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ASSAY QUALITY ASSURANCE-QUALITY CONTROL PROGRAM

FOR DRILLING PROJECTS AT THE PRE-FEASIBILITY TO FEASIBILITY REPORT


LEVEL (3rd edition)

Scott D. Long
Mineral Resources Development Inc.
1710 So. Amphlett Blvd., Suite 302
San Mateo, California 94402, USA
Tel: (650) 358-1116
Fax: (650) 349-2111
email: scott.long@agra.com; geochemist_qaqc@yahoo.com
September 2000

Mineral Resources Development Inc., U.S.A. 650 358-1116


SUMMARY OF CONTENTS
ASSAY QUALITY ASSURANCE-QUALITY CONTROL PROGRAM
FOR DRILLING PROJECTS AT THE PRE-FEASIBILITY TO FEASIBILITY REPORT
LEVEL

1.0 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
2.0 Definitions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
2.1 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
2.2 Sample Duplicates and Duplicate Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.3 Sampling Definitions by Gy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.4 Precision and Related Concepts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.5 More on Significant Figures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
3.0 Laboratories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.1 Selecting a Primary Lab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.2 Selecting an Umpire or "Check" Lab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
4.0 Obtaining or Making QA-QC Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
4.1 Standard Reference Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
4.2 Commercial Certified Standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
4.3 Creating Customized ("In House") Standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
4.4 Blanks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
4.5 Duplicate Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
5.0 Inserting Controls into Batches of Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
5.1 Batch Submissions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
5.2 Suggested Amounts of QA-QC Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
5.3 Maintaining the Anonymity of QA-QC Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
6.0 Quality Control Procedures and Criteria . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
6.1 The Concept of Accepting or Rejecting Batches . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
6.2 Types of Errors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
6.3 Identifying Outliers in Populations of Duplicate Results . . . . . . . . . . . . . . . . . . . . . . . 35
6.4 Deriving a Pass-Fail Look-up Table from Identified Outliers . . . . . . . . . . . . . . . . . . . . 36
6.5 Laboratory Drift . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
6.6 Practices to Monitor Quality . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
6.7 Suggested Levels of Accuracy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
6.6 Suggested Levels of Precision . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
7.0 Analysis and Presentation of QA-QC Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
8.0 Data Transfer Errors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
9.0 Common Mistakes and Pitfalls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
9.1 Lack of Vigilance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
9.2 Loss of Fines or Water-soluble Ore Minerals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
9.3 Mishandling of Standard Reference Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
9.4 Introducing Selection Bias . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
9.4 Preserving the Integrity of the Raw Assay Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
10.0 Quality Control of The Geologic Database . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
11.0 Geotechnical Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
11.1 Drilling Recovery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57

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11.2 Down-hole Contamination in Reverse-circulation Drilling . . . . . . . . . . . . . . . . . . . . . 57
11.3 Down-hole Surveys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
11.4 Bulk Densities . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
12.0 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

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1.0 INTRODUCTION

Resource estimation can be likened to a "house of cards" that has a foundation of sampling and
geological observation, with a first floor of sample preparation and geological classification, a second
floor of chemical analysis and geological interpretation, and a top floor consisting of geostatistics and the
resource model. Establishing levels of performance is a goal-oriented exercise which should be carefully
done at the outset and reviewed at appropriate intervals. Overly stringent quality requirements waste
money, since per-sample costs will be higher, while lax requirements tend to lose it, because work may
need to be re-done, including "downstream" work that is based upon flawed data.

The goals of a good QA-QC program are:

1. to prevent the entry of large errors into the database used for resource modelling,
2. to demonstrate that sampling and analytical variances are small, relative to the geological
variance, and
3. to provide assurance that the accuracy of data underlying the resource model can be confirmed,
within reasonable limits, by other laboratories, metallurgical testing, and ultimately, by mill and
mine production.

A feasibility document must include supporting evidence (quality assurance) that the data used to
construct the resource model are valid. Important data categories include assay, geological, and
geotechnical. This document focuses on assay quality, but touches upon a few geological and
geotechnical considerations.

Besides the fact that Quality Assurance - Quality Control (QA-QC) is a requirement for producing a
complete feasibility document, it also has intrinsic benefits. Quality Assurance provides a measurement of
the uncertainty in the underlying data. If the assay results can be demonstrated to be highly reliable, one
of the risks attached to the project is reduced, which may ultimately lead to more favorable financing or,
in the case of an internally funded project, a higher priority in relation to other projects considered by a
companys board of directors. More commonly, the lack of adequate Quality Assurance leads to delays
in project financing and development, while such evidence is collected, that adds to the cost of bringing
the project into production.

To the extent that Quality Control leads to corrections of errors or changes in procedures that improve
overall data quality, it may help produce a resource model that can categorize more ore as "measured and
indicated" (as opposed to "inferred") for a given drill hole spacing. This in turn may allow wider spacing
of additional drill holes. Such benefits can only be realized if Quality Control is done in a timely fashion.
Too often, the most cost-effective sampling and preparation procedures are not selected, and corrections
to the assay results are not completed, before modelling decisions are made on the basis of the available
data, regardless of its quality. Very often, quality control results are not analyzed, and no remedial
actions are taken, or are taken at such a late stage in the program that they incur delays.

The goal of a QA-QC program is to demonstrate and maintain good accuracy and adequate precision for
ore-grade samples. QA-QC programs are designed to monitor precision (reproducibility), and quantify

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any possible biases (accuracy). Emphasis should be placed on presenting a clear picture of the reliability
of the assay data, so that it can be demonstrated that there is a good match between the procedures used
in construction of the resource model, and the quality of the data used in that model.

There is a dichotomy between the analytical requirements of early-stage "grass roots" exploration and
resource definition that is sometimes overlooked. Grass-roots exploration requires high precision on low
concentrations and is more frequently concerned with results near the analytical detection limit. Because
most exploration samples are below ore-grade, there is less need to measure ore-grade samples accurately
on the initial analysis, because such samples make up a very small fraction of the samples tested and can
therefore be routinely re-analyzed at little additional cost. This allows the explorationist to confirm the
accuracy of "anomalous" values prior to engaging in the costly procedure of re-visiting and re-sampling
anomalous sites. Such selective re-assaying is appropriate in such cases, because the goal is to identify
anomalies, not to quantify ore grades.

In contrast, drill samples collected during resource definition ("in-fill drilling") are in many cases
predominately ore-grade, and many of the results below the ore-grade cutoff would usually be considered
anomalous in an exploration context. Hence the practice of re-analyzing samples with high values is no
longer practical nor appropriate. Biased estimates of average grade may be obtained in cases where
samples are selected for re-assay solely on the basis of their initial assay; this will be referred to as
selection bias, and will be discussed in detail later.

The following discussion mostly uses examples taken from QA-QC in gold drilling projects. Most of the
rules of thumb used here are applicable for establishing programs for other non-industrial minerals. The
levels of QA-QC suggested in this paper are sufficient to fulfill the requirements sought in most feasibility
studies presently performed. It is important to note that, as methods of sampling, assaying, and
processing data continue to improve, the requirements of feasibility studies can be expected to become
more stringent; the level of quality that needs to be demonstrated is dependent upon what is reasonably
obtainable, and this is changing.

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2.0 DEFINITIONS

2.1 General

In the context of this paper, Quality Assurance is information collected to demonstrate and quantify the
reliability of assay data. Quality Control consists of procedures used to maintain a desired level of quality
in the assay database. Quality Assurance can, to a certain extent, be added later in a program. Quality
Control, like safety, can only be performed in real time.

Thorough Quality Assurance - Quality Control (QA-QC) programs are intended to monitor routine
sampling and laboratory performance in an effort to control (minimize) the total possible error in the
sampling-splitting-analysis sequence. QA-QC on sampling and assaying is achieved by monitoring and
controlling four essential components of that sequence:

Field sample collection and splitting.


Laboratory sample preparation and sub-sampling (splitting).
Analytical accuracy and precision.
Reporting (clerical or data transfer) accuracy.

Sampling and assaying QA-QC programs integrate a program of routine insertion of quality control
materials, at several critical stages of sample collection, preparation and assaying, with analytical
determinations performed at a number of laboratories:

The routine insertion of quality control materials involves a number of different types of quality
control materials to monitor and measure laboratory performance. These include:
- standard reference materials (SRMs),

- blank material, consisting of material devoid of the element(s) or commodity of


economic interest, or devoid of a contaminant affecting a processing cost or
decision,

- duplicate samples.

A number of laboratories are used: the primary laboratory assays all of the samples. The results
of the primary laboratory are used. Projects of long duration or large size sometimes have several
different primary laboratories. Having more than one primary laboratory should be avoided if
possible, because it adds complexity to evaluating data quality, and introduces small (and
sometimes large) biases that are detrimental in the process of analyzing the data. The same is true
for major changes in analytical protocol at the same laboratory. Other, secondary laboratories,
analyze some of the samples to validate the primary laboratory results; when done in a timely
fashion, these provide a method of exercising quality control on the primary laboratory.

In practice, a QA-QC program is maintained by routine submission to the primary laboratory of project
("original) samples that are accompanied by blind intercalation of QA-QC materials. Blind means that

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the materials used to assess the laboratorys performance are indistinguishable from the submitted
samples, preventing such controls from receiving special treatment at the laboratory. Special treatment at
the laboratory can be as seemingly innocuous as the laboratory observing the performance of the clients
inserted standards, and deciding to re-run batches of the samples where the agreement appears poor; this
prevents the laboratorys client from obtaining an independent measure of the laboratorys performance.
All reputable commercial laboratories have their own internal quality control measures, and have no need
to incorporate their clients independent assessment of that performance.

Check assays are performed by the secondary (umpire) laboratory on a representative sampling of
previously analyzed pulps or other reject material. The combination of results from inserted standards
and check assays should be used by the project manager to accept or reject results from laboratory
batches of samples from the primary lab. It is widely accepted practice to stipulate that the check
laboratory use a similar method and sample size to that in use by the primary laboratory. The use of
umpire quality assays for the check assays is costly and is very seldom called for, except in cases where a
third opinion is called for and there are reasons (such as risk of legal action) to justify the expense.

There are two components to setting performance level goals, regardless of what is being analyzed.
Precision is the ability to consistently reproduce a measurement. Accuracy is closeness (on average) of
those measurements to the "true" value. A modern watch is more precise than a sundial at measuring
time, but the sundial will be more accurate if the watch is set for a location eight time-zones away. The
true value is never known, but in practice can usually be estimated to a sufficient level of confidence, or
confidence interval. A commonly used confidence interval is that corresponding to 95 percent; this is
the interval (plus or minus) around the mean that has a 95 percent chance of including the true value.
This 95 percent confidence interval is sometimes referred to as the standard error of the mean.

Another oft-used analogy is the shooting target, or bulls eye. If the pattern of arrows or bullet holes is
tightly grouped, the shooting is said to be precise, even if it is not centered on the bulls eye: the
observer can predict with some confidence the area in which the next shot is likely to strike. To be
accurate, the shots should be scattered evenly around the bulls eye, even if they are not tightly clustered.
When the arrows become more widely scattered about a bulls eye, it becomes increasingly difficult to
state with confidence that the shooting is accurate. Thus there is a connection between accuracy and
precision: if precision is poor, more measurements (i.e., more samples) are required to achieve an
accurate result, or an assessment of the accuracy of a set of results. Any demonstration that a set of
results is unbiased, or any effort to quantify a bias, has an uncertainty (a confidence interval) that is
related to precision of measurements.

2.2 Sample Duplicates and Duplicate Results

There is a lack of consensus in North America in what can be considered to be a duplicate sample, and
very often a lack of appreciation of the necessity of providing adequate descriptions of different types of
duplicate samples, and analyzing their results separately. There are a few fundamental principles which
the author believes should be honored in using the term duplicate:

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A duplicate sample has the same spatial location as the original sample. Thus the second
half of a drill core, even if taken on the same interval, is not strictly a duplicate because
it has a different, albeit small, location difference. The same is true of underground
channel and trench samples. These are sometimes referred to as re-sampling or twin
samples (most twins are not identical twins!) rather than duplicates. Similarly,
exploration geochemists sometimes collect field duplicates that are actually very closely
spaced samples. Duplicates can only be made by splitting representative samples from
broken ores because anything else has a spatial component.

An assay result may be said to duplicate another if the distinction between the original and
the duplicate sample is believed to be arbitrary. This circumstance is usually only
encountered where a laboratory analyzes a second sub-sample of the pulp within the same
batch. Some commercial laboratories refer to this as a replicate; because this term is not
widely used to refer to anything else, it is arguably a better term to use. It is better to
refer to check assays of sample pulp duplicates as same-pulp check assays, rather than as
duplicate results. Some measurable bias often exists between assay results performed by
different laboratories or different protocols within the same laboratory. Arbitrarily
swapping the duplicate and original results cannot be done, distinguishing these from
replicates. In some cases one discovers that, even though original and duplicate samples
have reportedly been processed in exactly the same way, there is a significant (i.e. real)
bias; this means the sample collection and preparation protocols are not providing
representative samples, a red flag!

Duplicates should be further described by the step in the process where they are collected. Duplicates
can only be made where a step in the process reduces the mass of the sample by taking a sub-sample (i.e.
the sample is split). In the case of field duplicates this requires the sample be split prior to processing.
This is commonly done in reverse-circulation drilling by collecting a second split (preferably of the same
size) of the uncollected portion of the drill cuttings.

Usually three types of sample duplicates can be made:

Pulp Duplicates: These are splits, or submission of the unused portion, of the sample pulps used
for the original assay. The splits are sent to the umpire laboratory, and can also be re-labeled and
resubmitted to the primary laboratory with a different sample number, and accompanying a
different batch of samples. These provide a measure of the accuracy of the initial determination
performed by the primary laboratory, and an estimate of the analytical variance + pulp sub-
sampling variance. Often the pulp splitting step is poorly done, which may impact results in the
case of gold assays with gold particles larger than about 20 microns.

Coarse-reject duplicates: These are splits taken at the point where the sample size (weight) is
first reduced; this often occurs after crushing the drill sample to -10 mesh. These splits are best
analyzed by the primary laboratory, as a check on the adequacy of the sample preparation. These
duplicates provide a measure of the variance included in the check laboratory duplicates, plus the
variance introduced by the sample preparation procedures, plus the sub-sampling variance of the

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coarse reject. Other names include: second pulps, resplits. In circumstances where more than
one crushing and splitting stage is used (for example, crush to -10 mesh, split, crush to -40 mesh,
split) the crush stage should be stated, e.g. -10 mesh resplits or second pulps from -40 mesh
reject..

Field (Drill Rig) Duplicates: These are duplicate splits (often c splits) collected at the drill site in
the case of rotary drilling. They should be given unique sample numbers on-site (or a suffix, such
as "A"). If carefully collected and analyzed at the same laboratory by the same procedure, these
splits can provide an estimate of the variance contributed by the entire sample collection,
preparation, and assaying process.

One other factor worth considering in special situations is whether the duplicates are processed together
in the same batch, or are run in separate batches. A comparison of same-batch versus different-batch
duplicates can be used to check for erratic laboratory performance. This is rare, and is seldom done
unless other information, such as performance on inserted standards, leads one to believe a problem
exists.

Here are some examples of adequate duplicate descriptions:

Laboratory replicates consist of duplicates created by the laboratory (non-blind) for use in their quality control,
consisting of 30 grams of P-95 150# material taken from the same pulp envelope as the original sample. These
were reportedly run in the same furnace load. Because the laboratory bases its decision on whether to release its
data in part on how well these duplicates agree, this duplicate performance shows what the laboratory considers
acceptable performance for this material and protocol. Because bad results are excluded in this process, these
performance data may indicate better performance than would be obtained by blind duplicate samples of the same
type.

These coarse reject duplicates consist of second riffle splits of the reject portion of jaw crusher output, found by
screen tests (see graph) to be approximately P-95 1/4 inch (median percent passing 10# was 78%), weighing
between 400 and 800 grams. Samples were re-labeled so that the laboratory did not know which sample was being
duplicated. These samples were submitted in the same shipment as their matching original samples, but are not
necessarily placed in the same furnace load as the matching original sample.

Rig duplicates consisted of collection of the entire rejected portion from a Gilson splitter used at the drill site (in
the case of dry samples) or from a rotating cone splitter (in the case of wet samples) mounted on the drill rig. In
the case of dry duplicates, the entire reject was passed through the Gilson splitter and then split repeatedly to
obtain a second (duplicate) sample of the same approximate mass (4 to 8 kg) as the original sample. Wet
duplicates were sent to the preparation facility for drying, after which they were split with a riffle splitter to
approximately the same sample mass as the original samples. Screening of 10 of the rejects selected at random
showed dry samples to be approximately P-95 3/4 inch and wet samples to be about P-95 inch.

2.3 Sampling Definitions by Gy

Pierre Gy (pronounced similar to, and rhymes with she), founder of modern sampling theory, provides
the following definitions:

Lot the total collection of material for which it is required to estimate some component.

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Component the property that we require to estimate using the sample, such as the grade.

