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NORANDA INC. - FALCONBRIDGE LTD. DRILL CORE SAMPLING AND ANALYSIS PROTOCOLS Version 2.0 July, 2003

NORANDA - Drill Core Sampling and Analysis Protocols

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  • NORANDA INC. - FALCONBRIDGE LTD. DRILL CORE SAMPLING AND ANALYSIS PROTOCOLS Version 2.0 July, 2003

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    Contributors: Version 1.0 Analytical Solutions Ltd. Lynda Bloom Analytical Procedures, Quality Control Noranda Inc. Lionel Martin Six Sigma: Variation Identification and Analysis, Capability Analysis (removed), Variable Gage R&R (removed) Robin Adair Drill Core Procedures Matt Rees Field Procedures Reviewed by: Noranda Exploracion Peru Diane Nicolson Noranda Pacific PTY. Ltd. Craig MacDougall Simon Tear Jock Gilfillan Noranda Inc. Rory Kempster Version 2.0 Charles Beaudry : Theory of Sampling and Sources of Error in Assays, Digestion, Integrated Variance Studies, Assays as a Measurement System, Measure of Variance in Assays. Reviewed by: B. Mercer, L. Vandamme, C. Moore

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    TABLE OF CONTENTS Preface to Version 2.0............................................................................................................................................... 1 Introduction .............................................................................................................................................................. 1 Terms of Reference................................................................................................................................................... 2 1. Theory of Sampling and Sources of Error in Assays ............................................................................................ 5

    1.1. Sampling and Assaying as a Process ............................................................................................................ 6 1.2. Accuracy and Bias....................................................................................................................................... 7 1.3. Precision and Variance ................................................................................................................................ 7 1.4. Sample Switching........................................................................................................................................ 9

    2. The QAQC Manager..........................................................................................................................................11 3. Specifying Preparation and Analytical Procedures ..............................................................................................13

    3.1. Laboratory Selection ..................................................................................................................................13 3.2. Laboratory Communication and Service Contract .......................................................................................13 3.3. Preparation of Pulp Standards and Round Robin Surveys ............................................................................14 3.4. Sample Preparation ....................................................................................................................................14

    3.4.1. Crushing and Splitting ........................................................................................................................14 3.4.2. Pulverizing .........................................................................................................................................17 3.4.3. Digestion ............................................................................................................................................17

    3.5. Selecting Geochemical Analyses or Assay Determinations..........................................................................18 3.6. Analysis for Deleterious or Secondary "Pay" Elements ...............................................................................19 3.7. Documentation...........................................................................................................................................20

    4. Quality Control at the Sampling Stage................................................................................................................21 4.1. Blanks........................................................................................................................................................21

    4.1.1. Preparation of Blanks..........................................................................................................................21 4.1.1.1. Materials Required ......................................................................................................................22 4.1.1.2. Procedure....................................................................................................................................22

    4.1.2. Insertion of Blanks..............................................................................................................................22 4.1.2.1. Materials Required ......................................................................................................................23 4.1.2.2. Procedure....................................................................................................................................23

    4.2. Pulp Standards ...........................................................................................................................................23 4.2.1. Purchased or Project Pulp Standards....................................................................................................23 4.2.2. Purchased Control Standards...............................................................................................................24 4.2.3. The Advantage of Control Standards Prepared from Project Materials .................................................25 4.2.4. Limitations of Using Control Standards Prepared from Project Materials.............................................26 4.2.5. Insertion of Pulp Standards .................................................................................................................26

    4.2.5.1. Materials Required ......................................................................................................................26 4.2.5.2. Procedure....................................................................................................................................26

    4.2.6. Sample Log ........................................................................................................................................27 5. Stage I, II, III Procedures ...................................................................................................................................29

    5.1. Stage I - Grassroots Projects .......................................................................................................................29 5.2. Stage II - Discovery Stage Projects .............................................................................................................30 5.3. Stage III - Advanced Exploration and Evaluation ........................................................................................31

