?

Criteria:
- Sudden change in PSA%
indicating change in sample
preparation conditions.

No
Calculate average
PSA and
percentage below
91%

Contact Manager
Geochemistry

No

Performance
acceptable?

Criteria:
- The average %passing should
be = 95%
- Fewer than 1 in 20 samples
with less than 91%passing

Yes

No action required

Acceptable
crusher
performance

OUTPUT

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

80

Selection of
samples from
existing pulps

INPUT

DELETERIOUS/BYPRODUCT ELEMENT &

ESH SAMPLING
PROCESS MAP

Determine list of
elements and
analytical methods

Select laboratory
and appropriate
standards

Submit samples to
lab for analysis

Discuss with
laboratory

No

QAQC data
acceptable?

Criteria:
- Use Standard failure flow chart
for guide to failure assessment.

Yes

Criteria:
- Target elements to be
determined with metallurgy,
mining, and ESH personnel.

Some samples with

unacceptable
values?

Yes

Criteria:
- Target elements to be
determined with metallurgy,
Some samples with
mining, and ESH personnel.
elevated
concentrations of
by-product
element(s)?

Contact
metallugist and/or
ESH specialist
and plan a
systematic
analysis program

No
Yes
Select a second
30 sample batch
near the end of
the program and
repeat

Plan a systematic
re-analysis program
for potential byproduct element(s)

Yes

OUTPUT

Assessment
of potential byproducts

Yes

Some samples with

unacceptable
values?

No

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

Criteria:
- Target elements to be
determined with metallurgy,
mining, and ESH personnel. No

No likely
deleterious or
ESH issues and
no potential byproducts

Assessment of
deleterious/
ESH elements
complete

OUTPUT

Some samples with

elevated
concentrations of
by-product
element(s)?

81

POST-DRILLING
CHECKLIST PROCESS
MAP

INPUT

Drilling
program
completed
Adequate No.
of core
duplicates?
Analytical
results for all
batches
received?

No

Contact
laboratories

No

No

Resolve issues or
contact Manager
Geochemistry

No

Upload data to
DDH database or
contact project
manager

No

Submit additional
pulps to
secondary lab

Yes
Adequate No.
of coarse
crush
replicates?

Conduct integrated variance

study and superimpose
replicate sets on RSD% vs
Grade diagram

Sampling for
metallurgy and
ESH
completed?

No

Complete
sampling and
interpret results

Complete retrieval
and storage of
pulps and coarse
rejects
Yes
Supervise storage
of core

Yes
Adequate No.
of pulp
replicates?

No

Yes

Yes
All results
uploaded to
DDH
database?

Integrated
variance study
completed?
Contact
secondary
laboratory

Yes
Any
outstanding
QAQC issues
unresolved?

No

Submit additional
core duplicates to
lab

Yes

Yes
Results of all
PSA batches
received?

No

Complete QAQC
report

Sampling
and analysis
process
complete

OUTPUT

Submit additional
coarse rejects to
lab

Noranda Inc. - Falconbridge Ltd.

QAQC Sampling and Analysis Protocols,
ver. 2.0, 2003

82

Appendix IV

List of Pulp Standards Prepared by Noranda and Falconbridge

The following is a list (clearly not exhaustive) of standards that have been manufactured
at different Noranda and Falconbridge sites in order to provide adequate accuracy
monitoring of batches. The data is printed from a small MSAccess database that will be
installed on the intranet and updated as new standards are manufactured. Any
information updates, corrections, or improvements are welcome.
If in need of one or more pulp standards you can scan the list and contact the Manager of
Geochemistry or the sites indicated in the header and referto the standard by name. It is
not kown however at this time how much material would be available for other projects.

83

Standard_ID

BA001(MRI73)

Material

Rock, Mineralized

Site

Matagami

Purpose

Pulp Standards for Matagami type deposits

Date_Manufacture

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Metallurgical

30

Se

464.3

ppm

32

6.89

Metallurgical

Te

543.9

ppm

17.6

3.23

Primary

Ag

39.571

gpt

2.11

5.34

Primary

Cu

1.6705

pct

0.0876

5.24

Primary

Pb

0.1164

pct

0.0072

6.19

Primary

Zn

11.17

pct

0.4566

4.09 Excellent Performance

Secondary

Au

0.91

gpt

0.1

11

84

Standard_ID

BA002(MRI72)

Material

Rock, Mineralized

Site

Matagami

Purpose

Pulp Standards for Matagami type deposits

Date_Manufacture

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Metallurgical

Se

348.1

ppm

37.6

10.8

Primary

Ag

28.488

gpt

2.22

7.78

Primary

Cu

1.1342

pct

0.0653

5.76

Primary

Pb

0.0856

pct

0.0064

7.42

Primary

Zn

5.78

pct

0.1114

1.93 Excellent performance

Secondary

Au

0.686

gpt

0.04

5.8 Omly one lab/. Not a true

standard.