Sample the part of a lot on which a determination of a component will be carried out, where each
part of the lot had an equal probability of being selected into the sample. Thus a sample
is representative of the lot.

Specimen part of a lot on which a determination of a component will be carried out, but for which
the rule of equal probability of selection has not been respected.. Measurements
performed on specimens cannot be used to typify the lots from which the specimens were
selected.

Increment some fraction of a sample (can be 1), selected from the lot with a single cut of the
sampling device. A number of increments may be combined to form one sample.

Twin Set of two or several intermediate samples of the same rank, obtained in similar
conditions, at the same time, often as the result of the splitting of a unique intermediate
sample. The relative difference between the mass and composition of the twin samples is
a random variable with zero mean. In commercial sampling, twin samples are distributed
to the parties, umpires, etc., or kept

These definitions are in some cases slightly different than those in commonly used in North America. For
example, the term twin is usually applied to drill holes that are drilled very near to another drill hole; Gys
twin is MRDIs duplicate; a lot is often called a batch; an increment is often called a split. Note the very
useful distinction between a specimen and a sample; because this distinction is not always made, one
sometimes sees the term representative sample (redundant in Gys nomenclature) to distinguish it from
samples that are actually specimens. In Gys parlance, a specimen cannot be used to estimate a
component of a lot.

2.4 Precision and Related Concepts

A first course in chemistry might introduce the topic of precision in terms of measurement error on
weighing some material. Supposing a balance provides readings in increments of 0.01 grams and one
wants to determine the moisture content of a sample. One weighs out 15.00 grams. In this first year
course, they tell you the uncertainty on that weight is 0.01 gram, the resolution of the balance, and that
is how you are instructed to write this in your lab book: 15.00 0.01. Your weight has four significant
figures: the number of meaningful digits. If you had written 15.000, you would be implying that you had
five significant figures, which is incorrect, as would 15.0, which is three. Thus the number of significant
figures has a connection with the implied precision.

After drying the sample and weighing it again, you obtain a weight of 14.91 grams, which is entered in
your lab book as 14.91 0.01. In this first-year course, they tell you to calculate the difference and add
the errors, from which you obtain 0.09 0.02. Everything has changed: your answer has only one
significant figure with a large error attached to it. Now you need to calculate the percent moisture

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content by dividing 0.09 by 15.00, which equals 0.6%, or is it 0.60% or 0.600%, and what is the error?
The units are in percent; you cannot use units of grams to express the error. The errors must be
converted into relative errors, which are expressed as percentages, so that they are independent of the
units. This is accomplished by dividing the error by the measurement. Thus 0.09 0.02 grams becomes
0.09 grams 22%, and 15.00 0.01 grams becomes 15.00 grams 0.0667%. The error on the moisture
content is then (0.0667+22)% which is still 22%, and the number of significant figures is determined by
the item that has the fewest, and is therefore one.

Although the answer is substantially correct in the above example, the methodology is in fact incorrect,
and a correct estimate of error using the above approach is only obtained in cases where one of the terms
has a much larger relative error than all the others. In all other cases, the estimated relative error
obtained by the above method of estimation will be much larger than the actual error produced by the
balance. The errors (estimates of precision for each measurement) stated as relative percentages are not
additive. Variances are additive, and these are proportional to the sum of squares of the percentages.
Thus a better estimate of the error (precision) in the above example is

s [(.00667)2 + (.22)2 ]

which is approximately

s(.22)2 = .22 or 22%.

Thus in this case, the method gave a correct result. It would not have given a correct result if the relative
errors were similar. For example, consider a case where, after drying the 15.00 0.01 gram sample, the
weight of the remaining material is 8.00 0.01 grams. Now the relative errors are .0667% and 0.125%.
Adding these together provides an error of .067+.125 = 0.19% which differs from taking the square root
of the sum of the squares,

s[(.00667)2 + (.00125)2 ] = 0.14%.

The other flaw in the laboratory exercise is slipped in right at the outset: the assumption that there is a
constant measurement error of 0.01 produced by the balance. This is unlikely to be so. If one wants to
know what the error actually is, one would need to take many measurements (of the same sample) and
obtain a distribution of the results. For the initial sample weight, there would be a lot of measurements
equal to 15.00, 15.01 and 14.99, plus a lower incidence of weights like 14.98 and 15.02. This is
sometimes a useful exercise to perform on gold balances, to see how reproducible the weighing is on
small beads.

The distribution of the weights about 15.00 grams would be roughly symmetrical, if plotted graphically as
a histogram. Whats the precision? If one uses the entire range of values obtained, the stated precision is
more a function of how many measurements one makes rather than anything intrinsic in the weighing
process. Consequently, it is better to use some other proportion of the population rather than 100
percent (the range of measurements).

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The most common convention is to express the precision in terms of standard deviations, sometimes
referred to as sigma (F).. It is important to remember that this is a convention, albeit one that has some
mathematical reasons behind it, and even within the context of the convention, precision is often
expressed in terms of some multiple of standard deviations other than one.

A statement of precision (e.g. 20%) without reference to the number of standard deviations (or
percentile) of the population associated with that precision, has no meaning.

The range determined by the mean plus or minus one standard deviation encompasses about 68 percent of
the population. Plus or minus two sigma encompasses about 95 percent. Plus or minus three sigma
encompasses about 99.8 percent. Another commonly used range is 1.65 standard deviations, because this
corresponds to 90 percent of the population. Another that will arise in this document, is 1.414 sigma,
which encompasses about 84 percent of the population. The number 1.414 comes from the square root
of two, which crops up often when dealing with pairs of duplicate results.

Precision becomes poorer for measurements of grade close to the analytical detection limit, a value set by
the assay laboratory for its analytical procedure; samples with concentrations (grades) below the
detection limit cannot be quantitatively measured with that analytical procedure, and are reported as less
than detection. These are often reported on assay certificates as the detection limit preceded by a less-
than sign (<) . One may hear an analytical chemist referring to a three-sigma detection limit or a two-
sigma detection limit. This has to do with the value at which the corresponding proportion of readings
detect the presence of the element being assayed. Thus a detection limit defined by a 3 sigma criterion is
much more reliable than one defined at 2 sigma. Conversely, given the same instrumental conditions, a 3-
sigma detection limit will be higher than a 2-sigma limit. Typically this fact is not presented in laboratory
brochures although detection limits are often stated.

Variances are additive; each step of sample collection, processing, and analysis adds variance. Sample
processing sources of variance can be measured and controlled by use of appropriate sampling and
analytical procedures. Geological variance is inherent in the nature of a given potential deposit and
cannot be controlled; high variance in the ore distribution is compensated for by collecting more
(decreasing drill hole spacing) and larger (larger hole diameter) samples.

Duplicate results show the variance contributed by all the steps in the process that follow creation of the
duplicate. Using a sufficient number of duplicate results from each stage in the process, it is possible to
calculate the variance contributed by each stage of the process by subtracting the variance calculated
from the following stage. Such comparisons are more reliable if the same samples are used to create
duplicates at each step, which is the common practice when performing experiments to optimize a set of
protocols. The comparisons are still valid even if different samples are used to make duplicates at the
different stages, so long as the method of selecting which samples are duplicated is the same for the
different stages, or is unbiased with respect to parameters which affect variance. Such parameters include
mineralogy and grade.

This information allows one to identify the stage in the process which is producing the most variance. If
one wishes to improve the precision of the assay database, time and effort should be focused on this step.

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Too often, time and money are wasted on improving the wrong stage of the preparation and assaying
process, as is subsequently revealed by negligible improvement in the precision of rig duplicates. In the
words of Pierre Gy, A bad sample has no memory; you cannot, for example, compensate for an
inadequate crushing protocol in sample preparation by improving the assaying protocol, nor will
improvements in crushing provide any benefit if the problem rests in the assaying protocol. Conversely, a
set of sampling, preparation and assaying protocols that show roughly equal contributions to variance
from each stage of the process can be described as having a balanced design and can be improved by
incremental improvements in any or all of the steps in the process. Improvements are usually obtained by
increasing the sample mass or decreasing the particle size, or both.

2.5 More on Significant Figures

A result has a certain number of significant figures: the number of digits which vary as a consequence of
measurement. These should not be confused with digits (always zero) used to hold place. For example,
an element having a detection limit of 10 units will typically have possible lowest values of <10, 10, 20,
30, and so on. These values have one significant figure even though it requires two digits to express
them using the selected unit of measurement.

Consider the case where a set of results has three significant figures, say covering a range of values from
0.100 to 0.999. In order for the last digit to have meaning, there must be a reasonable level of confidence
that the uncertainty in the measurement is less than 0.005 unit.

Thus the implied precision for three significant figures lies within 5/100 and 5/999, or 0.5 to 5 percent.
Note that this level of precision is for the final assaying step, obtained from the same sample solution, or,
in the case of a gravimetric gold fire assay, the same gold bead. It does not include sub-sampling
variance introduced by taking a different sample of pulp. Similarly, a result with two significant figures
implies a precision lying between 5 and 50 percent.

When a result has one significant figure, as is the case near the analytical detection limit, the uncertainty is
usually stated as one unit (rather than as half a unit, as was used for two and three significant figures).
This provides a precision of 100 percent at the detection limit (e.g. 1 1).

Sometimes one sees results near the detection limit reported in increments of 5 as for gold: 5 ppb, 10 ppb,
15 ppb, etc. This implies measurements that are no better than 5 units. Again, the precision at the
detection limit is 100 percent (5 5). In this case, a result of 100 ppb does not really have three
significant figures, and the precision is no better than 20 percent (100 5).

It should be clear from the above discussion that it is important to establish an analytical protocol that a
has a detection limit much lower than probable ore-waste cutoff grades, because measurements near the
detection limit have much poorer precision and are not reliable.

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3.0 LABORATORIES

Analytical programs should involve two or more laboratories, with one acting as the primary laboratory
for each project, with one or more additional laboratories serving as the check laboratories. There may
be several primary laboratories used by a company during a typical year, with each project dedicated to
one primary laboratory. The primary laboratory receives the majority of the analytical work for that
project, while the umpire laboratory receives only the check assay work. An umpire laboratory is one
used by two parties to form a consensus on the grade of material, such as a shipped ore or concentrate.
This term is also sometimes used to describe a third laboratory used to determine which of two
disagreeing laboratories is likely to be correct.

3.1 Selecting a Primary Lab

Primary laboratory selection is based upon a number of factors, including: quality of work, price,
convenience and service. The primary laboratory must provide results that are sufficiently timely, precise
and accurate for the projects needs at a competitive cost. Precision is typically not as good as that
offered by umpire laboratories, but must be sufficient for use in ore reserve estimates. Accuracy should be
sufficient for use in resource modeling without involving correction factors. To avoid correction factors,
there should be adequate evidence that the overall accuracy of the primary laboratory results is within 5
percent of the probable "true" value, as demonstrated by performance on inserted standards (mean
values) and agreement with check (and possibly umpire) laboratory results (comparing mean values).

In the case of feasibility studies used for seeking financing, it is preferable that the primary laboratory is
not affiliated with the umpire laboratory, and that the primary laboratory has no financial interest in the
project property. The primary laboratory may be very competitive in price and service; however, during
selection by the mining company, these attributes must not be weighed more heavily than the laboratorys
ability to routinely perform precise and accurate work, especially during times of high sample loads.

To select a laboratory from several candidates, one may submit a number of standard reference materials
to each of the candidates. At least five or six different materials should be submitted, and at least two
different submissions should be made on different days. The number of samples of each material should
be varied within each submission, but can equal a constant number when the results of all submissions are
combined. The assay protocol selected should be the one being considered for routine work.

How many measurements are necessary to characterize a laboratorys performance, and how many are
necessary to characterize a proposed standard reference material, is a debatable issue, where all agree that
"more is better". Generally, 30 or more determinations are needed. In the case of assessing a laboratory,
the 30 determinations might consist of, for example, assays on five aliquots from six different standard
reference materials. The variety of standard reference materials submitted to assess a laboratory should
reflect the variety of samples that will be submitted for the project. For example, it is unwise to submit
only gold-oxide ore standard reference materials if the project will include sulfide ores in its resource
model. Also the range of grades should be reflected, up to about a grade corresponding to the 90th to 95th
percentile of the population having grades above anticipated ore/waste cut-off. For example, if one has

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100 assay results that are anticipated to be classed as ore, these can be arranged in ascending order and
the 90th to 95th grade selected.

Where smaller numbers of each material are assayed by a laboratory, there are special statistical methods
for establishing confidence limits on mean values and estimates of variance. Where small numbers of
samples are submitted, small (statistically insignificant) differences in performance between different
laboratories should be subordinated to other considerations such as quality of the service (turn-around
time, quality of sample storage, etc.).

Once the results from all the laboratories are compiled, each candidate laboratory can be "scored" in a
number of ways. For precision, the standard deviation (or variance: either will provide the same relative
ranks) obtained by each laboratory on each reference material can be calculated. For each material,
laboratories can be ranked from high to low, with the highest rank (1) assigned to the laboratory with the
lowest variance on a given standard material.

For rating accuracy, the laboratory with the mean value closest to the certified value ranks first in
accuracy, the second-nearest is ranked second, and so on. Ranks are easily assigned by calculating the
absolute value of the difference between the laboratorys mean and the certified value, then sorting by this
calculated field.

In this manner, separate performance rankings for accuracy and precision are assigned each laboratory for
each standard reference material. The average rank scores for accuracy and precision obtained by each
laboratory can then be calculated, and separate overall rankings for accuracy and precision assigned. An
example is shown in the following table (Table 1). It should be emphasized that the number of results
shown is not sufficient to adequately characterize laboratories (or standard reference materials) but is
provided only as an illustration of one possible approach.

In this example, Standard 1 is a new material and does not have a certified value on which to establish the
relative accuracies of the laboratories; however, a ranking can be established by comparing the means of
the laboratories, and taking the median value of the means as the best value. Some statisticians will
recommend the mean rather than the median; the two should be nearly equal for an normal distribution.
Typically, however, there is at least one highly errant laboratory which will throw the mean off
substantially. Rather than agonize over whether a laboratorys results should be rejected for calculating
the mean, use the median.

In making the final selection one must examine the data closely. For example, in Table 1, Laboratory "A"
shows very good accuracy on oxide samples but very poor accuracy on the one sulfide sample, greatly
underestimating the certified value. This may indicate inadequate protocols for assaying sulfidic samples.
If sulfide samples are an important component of the project, then Laboratory "D" would be a better
choice for the project.

Where more than one assay is used in the resource model, it is best to perform assessments similar to
Table 1 on each. One can then weight the rankings by the estimated economic impact of each assay. For
example, if one anticipates that 80 percent of the value of the mineral inventory will come from gold and

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20 percent from silver, one can multiply the gold rankings by 0.8 and silver rankings by 0.2 and add these
two numbers together to get an overall ranking. This should make obvious an important point: precision
and accuracy on byproducts is much less critical than the principal commodity.

Sometimes there is an important contaminant that will affect the value of mined blocks, such as arsenic in
a copper deposit. This can be weighted in the same way as an element that adds value. For example, if
arsenic penalties are anticipated to subtract 10 percent from the value of the mined copper, the rankings
on arsenic could be weighted by multiplying by 0.1. Of course, one is forced to apply reasonable guesses
for any such weightings. For some projects, these can be based upon previous resource models of the
deposit, or other deposits in the district.

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Table 1. EXAMPLE OF AN EVALUATION OF SEVERAL FICTIONAL LABORATORIES
Standard 1: gold oxide, grade approx. 2.0 gm/ton, no best value Rankings
LAB Result 1 Result 2 Result 3 Result 4 Result 5 Mean Std. Dev. Accuracy Precision
A 2.16 2.06 2.22 2.14 2.09 2.14 0.062 1 1
B 2.22 2.13 2.20 2.13 2.42 2.22 0.119 2 3
C 1.73 2.03 2.14 1.70 1.90 1.90 0.189 5 4
D 2.25 2.22 2.39 2.07 2.20 2.23 0.115 3 2
E 2.09 1.46 2.56 2.50 1.32 1.99 0.575 4 5
Best Value (Median of Means) 2.14
Standard 2: gold oxide, certified value 1.49 gm/ton Au
A 1.61 1.57 1.48 1.53 1.47 1.53 0.059 2 1
B 1.76 1.66 1.64 1.48 1.80 1.67 0.125 4 4
C 1.51 1.67 1.51 1.57 1.50 1.55 0.072 3 2
D 1.39 1.59 1.48 1.45 1.53 1.49 0.076 1 3
E 1.33 1.26 1.19 1.57 1.20 1.31 0.156 4 5

Standard 3: gold sulfide, certified value 0.67 gm/ton Au


A 0.27 0.15 0.36 0.45 0.22 0.29 0.118 5 3
B 0.61 0.73 0.47 0.47 0.36 0.53 0.144 3 4
C 0.72 0.96 0.67 0.58 0.72 0.73 0.141 1 4
D 0.72 0.67 0.84 0.75 0.82 0.76 0.070 2 1
E 0.54 0.42 0.57 0.40 0.41 0.47 0.080 4 2

Composite Rankings Sum of Rankings Overall Ranking


Accuracy Precision Accuracy Precision
A 8 5 2 1
B 9 11 3 4
C 9 10 3 3
D 6 6 1 2
E 12 12 5 5

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3.2 Selecting an Umpire or "Check" Lab

A critical part of any QA-QC program is the check assays from an outside, or umpire laboratory. The
selection of a check laboratory involves more scrutiny than that required for selecting the primary
laboratory, as this lab(s) must perform exceptionally high quality, routine analytical work, while also
monitoring the following:

C Pulp fineness: Pulps received from the primary laboratory should be routinely checked for
percentage passing 100 (or 150) mesh. Typically every fifth or tenth sample, that is submitted for
check assay, is also checked by sieving (preferably wet) 10 or 20 grams of the pulp. Material
taken from the pulp bag for this test should be discarded, not returned to the bag.