    6. Procedures at the Drill and Drill Core Sampling .................................................................................................33 6.1. Communication with the Drill Company and Drill Crew.............................................................................33 6.2. Security......................................................................................................................................................33 6.3. Procedures at the Drill ................................................................................................................................33 6.4. Transportation ............................................................................................................................................34 6.5. Chain of Custody Management...................................................................................................................34 6.6. Drill Core Duplicates..................................................................................................................................37

    7. Submission of Samples to Primary Laboratory ...................................................................................................39 7.1. Submitting Samples to Primary Laboratory.................................................................................................39

    7.1.1. Materials Required..............................................................................................................................39

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    7.1.2. Procedure ...........................................................................................................................................39 7.2. Batch Size..................................................................................................................................................40 7.3. Data Entry and Database Management........................................................................................................40

    8. Review of Quality Control Data .........................................................................................................................41 8.1. Control Charts............................................................................................................................................41 8.2. Logic Table of Failures...............................................................................................................................42 8.3. Table of failures .........................................................................................................................................44

    9. Quality Control Failure: Request for Repeat Analyses ........................................................................................45 10. Additional Quality Control Procedures ...........................................................................................................47

    10.1. Coarse Crush Particle Size Analysis........................................................................................................47 10.1.1. Sample Selection ................................................................................................................................47

    10.2. Pulp Check Assays .................................................................................................................................47 10.2.1. Submission of Pulp Replicates to the Secondary Laboratory................................................................47 10.2.2. Analytical Methods.............................................................................................................................48 10.2.3. Sample Selection ................................................................................................................................48 10.2.4. Sample Submission.............................................................................................................................48 10.2.5. Comparison of Results for Checks Assays ...........................................................................................49

    10.2.5.1. X-Y Plot and Regression .............................................................................................................49 10.2.5.2. Mean vs. the %Difference Plot ....................................................................................................50 10.2.5.3. Paired t-Test................................................................................................................................51

    10.2.6. Corrective Action ...............................................................................................................................51 10.3. Reject Replicates ....................................................................................................................................52

    10.3.1. Submission of Reject Replicates for Check Analyses...........................................................................52 10.3.1.1. Sample Selection.........................................................................................................................52 10.3.1.2. Sample Submission .....................................................................................................................52 10.3.1.3. Analysis of Results......................................................................................................................53

    10.4. Integrated Variance Studies ....................................................................................................................53 11. Measurement System Analysis .......................................................................................................................55

    11.1. Assays as a Measurement System ...........................................................................................................55 List of References and Selected Bibliography ............................................................................................................57 Appendix I Glossary of Terms ..............................................................................................................................59 Appendix II Guidelines for Preparation of Analytical Service Contract ...................................................................63 Appendix III Detailed Process Maps ....................................................................................................................65 Appendix IV List of Pulp Standards Prepared by Noranda and Falconbridge.........................................................83 Appendix V Laboratory Audit Guidelines.............................................................................................................111

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    List of Figures Figure 1 : Typical simplified flow chart of sampling and assaying process. ................................................................. 6 Figure 2 : Rhino Jaw crusher with 10mesh sieve attachment.......................................................................................16 Figure 3 : Process map for homogenization of sample in a Jones splitter.....................................................................16 Figure 4 : Methods for preventing and detecting tampering. ......................................................................................35 Figure 5 : Samples should not cross geological boundaries. .......................................................................................36 Figure 6 : Standard Control Chart .............................................................................................................................41 Figure 7 : X-Y plot of Check Assays (Cu2_pct) vs Original Assays (Cu_pct). Blue line is for X=Y (slope of 1). Black

    dashed line is actual regression line for the least squares trend between variables. ...............................................50 Figure 8 : Mean (Cu_pct) vs percent Cu difference plot.............................................................................................50 Figure 9 : Absolute difference vs mean concentration plot. Results indicate a distinc grouping of samples with higher