85

Standard_ID

BM134

Material

Site

Brisbane

Purpose

Date_Manufacture

Rock, Mineralized

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Metallurgical

39

As

1449

ppm

97

6.7

Primary

47

Cu

6577

ppm

296

4.5 Excellent

Primary

46

Zn

153

ppm

10

6.5 Excellent

Secondary

43

Ni

107

ppm

13

12.1

Secondary

46

Pb

105

ppm

14

13.3

86

Standard_ID

BM135

Material

Site

Brisbane

Purpose

Date_Manufacture

Rock, Mineralized

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Metallurgical

39

As

541

ppm

35

6.5

Metallurgical

39

As

5975

ppm

290

4.9 Excellent

Primary

51

Cu

4624

ppm

249

5.4 Excellent

Primary

40

Ni

839

ppm

49

5.8 Excellent

Primary

45

Pb

1862

ppm

149

8.8 Acceptable

Primary

47

Zn

1058

ppm

64

6 Excellent

87

Standard_ID

BM153

Material

Site

Brisbane

Purpose

Date_Manufacture

Rock, Mineralized

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Primary

52

Cu

13900

ppm

698

Primary

49

Zn

259

ppm

23

8.9

Secondary

45

Ag

5.4

ppm

1.2

22.2

Secondary

42

Ni

83

ppm

10.8

Secondary

46

Pb

773

ppm

57

7.4

Comment

5 Excellent

88

Standard_ID

EM1

Material

Rock, Mineralized

Site

Santiago

Purpose

El Morro project

Description

Blank sample

Date_Manufacture

12/12/2001

Date_Validation

12/12/2002

Category

Primary

Number
Element
Laboratories
6

Au

Value

Units

0.0083

gpt

Standard
Deviation
0.0025

RSD%

Comment

30.4 Near detection limit. Do not

use.

Primary

Cu

0.006

pct

0.0003

4.2 Very low concentration.

Secondary

Mo

0.0006

pct

0.0002

34 Near detection limit. Do not

use.

89

Standard_ID

EM2

Material

Rock, Mineralized

Site

Santiago

Purpose

El Morro project

Description

Oxide zone

Date_Manufacture

12/12/2001

Date_Validation

12/12/2002

Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Au

0.2108

gpt

0.0199

9.5 Acceptable.

Primary

Cu

0.0133

pct

0.0006

4.41 Excellent. Very low grade.

Secondary

Mo

0.0048

pct

0.0006

13.6 Very low concentration. Use

with caution.

90

Standard_ID

EM3

Material

Rock, Mineralized

Site

Santiago

Purpose

El Morro project

Description

Supergeme enriched zone

Date_Manufacture

12/12/2001

Date_Validation

12/12/2002

Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Au

0.319

gpt

0.0022

6.98 Excellent

Primary

Cu

1.0639

pct

0.0311

2.92 Excellent.

Secondary

Mo

0.0047

pct

0.0007

14.2 Very low concentration. Use

with caution.

91

Standard_ID

EM4

Material

Rock, Mineralized

Site

Santiago

Purpose

El Morro project

Description

Cutoff grade hypogene

Date_Manufacture

12/12/2001

Date_Validation

12/12/2002

Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Au

0.195

gpt

0.011

5.85 Excellent

Primary

Cu

0.313

pct

0.008

2.53 Excellent

Secondary

Mo

0.0047

pct

0.0006

13.6 Near detection limit. Poor

standard.

92

Standard_ID

EM5

Material

Rock, Mineralized

Site

Santiago

Purpose

El Morro project

Description

Average grade hypogene

Date_Manufacture

12/12/2001

Date_Validation

12/12/2002

Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Au

0.601

gpt

0.033

5.42 Excellent

Primary

Cu

0.621

pct

0.01

1.65 Excellent

Secondary

Mo

0.0012

pct

0.0005

41.7 Near detection limit. Do not

use.