C Condition and Orderliness of sample transmittals: Samples received from the primary laboratory
should be contained in legibly marked and undamaged packets, ordered correctly, and
accompanied by an organized sample transmittal sheet. This is a reflection on sample handling
conditions within the primary laboratory.

The goal of the check assay program is to increase confidence in the primary laboratorys accuracy.
Hence it is important to select an Umpire laboratory that is widely recognized within the industry as
having good accuracy.

A consensus is forming within the mining industry that check assays should be performed only by
accredited laboratories. Widely recognized organizations conferring accreditation include the
International Standards Organization (ISO) and the recently created Guide 25 program of the Standards
Council of Canada (SCC) that is administered by the Canada Centre for Mineral and Energy Technology
(CANMET). Accreditation by no means proves that the assay work done on a particular submission of
samples is adequately precise and accurate, nor does lack of accreditation indicate a laboratory does poor
work. The down-side of accreditation programs is their resistance to innovations which might improve
precision or accuracy.

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4.0 OBTAINING OR MAKING QA-QC MATERIALS

QA-QC programs include controls; this term is sometimes used to refer to any inserted QA-QC material,
and sometimes used to refer to materials with a well-established grade of the commodity. To avoid this
ambiguity, materials of known grade will be referred to as Standard Reference Materials, or SRMs for
short. Other QA-QC materials include duplicates and blanks. There may be various re-sampling programs
and twin (as in drill hole twin) studies as well. Standard reference materials, usually consisting of
pulverized rock, should not be confused with calibration standards, which are solutions of known
concentration used by the laboratory for instrument calibration, nor should they be confused with standard
weights, used to check laboratory balances. The problem with using the term Standards is that this is
sometimes used to refer to the methodology used to prepare and assay samples. To avoid this confusion,
it is better to refer to a methodology as a protocol.

4.1 Standard Reference Materials

An ideal standard reference material has a matrix identical to the samples being assayed, has extremely low
heterogeneity, has a value (grade) within the range used for categorizing ore, and has a reputation for
being reliably prepared and accurately characterized. Category boundaries can be real, as in the case of an
ore/waste cutoff, or more theoretical, as in the case of capping grades used in resource modelling. Ideally,
a suite of standards brackets every such category boundary, combined with every important difference in
sample matrix. The suite should include standards that have grades on both sides of any important
procedural steps in the laboratory, such as dilution steps or changes in instrument set-up and calibration
standards. Important sample matrix differences almost always include oxide and sulfide samples, because
fire assay procedures utilize flux adjustments and/or sample weight changes when processing sulfide-rich
samples, and copper projects often have assays to help distinguish copper oxide from other ore types.

Such procedural changes can affect both accuracy and precision. Other potential matrix differences might
include high and low levels of copper, silver, platinum group elements, bismuth, tellurides, etc., presence
or absence of hydrated minerals, high and low amounts of total sulfur in non-oxide samples, varying levels
of carbon. Not all these factors may be clearly understood at the time standards are first created; what is
known at the time the standards are created should be reflected in the grades and matrices of the materials
selected. Geological and metallurgical concerns should also be clearly reflected in the materials selected
for standards.

4.2 Commercial Certified Standards

Standard reference materials are readily available for purchase, but can be expensive. Commercial sources
(in North America) for standard reference material include:

Brammer Standard Co. Inc.


14603 Benfer Rd.
Houston, TX 77069-2895
tel. 281 440 9396 fax 440-4432
website url: www.brammerstandard.com
Comment: ISO certified supplier. Sells standards acquired from agencies throughout the world.

Canadian Certified Reference Materials Project (CCRMP)


Canada Centre for Mineral and Energy Technology (CANMET)
555 Booth Street

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Ottawa, Canada K1A@0G1
tel. 613 995-4738 fax 943-0573
Comment: best known in North America; extensive and expensive

Nevada Bureau of Mines and Geology


University of Nevada, Reno
Reno Nevada, 89557-088
tel. 702 784-6691.
Comment: Limited number of gold and silver SRMs.

West Coast Minerals


lwtaites@chemex.com
Comment: Limited number of off-the shelf SRMs available.

CDN Resource Laboratories Ltd.


225 Springer Ave.
Burnaby, B.C. V5B 3N1
(604) 291-1303 Fax -1392
nfuge@direct.ca
Comment: Limited number of gold standards.

LQSI (Chicago)
708 331-3249
Comment: Does expensive round-robin laboratory evaluations, materials may not otherwise be
available. Has very large rotary splitter for expensive custom work.

Vendors outside North America include:

Geostats
Freemantle, Australia
Info., and to order outside North America: http//geostats.copl.com.au
to order in North America: FPSC@aol.com
Comment: large selection; repackages and characterizes Gannet materials

Gannet Holdings Pty. Ltd.


43 Frederic Street, Naval Base
Western Australia 6165
P.O. Box 329, South Perth
Western Australia 6151 AUSTRALIA
Comment: Widely known in Australia. Sells in bulk. Does Round Robin of Australian labs to
certify its materials.

Rocklabs Ltd.
P.O. Box 18-142
Auckland 6, New Zealand
64-9-634-7696 fax -6896
http://rocklabs.com/
Comment: best known for sample prep. equipment. Small selection Au and Ag SRMs at very
reasonable prices.

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Ore Research & Exploration Pty Ltd (OREAS)
Unit 23, 993 North Road
Murrumbeena Vic 3163
Australia
Ph: +61-3-9570 5300
Fax: +61-3-9570 5221
email ore@mira.net
Comment: Limited selection, but higher quality than most; uses proprietary preparation technique.

There are many SRMs available from Brammer Standard, often allowing for selection of a material similar
to that present in the project area. There are over 5,000 materials in their catalog. While many of these
are not relevant to geoscience, they probably have the most extensive listing of geologic materials from
governmental and quasi-governmental organizations. The Brammer catalog contains an extensive listing
of governmental organizations that provide standards; the catalog is free by request and is shipped
overnight.

CANMET materials have been demonstrated, as part of their certification process, to be sufficiently
homogeneous and well behaved: most usually provide results that can be reproduced at levels comparable
to those obtainable for "Carlin type" gold samples.

The Nevada Bureau of Mines and Geology (NBMG) provides a few standard reference materials collected
from selected mine sites in Nevada. The NBMG material is not as homogeneous as the CANMET
material, not quite as expensive, and is restricted to gold and silver standards only.

One advantage of commercial standard reference materials, that they are widely known, is also a
disadvantage, since commercial laboratories are quite familiar with the grades and appearance of most
commercial reference materials. It is difficult to submit them blind to the laboratory intercalated with the
projects samples, if the analytical laboratory also manages the sample preparation facility, which is usually
the case. The laboratory will recognize them as being pulps, and therefore likely to be standard reference
material, from which it is a short hop to deducing exactly what commercial material it likely is. Some
possible approaches to maintaining the anonymity of standard reference materials are discussed in Section
5.3.

If using commercial standards, it is important to review the appropriateness of the material, and to review
the report detailing the certification. The brief specification sheet provided with such materials does not
always provide sufficiently detailed information. For example, CANMET standards state the standard
error on the jars, but not the average standard deviation; reasonable pass/fail limits cannot be established
on the basis of the standard error, since this is a function of the number of times the material was analyzed
during the certification process, and is not a direct measure of the variability of the material itself.
Detailed review of the reports may also reveal shortcomings in the stated certified value; for example,
some materials may have a "certified" value that includes some determinations using procedures that are
inappropriate to the material, providing results that are clearly biased either high or low relative to the
industry-recognized determinations (e.g., fire assay). Including these questionable results when calculating
the average, may change the certified value to such an extent that inappropriate pass/fail limits will be set
for a standard.

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4.3 Creating Customized ("In-House") Standard Reference Materials

If creating a new standard from site materials, it is important to include all of the following steps.

Collect sufficient amounts (see section 5.2) and types of material for the projects needs. It is better to
have a set of several standards that are used throughout the project, rather than different standards at
different times. Having the same standards provides a more sensitive check on laboratory "drift". If a
sufficient amount of material cannot be collected at the outset, it is important to overlap standards (ie.,
include submissions that contain an old standard that is starting to become exhausted with a new
standard). One should attempt to collect a number of bulk samples. These might include:

A standard with a grade near the anticipated ore-waste cut-off.


A standard with a grade between the 85th to 90th percentile of all ore samples.
Standards with grades near any other potential "decision points", such as a mill grade/heap leach
cutoff.
Standards covering adjustments in analytical procedure, such as both oxide and sulfide standards,
since sulfide samples require flux adjustments.
Standards covering a substantial portion of the ranges of any other routinely analyzed elements.

Establish the level of heterogeneity of a proposed standard reference material prior to attempting to
establish its "best" value. This is done by taking 24 to 48 randomized "grab" samples1 or representative
splits of the pulp material and submitting them to the umpire, or other high-quality laboratory. For the
purposes of this test only, the laboratory should be advised of the estimated grade range of the material
and the nature of the mineralogy. The analytical procedure used should be the best available for the
material (using the anticipated sample size, such as 1 assay-ton, that will be used routinely), and the group
of samples should be run together all in one or more batches, without the presence of any other materials
(to avoid potential sample mix-ups). This test is not used to establish the most accurate value, but only to
establish that the material has been adequately prepared (homogeneity).

As a rule, if the relative standard deviation (standard deviation / mean) exceeds what the laboratory claims
is obtainable for that analytical method and grade-range, additional processing of the material should be
undertaken to reduce the materials heterogeneity, or the material should be discarded. For materials
having grades well (more than 20 times) above the detection limit, this typically translates to 90 percent of
results (1.65 sigma) lying within five percent of the mean value and all results lying within 10 percent of
the mean value. In relative percent terms, more latitude must be given to low-grade materials, particularly
those with average grades less than 20 times the detection limit of the analytical method used. Because of
the extensive precautions taken to insure that sample mix-ups and clerical errors are unlikely, it is unwise
to discount one (let alone two!) erratic results. Such occurrences are what one would expect if there are
some large gold grains, for example, in the material.

Not all deposits have material that can be easily made into standards with such tolerances; in particular,
coarse-gold deposits provide many challenges. Since the purpose of the standard is to assure accuracy as
well as precision over time, it is inadvisable to make standards from such materials. Sometimes this
limitation can be overcome by screening the material through a 100 mesh or finer screen and discarding
the oversize material, followed by re-grinding of the undersize. Often in such cases, one is better off

1
Some statisticians recommend the number of tested samples be equal to the cube root of the number of
samples in the lot; this guideline would test 10 samples out of 1000, for instance. MRDI believes this number is
only valid if there is no nugget effect, and in any case will provide overly uncertain estimates of variability.

Mineral Resources Development Inc., U.S.A. 650 358-1116 19


purchasing commercial standards, even if there are some differences in mineralogy, or obtaining better
material from another project or mine, if such is available. The coarse gold problem can be better
monitored with sample duplicates if the laboratory performance is accurately measured by use of a reliable
standard. A standard with high heterogeneity is less effective at detecting problems like laboratory drift.
Even obvious mistakes such as sample swaps and transposed digits are more likely to go undetected if the
variability of the standard reference material is high.

A detailed description of testing the adequacy of the material preparation can be found in the appendices
of most CANMET reports, such as Appendix A of CANMET report 82-14E, for the reference ore MP-
1A. Once the variance of grab samples indicates the material appears to have a sufficiently low level of
heterogeneity, the material can be carefully split with a rotary splitter into individual sample packets. At
this point, it is prudent to repeat the test, by analyzing another two dozen randomly-selected packets.
Dividing the material into individual samples and placing these in a random order is an important, but often
neglected step in creating in-house standards.

Establish the "best value" (also sometimes referred to as the "sought" or "certified" value) and reasonable
"pass/fail" limits by submitting the material to a number of different reputable laboratories. This should
include any laboratories involved in performing metallurgical work (if such work includes, for example,
gold fire assays to establish head grades), plus the primary and umpire laboratories (or candidates), plus
laboratories widely recognized by the industry as performing quality work.

If there are active mill laboratories within the company that are routinely analyzing the projects
commodity, these too should be utilized. Include blind (anonymous) insertion of some commercial
standard reference materials having certified values in these round robin submissions to laboratories.
These will provide additional validation of the new materials' values, and will help determine if a
laboratorys results should be excluded when setting pass/fail limits. Request, from each laboratory, the
analytical procedure they describe in their price list that most closely resembles the anticipated procedure
to be used in the project; try to avoid introducing a new procedure to the laboratory. For gold, the choice
of procedures typically requires a selection of analytical sample weight (such as one assay-ton) and "finish"
(gravimetric or atomic absorption). Laboratories should not be alerted as to the samples nature (that these
are standard reference materials, or what the expected grades of each are).

Materials should be submitted in at least two separate lots on different days, the number of samples of
each material varying in each lot, but totaling to the same number (typically 8 to 10 determinations by each
laboratory on each material) when all submissions are combined. In this way, variance between batches is
included. For example, the first submission sent to Laboratory "A" might contain 5 samples of standard 1
and 3 samples of standard 2, and the second submission would then include 3 samples of standard 1, and 5
samples of standard 2, so that a total of eight samples of standard 1 and eight samples of standard 2 are
analyzed. This makes it a bit less obvious to the laboratory that the same material is being submitted
multiple times. Anonymity can be further enhanced by including drill sample pulps that are sent for assay
check, if there is an on-going program.

Some laboratories try to make a good impression by analyzing each sample several times when they know
that the material is for quality control. This does provide a more reliable estimate of the best value, but
misleads one into establishing unreasonably stringent pass/fail limits on the material. If this circumstance is
suspected, the sample weight should be carefully restricted.

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The "best value" can either be the mean value of all results remaining after discarding outliers (typically
those results more than 3 standard deviations above or below the mean), or the median of the population
of laboratory means can be taken (Section 3.1). The second approach is best if the number of assays
performed by different laboratories varies.

Establishing pass/fail limits for a Standard Reference Material is more problematical than establishing a
best value. Many commercial Standard Reference Materials do not state pass/fail limits. For example,
Canmet standard reference materials have confidence limits stated on their labels. These cannot be used as
pass/fail limits; they are the standard error of the mean, narrow limits that narrow further as more
assays are used to calculate the mean, and are therefore not a direct measure of the intrinsic variability
between sub-samples of the material (plus typical measurement errors contributed by the assay procedure).

The problem with establishing pass/fail limits is that a given laboratorys performance is likely to have a
small bias relative to the best value; consequently, the standard deviation calculated from all the round
robin results (even when excluding outliers) will incorporate many small relative biases. Thus, if all the
accepted data are used to calculate the limits, the limits will be set much wider than that typically obtained
by a single laboratory, and if the limits are set relative to the best value, a particular laboratory, having a
relative bias to that best value, will show failures that are partially a consequence of the relative bias rather
than a loss of precision. This is typically seen as tendency for nearly all the failures to occur on one side
(either the lower or upper limit) of the best value, and to be outside the limit by amounts similar to the
difference in the best value and that laboratorys mean for that material.

One way around this, used by some major mining companies, is to establish two pass/fail limits. The wider
set of limits are ones where there is a high degree of probability that some gross error has been committed
(probable Type I errors, such as sample mix-ups), and the narrower set is used to detect laboratory drift
and possible Type I errors. Results falling outside the outer limits always trigger remedial actions,
whereas results falling outside the inner pass/fail limits prompt action only if they occur with an unusually
high frequency.

If this approach is used, the large failure limits can be established from the population of all results
(including outliers) by finding the range that includes 95 percent of all the results. To do this, arrange all
the round robin results in order by grade and remove the lowest and highest 2.5 percent of results, then
take the maximum and minimum values of the remaining population. If the round robin results are
representative of the material plus the relative biases between laboratories, then these limits should be
exceeded not more than 5 percent of the time, regardless of the laboratory. The limits may be skewed
around the best value, particularly if the sample is low in grade. This may reflect heterogeneity in the
material, and thus it is arguably valid to have such an asymmetry. This approach works best if one has a
large amount of data (such as that provided in a CANMET report).