    variance, possibly due to erratic or nuggety copper. ......................................................................................53 Figure 10 : Thompson and Howarth Plot. ..................................................................................................................54 List of Tables Table 1 : Definition of accuracy and precision............................................................................................................ 5 Table 2 : Selecting an Analytical Method ..................................................................................................................19 Table 3 : Noranda - Falconbridge, recommended rates of insertion of control materials..............................................21 Table 4 : Example of a Sample Log ..........................................................................................................................27 Table 5 : Example of logic table of failures ................................................................................................................43 Table 6 : Example of table of failures to keep track of what controls failed in which batches and what actions were

    taken..................................................................................................................................................................44 Table 7 : Regression analysis of check assays against original assays (X Variable 1). The pertinent outputs are the

    coefficients for the intercept (X0) and for the X variable (k) (see bottom second column) to be used in the linear function Check Assay = k(Original Assay) + X0. The P-value for the intercept is >0.05 and is therefore not significantly different than 0. The P-value for the X variable and the R-square are meaningless in this case because of the naturally strong relation between the variables. ............................................................................49

    Table 8 : Example of output from paired t-Test calculation in Excell. In this case there is bias between the two datasets because the P-value for the two-tailed test is less than 0.05. The check assays are on average 5.7% higher than the original assays. ..................................................................................................................................................51

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    Preface to Version 2.0 The following document is a revised version of the Drill Core Sampling and Analysis Protocols v1.0, published in April 2000 by Lionel Martin with contributions from numerous collaborators. This publication is a result of a second Six Sigma project that focused on reducing the sources of variance in Noranda and Falconbridge's diamond drill core assays and used a centralized QAQC database as a source of data to analyze the performance of assays from different projects. A number of experiments were undertaken to study the effects of different equipment and procedures on variance and bias of assays. Where conclusive the results of these experiments have been included as recommended equipment or operating procedures that are expected to help to reduce the variance and prevent bias in assaying procedures. Introduction This manual describes the Noranda and Falconbridge protocol for the collection, sampling and analysis of diamond drill core, and the auditing of analytical results. It is the responsibility of management and the project manager/geologist to ensure this protocol is diligently applied to exploration, evaluation and feasibility stage projects. Diamond drill core sampling is mandated as the sampling method for a mineral body of potential economic significance where ground quality permits acceptable recoveries. The project manager is responsible for the quality assurance (QA) of the sampling procedure, shipping of samples, chemical analyses (including selection of appropriate analytical method) as well as the quality control (QC) and security of both the core and analytical samples. Project managers must ensure there is complete documentation (both hard copy and digital) of all procedures and results at all stages of the project to provide a clear audit trail for subsequent (and possibly external) reviews. Implementation of standardized quality control procedures for all of Noranda and Falconbridge's exploration and development offices is a key objective. Although the approach to quality control described in this document can be applied to rock samples, core, RC samples, soil/silt samples and lithogeochemical samples this document pertains only to drill core and the quality control program consists of:

    The submission of blanks to monitor contamination and data accuracy. The submission of control samples (i.e. pulp standards), of known metal

    concentration, to monitor data accuracy. Acquisition of data for laboratory internal pulp replicates to monitor analytical

    precision. Collection and review of all internal laboratory data for blanks and in-house

    control standards to monitor accuracy. The submission of reject replicates to monitor sample homogeneity and

    preparation procedures.

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    The submission of pulps to a secondary laboratory (also referred to as cross-checks) to verify analytical methodology, laboratory bias and data accuracy.

    Submission of coarse crush rejects to a secondary laboratory for coarse crush particle size analysis to monitor preparation procedures.

    Submission of core duplicates to monitor total sampling and analysis variation.