93

Standard_ID

EP1

Material

Rock, Mineralized

Site

Santiago

Purpose

Pulp standard for El Pachon

Date_Manufacture

12/12/2002

Date_Validation

12/12/2002

Category

Number
Element
Laboratories

Description

Value

Units

Primary

Cu

0.947

pct

Secondary

Au

36.8

ppb

Secondary

Mo

0.0008

pct

Standard
Deviation
0.015
4.4
0

RSD%

Comment

1.59 Excellent
12 Acceptable
0 Near detection limit. Do not
use.

94

Standard_ID

EP2

Material

Rock, Mineralized

Site

Santiago

Purpose

Pulp standard for El Pachon

Date_Manufacture

12/12/2002

Date_Validation

12/12/2002

Category

Number
Element
Laboratories

Description

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Cu

1.268

pct

0.029

2.3 Excellent

Secondary

Au

31.55

ppb

3.38

10.7 Acceptable

Secondary

Mo

0.0095

pct

0.0005

5.3 Near detection limit. Do not

use.

95

Standard_ID

EP3

Material

Rock, Mineralized

Site

Santiago

Purpose

Pulp Standards for El Pachon

Date_Manufacture

12/12/2002

Date_Validation

12/12/2002

Category

Number
Element
Laboratories

Description

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Cu

1.727

pct

0.061

3.55 Excellent

Secondary

Au

31.56

ppb

16.66

42.1 Poor.

Secondary

Mo

0.036

pct

0.002

4.96 Excellent

96

Standard_ID

GBM3008

Material

Site

Navan

Purpose

Date_Manufacture

Rock, Mineralized

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Pb

9590

ppm

588

6.13 Good

Primary

Zn

30249

ppm

1937

6.4 Good

Secondary

Cu

123

ppm

6.5 Excellent

97

Standard_ID

GBM3998

Material

Site

Navan

Purpose

Date_Manufacture

Rock, Mineralized

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

ppm

Primary

Zn

280072

Secondary

Cu

124

Secondary

Pb

13817

ppm

Standard
Deviation

RSD%

Comment

17075

6.1 Good

10

8.06 Good

657

4.75 Excellent

98

Standard_ID

GBM9967

Material

Site

Navan

Purpose

Date_Manufacture

Rock, Mineralized

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Cu

23362

ppm

1596

6.83 Good

Primary

Pb

39189

ppm

2818

7.19 Good

Primary

Zn

110402

ppm

5910

5.35 Excellent

99

Standard_ID

MR1

Material

Rock, Mineralized

Site

Raglan

Purpose

For chromitite-type PGE deposits

Description

Merenski reef

Date_Manufacture

12/12/2002

Date_Validation
Category

Metallurgical

2/1/2002

Number
Element
Laboratories
1

As

Value

1.6

Units

ppm

Standard
Deviation
0.37

RSD%

Comment

23.8 Near detection limit. Do not

use.

Metallurgical

Pb

3.5

ppm

1.3

37.5 Poor standard. Do not use.

Metallurgical

782

ppm

111

14.2 Poor agreement between labs.

Use with caution.

Metallurgical

Zn

66

ppm

8.32

12.6 Near detection limit. Do not

use.

Primary

Au

46

ppb

3.6

7.9 Good

Primary

Cu

150

ppm

11

7.3 Good

Primary

Ni

583

ppm

25

4.4 Excellent

Primary

Pd

281

ppb

18

6.5 Excellent

Primary

Pt

654

ppb

52

7.9 Good

Secondary

Ag

0.1

ppm

0.04

39.2 Near detection limit. Do not

use.

Secondary

Co

66

ppm

4.9

Secondary

Cr

2849

ppm

607

7.5 Good
21.3 Poor recovery compared to
INAA. Poor standard.

100

Standard_ID

MR2

Material

Rock, Mineralized

Site

Raglan

Purpose

For chromitite-type PGE deposits

Description

Merenski reef

Date_Manufacture

12/12/2002

Date_Validation
Category

Metallurgical

2/1/2003

Number
Element
Laboratories
0

As

Value

3.7

Units

ppm

Standard
Deviation
2.1

RSD%

Comment

56 Poor standard. Low

concentration. Do not use.