If the data are limited, and do not have a serious assymetry problem (or one chooses to ignore it) one can
discard results that are more than 3 standard deviations from the mean of all results, then recalculate the
standard deviation on the remaining data. If a skewed distribution has a log-normal appearance, one can
convert the results by taking their logarithms, calculate the standard deviation of the logarithm values
(omitting any results more than 3 standard deviations out in the converted population, which very rarely
happens) then convert the limits back by taking the antilog. This will insure that the lower pass/fail limit is
always a positive number. However, if one has to go through this gyration to calculate boundaries, it
usually means one has a poor material for a standard.

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The narrower set of failure limits can be tailored to the particular laboratory being used, taking into
account any relative bias (relative difference between the mean value that laboratory obtains on that
standard reference material and the best value for that material) by using that laboratorys mean rather
than the best value. This should only be attempted if the uncertainty in the mean obtained by the
laboratory is small, as measured by the standard error of its mean. If the uncertainty of the mean exceeds
about two percent, more results from the laboratory in question are required, before a mean value can be
established. The uncertainty in the mean should decrease proportional to the square root of the increase in
the number of measurements; for example, quadrupling the number of results should roughly halve the
uncertainty of the mean.

One can then take the typical standard deviation shown by the round robin laboratories and use it to
place evenly spaced boundaries around that laboratorys mean value for that standard reference material.
The median of the round robin laboratory standard deviations is the value for which half the participating
laboratories showed better precision and half worse, and is arguably a fair choice. If this median standard
deviation is multiplied by two and the resulting number added to the laboratorys mean to make an upper
limit, and subtracted to make a lower limit, then the laboratory should only exceed these boundaries five
percent of the time, provided it is as good as half the participating laboratories. If it has better precision
than half the laboratories, it will show a lower rate of failure.

The data in Table 1 (Section 3.1) can serve to illustrate. Standard 1 has a mean of 2.09 and a standard
deviation (all data) of 0.290, giving a mean 3 sigma range of 1.22 to 2.96, which encompasses the entire
range of results (1.32 to 2.56). Therefore, no datum can be excluded on the basis of being more than 3
standard deviations from the mean.

The 2 sigma pass/fail range is 1.51 to 2.57. The alternative method of excluding the uppermost and
lowermost 2.5 percent of the population cannot be easily applied to a population of 25 results because
each result constitutes four percent of the population. The range using this method must therefore lie
between excluding no results and excluding two results (i.e. the highest and lowest results) which defines a
lower boundary located somewhere between 1.32 and 1.46, and an upper boundary between 2.50 and
2.56. These are awfully wide limits. One should in practice have a material better behaved than the one in
this example.

The inner pass/fail boundaries for Laboratory A would be symmetrically spaced about the mean of
Laboratory A results for Standard 1, which is 2.13. The median of laboratory standard deviations for
Standard 1 is 0.119, giving boundaries for Laboratory A of 2.13 0.238, or 1.90 to 2.37. By comparison,
the equivalent boundaries for Laboratory C are 1.90 0.238, or 1.66 to 2.14.

Ideally, a laboratorys relative bias will be small, because a laboratory should not be selected for a project
if it shows a large bias. Laboratories (or assay protocols) showing biases exceeding five percent on ore
grade samples (of the principal commodity) should be avoided. In any case, the amount of bias that is
acceptable is dependent upon the context provided by the resource model and viewpoint of the readers.
Those who would finance the venture are not perturbed by using under-estimates, while those who are
promoting the property are. Biases should be viewed on the basis of all the assays on the standard
reference materials, and can also be viewed on the basis of prolonged periods of high or low results
(laboratory drift). As a rule of thumb, for the principal commodity, a bias (using the average of all the
standard reference material results) of less than five relative percent is widely accepted, and a bias of more
than ten percent is widely rejected. Worse biases are sometimes accepted for byproducts and
contaminants, commensurate with their smaller impact on valuations.

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There have been several instances where mining companies, in making their own standards, have relied
primarily on rolling and shaking a material to reduce its heterogeneity. They have then removed the
material from a cement mixer (or a bucket they have rolled around on the laboratory floor), a bucketful (or
a scoopful) at a time, and put it into numbered jars, which they have then proceeded to use in sequence.
Later, when a jar was exhausted and they began using the next jar (an event that is seldom recorded
anywhere), it appeared that the laboratory had drifted in its performance, slightly higher or lower. In fact,
the laboratory is unchanged; what has changed is the grade of the standard reference material sent to the
laboratory.

The best way to prevent this situation is to split the material up into the lot sizes that will be used in its
submission (typically about 100 grams of material). The packets of material must then be placed in
random order, so any heterogeneity does not become clustered into different time periods, and instead is
appropriately observed as part of the intrinsic variability of the material.

It is important that, during the certification process of a proposed standard reference material, care is
taken to sample from every part of the material. With powders, this can be achieved with a vibrating riffle
splitter, although a rotary splitter is capable of producing a much superior product, when operated at a
slow feed rate. Although riffle splitting cannot surpass rotary splitting, it can be improved by passing the
material through the splitter and recombining it several times prior to making the split. Also, as the
number of fences in the riffle splitter is increased, the quality of the riffle split improves.

Finally, all the assay certificates, compilation and analysis of data should be properly archived so that it is
available for review by auditors. More often than not, this documentation is lost, which makes a
laboratorys performance on a particular material a baseless claim of accuracy. The error is compounded
by completely exhausting the material, so that there is nothing left to submit to other laboratories, in order
to demonstrate the best value is valid. Often, too, when a property changes hands this information is
never requested and never provided, a lack of diligence that sometimes has dire consequences.

4.4 Blanks

Blanks are samples of material devoid of the element undergoing analysis. Blanks help to monitor carry-
over contamination and mis-sequencing of samples during sample preparation and analysis. Blanks may be
submitted as coarse material (coarse blanks) consisting of nominal 1/4 inch barren material which is
inserted into the sample stream at the drill site (in the case of rotary cuttings) or during core splitting. This
material is then subjected to the same sample preparation steps undergone by a project sample. Another
type of blank consists of pulped material, such as Ottawa sand, or other high-purity sand, or reliably
barren material collected from the project drilling, that has been made into a pulp. These pulp blanks are
submitted into the sample stream after sample preparation has been completed.

The mineralogy of the blank should resemble that of the material being routinely analyzed (e.g. barren drill
cuttings); however, this is not as critical for blank material as it is for standards. A coarse blank should be
sufficiently hard and of large enough mesh size to allow effective grinding of any contaminant material
(from previous samples) adhering to the sample preparation equipment. Elsewhere in the laboratory, this
blank material will reveal: the presence of unacceptably high levels of background concentrations caused
by cross-over contamination (dust, boil-overs, etc); poor lab-ware cleaning; or, in circumstances where
below-detection results are infrequent, mis-ordering of samples.

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As a rule of thumb, coarse blanks should return values less than or equal to twice the detection limit value
80 percent of the time. Pulp blanks should return values less than or equal to twice the detection limit
value 90 percent of the time. After correcting any sample swaps and replacing results from any failed
batches with new results, the mean value of pulp blanks (assigning a value of "0" to samples reported as
below detection) should not exceed the detection limit.

4.5 Duplicate Samples

A group of duplicate samples can be created from any point in the sampling process where the mass of the
sample is being reduced (i.e. the sample is split and a reject is created). In the initial stages of establishing
sampling, sample preparation, and assaying protocols, duplicates should be collected frequently at all these
stages, in order to generate sufficient data to obtain estimates of the variance introduced by each step.
Sampling theory is useful at predicting how best to optimize the process by which estimates of grade are
obtained, but it does not operate in a vacuum. It must be supported by experimental data (as obtained
from analysis of duplicates) and observation (such as mineralogical reports on the distribution of gold
particle sizes). Once the process has been established and tested, the number of duplicates can be reduced
to a modest percentage of the samples, in order to monitor the process (quality control) and demonstrate
its adequacy (quality assurance).

One can sufficiently describe types of duplicates by an appropriate measurement of the particle size at
which the material is divided (split), and the mass of the split. Gy (1992) has made an extensive
investigation, utilizing many different kinds of crushing and grinding equipment, to ascertain what
measurement of particle size best characterizes a sample. Gy found that the screen size that allows 95
percent of the sample to pass is the measure which is most independent of the method by which the
material was crushed or ground, and most independent of the range of particles sizes (i.e., it applies well
to both fine and coarse materials). More recently, Francois-Bongarcon (MRDI, personal communication)
has provided a theoretical explanation of why this is so.

This is backwards from what is usually the case of how a sample size is described. Often, a crushed
material is described as 10 mesh for example, without any description of what percentage of the sample
passes 10 mesh. Often a material prepared by a commercial laboratory and described by them as 10
mesh is in fact, about 50 to 60 percent passing 10 mesh. Metallurgists often refer to the D-50 size,
particularly in Australia: the screen size that allows half the sample to pass. North American metallurgists
and sampling experts sometimes use P (for passing) followed by the percent passing; the most common
criteria are P-80 or P-90 for 80 and 90 percent passing, respectively. These are followed by the mesh
size, as in P-80 10# or P-90 1/4 inch.

The most common practice of commercial assay laboratories is to describe crushing output as 10 mesh
followed by some percent passing, rather than to determine the screen size which allows 95 percent of the
material to pass. This sometimes conceals problems that may be present in a given material, such as the
presence of large (more than 2 or 3 inches in longest dimension) pancakes or splinters from a rolls
crusher, which may be detrimental to sample precision. If sampling theory indicates a process should
provide a level of precision that duplicate results indicate is not being achieved, particle size distribution is
the first place to look for a problem.

A second important parameter when describing duplicates is the sample mass. This is often easily done as
a range of a factor of two, such as 4 to 8 kg, or 200 to 400 gm, if a riffle splitter is being used, because
these, when used properly, split the material into two equal sample masses. Consequently, unless a

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complex routine of splitting and recombining is practiced, one is left with the option of splitting one more
time, or not. Hence the factor of two in the range. In some other scenarios, such as using a rotary
(rotating riffle) splitter or collecting material from a mat, a tighter range of masses may be achieved. If
sampling theory indicates a process should provide a level of precision that duplicate results indicate is not
being achieved, this is the first place to look for a problem in the case of drill site duplicates, and the
second place (after particle size) to look in the case of other duplicate types.

Although not truly duplicate samples, other samples, sometimes referred to as "duplicates" include the
other half of split drill core, and twinned drill holes. Split core includes more variability than rig
duplicates (from a rotary drill hole) because there is a small but quantifiable spatial separation of the two
samples; this contributes variance which is a function of the geology of the deposit and not of the sampling
method. For split core, a random selection of ore-grade intervals can be analyzed, to establish that the
selection process of the drill core halves was unbiased.

Some geostatisticians find it useful to examine the level of variance in this type of duplicate sample when
completing variography (for an independent estimate of nugget effect at centimeter-scale separation of
samples). Twinned holes have even more spatial separation and are often difficult to evaluate. This is
because samples cannot be easily paired between the two drill holes, because ore controls are not always
horizontal, and are frequently quite variable on a scale of meters.

Because of difficulty in matching intervals to create pairs in twinned holes, even when drill holes have been
subjected to detailed down-hole surveys, it is advisable to compare twinned holes on the basis of similarity
of the distributions, such as is done with a quantile-quantile (Q-Q) plot. In some cases, comparing two
different drilling techniques reveals the presence of sampling biases, caused by such factors as down-hole
contamination during wet rotary drilling, or selective ore loss during core drilling, compared to dry rotary
drilling. Pairing data or comparing means is even more problematical in such circumstances, because the
sample sizes are usually unequal.

Given two populations of samples taken from the same lot, but of different sample mass, the population of
smaller samples will have a distribution with a longer tail, i.e., it will be more assymmetric than the
population of larger samples. Both populations will have the same mean, or nearly so, if the samples are
collected properly, and the population size is large enough. This effect is sometimes described as change
of support: increasing the support has the effect of reducing the spread of the assay values, but in such a
way that the mean does not change. One may encounter it when comparing blast hole to exploration drill
hole results, or drill core holes of different diameter, or when comparing drill core to reverse-circulation
drill holes.

Another option is to make several different sets of pairings using matching geologic observations between
pair members and varying offsets in sample elevation. This allows for the possibility that the trend of
mineralization is not horizontal over the short separation distance between two drill holes. The various
match-ups, offset by 0, 1, 2 or more drill sample interval lengths, can then be processed separately to
obtain a range of estimates for comparing the twins.

Averages can be calculated for geologic units, either average grade or average metal content (summation
of grade times length) for each geologic unit. This may be most useful where ore-bearing units are varying
in width over short distances. The boundaries of the geologic units must be based upon geologic
observations not influenced by assay results.

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5.0 USING QA-QC MATERIALS

5.1 Batch Submissions

A "batch" is an imprecise term, but can be defined as a group of samples that undergoes processing (for
example, firing in a furnace, heating on a hot plate) as a group.

It is useful to know the number of samples in each laboratory batch; and how the number varies by
analytical technique. These numbers will vary by laboratory. Standards should be submitted to the
laboratory in sufficient number and frequency such that each laboratory batch contains at least one ore-
grade standard, plus one blank, plus one low-grade standard or pulp duplicate. The laboratorys internal
QA-QC program should include at least one duplicate sample and/or control sample, and one blank; this is
a widely used QA-QC procedure at commercial laboratories. If the laboratory does not include a blank in
each batch of samples, then blanks should be submitted with sufficient frequency so one is included in each
laboratory batch. There is a special circumstance where the project geologist should submit blind blanks
into every batch, even though the laboratory routinely inserts blanks into batches as part of its quality
control: if there is not at least one sample below detection in nearly every batch processed. Such a
situation is atypical for most gold deposits.

In any case, every submission (shipment of samples) to the laboratory should include at least one coarse
blank. Blanks become more critical as a method of controlling laboratory error as the ore-waste cutoff is
pushed closer to the detection limit. As a rule of thumb, if the ore-waste cutoff is less than 15 times the
detection limit, one should insert blanks into every batch of samples. It is, however, better to avoid assay
protocols that have detection limits so close to the ore-waste cutoff.

Coarse blanks should be submitted to the sample preparation laboratory in sufficient quantity to insure at
least one such blank is processed during every operating shift of the preparation facility. The geologist or
technician overseeing rig sample collection should watch for significant footages (typically four or more
sample intervals) of visually-identified probable ore-grade material, and insert the allotted coarse blanks
into the sample stream within or just after some of these "runs"; there is little value in placing coarse
blanks into the sample stream after barren material, since cross-contamination cannot be detected unless
previous samples have detectable levels of the element of interest.

Low-grade SRMs should have grades close to the anticipated cutoff grade (for gold, say 0.4 to 0.8 gm/t,
or 0.012 to 0.023 oz/short ton). A high-grade SRM should be above any anticipated mill-ore/leach-ore
cutoff grade or around the 85th percentile of all ore-grade samples previously assayed. Assay precision in
this concentration range is very important in order to minimize mis-classification of material.

Another high-grade standard should have grades at or above the routine "linear range" routinely used by
the atomic absorption spectrometer (if this procedure is used); that is, above the threshold at which the
laboratory must dilute the sample, or re-calibrate its instrument with a different (higher concentrations) set
of calibration standards. For gold this is often in the 3.5 g/mt (0.102 oz/short ton) range, but the threshold
will vary by laboratory. This high-grade standard allows the detection of incorrect or inaccurate dilution
or re-calibration, which often occurs at some point in time if a project is large. Whether such an SRM is
warranted depends upon the frequency and reproducibility of ore-sample results above this grade.

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Other "high-grade" standards might be selected at the median grade of ore-grade samples for the deposit,
or at median grades of oxide and sulfide samples in the deposit, if there is a great disparity between grades
in the oxide and sulfide zones.

5.2 Suggested Amounts of QA-QC Materials

As a minimum program, MRDI recommends the following:

An ore-grade standard (of appropriate oxidation state), and a below-ore-grade or blank sample
should be analyzed in each laboratory batch. The total of such insertions should comprise about 5
percent of the samples being submitted to the laboratory.

Blanks should occur in each lab-batch. If the laboratory does not insert blanks as part of its quality
control, then these must be submitted at a rate of one blank per batch by the project manager.
Additional coarse blanks should be occasionally inserted within or immediately following visually
identified high-grade samples.

Coarse-reject duplicates should constitute five percent of the samples submitted to the laboratory.
As much as five percent of renumbered (same-pulp) drill samples should be re-submitted with the
standards, if the same organization performs sample preparation and assaying, in order to better
maintain the anonymity of the standards. In reverse-circulation drill sampling, drill rig duplicates
can be used instead of coarse-reject duplicates.

Some projects routinely submit all drill samples for assay, including rock units known to be barren,
such as the leached cap of a coppery porphyry deposit. In cases where these units can be reliably
identified without assaying, they can be excluded from duplicate selection process.

Analytical results from the standards will be used to evaluate the analytical data and to accept or reject
laboratory batches of results. Coarse reject duplicates are used to evaluate the sample preparation
performance. Coarse blanks are used to evaluate both sample preparation and assaying. It is preferable
that duplicate samples be analyzed in a different batch than the original sample, because most laboratories
include their own duplicates in each batch. If some processing error affects all members of a batch in an
identical fashion, duplicates in the same batch will agree, but duplicates assayed in different batches will
not.