    Management and review of all quality control data. The purpose of documenting the procedures, and any revisions, is to ensure consistency. Written protocols ensure that all project employees can reference the protocols if they are not clearly explained or if forgotten. Jobs are clearly defined and procedures are consistently applied. The project manager assigns responsibility for different procedures to specific individuals so that there is accountability for each aspect of the quality control program. Any changes to the procedures and the date of the change must be recorded. Protocols exist for all stages of exploration, and are particularly important for projects where pre-feasibility or feasibility studies are planned. Third party engineering firms, investment bankers and other individuals from outside the company may request documentation of the sampling, sample preparation and quality control procedures. Compliance with these protocols will be monitored and reported to senior management, or in the case of feasibility studies, third parties. Inclusion of quality control samples such as blanks, control standards and replicates will allow laboratory errors to be readily identified and corrected. This approach provides a high quality database that will improve confidence in the decisions based on these data. The procedures documented in this manual are general guidelines. It is envisioned that the procedures may be modified with experience and new technological developments, however documentation of all changes is necessary. Terms of Reference In response to the Best Practices Guidelines proposed by the Toronto Stock Exchange and Ontario Securities Commission (TSE/OSC) Mining Standards Task Force, Noranda and Falconbridge implemented a review of the company's quality control practices with respect to the submission of samples for analysis. A series of documents were distributed internally for discussion including notes from a 1998 PDAC short course, "Practical Application of Exploration Geochemistry", written by Lynda Bloom, Stephen Amor and Peter Ward as well as a paper titled "The Role of Economic Geologists in Evaluating Data Quality" by L. Bloom (1998). This document applies to drill core only, however protocols for rock sampling (grab, outcrop, channel, etc.), lithogeochemistry (whole rock) and sediment sampling (soils, silts, HMC's) can be adapted from this protocol as many of the procedures will be similar.

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    The quality control guidelines described in this document are designed to maintain a high level of confidence in analytical results for Noranda and Falconbridge management and geologists, joint venture partners, regulatory authorities and the public domain. Adequate mineralogical and metallurgical testing and geotechnical measurements also need to be introduced at specific stages to identify negative economic consequences early in the exploration process. The additional objective of this protocol is to characterize potential ores early in the process and, where appropriate, testing can be used to compliment preliminary predictive metallurgy reviews. The results are to be carried to the advanced metallurgical testing stage with the clear identification of potential negative impacts of deleterious elements and complex mineralogy early in the process. The components of a quality control program will vary according to commodities, deposit type and location. The number of quality control checks will increase as a project advances and the financial exposure to the risk associated with the project also increases. This protocol envisions that the exploration process is governed by three principle stages that reflect increasing success from grassroots through to feasibility. Each stage represents the progressive addition of quality controls with increased success as well as the concomitant implementation of metallurgical, mineralogical, and rock physical property measurements (e.g. RQD). Stage I, Stage II or Stage III are briefly described as follows: Stage I - Grassroots Exploration: Stage I projects primarily involve drill testing geophysical, geological and/or surface geochemical targets. These projects may not encounter mineralized zones and, in the absence of significant mineralization, the focus is identification of anomalous metal values and alteration patterns. Geochemical multi-element ICP analysis may be used to estimate the metal content of drill core as a less expensive alternative to assaying. Significant mineralization will automatically be assayed as described for Stage II and III projects, as will any indication of gold, silver or platinum/palladium. QC procedures are applied to develop a reasonable baseline confidence level with respect to chemical analyses. Control standards, blanks and replicates are submitted and monitored. QC data are verified as each set of analyses is received. With increased success, Stage I projects evolve into Stages II and III with the addition of further QC checks as well as the initiation of metallurgical and geotechnical data collection. Stage II - Discovery-Stage Projects: Stage II projects essentially represents a transitional stage that is initiated upon first discovery of potentially economic mineralization. It is directed towards additional QC checks, as well as the beginning of the characterization of a potential ore body. It is acknowledged there will be initially limited sample availability. The discovery of potential economic mineralization automatically implies that assay methods are to be used for all samples within a mineralized interval in place of