Metallurgical

Pb

59

Metallurgical

1358

Metallurgical

Zn

112

ppm

0.88
147

ppm

19

14.9 Poor standard. Low

10.8

concentration. Use with

caution.
Accaptable

16.6 Poor standard. Low

8.6

concentration. Use with

caution.
Good

Primary

Au

81

ppb

Primary

Cu

257

ppm

17

6.5 Excellent

Primary

Ni

803

ppm

30

3.8 Excellent

Primary

Pd

542

ppb

36

6.6 Excellent

Primary

Pt

1304

ppb

75

5.7 Excellent

Secondary

Ag

0.15

ppm

0.03

22.4 Poor standard. Near detection

limit. Do not use.

Secondary

Co

7.5

ppm

5.4

Secondary

Cr

5444

ppm

1214

7.1 Good
22.3 Poor recovery compared to
INAA. Poor standard. Use
with caution.

101

Standard_ID

MR3

Material

Rock, Mineralized

Site

Raglan

Purpose

For chromitite-type PGE deposits

Description

Merenski reef

Date_Manufacture

12/12/2002

Date_Validation
Category

Metallurgical

2/1/2003

Number
Element
Laboratories
2

As

Value

4.8

Units

ppm

Standard
Deviation
4.9

RSD%

Comment

101 Poor standard. Near detection

limit. Do not use.

Metallurgical

Pb

5.2

ppm

0.2

3.8 Poor standard. Near detection

limit. Do not use.

Metallurgical

3289

Metallurgical

Zn

103

ppm

414

12.6 Acceptable

19.6

18.6 Poor standard. Low

6.5

concentration. Use with

caution.
Excellent

Primary

Au

182

ppb

11.9

Primary

Cu

637

ppm

39

6.2 Excellent

Primary

Ni

1527

ppm

59

3.8 Excellent

Primary

Pd

1031

ppb

77

7.4 Excellent

Primary

Pt

2774

ppb

171

6.2 Excellent

Secondary

Ag

0.27

ppm

0.03

9.9 Poor standard. Near detection

limit. Do not use.

Secondary

Co

93

ppm

5.6

Secondary

Cr

6708

ppm

1167

6 Excellent
17.4 Poor recovey compared to
INAA. Use with caution.

102

Standard_ID

ST205

Material

Site

Brisbane

Purpose

Date_Manufacture

Rock, Mineralized

Description

Date_Validation
Category

Primary

Number
Element
Laboratories
81

Au

Value

1.48

Units

gpt

Standard
Deviation
0.06

RSD%

Comment

4.05 Excellent

103

Standard_ID

ST292

Material

Site

Brisbane

Purpose

Date_Manufacture

Rock, Mineralized

Description

Date_Validation
Category

Primary

Number
Element
Laboratories
82

Au

Value

0.41

Units

gpt

Standard
Deviation
0.04

RSD%

Comment

9.76 Good

104

Standard_ID

StrathA

Material

Site

Sudbury

Purpose

Date_Manufacture

12/12/2002

Date_Validation

12/12/2002

Category

Number
Element
Laboratories

Rock, Mineralized

Description

Value

Units

Standard
Deviation

RSD%

Comment

Metallurgical

5.72

pct

0.28

Primary

Cu

5.21

pct

0.09

1.72 Excellent performance

Primary

Ni

0.3

pct

0.01

3.33

Primary

Pd

1.83

gpt

0.19

10.4

Primary

Pt

1.12

gpt

0.15

13.4

Secondary

Au

0.37

gpt

0.08

21.6

Secondary

Co

0.0007

pct

0 Below detection limit. Do not

use as standard.

105

Standard_ID

StrathB

Material

Site

Sudbury

Purpose

Date_Manufacture

12/12/2002

Date_Validation

12/12/2002

Category

Number
Element
Laboratories

Rock, Mineralized

Description

Value

Units

Standard
Deviation

RSD%

Comment

Metallurgical

28.7

pct

0.74

2.58

Primary

Cu

25.3

pct

0.36

1.42

Primary

Ni

0.93

pct

0.02

2.15

Primary

Pd

7.54

gpt

0.29

3.85

Primary

Pt

3.52

gpt

0.28

7.95 Excellent performance

Secondary

Au

0.18

gpt

0.03

16.7

Secondary

Co

0.016

pct

0.003

18.8 Very low grade. Poor percision.

Do not use.