A rough estimate of the minimum amount of ore-grade standard reference material needed for a drilling
campaign can be obtained from the formula:

0.02625*w*D/l

where w= average weight of a submitted sample of standard, D=total meters of drilling planned, and
l=average drill interval length of samples. This number includes the insertions of standard reference
material in submissions to the check assay laboratory. Hence 10,000 meters of drilling sampled on an
average interval length of 2 meters would require a minimum 132 insertions of ore-grade standard that, if
sample weight averaged 100 grams each, totals 13.3 kilograms of material. A similar amount of low-
grade+blank material would be required. If the batch size is less than 40, more material is required in
order to insert one ore-grade sample (and one blank or low-grade sample) into each batch. In such a case,
the minimum amount of ore-grade standard reference material can be estimated from

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w*D/(l*n) + .05*w*D/(l*m)

where n is the number of samples processed in each primary laboratory batch and m is the number of
samples processed in each umpire laboratory batch.

5.3 Maintaining the Anonymity of QA-QC Materials

Typically, sample preparation is handled at the same facility doing the analytical work (the primary lab).
This facilitates, minimizes and expedites sample handling and receipt of assays. Also, cost-savings are
obtained from: reduced time spent in sample tracking (phone calls); sample shipping (air freight of pulps);
and work volume discounts.

Because all standard reference materials are usually submitted as pulps, it is impossible to keep their
identity secret from a primary laboratory that is otherwise receiving variably sized geological material.
Blind submission of standards to the primary laboratory would be facilitated if sample preparation were
handled by a facility other than the primary assay laboratory. If this is done, all samples that arrive at the
primary laboratory will be pulps and the intercalated standards will be more easily concealed from the
laboratory. Most commercial laboratories will, under duress, do sample preparation only; however,
preparation alone can be expensive, since advertised preparation prices are often leveraged by the
analytical prices which have more profit margin for the laboratory. Laboratories are reluctant to perform
sample preparation without obtaining the analytical work as well, because sample preparation can become
a bottleneck that prevents the laboratory from obtaining more remunerative work that includes both
preparation and analysis.

The options of completing preparation at a separate facility should be explored. There are a few "prep-
only" laboratories established that offer customized preparation. Some major laboratories that routinely
perform both preparation and analysis will do sample preparation only for a very substantial surcharge
(around 100 percent). Alternatively, for large-scale programs of sufficient duration, construction of a
sample preparation facility should be evaluated.

If there are any doubts as to whether "blind" controls may be identified and singled out for special
treatment, pairs of standards, that differ from each other in assay value by 1.5 F (1.5 times the standard
deviation obtained for the standard to be diluted). This is typically four to eight relative percent, with a
higher relative percent difference for standards having grades nearer the analytical detection limit. Near
the ore/waste cutoff, such a pair of standards might have values of 0.48 and 0.52 gm/ton Au (a relative
difference of 0.04/0.50, or 8 percent). A pair of "high-grade" standards might have values of 2.04 and
1.96 gm/ton Au (a relative difference of 0.8/20.0, or 4 percent). Such differences are difficult for a
laboratory to identify with certainty on the basis of a single assay. Where such an approach is used, the
two standards of each pair can be graphed on the same control chart, as separate lines.

In addition to this, a percentage of previously assayed sample pulps ("same-pulp duplicates"), repackaged
and renumbered by the projects expediter so as to be indistinguishable from packets of standard material,
should also be included in the QA-QC materials supplied to the laboratory for insertion. Typically, most
QA-QC programs use two or three standards (cutoff, average grade, special treatment grade) for each ore
type (e.g. "oxide" and "sulfide" ores in a gold deposit). In order to insure that one high-grade and one
low-grade or blank is inserted into most batches of samples, the laboratory can be provided with two
boxes of pulps for insertion: one containing blanks, low-grade standards and pulp duplicates with initially

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low assays, and one containing high-grade standards, and duplicates of pulp duplicates with high-grade
results.

Where laboratories are provided with standard reference materials for insertion, it is important to check,
whenever visiting the laboratory, to be sure the materials are being inserted into each batch, and are not,
for example, being run separately in duplicate or triplicate and the average results entered in the final
report.

It is a good practice to pre-assign and pre-number standards under very controlled conditions so that the
likelihood of mislabeling or mis-recording is reduced:

When this is possible, a key list should be maintained of each samples "SRM identity". Just as for
samples, each insertion of an SRM should be accompanied by a unique sample number.

To maintain anonymity and to control the location of SRMs in the sample stream, sample numbers
can be reserved in printed sample number books, if such are used. This can be done by using a
rubber stamp "STANDARD: _________" on selected pages, such that each group of samples
(equal to the batch size) has two places reserved for SRMs..

The selection of sample numbers used for assignment can be varied slightly by, for example, adding
a randomly-selected integer between -4 and +4 to a constant number equal to the batch size. A list
can be very easily generated in a spreadsheet such as Excel or Quattro-Pro, that is then imported
to the database to make an SRMS table.

A list is also printed and kept with the sample books; thus the identity of the standards inserted can
be filled out. The filled-in list is then returned, and the SRMS table is up-dated.

To avoid introducing clerical errors, it is advisable to incorporate some redundancies into the task,
such as having a removable (paper-clipped) tag on each standard, that must be removed and
marked with the sample number, at the same time as a sample number is written on the standard
materials envelope. These tags can then be placed in an envelope with the date of shipment, and
kept until the results are back. If a question arises about mixing up inserted standard reference
materials, the appropriate envelope can be checked. Writing the information down on a clipboard
does not seem to work as well, possibly because people forget to do it when they are in a hurry. If
a technician forgets to remove a tag, the laboratory will know the standard identity for that sample,
but at least it will not have been misidentified.

It is important to provide feedback to the technicians involved in the task, alerting them if mistakes
are being found, so they will be vigilant.

It then becomes the responsibility of the supervising geologist or geotechnician to enter the identity of the
SRM inserted in the sample booklet (rather than a drill meterage interval) and on the SRMS list. It is
worthwhile to make some effort to insert an appropriate standard into the sequence, based on what is
logged for nearby samples. For gold samples, efforts should be made to insert an oxide (typically red in
color) standard with oxide samples, and sulfide (gray or black) standards with sulfide samples, so that the
SRM and samples will receive the same flux adjustments prior to the firing process.

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Where drill footages are used as sample numbers, SRMs cannot be easily inserted. Using fictitious drill
footage intervals is a potential source of confusion, and is not recommended. If this approach is adopted
anyway, the fictitious drill footages should be assigned a zero length (i.e. the from should equal the to) so
that they will receive zero weighting (and be discarded) if mistakenly incorporated into the resource
model.

An alternative is to append a suffix to the drill interval which precedes the insertion point, and assign this
to the control; this somewhat compromises the anonymity of inserted control materials. When using this
approach, do not routinely insert a duplicate right next to its original sample. One can use "peel-off"
labels, preprinted with the standards identity; because the sample already has a distinct suffix, the
presence of the label backing gives nothing additional away. The label is then peeled off at the time of
insertion and labeling of the bag of standard material, and the peeled labeled pasted into the sample book,
or onto a key list, that identifies the standards. A similar approach can be used for insertion of coarse
blanks.

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6.0 QUALITY CONTROL PROTOCOLS AND CRITERIA

6.1 The Concept of Accepting or Rejecting Batches

A critical aspect of a Quality Control program is the decision process for accepting or rejecting data from
the laboratory. Data are often reviewed on a lab-batch basis; a number of lab-batches may constitute an
entire laboratory job. Therefore, it is rarely necessary to reject an entire job; rather, individual batches
from laboratory jobs are all that, under ideal conditions, will occasionally need to be rejected.

Usually it is impractical to exercise batch control from outside the laboratory. The project manager does
not usually know where one batch ends and another begins, and so must typically reveal the identity of the
control sample (if it is not already known) so that the laboratory can identify the batch. Instead, the
project manager should request re-assay of a small group of samples (five to ten) that include the inserted
standard, such that the position of the standard is not at the beginning nor the end of the sequence, but
otherwise varies with each re-assay request. The laboratory will, after investigation, often be able to
identify to the project manager the type of error it has committed (batch, sample swap, etc.) and perform
the appropriate action (re-analyze the appropriate batch if a batch error, issue a corrected assay
certificate).

The idea of quality control by batch is that an entire batch may have been subjected to an improper
procedure and so the entire batch is "bad". This is sometimes, but not usually the case. The most
common kinds of errors in assays are episodic errors, which occur at random. Examples are misreading a
number on a balance or instrument, transposing digits when recording a number, misplacing a decimal
point, spillage or "boil-over" of a single sample, a transient partial blockage in fluid flow to the
spectrometer, contamination from drips occurring in a dirty furnace, re-use of a contaminated crucible,
and so on.

Usually, the second-most common kind of error involves switching two samples, which results in two
nearby samples having incorrect results. Having a "bad batch" is usually a rare event. Examples include
"reading" (on the instrument) a rack of samples backwards, reading the wrong rack of samples, heating a
group of samples for too long or too short a period of time or at the wrong temperature, using the wrong
reagents or improperly calibrating an instrument. Because these are procedural errors that can be
eliminated by introducing good procedures, good laboratories have few bad batches. The other types of
errors are more difficult to prevent, but can be reduced through the use of computers (connected to the
spectrometer and balance, for example, to prevent transposing digits).

It is good business practice to make an agreement with the laboratory specifying the required levels of
laboratory performance, how they will be measured, and what remedial actions are required under
different outcomes. The specific arrangements will vary, but typically the laboratory will agree to re-assay
batches failed by the project manager at no additional charge. This agreement will erode if the Quality
Control program is poorly managed as evidenced by, for example, the frequent occurrence of sample
swaps made by project personnel responsible for labeling and inserting blind standards and duplicates. For
certified standard reference materials, the "tolerance" (range around the sought value of a standard
deemed acceptable) should be based upon what has been attained by other laboratories using similar
analytical procedures, as published in the certification report. Reasonable limits typically encompasses
about 95 percent of the determinations obtained during the certification process, not the standard error of
the mean (the uncertainty in the estimate for the certified value) as is printed on some commercial labels,
including CANMET standards.

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In the case of umpire check assays, the original and check results commonly exhibit systematic differences
of a few relative percent (i.e. one laboratory returns values very slightly higher than the other, on average,
over time). This component of relative bias between the laboratories is typically factored into statements
of standard deviation in certificate reports. Samples that have grades near the detection limit must be
given even larger tolerances (in terms of relative percent of the grade). This effect should be minimized as
much as possible by selecting a primary and umpire laboratory that show good agreement with other
laboratories and very good agreement with each other.

A result can be described as passing limits if:

For standard reference materials, the accepted range should be the sought value 2F (nominally 95
percent confidence interval). This is a generous tolerance. One may expect that, if the laboratory
is performing above average and samples are not mislabeled prior to submission to the laboratory,
that less than five percent of submitted standards will be outside this range.

Pulp blanks should return values less than or equal to twice the detection limit. Coarse blank
material should not exceed three times the detection limit.

Placing pass/fail boundaries on duplicate results is more problematical because less is known about the
reliability of duplicate pairs. What may seem a very demanding requirement for one deposit may be easily
obtainable for another. Some rough rules of thumb specify that 90 percent of duplicates pairs meet one
of these criteria:

Duplicate results (results A and B) performed on coarse rejects should be within 20 relative
percent (pair difference divided by pair mean):

/ 0.5*(A+B) /
A-B < 0.2

Duplicate results (A and B) performed on pulps should be within 10 relative percent:

/ 0.5*(A+B) /
A-B < 0.1

In the above formulae, results below detection are assigned a value of zero. The equations are undefined
where both values are below detection. Pair mean values (0.5*(A+B)) which are less than 15 times the
detection limit are allowed wider relative limits:

For pulps, if the absolute value of A - B is less than or equal to twice the detection limit, it passes.

For coarse rejects, the value *A-B* should be less than or equal to three times the detection limit,
in order to pass.

How well these "rules of thumb" work for duplicate results near the detection limit depends upon how the
laboratory defined its detection limit; these rules are consistent with those stated for blank samples.

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These rules are quite effective at identifying pairs of results that are passable. A laboratory that has a high
proportion of results near the detection limit which do not fulfill the above criteria, but good performance
for higher grade samples, may be understating its (practical) detection limit. Several papers by Thompson
and Howarth discuss this problem in detail. One solution is to redefine the "practical" detection limit at a
higher level than the level stated by the laboratory (for example, doubling it). There is little risk to
resource estimations, so long as the "new" detection limit is still well below any possible ore-waste cutoff
anticipated for the project. If the ore-waste cutoff is less than 15 times the redefined detection limit, the
adequacy of the analytical method must be carefully reviewed.

6.2 Types of Errors

Errors in data can generally be categorized into three different types: those that we think of as
mistakes, those that are a consequence of the limitations of process, and flaws in the process which
provide consistently wrong answers.

Mistakes include actions such as transposing digits when recording a reading, mixing up samples, or
forgetting to apply a dilution factor when calculating an answer, electronic or mechanical failure of a
measuring instrument, and mismatching results to sample numbers, to name but a few. This type of error
is sometimes referred to as Type I. Results with such errors bear no predictable relationship to results
without mistakes. That is to say, given a list of results, all of which contain this type of error, one can
make no prediction about what the results would be without these errors. The difference between the
erroneous result and the true value may be very large or very small. Some of the errors of this type can
be quantified by their frequency of occurrence. For example, by checking some of the entries in a database
against source documentation, one can find what percentage have data entry errors.

Measurement and sampling errors, sometimes called Type II errors, are more predictable. A sufficiently
large population of these errors has a mean of zero (positive and negative errors tend to cancel out). For
these type of errors, one can calculate confidence intervals and the like. These types of errors do not
prevent one from obtaining the right answer. Measurement and sampling errors cannot be prevented,
only reduced in size.

The third type, systematic errors are also predictable, but provide the wrong answer. For example, if
the calibration on a balance used to weigh sample aliquots is 5 percent low, then the average of results
from samples weighed on that balance will be 5 percent high, because each sample aliquot weighed on
such a balance has on average five percent more sample mass than is used for calculating the grade of the
sample. Small systematic errors exist in any process; they are the reason different laboratories will obtain
slightly different average results on the same set of samples. Large systematic errors in assaying or
sampling can be fatal flaws in a resource model.

These three different types of errors all coexist in a set of quality control data. Effective quality control
takes this into account.

The first item to locate are large Type I errors. These are the outliers on scatter plots of duplicate
results. These can be visually located from scatter plots. If they can be identified and removed, the
remaining data contains small Type I errors that are indistinguishable from Type II, and Systematic Errors.
After removing outliers, duplicate data can be used to construct a table to accept or reject any pair of
duplicate results.

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6.3 Identifying Outliers in Populations of Duplicate Results

Precision, expressed in terms of relative difference between two measurements on duplicate samples,
varies with grade. Precision in the neighborhood of the detection limit will be poorer than precision at
higher grades. This can occur when some measurement errors are constant. For example, if a set of
instrument readings has increments of 0.1, with an uncertainty (say at 2 sigma) of 0.1, the precision at 2
sigma is 100 percent for a sample producing a reading of 0.1, whereas a sample producing a reading of
1.0 has a 2 sigma precision of 10 percent.

Consequently, if one does not take grade into account, the relative difference between pairs will reject a
disproportionate number of pairs from some grade neighborhoods. Other measurement errors are not
constant, such as, for example, diluting a sample. A 1 percent error in dilution produces a difference of
0.01 in a sample having a grade of 1, and a difference of 0.001 in a sample having a grade of 0.1.

One should evaluate the data set to define what level of precision is acceptable for a given grade. Heres
one approach. Place the duplicate results in columns A and B of a spreadsheet. Calculate the pair means (
[A+B]/2) in column C, and the differences (A-B) in column D. Then:

1. Sort the data by pair means.

2. Calculate the variance of each pair in a new column, e.g. E32: =VAR(A32,B32).

3. In another column F32, using a reasonably-sized neighborhood (usually more than 32 pairs but less
than 10 percent of the population you need a lot of pairs for this), calculate a moving window of
the median of the pair variances. Make sure the moving window is properly centered so that half
the pairs in it are above and half below; for E32 a 33 pair moving window would be
=MEDIAN(E16:E48).

4. Pairs with average grades near the detection limit lack outliers because, if one of the values was
much larger than the other, the pair average places them farther from the detection limit.
Consequently, estimates of precision near the detection limit cannot be made in this way.
Proceeding down column E, delete entries until the results peak and start to decline. Pairs with the
highest average grades also have a problem: there are no pairs in the neighborhood above them.
Consequently, the formulae in the last cells must be altered by fixing the range used to calculate the
median. For example, if the data end at row 340, the formula for cell E320 is not
=MEDIAN(E316:E348); its =MEDIAN(E16:E$340).

5. Calculate the ratios of each pair variance to the median of its neighborhood; for example, G32
=E32/F32.

6. Copy the values (paste special - values) of this worksheet to another worksheet and sort in
descending order by the ratios in column G. The outlier candidates are now sorted to the top of
the list.