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

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

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

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

    Precision Amount of dispersion of repeated

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

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

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

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

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

    Split Core Crush Split & sub-sample

    Pulverize Sub-sample Digest Analyze

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

    1.3. Precision and Variance As mentioned above, variance is a consequence of sub-sampling and it is additive through the sampling and assaying process. Information on variance is contained in the duplicate analyses of core, coarse crush and pulps material and is directly obtainable from the distribution of assay results of pulp standards. Under conditions of grade constant variance (only true for narrow grade ranges), the variance is calculated as followed:

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    s 2 = S (2nd assay - 1st assay)2 / 2N (1) Unfortunately variance is also a function of grade and is a second-order polynomial of the form of equation 2 (Franois-Bongaron, 1998b): s 2 = (s 2(0) + Beta Grade2) + s 2(s) Grade , (2) where, s 2 (0) = The variance at a grade of zero or constant analytical variance s 2 (s) = The sampling variance independent of grade as in 1 above Beta = The coefficient of proportionality of analytical variance. The square root of equation 2 becomes: s (c) = s(0) + k Grade (3) This equation is equivalent to equation 1 of Thompson and Howarth (1978) and is used to estimate parameters Std(0) and k in their equation 2 which translates as follows: Pc = 2 s(0) / Grade + 2 k (4) From this equation we can calculate the precision (Pc) or relative standard deviation (RSD%) (the two are equivalent) for any grade. The variance arising specifically from the act of sub-sampling has been analyzed in detail by Gy (1982) and is summarized by Franois-Bongaron (1998b). In his simplified equation Gy expresses the variance of sampling error as a function of particle size (dN) and masses of the sample (Ms) and the lot (Ml) as follows: s (FSE) 2 = (c l) (f g dN3) * (1/Ms - 1/Ml), (5) where, c = mineralogical factor related to grade of the lot and densities of the mineral of interest and the rest of the rock, l = liberation factor related to size distribution and arrangement of mineral grains within rock fragments, f = shape factor, g = granulometric factor, and dN = nominal size. The importance of this equation comes from the fact that certain conditions are required for it to be applicable. The most important is factor "g" that requires that the PSA be 95% for it to be constant (Franois-Bongaron, 1998b). For this reason it is essential that PSA specifications always be defined in terms of the sieve size for which 95% of the material passes through.

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

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    2. The QAQC Manager Each drilling project shall have a QAQC manager. In early stage projects this role will typically be cumulated by the project geologist. On advanced projects and depending on the situation, a person may be assigned the task and responsibilities of ensuring all quality procedures are followed. The QAQC Manager must be a "Qualified Person" as per the definition in NI 43-101. The QAQC manager is responsible for the following aspects of the drilling program:

    Identify adequate pulp standards or, if required, the collection of project materials to be used to prepare standards, the supervision of the round robin validation of the standards, and the calculation of the accepted values for the standards.

    The collection and validation of blank material. The identification and validation of the primary and secondary laboratories. The planning of the sampling program including the schedule of control

    insertion and collection of duplicate samples. The validation of batches for accuracy using standards and blanks. The additional validation of the primary lab using check pulp assays at the

    secondary lab. The estimation, as required, of precision of crushing and core sampling from

    duplicate samples. The supervision of the storage of core boxes and pulp and reject materials. The preparation of the QAQC report to be included in the project drilling

    report. Refer to Appendix III for detailed process maps of the activities necessary to ensure compliance with the protocol.

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

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

    3.2. Laboratory Communication and Service Contract It is preferable to negotiate a contract with a commercial laboratory that clearly defines the services required, reporting formats, quality control parameters, pricing, turnaround time and penalties in the case turnaround times are not respected. Laboratories should be asked to report on the following:

    Analyses of the second quartz chip sample (i.e. cleaner) to be passed through the pulverizer equipment prior to each batch of samples being prepared. Some labs do not routinely analyze the pulverizer blanks.