106

Standard_ID

ZnHigh

Material

Rock, Mineralized

Site

Bathurst

Purpose

For Bathurst camp deposits

Date_Manufacture

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Ag

173.2

gpt

9.9

5.7

Primary

Cu

0.5378

pct

0.0158

2.93 Excellent performance

Primary

Pb

5.4713

pct

0.1345

2.46

Primary

Zn

13.5338

pct

0.228

Secondary

Au

683.2

ppb

67.3

1.68 Exce;;ent Performance

9.85

107

Standard_ID

ZnLow

Material

Rock, Mineralized

Site

Bathurst

Purpose

for Bathurst camp deposits

Date_Manufacture

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Primary

Ag

35.076

gpt

3.983

Primary

Cu

0.1111

pct

0.0044

Primary

Pb

1.1152

pct

0.028

2.53

Primary

Zn

2.7529

pct

0.0982

3.57

Secondary

Au

148.5

ppb

12.94

8.66

Comment

11.4
3.92 Excellent performance

108

Standard_ID

ZnMed

Material

Rock, Mineralized

Site

Bathurst

Purpose

For Bathurst camp deposits

Date_Manufacture

Description

Date_Validation
Category

Number
Element
Laboratories

Value

Units

Standard
Deviation

RSD%

Comment

Primary

Ag

86.6

gpt

3.97

4.58 Excellent performance

Primary

Cu

0.2642

pct

0.0077

2.9 Excellent performance

Primary

Pb

2.7093

pct

0.0679

2.51

Primary

Zn

6.713

pct

0.2094

3.12 Excellent performance

Secondary

Au

350.1

ppb

24.01

6.86

109

110

Appendix V

Laboratory Audit Guidelines

Sample Preparation
Lab Name :
Equipment required for audit:
- Flashlight
- Digital camera
- Ruler/measuring tape
- Protractor/compass
- Notebook
Building
- Security
- Safety
- Location
- Address
- Access
Manager
- Name
- Phone
Sample Receiving and Sorting
- Organization of work space
- Work order book
- LIMS?
Sample Preparation
- Space
- Cleanliness/Dust level during visit
Dust Control system
- Description
Drying Facility
- Description of ovens, number
- Heat source
- Capacity
- Description of drying procedures
Crusher equipment
- Types/Models and number
- For each machine:
- Condition
111

- Sieve attachment present?

- Description of crushing procedures
- Dust control
- Type of reject bags
Pulverizer equipment
- Types/Models and number
- For each machine:
- Condition
- Description of pulverizing procedures
- Dust control
- Type of pulp bag
Cleaning material for crusher and pulverizer
- Source
- Scheduled usage
Splitters
- Types and number
- For each splitter:
- Overall length and width
- Vane spacing
- Angle of chute
- Description of splitting procedure
- Dust controls
Air hoses and compressor
- Air pressure

Preparation QC methods
- Frequency of preparation duplicates
- Crusher
- Pulverizer
- Frequency of PSA tests
- Coarse rejects
- Pulps
- QC log book for preparation
- Specifications for crusher
- Specifications for pulverizer
- Control charts plotted?
Preparation blanks
- Source
- Frequency of analysis
- Analysis of wash material?

112

Analytical Laboratory
Lab Name :
Equipment required for audit:
- Digital camera
- Notebook
- Pulp Standards to be submitted
Building
- Security
- Safety
- Location
- Address
- Access
Manager
- Name
- Phone

Fire Assay
Description of Facilities:
Fusion Furnaces:
Number:
Size:
Condition:
Cupel Furnaces:
Number:
Size:
Condition:

Source of litharge:
Method of mixing:
Method of order control:
Method of inquart:
Ventilation and Safety:

113

Management of crucibles (reject levels):

Wet Chemistry
Distilled Water:
Calibration/testing:
Hot Plates:
Auto-pipettes:
Make:
Calibration:
Glassware:
Instruments:
Makes and Models:
Calibration Standards:
Weighing Room:
Balances (makes and models):
Room isolated?
Balance tables?
Calibration:
Frequency:
Warehouse and Storage:
Pulps:
Rejects:
Organization:
Quality Control Methods:
Standards:
Frequency:
Round Robin Limits:
In house Standards:
Preparation Duplicates:
Frequency Analyzed:
Pulp Duplicates:
114

Frequency Analyzed:
Blanks:
Frequency Analyzed:
Laboratory QC Manager:
Usage of control charts:
Reporting:
LIMS?
Database?
Fax/E-mail?
Custom reporting formats?
Personnel:
Total:
No trained technicians:
No. shifts:
Description of procedure used for samples:

115