7. If one knew what percentage of the pairs have large clerical or other Type 1" errors, one could
then just select the appropriate number of pairs at the top of this list as probable outliers. In the
absence of any such estimate, a fixed percentage could be selected, or the scatter plot made and
varying numbers (from the top of the list down) plotted as outliers. This is a refinement on a

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simple visual approach, in that one makes a subjective judgement in this case on the number of
outliers, but does not choose which points are outliers. It is therefore arguably a more objective
selection. If doing a strictly visual selection, it helps to keep the x and y scales the same, or switch
which data set is x and which y.

8. If the outliers selected disagree with common sense, remember that common sense rules: adjust the
size of the neighborhood upward or downward by at least 20 percent and look for improvement.
This can be quickly done by editing the formulae in column F32 (step 3). Dont forget to edit the
formula for the highest values (step 4).

Sometimes, a disproportionate number of outliers are found at the very highest grades (where the moving
window is shrinking as the end of the grade distribution is reached). This can be the consequence of
certain Type I errors, such as misplacing the decimal point or failing to convert results from one unit of
measurement to another (e.g. a few results are in ppb and most are correctly in gm/t). It can also occur
because the scatter is increasing, but the estimation method near the tail-end of the distribution lacks
sufficient data to properly extrapolate.

6.4 Deriving a Pass-Fail Look-Up Table Based Upon Identified Outliers

The most common missing feature of Quality Control using duplicate data is a documented procedure for
failing the duplicates. Many commercial laboratories have rather sophisticated algorithms built into their
LIMS (Laboratory Information Management Systems) that set off alarms when processes go out of
control. Because these involve a stream of data that usually comes from a number of different clients, it is
not practical for them to present these data and maintain confidentiality over their clients data. At least,
this is one argument that has been made.

Such systems monitor both the frequency and magnitude of deviations (typically in units of standard
deviation) from optimum values. For example, a single result one standard deviation higher than the best
value (mean) should be expected to occur with a certain frequency. If seven consecutive results are out
by more than one standard deviation, this is improbable, and will trigger an alarm in some systems. In
contrast, a single result out by 3 standard deviations typically triggers an alarm.

The laboratory can exercise control over batches of samples. It is usually impractical for the geologist to
attempt to do so. However, once one has a hundred or so duplicates of some kind, one can generate a
table for deciding whether a pair of duplicate results are sufficiently close to be acceptable. Such a table
will show acceptable amounts of differences for grade ranges, as estimated by the pair average. All the
state laboratories of the former Soviet Union were operated on one look-up table. In that cost-insensitive
environment, all samples were assayed for gold in duplicate. Then the official table (Table 6.1) is
consulted2. Does the sample pass for the class of laboratory you are? If not, back it goes for two more
assays.

2
from: Branch Standard: Control of Quality of Analytical Work, Operational lab control of coincidence (repetition)
of the results of quality analyses of mineral raw materials, OST 41-08-214-82 Official Issue. Approved by the Order of
Ministry of Geology of USSR Sept. 9, 1982. Introduced into work July 1, 1983.

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Table 6.1
Official State-Prescribed Tolerance Limits
Grade Range, Au Tolerance in percent*
g/t Laboratory "Class"*
min max a b c
50 99 8.9 18 25
20 49 15 25 33
10 19 23 33 55
5 9.9 33 50 75
2 4.9 50 75 83
0.5 1.9 75 83 83
0.2 0.49 83 83 83
* | Pair Difference | / (Pair Mean)

The drawback to this approach (besides its low cost-effectiveness) is that geologic deposits do not
conform to socialist ideology: some have visible gold, giving a strong nugget effect, and some do not.
Thus the table, which one might at first glance think would be a cake walk for a commercial assay
laboratory in the West, would in fact, for coarse gold deposits, become a nightmare of repeated assaying.
A possible socialist solution to this dilemma is to fob off the deposits with a strong nugget effect on the
Class C laboratories, rather than risk losing ones Class A status. The probable ironic result is that the
samples most difficult to assay wind up at the laboratory least equipped to handle them.

A better approach is to tailor a pass-fail table to the material and protocols being used. Once a program
has a large number of duplicate pairs of the same type, including some outliers, visual identification of the
outliers can be used to establish the pass-fail criteria for a look-up table. This is achieved by some
additional work using the procedure to identify outliers (sect. 6.3). The variances calculated for the pairs
of duplicate results are equal to [a-b]2, where a and b are the two duplicate results. Using the criterion
ratio (steps 5 and 7 in sect. 6.3) selected for what defines an outlier, one can calculate the acceptable
difference (a-b) for each pair mean.

In most cases (exceptions occur for some deposits that have more than one population of ore minerals that
have very different particle size distributions), the variance can be expected to increase or stay the same
with increasing grade. The precision goes down, because it is proportional to the square root of the
variance divided by the mean, but the variance creeps ever upward (it is monotonicly increasing with
respect to grade).

Proceeding on from the steps in Section 6.3:

9. Find the lowest ratio of [pair variance] / [median pair variance] (call it p) in the outlier population
(i.e., the smallest ratio needed to qualify as an outlier).

10. In a separate column, say column H, calculate the criterion variance for a pair failing from
p*median variance. To smooth this into a monotonicly increasing function, use (for example, in
cell H23): =max(h22,p*E22) where E22 contains the median pair variance of the neighborhood
(see steps 3 and 4).

11. Calculate the pass/fail pair difference (a-b) in a separate column I. Continuing the example, I32
contains the formula =SQRT[2*H32]. Round these differences off to match the source data, for
example if the source data have 2 places after the decimal point, the pair differences should also.

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12. You now have a step-shaped function. The largest acceptable pair difference will be constant for a
range of mean values, then increase. From this, construct a table, by finding the minimum and
maximum pair means for each pair difference. This produces a look-up table having the structure
of the example in Table 6.2

Table 6.2
Example of part of a Pass/Fail Table for Duplicates
If Pair Mean is and |Pair Difference| Must Be
>= < <=
0 0.2 0.1 (all pass)
0.2 0.6 0.2
0.6 1.1 0.3
1.1 1.7 0.4
1.7 1.9 0.5

One now has a table that a clerical person can use to identify failures in returning data. This is much more
effective and consistent than scanning the duplicate results for big differences.

Outliers identified using such a table should be fairly rare occurrences that are related to large Type I
errors. The first action to take with these is to look for probable data entry errors and sample mix-ups. It
may be necessary or desirable to request re-assays of these pairs of samples. If the disparity is a result of a
reporting error (such as transposing digits while reading the instrument) or assaying error (spilling or boil-
over), reassays of the two duplicate samples will provide results which agree with each other, and with
one of the two original duplicate results. If re-assay gives two disparate results similar to the first pair of
results, it indicates the samples have been mixed up. It is very useful to distinguish these two conditions,
so that the appropriate remedial action can be taken.

6.5 Laboratory Drift

For each report, it is important to plot the running average of each SRM against a time sequence, so that
laboratory drift can be monitored. The difference between the averages in the original and check assays
can also be plotted against a time sequence. These two plots will detect any laboratory drift that may
occur. Where there have been failures and laboratory reports have been revised, the old data should be
excised and replaced with the new before calculating the result. Prolonged differences (over a time-span
of 10 or 20 SRMs) of more than five relative percent are generally unacceptable. The laboratory should
be made aware of the drift, but without disclosing confidential information about the identity and grades of
the blind SRMs. This is usually best done by supplying information on the check assays rather then the
standard results. The blind SRM results should only be used as a "last resort" when attempting to resolve
a problem with the laboratory; first ask the laboratory to present the performance of its own inserted
standards for the time frame in question.

6.6 Practices to Monitor Quality

Sample pulps should be re-homogenized if the samples are shipped any distance. MRDI recommends that
the pulps be passed through a ring-and-puck pulverizer for 10- to 20-seconds prior to weigh-out; this
reduces segregation that may have occurred by settling of denser particles, segregation by particle size or
shape, caking, etc. Obviously, samples selected to monitor the grind quality of pulps should have aliquots
for this test removed prior to re-mixing the pulp in a pulverizer. In this case the fraction taken for the
screen test should be collected by rolling and spreading the pulp on a small mat and taking many small

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grab samples. A better sample is obtained by passing the sample through a vibrating micro-splitter, but
this is rarely done; most laboratories do not have one. The subsample used for the wet screen test should
be discarded, never returned to the sample pulp bag.

Most commercial laboratories complete fire assays of low-grade samples with an AAS-flame finish as
opposed to weighing the bead (gravimetric finish). The check laboratory should routinely finish fire
assays grading in excess of 1 to 2 gm/t by gravimetric method, because it is more precise for high-grade
gold samples. This provides a good check on the primary laboratorys AA-flame finish, which can be
affected by dilution and calibration errors.

As mentioned previously, the umpire laboratory should measure the pulp quality (fineness) of some of the
pulps sent to it from the primary laboratory. A measurement of quality is much better than a qualitative
feel, which cannot easily be documented. Usually testing one pulp in 10 (of pulps submitted for check
assay) is sufficient. Since the umpire laboratory is provided with approximately five percent of all pulps
for check assay, this means that about one-half of one percent of pulps will be tested for adequate
pulverization. Pulps should be tested using the screen size expected to allow 95 percent of the sample (by
weight) to pass through. This should be done by weighing out 10 or 20 grams of dry pulp reject and wet-
sieving it through a small screen, drying and weighing the oversize fraction and calculating the percent
passing the screen. This is a quality control step; the purpose is to maintain quality during the project.

If the primary laboratory does not quote the percentage of material expected to pass its specified screen
size, convention is to assume that 95 percent should pass that size (P-95). This passing percent has been
found through experiment to provide the most reliable estimate of average particle size regardless of the
grinding technology employed. Sometimes the word "nominal" is used for the screen size, as in "pulps are
ground to a nominal -150 mesh", that, in this context, means "in name only". This is not acceptable.
Instead, a specification that states the screen size through which 95 percent of the sample (by weight)
passes, should be obtained from the primary laboratory. The laboratory should be required to meet their
own specification with a failure rate (determined by random routine testing performed by the umpire
laboratory) of less than five percent. The P-95 screen size should be that size which achieves reproducible
results on pulp duplicates (as previously stated, within 10 relative percent, 90 percent of the time).

In the case of gold deposits, the particle size is much more critical than, say, in the case of copper
deposits, where reproducible results can be obtained even with relatively coarse pulps. For gold, a starting
point might set a specification of 95 percent of the tested pulp reject passing a 150 mesh screen. Again,
requirements of sampling theory make it necessary that the criterion be stated in terms of P-95;
performances stated in terms of other percentages (such as "85 percent passing a 200 mesh screen, or 100
percent passing a 100 mesh screen") should not be used. If the primary laboratory uses a specification
other than P-95, it can be accommodated by using 2 screens, one for the probable P-95 size and the other
for the laboratorys stipulation.

It is also critical to obtain a consistent and adequate size reduction during crushing of drill samples prior to
taking a split for grinding down to a pulp for analysis. The sample preparation facility should dry screen
one split of coarse reject from a randomly selected sample during every shift it operates, and adjust the
crushing equipment when necessary. "Nominal -10 mesh" crushing is typically more deplorable than
"nominal -150 mesh" pulverization in its departure from the 95 percent passing requirement. It is not
unusual to discover that a preparation laboratorys " -10 mesh" crush translates to be only 50 percent -10
mesh. Not only should the preparation facility perform this test every shift, but it should routinely plot

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each test result on a graph posted in the sample crushing room; this is very rarely done except for
laboratories that are complying with ISO practices.

Within practical limits, the project geologist and company geochemist (or person charged with monitoring
quality control) should make periodic, unannounced visits to the primary laboratory and sample
preparation facilities to review procedures, and examine overall facility organization and cleanliness. This
should include making sure that inserted quality control materials are receiving the same treatment as drill
samples, and that stipulated particle sizes are being measured and maintained. A brief memorandum
documenting their visit is a useful addition to the QA QC file.

On visits to the sample preparation facility, a random sample of coarse reject should be tested to ascertain
if the crushing is adequate. Sometimes, one discovers that the preparation facility does not even have a
screen to perform such a test.

6.7 Suggested Levels of Accuracy

For use in resource models where outside financing is sought, MRDI recommends that the average grade
of all the check pulps should be within 5 percent of the average grade of all the original pulps so checked
(this criterion is in addition to the quite different criterion of less than 10 percent of check assays having a
relative difference exceeding 10 percent). If it is not, an umpire laboratory can be used to assay the
samples with the largest disagreements between laboratories. It is less costly to monitor laboratory
performance and correct procedural flaws than to engage in an extensive re-assay program late in the life
of the project.

Any outliers should be identified and omitted before calculating the averages used to compare the original
and check assays. However, the outliers should be accounted for by requesting re-assays be performed by
the check assay laboratory. This is easily done if the results are evaluated shortly after they are received.
If the check assay laboratory gets nearly the same result on re-assay as its first assay, the outlier can be
considered to be an error made by the original assay laboratory. The frequency of such errors should be
reported, and should not exceed five percent of the original assay population. If it does, protocols should
be modified in order to reduce Type I errors.

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6.7 Suggested Levels of Precision

Poor precision has many subtle effects on the resource model; it reduces the certainty with which any
particular block in a resource model can be classified as ore, makes production schedules less reliable, and
can lead to a mineral inventory where fewer tons are placed in the proven and probable or measured
and indicated categories and more tons are placed in the inferred or possible category. Sometimes
the distribution of ore in the deposit is problematic, and efforts to improve the precision of the sampling,
preparation and assaying are largely unsuccessful. In other cases, the Project Geologist or other
competent person jumps to the conclusion that the ore distribution is responsible for the problems of
precision, and makes no effort to improve sampling, preparation, and assaying protocols that would
improve the resource model.

Precision becomes very poor when the number of ore particles in the sample aliquot undergoing assaying
drops below 20 (Bacon, et al). In such a case, the addition or subtraction of one particle can change the
grade by more than five percent. This problem is largely restricted to diamond and precious metal ores.

For any ore, the precision becomes problematical as one nears the analytical detection limit, where
precision is plus or minus 100 percent (usually stated for 2 or 3 standard deviations). If the anticipated
ore-waste cutoff is less than 15 times the analytical detection limit, there will usually be trouble.

As a rule of thumb, if 90 percent of same-pulp duplicates or replicates with pair mean grades above the
anticipated ore waste cut-off have a relative difference (pair mean divided by pair difference) within 10
percent, then the pulp grind, assay aliquot size, and assay method can be described as providing good
precision. Similarly, if 90 percent of the coarse(st) reject duplicates have a relative difference within 20
percent, the preparation protocol can be considered to provide good precision.

If 90 percent of duplicate samples collected at the drill site agree within 30 percent, the overall precision
can be considered sufficient, provided the average length associated with a sample is less than half the
anticipated mining bench height; if the mining plan is very selective, the precision has to be better in order
to support it.

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7.0 ANALYSIS AND PRESENTATION OF QA-QC DATA

It is advisable to maintain a visual record of laboratory performance updated as new data are received.
Graphical representations, if done well, summarize the entire project history and thereby provide useful
context for the current results. Personal preferences play an important role in the precise nature of such
graphs. The following examples are ones that MRDI finds useful.

The most common kind of control chart is one that displays the performance of a standard over time. This
is usually done as a line graph (not an xy graph) so that the performance is plotted in sequence, but the
spacing is not proportional to the time between analyses. It is useful if large time gaps, changes of
procedure, etc., are annotated on such a chart. It is also quite useful to have the sought value, and the
upper and lower tolerance (pass/fail) limits drawn on the chart as three horizontal lines. A moving average
can be plotted to show any laboratory drift. An example of such a control chart, using synthesized data, is
shown in Figure 1.

A scatter plot of check assay results is practically a must. In this graph, the check assay result is plotted
against the original result (Figure 2). For reference, the x = y line and/or the lower and upper pass/fail
limits should be included. The mean obtained from each laboratorys results should be stated. After
excluding outliers (either visually or statistically) a "best fit" regression line can be calculated for the data
and the correlation coefficient r can be calculated. Any outliers that were excluded from statistical
calculations should be marked on the chart so that others can judge the reasonableness of their rejection.

For the best fit calculation, the method of Reduction to Major Axis (RMA) is recommended (Agterberg
1974, Davis 1986). This approach does not introduce any underlying assumption about which data set is
correct, and makes an allowance for any difference in population variance between the two data sets. The
RMA slope is the ratio of standard deviation of the y population to that of the x. The intercept b is
calculated by solving the linear equation, y = mx + b, for b, using the mean of the x population for x, the
mean of the y population for y, and the RMA slope for m.

A final addition to the xy plot can be a line showing a pairing based upon arranging the x and y sets in
ascending order. This trace can often include the outliers, because outliers are often the result of sample
mix-ups. This line is sometimes referred to as a quantile-quantile (Q-Q for short) plot because it matches
percentiles of the x and y data sets.

Another graph that is effective at characterizing precision is made by plotting the sorted absolute value of
relative percent differences against percentile rank (Figure 3). To make this plot, calculate the absolute
value of the difference and divide by the mean of the pair, as in the formula:
absolute value [ 2*(A-B)/(A+B)].