    Laboratory pulp replicate results. Blank and control standard results. Lab blanks are often solution blanks. Results of coarse crush particle size analysis performed by the laboratory to

    monitor sample preparation quality. Results of participation in round robins.

    The contract should also specify the number of significant digits to be reported. The rule is that one additional digit should be reported. For example, if results are significant to two decimal places, three digits should be reported to the right of the decimal place.

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

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

    3.4. Sample Preparation

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

  • 15

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

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

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

    CrushedCrushedSampleSample

    SplitterSplitter

    50%50%50%50%

    25%25%75%75%

    37.5%37.5% 62.5%62.5%

    11

    22

    33

    SampleSample 100%100%

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    Some commercial laboratories may be equipped with other types of crushers; however, it is up to the QAQC manager to ensure that the equipment that is to be used is both unbiased and introduces acceptable variance. If in doubt consult with the Manager Geochemistry or an experienced professional.

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

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

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

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

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

    Analytical Procedure Geochemical Analysis Assay Sample Weight 0.2 0.5 g 0.25 1.0 g Sample Dissolution Selective extractions

    Aqua regia digestion HCl+ HNO3+ HClO4 HF Alkaline fusion

    Elements Compromises used to achieve maximum no. of reported elements

    Optimized for single elements

    Dilutions Usually imprecise and performed in test tubes

    Precise and performed in volumetric flasks

    Upper Limit of Detection Precision is poor at upper limits of detection

    No upper limit of detection

    Lower Detection Limit Generally less than 1 ppm or 0.0001% for major elements

    Usually 0.01% for base metals

    Instrumentation A.A.S. , I.C.P.-O.E.S., I.C.P.-M.S., neutron activation

    A.A.S., I.C.P.-O.E.S., XRF, fire assay

    Specialized Methods Includes analysis of water, biogeochemical samples, gases, MMI, Enzyme Leach, etc.

    Colorimetry and gravimetric techniques may be used for high grade samples or concentrates

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

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

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

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

    4.1. Blanks

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

    Stage I Stage II Stage IIIStandards >= 1% >=2% 1 per batch or 1:40Blanks >= 1% >=2% 1 per batch or 1:40

    Pulp Check Assays >= 5%>= 5% of mineralized samples >= 5% of mineralized samples

    Coarse Crush Replicates Optional >= 5%>= 5% initially until 55 samples collected, afterwards 1%

    Core Duplicates Optional Optional>= 5% initially until 55 samples collected, afterwards 1%

    Reject PSA Optional >= 5%

    >= 5% initially until about 30 samples show PSA is aceptable, afterwards 1%

    Noranda/Falconbridge Protocol

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

    4.1.1.1. Materials Required Unmineralized quartzite or sandstone (for example) 20-litre pails

    4.1.1.2. Procedure A geologist locates a source of suitable material (typically from a quarry or unmineralized drill core). Determine how much material to collect by (a) dividing the total of number of samples by the frequency of blank insertion to determine the total number of blanks for the program and (b) multiplying by 2 kg (the approximate weight of material submitted). Store the blank material in pails so that it is ready for routine core sampling. Record a description of the material and its origin. Submit five 200-500 gm sub-samples of the "blank" material to the primary laboratory to confirm low metal values. Blank material is not processed in advance of its insertion into sample batches. Individual pieces of rock should be no larger than 5 inches by 5 inches so that they are small enough to pass the hopper of the crusher. It is up to the QAQC manager in discussion with the project manager to determine the defect threshold concentrations for the blanks. This may vary according to project, mineralization type, and the average grades encountered but should always be less than 1/20th of the anticipated cut-off grade.

    4.1.2. Insertion of Blanks A blank sample is inserted routinely into sample batches. When the sample is analyzed, the reported analytical values should be near the detection limit of the method. If the reported values are higher than expected, contamination of the samples during crushing, pulverizing or analysis may be indicated. Sample preparation procedures would be reviewed to isolate the cause of contamination and corrective action taken.