For pairs of data performed by the same laboratory, this equation is equal to twice the relative standard
deviation. Convert these values to percentages and sort them into ascending order. This provides the y
values for an xy graph. For the x values, calculate the corresponding percentile for each value. For
example, for a population of 130 such pairs, the percentile rank of the first (lowest difference, typically 0
percent) pair is 1/130 = 0.77 percent. This amount is then added to the previous x value to produce a set
of ascending percentile values. If done correctly, the last x value has a value of 100 percent.

Mineral Resources Development Inc., U.S.A. 650 358-1116 41


There is also a percentrank function in some software spreadsheets. These provide a less smooth graph
because ties are given the same percentile rank, then the percentile value makes a larger jump at the next
increase in absolute value of relative difference.

Because the relative percent differences are large near the detection limit, it is wise practice to discard data
pairs that are near (less than 10 to 15 times) the detection limit when making this kind of graph, or to
make 2 separate lines on the same graph, one of which excludes paired values with a pair mean near the
detection limit.

Precision varies with grade. Thompson-Howarth graphs (see references of same name) are one approach
for showing how they do so for a particular set of x,y pairs. Because they have an underlying assumption
that is not always correct, this approach sometimes fails, and sometimes misleads. The underlying
assumption is that there is a linear trend to pair variance with increasing grade. This is true in geological
systems where the particle size is constant. For example, if increasing grade of gold ore samples in a
deposit is proportional to the number of particles, then this approach works. However, higher-grade
samples often have larger particles rather than a large number of small particles. In such a situation, the
pair variance cannot be approximated by a linear trend.

A more flexible approach is therefore to plot moving averages, and thus show a less-idealized
interpretation of how precision varies with grade. This requires a large set of xy data, at least a few
hundred pairs. Outliers must first be identified and removed from the data set. The difference and mean
of each pair are calculated in a software spreadsheet, and the pairs are sorted by pair means. A suitable
window (typically more than 16 put less than 1/10 of the population) is chosen, and the standard
deviations of the pair differences and means of the grade are calculated for the window. The formulae are
copied down the rows so that the last entries have a moving window that ends with the last (highest mean
grade) pair. Finally, in each row, the ratio of the moving window of standard deviation is divided by the
mean grade (of the same window) in order to state the standard deviation as a percentage; these numbers
are plotted against the average grade number to create a curve of the general form y = m/x + b. An
example of such a curve is shown in Figure 4. In this example, one is alerted to worsening precision at
higher grades. A Thompson-Howarth interpretation would not reveal this fact.

Mineral Resources Development Inc., U.S.A. 650 358-1116 42


QA-QC Guidelines

STANDARD CONTROL CHART


STANDARD NUMBER 1

2.4

Overall 4% low bias. Drift exceeding 10% low:


Acceptable in most unacceptable if it continues. Data

cases.

2.2 9-point moving average


GOLD IN GM/TON

Best Value

2 LAB. MEAN

P/F INNER

1.8
Preferred Range:

FAILURE

Best Value +/- 5 %

1.6
934458 934979 935141 944424 945525 946125 946242 947039 9421879 9421885 9321933
LABORATORY CERTIFICATE NO.
Figure 1. Use of a moving average on a control chart to show laboratory drift.

Mineral Resources Development, U.S.A. (650) 358-1116


QA-QC Guidelines

SAME-PULP GOLD ASSAY CHECKS


N=55. Mean LAB C = 0.96 gm/ton, Mean LAB A = 0.95 gm/ton.

Data

6
x=y
LAB A Au (g/t)

4 Q-Q

RMA fit
2

0
0 2 4 6 8
LAB C, Au (g/t)

Figure 2. An x-y scatterplot comparing two laboratories.

Mineral Resources Development, U.S.A. (650) 358-1116


QA-QC Guidelines

"COARSE GOLD" PROJECT, SA


LAB A INTERNAL PULP REPLICATES
180%

160%
ABS. RELATIVE % DIFFERENCE

140%

120%
Recommended precision is +/- 10% for 90% of the data.
100%

80%

60%

40%

20%

0%
0% 10% 20% 30% 40% 50% 60% 70% 80% 90% 100%
PERCENTILE RANK

Means >0.45 gm/ton Au, N=465 All data, N=718

Figure 3. Example of a graph to assess laboratory precision.

Mineral Resources Development, U.S.A. (650) 358-1116


QA-QC Guidelines

Sorted by pair means, groups > 0.01 oz/st Au

100%
[Std.Dev.16 Pair Diffs.] / Mean

80%

60%
Rig
Pulp
40% Coarse Rej.

20%

0%
0.00 0.05 0.10 0.15
Mean of 16 Pairs, Au oz/st

Figure 4. Assessment of precision versus grade using moving windows of standard deviations of pair differences divided by
mean grade, versus mean grade.

Mineral Resources Development, U.S.A. (650) 358-1116


8.0 DATA TRANSFER ERRORS

Reporting errors frequently occur when data are transferred from paper copies of laboratory assay
certificates into computers (or onto maps or cross-sections). For assay data, there are six common types
of reporting errors:

Shifting results by one drill hole sample interval


Shifting the location of the decimal point in a result to the right or left
Entering data into the wrong field
Transposing digits
Misreading (guessing) results off illegible facsimiles, photocopies, or hand-written notes
Handling data below detection limit inconsistently.

While these different types of errors can be sought, it is better to find and detect all data entry errors.
Such errors committed outside the laboratory can be virtually eliminated by obtaining laboratory reports as
computer files. In cases where data have been hand-entered, efforts should be made to obtain computer
files from the assay laboratory to correct these data. This may require reformatting of the laboratory
computer files, which can be quickly done by someone skilled at manipulating computer data. Data can
then be completely cross-checked using one of the many database software programs, such as Rbase,
Foxpro, dBase, Paradox, Access, Informix, etc. Cross-checking data is not practical using spreadsheet
software such as Lotus, Quattro-pro, Excel, etc.

Where data are unavailable from the laboratory in computer format, the error rate within the assay
database should first be evaluated by checking a random selection of five percent of the intervals from
each drill hole. These should be checked against a completely legible (not a facsimile or poor-quality
photocopy) copy of the assay certificate. If the error-rate of data to be utilized in resource modelling
exceeds five errors per thousand entries (one-half of one percent) the data should be re-entered from good
quality copies, the two data-sets cross-checked using database software, and all errors thus located and
corrected.

In addition, a separate check of the highest top 3 percent of results should be made. If a high error rate is
found amongst these results, then the next-highest 3 percent of data should also be checked and corrected,
and so on until the error rate is below 0.5 percent.

In an on-going project relying on hand-entry of assay data, it is advisable to routinely enter all data twice.
Two different people should be used so that the same person does not enter the same data twice. The
same person is more likely to repeat the same mistake, for example, misreading a "7" as a "1".
Precautions should be taken to insure that all data are indeed entered twice and not copied from one file to
the other, which defeats the purpose of dual entry. The two sets of entered results are then transferred
into two database tables, cross-checked for inconsistent entries, and every such disparity located to
determine the correct entry and make a final database free of data entry errors.

48
9.0 COMMON MISTAKES AND PITFALLS

A number of sources of error occur repeatedly in the industry. Some of these are a result of unforseen
consequences or misapplication of policies known to be appropriate for other situations. Others are a
result of insufficient failsafes being put in place.

9.1 Lack of Vigilance

QA-QC programs must be monitored on an on-going basis, as the exploration or drilling program
progresses. Review must not await completion of program or year-end analysis. When everything goes
right, those who elect to defer this task until the end of the project are encouraged to do so again on their
next project. Sooner or later, everything does not go right, and the project suffers from their wishful
thinking and procrastination.

Without feedback there is no quality control. Frequent monitoring of preparation and analytical
performance prevents systematic errors. If stipulated levels of precision are not sustainable, then changes
can be made to sample preparation procedures (e.g. second-stage crushing in a rolls crusher; making a
larger pulp; etc.) or the analytical methods (e.g. changing from a 1 assay-ton to a 3 assay-ton or screened-
fire "metallics" assay, etc.)

Changes in staff at the sample preparation or assaying facility or at the point of collection at the drill site,
increase the likelihood that changes in sample handling protocols will be made, out of ignorance. MRDI
has encountered many examples of this:

A simple blast-hole sampling device, shaped like a triangular slice of pie with the tip cut off, was designed
to obtain a more representative sample: by orienting the tray like a pie slice, with the narrow end next to
the hole, proportional amounts of lighter (thrown farther from the blast drill hole) and heavier particles are
collected. A later visit found the device in use, but the sampling tray was thrown down next to the drill
hole with no particular orientation, making it worse than useless.

A visit to one of a major international laboratorys sample preparation facilities, conducted with two days
advance notice, found a technician riffle-splitting samples in a manner suggesting he had never been given
the two minutes of instruction required to perform this critical task properly. He was pouring the sample
out of the corner of the pan through a few of the center chutes of the splitter. When questioned, it was
found there was presently no sample preparation manager; no one was in charge.

A laboratory, asked to perform both cyanide-soluble and fire assay gold determinations, routinely replaced the
cyanide-soluble result with the gold fire-assay result, if it exceeded the fire assay result, because it was impossible
for the CN-Au result to be higher, thereby creating a low bias in the cyanide-soluble gold results within the oxide
zone. Original assay data had been discarded.

A set of check assays showed a substantial low bias relative to the original assays until it was discovered
that the person processing the check assay data had simply removed all the > signs from the check assay
reports, so that the highest grade samples, having grades exceeding the upper limit of the assay method,
were misrepresented as having grades equal to that upper limit.

49
A set of copper check assays was subjected to numerous highly sophisticated statistical tests and numerous
reports were written, providing a conclusion that although there were marked differences between the two
sets of results, the difference could not be considered statistically significant. Upon changing the scale of
the xy plots, MRDI discovered that the laboratories agreed closely for the samples low in copper (waste
grade) which constituted about 80 percent of the assays, but had a large disagreement (bias) for the ore-
grade samples. The authors of the statistical treatises had failed to examine the data closely enough, by
changing the scale on a graph, to find this fatal flaw.

The mine laboratory of a highly successful mine never sent any of its samples out for check assay, nor did it
periodically evaluate its accuracy using certified reference standards. Subsequent check assays revealed
this laboratory had been underestimating the grade of its commodity by more than five percent for years.
An audit of the laboratory uncovered an incorrect conversion factor used to calculate the grade of its
calibration standards; the wrong factor had been used to make up calibration standards for more than five
years.

The most disastrous quality control failures involve poor sample collection, because if the collected sample
is not representative, re-assaying it provides no benefit. Disasters also occur when the person splitting
core intentionally cuts the core to obtain pieces of unequal grade, either because nice specimens are being
preserved, or to obtain higher assay results.

9.2 Loss of Fines or Water-soluble Ore minerals

Loss of fines impacts the accuracy of ore estimation when the grade of the fines, on average, differs
significantly from the grade of the rest of the sample. A statistically significant difference can be
established by an appropriate statistical test, such as the Sign Test or a t-test. With large sets of data, it is
sometimes possible to establish a statistically significant difference that is not economically significant (i.e.,
the bias created is too small to impact the model).

Try to avoid this quagmire by minimizing losses of fines while also testing for the effect. This should
include not allowing sample collection buckets to over-flow during wet reverse-circulation drilling.
Similarly, during initial core in-fill drilling, drill muds should be sampled for several holes, to ascertain if
their grade differs greatly from the associated core.

In some circumstances, such as drilling copper oxide deposits with water-soluble minerals, a more
representative (and higher grade) sample may be obtained by reverse-circulation rather than core-drilling,
because of losses caused by water. For some deposits, dry reverse-circulation drilling may be more
difficult, but necessary in order to obtain a representative sample. In many such cases, the dust recovery
system on the drill rig must be upgraded beyond what is normally used. In other cases, the presence of
groundwater precludes the option of drilling dry; careful use of drilling additives and adjustment of drill
operational parameters can reduce the probable bias.

In cases where water is biasing a sample, using a rock saw to split core only worsens the problem. In
such situations it is preferable to use a core splitter, even though it provides a much more uneven split.
Which half is taken for assay should be alternated, because the two sides of a core-splitter or a saw blade
are never identical (for example, one will pluck more than the other). In some production situations, it is

50
reasonable to prepare the entire core for assay (the core is not split). This practice is frowned upon
because it was one of the important components of the Bre-X fraud.

Dust losses during sample preparation can also be appreciable. These should be monitored by selecting
one or two samples each shift and weighing all the components (weight of sample in, weight of sample and
rejects out) to determine the effect. This will be a function of rock type; the results should be analyzed
accordingly. It is not uncommon to find steps in the preparation procedure that have more than 10
percent sample loss. Where dust losses are high, adjustments and maintenance are indicated, such as
replacing o-ring seals on pulverizer bowls and adjusting the ventilation of the dust-control system.

9.3 Mishandling of Standard Reference Materials

Solids are very difficult to mix. In fact, a highly homogenous solid mixture of powders containing several
components with different physical properties (especially density and particle size) is in a very unnatural
state; any shaking or rolling of such a material will result in a decrease in its homogeneity (that is,
producing an increase in its heterogeneity, or segregation). However, if a material is in a highly
segregated state, rolling or shaking it will probably reduce the segregation. Hence whether this treatment
is helpful or not depends upon the initial state of the material; it may be helpful to briefly roll or shake a
material that has just been screened for a metallic (screen) fire assay, because the screening has created a
highly segregated condition in the (undersize) sample. On the other hand, rolling or shaking a sample that
has just been passed through a high-quality splitter will likely result in a worse condition than if the
material was not so processed. And, in the case of rolling and shaking, more is not necessarily better
(Campbell, 1966). Where practical, instead of rolling and shaking, material should be passed through a
riffle splitter and recombined several times, and then a final split taken with a riffle splitter or, preferably, a
rotary splitter.

With certain materials, storage can become an issue. On the face of it, one would think that a gold
standard would be highly stable; the gold is certainly not going to volatilize out of the material at room
temperature, nor is it likely to oxidize. Unfortunately, the matrix may not be so stable. For a sulfide-rich
gold standard, the sulfides in the material will react with oxygen and water in the air, effectively diluting
the gold grade of the material; a kilogram of sulfide-rich material containing say 500 milligrams of gold
may, over time, become 1.1 kilograms of mixed oxide and sulfide material still containing 500 milligrams
of gold. The observed gold grade is then 10 percent lower than it was previously. The rate at which this
happens can be greatly reduced by keeping the materials extremely dry. Unstable standard reference
materials used for special assays may require additional care in storage, but for the majority of situations it
is only necessary to store thoroughly dried material in air-tight bags, or in an air-tight container that
contains a drying agent (desiccant).

It is very common for technicians inserting standard reference materials into laboratory shipments to
improperly record which SRM they insert. There have been many instances where over ten percent of the
SRMs were misidentified, and others where no identification of the SRM was made, other than "standard",
when there were several possible choices. This makes the performance charts look terrible, and of course,
one should re-assay all such mix-ups to be certain this is not a laboratory error.

51
9.4 Introducing Selection Bias

One practice, which is sometimes useful in some exploration programs, should be avoided in drilling
programs for a feasibility study. This is the practice of routinely selecting samples for re-assay based upon
the results of the first assay. This practice can be useful in, for example, a stream sediment sampling
program or with soil samples, because it will reduce the number of false anomalies, or "false positives"
that are a consequence of laboratory error. As a consequence, the explorationist can set priorities on
which anomalies are most promising.

There are instances where an exploration geologist has requested re-assay of all his gold anomalies only to
find that all his anomalies have disappeared. Human nature is to immediately blame the assay laboratory.
It is more probable that the disappearance of all the anomalies is a consequence of inadequate sampling
(usually too small a sample size) and/or inadequate sample preparation, coupled with a large average gold
grain size.

Selecting out the samples with the highest results in a resource definition drilling program will almost
always result in lower estimates of average grade in the re-assay results than in the original results. The
relative difference between the two sets of results will be larger when the sampling variance is high, and
lower when it is low. This happens because the selection of which samples to re-assay is not independent
of the variable being checked: the original assay. Large positive errors in the original results will be found,
but large negative errors will not. If there are a lot of large errors (that is, the assay precision is low) then
the average of the second set of assays will be markedly lower than the first.
If there are very few large errors, then the average of the second set of assays will be very close to the
first.

A simulated distribution may serve to illustrate this effect. Assume you are provided with a set of 1,000
results that contains 30 very large sampling errors where the result differs from the true value by a factor
of ten or more, half the time ten times smaller, and half ten times larger. If you re-assay the highest 50
results, you are quite apt to include many of the errors where the sampling error was ten times higher, but
none of the errors where it was ten times lower. Large errors have been detected and corrected, but the
average grade is now lower than it was before the errors are found, and lower than it would have been if
all the large sampling errors had been corrected.

Even where large errors are absent, there will be selection bias. This can be envisioned by another thought
experiment. Imagine that you have a thousand samples that you have analyzed twice. You arbitrarily
separate each pair of results into two columns, A and B, and find the two columns have identical means
equal to 2 grams/ton. You then decide to just select the pairs of results where the result in the A column
is above 4 grams/ton (this is equivalent to a re-assay criterion of 4 grams/ton). While most of the results
in the B column are also above 4 grams/ton, there are also a few values that are below it; all of the A
results below 4 grams/ton have been excluded but not all of the B results. Hence it is not surprising to
find the means of the two columns for this shorter list of samples are no longer equal, with column A
having a higher mean than column B.

52
Selection bias can be quite severe when coarse gold is present in the deposit, due to the "nugget effect".
This is because the sampling error is large. The majority of samples are below the (arithmetic) average
grade. Within this large group of low-grade samples, if it were to be re-assayed, are a small number of
samples that will return a much higher grade. In this situation, if one wishes to demonstrate the validity of
the original assays, one must make a selection that is not based on the original assay. It can be based on
geology, or on an "ore envelope" that encompasses ore grade intervals plus some adjacent intervals
irrespective of their grade. From this, a random selection of intervals can test for bias in the original
assays.

The safest approach to avoiding selection bias is to make a random selection for assay check, or to make a
uniform selection (e.g. every 20th drill sample) that is random with respect to grade. It is nearly as safe to
exclude some barren rock types from selection. The use of ore envelopes can be abused, and should only
be considered where the geology is well defined and can be used with confidence to distinguish ore from
waste with a fairly high degree of confidence. Where ore envelopes are employed for sample selection,
they should not be narrower than the largest contemplated bench height (or small mining unit dimension).

9.5 Preserving the Integrity of the Raw Assay Data

An assay database that accurately reflects values as reported on assay certificates should be maintained.
There is a common problem with samples which are reported with a "<" since the "less-than" sign is not
recognized as a numeric character by most software. The best convention to use is to replace the "<" with
a minus sign "-". This should be stated in the documentation accompanying the database. Another
problem arises with samples which were not analyzed, and appear as entries on the assay certificate such
as "n.a.", "insufficient sample", "not received", "missing", etc. The best convention to use is to replace all
such entries with the numeric entry "-99.9", since this value is very unlikely to correspond to the analytical
detection limit of any result. Other software, such as MEDS, may later require a different convention for
such data, such as "-1", but this should be avoided in the "raw" assay database because some assay results,
such as silver, may have an analytical detection limit equal to 1 gram/ton, and hence a value of "-1" in such
a case would be ambiguous. A very sophisticated database might use different codes for different types of
non-numeric information; for example insufficient sample might be represented as -99.8 while
missing sample might be entered as -99.9. These may be useful for compiling operational statistics,
such as the percentage of samples that were lost; or relating insufficient sample to poor drilling recovery
or mistakes in sample preparation.

The use of values other than that obtained by replacing the "<" with a minus sign is not recommended
because large databases sometimes contain assay results where the analytical detection limit has changed
over time. Hence information will be lost which is not easily recovered and worse, misinterpretation of
assay results is possible. For instance, an assay database may contain arsenic results, some groups of
which have been analyzed with a 50 ppm detection limit, and other groups of samples which have a 5 ppm
detection limit. If results below detection are replaced with a value equal to half the detection limit, some
below-detection results in the first group may then be confused with samples having a 25 ppm result in the
latter group. The convention of assigning a value of "0" to results below detection should also be avoided
for this reason (in the case sited, a "0" entry is ambiguous because it may mean either less than 50 ppm, or
less than 5 ppm). Also, "0" entries are risky because in transferring data between different computer

53
software, this value is sometimes assigned by the software where a field is blank. If this happens, it is
possible that samples which were not analyzed will be mis-interpreted as having been analyzed and found
to be below detection. Such an error could have severe repercussions on a resource model constructed
from such data.

Sometimes intervals are not sampled and assayed because they are judged barren by sample inspection.
This should be avoided in cases where the geologic log data are unclear which samples would not be
assayed; i.e. that a hard boundary can and will be drawn in the geologic interpretation used to make the
resource model. If not, a very low value for the grade of any ore must be assigned to the unsampled
intervals, in order to prevent the interpolation of higher grades. In such cases, to avoid confusion, a table
should be maintained which lists the assignment of barren grades to unsampled intervals, or a unique code
must be used in the database. One cannot assign low grades to contaminants (i.e. components that incur a
penalty); in such cases the grade should be interpolated from nearby intervals assayed for the component.

An assay database that closely reflects the results shown on the assay certificates should be maintained.
Any subsequent manipulations of these results should be preserved in a separate database, along with
documentation on what manipulations were performed. The only exception to this should be the handling
of non-numeric characters in the results. Conversion of results to different units (such as ounces per short
ton to grams per metric ton) is best handled by adding a new calculated field to such a database. This
allows more straightforward auditing of the database.

Sometimes, in the case of solubility determinations, the raw data are compromised by a well-intentioned
geologist. A common example occurs in using dilute acid to estimate recoverable copper in an acid heap
leach. Typically, the geologist finds some results in the oxide zone where the soluble copper result
exceeds the total copper result. Knowing this to be impossible, he sets the soluble number equal to the
total copper number. While this is a little better than say, increasing the total copper number to match the
soluble copper number, it is just as invalid a practice.

The soluble copper and total copper assays are separate unbiased estimates of two different, but related,
components of the sample. If the soluble copper determination has a one-sigma precision of 10 percent
and the total copper assay has a one-sigma precision of 5 percent, for some copper grade, there will be
some occurrences where the soluble copper values exceeds the total copper value by 15 percent. The
frequency of this occurrence can be estimated by multiplying the probability of obtaining a soluble copper
value high by 10 percent by the probability of a total copper number being low by 5 percent. Since this is
one-sigma in both cases, there are about 16 percent for each of these, and the probability of both occurring
together is about 0.16 x 0.16, or about 2.6 percent of the pairs.

Because there will also be a roughly equal frequency of occurrences where the soluble copper number is
low by 10 percent and the total copper number is high by 5 percent, the data are unbiased. The geologist
cannot identify these pairs; he only sees the ones where the soluble copper result is too high.
Consequently, when he modifies the soluble copper results, he biases the population. The average soluble
copper grade, the distribution of ratios for oxide samples, and other aspects based on the soluble copper
population will now be incorrect and misleading.

54
Sometimes a laboratory will modify the soluble copper results so that no value exceeds the total copper
results. The absence of any pairs in the database where soluble copper exceeds total, in a large population
of data, is strong evidence that they have falsified some of their soluble copper results.

This misguided practice is also sometimes found to occur in the following data sets:

drilling recovery greater than 100 percent changed to 100 percent.

cyanide-soluble gold results exceeding fire assay gold results changed to fire assay value.

Raw results should never be modified to make them look better. In the process of subsequently
analyzing these data, such manipulations can be practiced, but the integrity of the source data should be
maintained (except for the use of unique numeric codes to transform non-numeric entries into a
compatible format, as previously described in this section). Any manipulations of that source data should
be placed in calculated fields and the rules of calculation clearly documented. This affords others the
opportunity to modify the original assays using a different set of rules.

Probably the most common and time-consuming problem in managing resource data concerns the lack of
consistently maintaining sample identities. This usually take the form of hyphens, extra spaces, mistyped
prefixes, and the like, but can also include using the same sample identifier for different samples collected
at different times.

55
10.0 QUALITY CONTROL OF THE GEOLOGIC DATABASE

Geologic information can usually be described as either observation (facts) or interpretation. For example,
an outcrop map typically is limited to observations. An interpretative layer, which interpolates geologic
boundaries from the outcrop map, is mostly interpretation. Geologic logs are the most common source of
geologic information used in resource models, and usually contain both facts and interpretations.
Typically, the rock type and alteration are interpretations that are based upon observed facts such as
observed minerals and proportions and alteration of those minerals (replacement of one mineral with
another, etc.).

Consistent reliable observation and interpretation is necessary in order to obtain useful parameters for use
in constructing a resource model. This often happens where many different geologists perform the
logging, using a logging form which does not provide sufficient guidelines as to what measurements are
needed for the deposit. A critical aspect of controlling the quality of geologic logs is a properly designed
logging form. The best designed forms are tailored to the deposit. Generic forms tend to produce
generic results. The most useless geologic logs can be produced when there is no logging form and the
logging is done by numerous geologists who do not read the previous logs nor agree with them.

Control of quality is better maintained if observations and interpretations are kept separate. This may
allow speedier modification of geologic interpretation. When the observations are absent and only an
interpretation is provided, it is usually necessary to re-log all the drill holes in order to successfully
upgrade the geologic interpretation of the deposit.

Logging and any re-logging or re-interpretation of drill holes should be fully documented with the identity
of the person performing the task and the date. If the data are computerized, this information should be
included in the computer database, because it allows the data to be analyzed statistically for biases which
may be a function of who has logged the drill hole. Differences in the frequency of particular observations
by different logging geologists can then be assessed for groups of nearby drill holes. Highly disparate
frequencies (especially occurrences of zero instances) by one geologist may point to mistakes in mineral
identification. Semi-quantitative observations (such as estimated percent sulfides) can be normalized to
the observer making them, when cross checking them against assay or geotechnical data for a given rock
type or geo-metallurgical zone.

Quality Control is enhanced by maintaining a training set of selected core boxes. These examples,
selected to present or remind the logging geologist of the variations present in the deposit, are logged, and
the results compared to a previously established consensus log for these example boxes. Logging
geologists returning from extended breaks or other duties should re-log these holes prior to commencing
on new drill holes.

The incidence of clerical errors has been greatly reduced in the last decade as a consequence of the
widespread use of computerized data transmission. This has avoided the introduction of keyboard entry
errors which took place when paper (or worse, facsimilie transmissions) copies of assay certificates were
entered by hand. Computerized entry of geologic data has not benefitted from this advance. In most
cases, there is little productivity to be gained by providing logging geologists with electronic devices for

56
direct entry of geologic information. However, thoughtful design of the system by which data are
arranged on a geologic log form, and subsequently entered into a computer, can reduce the incidence of
clerical errors.

An operation is more productive if the clerical entry does not require skills other then keyboard entry of
data. Written descriptions are seldom very useful for conducting the exploratory data analysis that
precedes formulation and checking of a final geologic resource model, whereas codes, indicating, for
example, what minerals are present, are quite useful.

Errors are reduced if the data entry form, which can be as simple as a few strings of digits and letters,
closely follows the way the data appears on the geologic form. Plucking bits of data from here and there
off a geologic form and then re-assembling them on the fly, mentally translating one code to another
before entering, or one code for several, or creating codes for varying combinations of information on the
form, will result in much higher error rates. These functions are best left to the computer, by applying
rules to the information entered from the logging form. It is also a much simpler task to audit the quality
of the data entry if there is a one-to-one relationship between the entered data and what appears in the
geologic logs.

Errors can be trapped in fields identified as having critical information by the double-entry of that
information. The two sets of entries can then be cross-checked using relational database software to
identify all entries that disagree. Disagreements are then resolved by a final examination of the drill logs
with entry errors.

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11.0 GEOTECHNICAL CONSIDERATIONS

In terms of the resource model, important quality issues include drilling recovery, bulk density
determinations, and in the case of reverse-circulation drilling, down-hole contamination.

Some geotechnical measurements, such as Rock Quality Data (RQD) can be affected by core handling and
transport after drilling. Results from different drill holes can under some circumstances be more a
consequence of how the core was handled during transport than of variations in RQD within a given
lithological unit. In such cases it is best to take at least some of the measurements in the field immediately
after the core is collected, in order to have a check on the effect of handling. These check boxes can then
be compared to the routinely collected data. This serves as a check on both the technicians routinely
performing the task, and on the effect of handling.

11.1 Drilling Recovery

Drilling recovery is nearly always measured for drill core. The boundaries of each core run are typically
marked with wooden blockes, upon which the drilled depths are written. A technician then sums up the
lengths of core between the blocks, and records this information along with the two hole depths; the ratio
of the core measured to the difference in depths written on the two blocks is the core recovery. As simple
as this is, there are cases where this has been done incorrectly, indicating the person assigned the task had
no understanding of the task. Once again, the best practice is to have an experienced geologist make some
independent measurements of recovery for a few selected boxes, and compare these to the routine
measurements.

Drilling recovery should be stated for separate geologic units. This should at the very least consist of a
statement of what the drilling recovery is within the different ore zones, compared to the overall recovery
and the recovery in waste zones.

Some lithological units (typically limestones) may have large naturally occurring open spaces (voids).
Efforts should be made to clearly distinguish and separate these occurrences from core loss as a result of
drilling technique. Projects in areas containing old workings sometimes also locate voids. These should
be very carefully recorded because they occur within ore zones and, if misinterpreted as bad core
recovery, can lead to wrong conclusions about the adequacy of the drilling recovery.

One should check for a relationship between drilling recovery and grade. Methods for performing such
evaluations are the subject of a separate MRDI document.

11.2 Down-Hole Contamination in Reverse-Circulation Drilling

The one piece of evidence most critical and most often absent for performing an evaluation for potential
down-hole contamination is the location of additions of drill rods. Good programs routinely mark on the
drill sampling logs the position of each rod addition, and important events such as bit changes, addition of
polymer, loss of circulation, etc.

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Methods of examining for down-hole contamination consist of looking for asymmetric distributions of
grade down-hole, and for regularly-spaced (drill rod length) spikes in grade.

11.3 Down-Hole Surveys

For inclined drill holes, or for holes that are deeper than 600 feet, it is advisable to collect at least some
down-hole survey measurements. If these indicate severe deviations are occurring, such measurements
need to be performed routinely. Where this is discovered late in a project, and some drill holes can no
longer be surveyed, the possibility of applying corrections to azimuths and dips in unsurveyed drill holes,
along with discarding data below certain depths, should be explored.

Devising corrections to unsurveyed drill holes, based upon surveyed drill hole deviations, is addressed in a
separate MRDI document.

For magnetic surveys, it is important to apply the correct declination for adjusting the readings to true
north. In some areas, the declination changes enough, and the project has been on for a long enough time,
that different corrections should be applied for holes drilled in different years.

11.4 Bulk Density Measurements

Bulk densities must be calculated on a dry weight, because the assays are done on a dry weight basis. It is
important not to lose sight of the goal of making an unbiased connection between the sample volumes of
the resource block model, the weight of rock associated with the block model volumes (the tonnage factor
or bulk density) and the assays (done on dry weights). What constitutes a dry weight in some deposits
(e.g. saprolites and laterites) must be carefully defined and the definitions adhered to.

Samples that have porosity must be thoroughly dried and then sealed before weighing in water.
Otherwise density measurements of porous rocks will be too high. Because of the role of porosity, bulk
density cannot be inferred from specific gravity measurements on powders, unless the porosity of the rock
is also accurately known.

A good program will dry to a constant weight for at least some samples in each group being dried: this is
done by weighing the selected dried sample, returning it to the drying oven for an hour or more, then
weighing it again to determine if the weight has changed. This is repeated for the batch until there is a
sufficiently small change in weight that the calculated bulk density is not affected. Drying to a constant
weight is much more problematical for saprolite and laterite samples.

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12.0 REFERENCES

Agterberg, F.P., 1974, Geomathematics; Developments in Geomathematics 1, Elsevier Scientific Publ.


Co., Amsterdam, 596p.

Bacon, W.G., Hawthorn, G.W. and Poling, G.W., Gold analyses - myths, frauds and truths, CIM Bulletin,
November 1989, vol. 82, no. 931, pp 29-36.

Campbell, H. and W.C. Bauer, 1966, "Cause and cure of demixing in solid-solid mixers.", Chemical
Engineering, Sep 12, 1966, 179-185.

Davis, J.C., 1986, Statistics and data analysis in geology (2nd ed.); John Wiley and Sons Inc., New York,
646 p.

The Canadian Mineral Analysts (John Labrecque, Ron Connell, Wes Johnson, Clint Smith), 1992, "A
Manual for to Quality Control and Quality Assurance in Analytical Chemistry".

Francois-Bongarcon, Dominique, 1996, "Extracting error variance information from paired data and
applications to sampling theory", Mineral Resources Development internal report, October, 1996.

Davis, B. and Widham, C., 1996, "Statistical control for the production of assay laboratory standards",
Mining Engineering, 48, No.3, 73-76.

Gy, Pierre, 1992, Sampling of heterogeneous and dynamic material systems: theories of heterogeneity,
sampling, and homogenizing, Elsevier Science Publishers B.V.: Netherlands. ISBN 0-444-89601-
5.

Thompson, Michael and Richard Howarth, 1973, "The rapid estimation and control of precision by
duplicate determinations", The Analyst, 98, 153-160.

Thompson, Michael and Richard Howarth, 1976, "Duplicate analysis in geochemical practice Part 1:
Theoretical approach and estimation of analytical reproducibility.", The Analyst, 101, 690-698.

Thompson, Michael and Richard Howarth, 1976, Duplicate analysis in geochemical practice, "Duplicate
analysis in geochemical practice Part 2: Examination of proposed method and examples of its use",
The Analyst, 101, 699-709.

Thompson, Michael and Richard Howarth, 1978, Duplicate analysis in geochemical practice, "A new
approach to the estimation of analytical precision", J. Geochemical Exploration, 9, 23-30.

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