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    4.1.2.1. Materials Required Sample bags Sample tags "Blank" material

    4.1.2.2. Procedure

    Two sample tags in each group of 100 tags are reserved for blanks. Reserved numbers usually end in "-10" and "-60" or, better still, two numbers chosen at random from each series of 100 sample numbers. The insertion of blanks randomly is a more robust test of the laboratory but requires careful training and record keeping.

    Prior to moving samples to a sample preparation facility, coarse blank samples are added as follows: a) label a plastic sample bag with the sample tag ending in the number "-

    10" or "-60" or the pre-selected random number. b) insert the sample tag in the sample bag. c) add an amount of "coarse blank" material to the bag that is similar to

    that submitted for samples. Sort all samples into consecutive numerical order. Submit the "blank"

    sample to the sample preparation facility with the samples. Note: Plastic bags can be filled with blank material in advance, then labeled and the sample tag added when preparing samples for shipment. Where possible, barren drill core is submitted so that the laboratory cannot recognize the "blank" material.

    4.2. Pulp Standards

    4.2.1. Purchased or Project Pulp Standards In different circumstances it may be appropriate to purchase control standards or prepare control standards from materials on the property.

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

  • 25

    available reference materials. This list will be implemented on the intranet later in 2003 and updated on a regular basis.

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

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    4.2.4. Limitations of Using Control Standards Prepared from Project Materials Once the material for the control standards is received at a laboratory it is likely to take 4-6 weeks to complete the preparation and analytical stages. An approximate cost to prepare a 50 kilograms control standard is in the order of four to five thousand dollars per pulp standard, depending on the number of variables being determined. Typically, half the cost is related to submission of the material for determination of "acceptable" values and measurement of homogeneity. This becomes a significant expense and the time delay is not always manageable. In certain cases, it may be difficult to prepare a control standard that has sufficient homogeneity. It can be particularly difficult to prepare a control standard homogeneous with respect to gold or other metals that are distributed as nuggets or discrete grains. The insertion of control standards where metal concentrations cannot be anticipated reduces the effectiveness of a quality control program. It may be preferable to use purchased control standards in such cases.

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

    4.2.5.1. Materials Required Fully-prepared (crushed, pulverized, homogeneous and certified) control standards Small sample bags (approximately 10 x 16 cm) Sample log (see Note below)

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

  • 27

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

    4.2.6. Sample Log Complete the internal sample log that records a minimum of the following information:

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

    was inserted. sample numbers assigned for drill core duplicates, if used.

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

    Sample Number

    Hole-ID From To Shipment Shipped Date Recd/Cert #

    1001 DH-06 100 101 33BH Oct.3 Oct.12 A990343

    1002 DH-06 101 103.4 1003 DH-06 103.4 104.87 1004 DH-06 104.87 105.5 1005 DH-06 105.5 107 1006 DH-06 BLANK 1007 DH-06 107 108 1008 DH-06 108 110 1009 DH-06 110 111 1010 DH-06 113 113.5 1011 DH-06 113.5 114 1012 DH-06 114 115.23 1013 DH-06 115.23 115.9

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    1014 DH-06 115.9 116.8 1015 DH-06 Control STD05

    BM&S

    1016 DH-06 116.8 117.33 1017 DH-06 117.33 118.75

  • 29

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

    5.1. Stage I - Grassroots Projects Stage I projects primarily involve drill testing geophysical, geological and/or surface geochemical targets. These projects may not encounter mineralized zones and, in the absence of significant mineralization, the focus is identification of anomalous metal values and alteration patterns. Generally, geochemical multi-element ICP analysis is acceptable for Stage I projects to evaluate the metal content of zones of interest. Analytical technique may vary on a project basis. Potential economically significant intersections will automatically move the project to Stage II. One control standard and one blank sample are submitted with each sample batch with a minimum of one each per every 100 samples. Coarse reject replicates, coarse crush particle size analysis, and drill core duplicates are optional. Cross-check analysis of pulps at a secondary laboratory is recommended for 5% of mineralized samples. Quality control results are verified upon receipt of analysis and the lab contacted immediately upon failure at any point. Under Stage I and specific to ICP analyses and geochemical analysis for gold, the following guidelines are recommended.

    Samples with reported base metal results greater than 10,000 ppm and silver values greater than 10 ppm are automatically assayed.

    Samples analyzed for gold using a geochemical analysis (MIBK-A.A.S. or fire assay with an instrumental finish) that report gold values greater than 1000 ppb are automatically fire assayed using a gravimetric finish.

    Intervals selected for assay, based on the above criteria, shall include lower grade samples on each end of the interval so that the "cut-off" grade for the mineralized interval is determined using the same analytical method.

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

    Complete multi-element (deleterious) chemical characterization analyses on individual representative samples. If practical, characterize all samples that comprise composite. Do not rely on a standard suite of deleterious elements for any mining camp to determine characterization of deleterious elements.

    As an indication of a potential resource develops, initiate optical predictive metallurgical characterization and compare results with chemical analyses. Microprobe work can compliment this type of study by locating host minerals of deleterious elements.

    Begin collection of geotechnical data.

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

    Assays to be used for all samples. The selection of deleterious elements may vary for different parts of an ore

    body and the analytical requests must reflect a detailed investigation to document these variations.

    Specified sample preparation protocols must be adhered to. Samples required for metallurgical testing may require different sample preparation procedures.

    Initiate systematic predictive metallurgy prior to advanced metallurgical analyses and compare results with chemistry. Microprobe work may

  • 32

    compliment this type of study by locating host minerals of deleterious elements.

    Assays of metallurgical re-samples (either assays of reject or re-sampling of drill core) are compared immediately with initial results. Deleterious results from the metallurgical flow test are compared with geochemical data of the original samples.

    Initiate a statistical review of the spatial (hole to hole) variance of the assay data.

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    6. Procedures at the Drill and Drill Core Sampling

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

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

    6.3. Procedures at the Drill

    Core boxes are labeled, and arrows drawn so that the core is systematically laid in the box.

    The core box is placed away from any source of contamination. A wooden or plastic marker is placed in the core box after each run. The

    meterage/footage is written on the marker. Transfer of the core from the core barrel to the box should be done as

    carefully as possible. No core is allowed to fall onto the ground. Core is directly placed in the core box and a plastic mallet is used to loosen core in the core tube. Breakage of core will produce inaccurate geotechnical measurements.

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    Photographs of the core at the drill site will be beneficial for geotechnical analyses in a number of circumstances where transportation may result in degradation of the core.

    Document intervals of ground core and immediately address inaccuracies in depth labeling in the core boxes. A rod count must be conducted immediately to accurately measure the depth of the hole (this is at the drill company's cost if poor attention to labeling is indicated).

    Rod counts should be done at each bit change as a matter of course. If the core is being orientated, the core is systematically marked to indicate

    base of hole. As soon as a core box is full, a lid is properly secured so that no accidents

    occur. Poor quality or broken core boxes must be discarded.

    6.4. Transportation Sample collection and transportation procedures may vary between projects. Differences are commonly related to access, climate, local infrastructure and region. Sample collection and transportation procedures must be documented and made available to field staff. These procedures are recommended to address the following issues where applicable:

    Transportation of core from the drill site to the logging facility must be in a manner to minimize or eliminate shifting of material in the core boxes.

    Transportation and storage of cut or split core must ensure that the remaining core does not shift and that marked sample intervals remain intact.

    Appropriate measures must be taken to eliminate the possibility of sample tampering through proper chain of custody management.

    6.5. Chain of Custody Management It is essential that proof be obtained that the samples were not tampered with between the time of sampling and arrival at the laboratory. Depending on the project this may be trivial issue or a very complicated one. All movement of samples from the drill