PTP Mal Gui Eng

CANADIAN CERTIFIED REFERENCE MATERIALS PROJECT
DESCRIPTION OF THE
PROFICIENCY TESTING PROGRAM FOR
MINERAL ANALYSIS LABORATORIES
(PTP-MAL Guide)

Scope of Accreditation No. 420

Accredited by the Standards Council of Canada as a
Proficiency Testing Provider for specific mineral analyses parameters.

Prepared By: Diane Desroches
PTP-MAL Coordinator

Approved By: David Koren
Manager-Laboratory Services/CANMET-MMSL

Issued By: Saman Amarakone
Manager- Quality Systems/CANMET-MMSL

Copyright: This Manual is the property of the Government of Canada.
Crown Copyrights reserved.

Proficiency Testing Program - Mineral Analysis Laboratories (PTP-MAL)
CANMET Mining and Mineral Sciences Laboratories, Natural Resources Canada,
555 Booth Street, Ottawa, Ontario K1A 0G1Tel.: (613) 995-4738, Fax: (613) 943-0573
ptp@nrcan.gc.ca / www.ccrmp.ca

PTP-MAL Guide version 13 Page i of iii
Step by Step Overview

1. The PTP-MAL Coordinator sends a letter of invitation to participate in the next PTP-MAL cycle
to all intended participants approximately three weeks before the cycle starts.
2. Participants fill in the Order Form. Payment can be made by Visa, MasterCard, Cheque or
Wire Transfer.
3. Samples are shipped to all participants.
4. An input file is emailed to all participants.
5. Using the input file provided, participants submit their results within one month from date of
shipment of the samples. Confirmation of receipt of results is emailed within three working
days.
6. Results must be reported to at least two (2) significant figures.
7. No modification of results is allowed later than three days after the deadline for submitting
the results.
8. The Performance Report is issued to each individual participant approximately 5 weeks from
the receipt of the analytical results.
9. The Comprehensive Cycle Report is issued to participants approximately one month after the
delivery of the individual Performance Reports.
10. A certificate of successful participation in proficiency testing is delivered.

Standards Council of Canada (SCC)-Accredited Laboratories and Action Requirements

Laboratories accredited by SCC under the Mineral Analysis Testing Program Specialty Area are
required to participate in PTP-MAL as fully described in CAN-P-1579. Any questions concerning
CAN-P-1579 proficiency testing performance requirements should be addressed to SCC and not to
PTP-MAL.

The CAN-P-1579 can be viewed on the SCC website at:

http://www.scc.ca/

Note: rules for accreditation by SCC are quite different from the criteria to obtain the PTP-
MAL certificates. Only the individual and absolute z scores value are used by SCC. The Mineral
Analysis Laboratories Working Group (MAWG) of SCC has requested the proficiency testing
provider to continue to calculate and report the RSZ (Re-scaled Sum of z-Scores) and SSZ (Square
Sum of z-Scores) values and evaluate them in their reports. Please consult SCC website.

PTP-MAL Guide version 13 Page ii of iii
TABLE OF CONTENTS

Step by Step Overview......................................................................................................................... i
Standards Council of Canada (SCC)-Accredited Laboratories and Action Requirements...................... i
1.0 CANADIAN CERTIFIED REFERENCE MATERIALS PROJECT (CCRMP) ...................................... 1
2.0 INTRODUCTION............................................................................................................................... 1
3.0 DESCRIPTION OF PTP-MAL ........................................................................................................... 1
3.1 Operation of PTP-MAL..................................................................................................................2
3.2 Extended Proficiency Testing Program..........................................................................................2
3.3 Accreditation by SCC ....................................................................................................................3
3.4 Submission of Results...................................................................................................................3
3.5 Correction of results submitted......................................................................................................3
4.0 REPORTS TO PARTICIPANTS........................................................................................................ 4
4.1 Performance Report......................................................................................................................4
4.2 Comprehensive Report..................................................................................................................4
4.3 Confidentiality............................................................................................................................... 4
5.0 PARTICIPATION IN PTP-MAL ......................................................................................................... 4
5.1 New participants............................................................................................................................4
5.2 Previous participants.....................................................................................................................5
6.0 FEE................................................................................................................................................... 5
7.0 UNSATISFACTORY LABORATORY PERFORMANCE.................................................................... 5
8.0 FEEDBACK AND PARTICIPANT COMPLAINTS ............................................................................. 5
9.0 SCC-ACCREDITED LABORATORIES AND ACTION REQUIREMENTS ......................................... 6
10.0 ASSESSMENT OF PROFICIENCY................................................................................................. 6
10.1 Rules...........................................................................................................................................6
10.2 Estimation of Statistical Parameters............................................................................................7
10.2.1 Consensus value..................................................................................................................7
10.2.2 The standard deviation of the consensus value....................................................................7
10.2.3 Calculation of z-score for an analysis ...................................................................................7
10.3 Scope of Assessment of Proficiency............................................................................................8
10.4 Tests for Assessment of Proficiency............................................................................................... 8
10.4.1 Assessment of proficiency: z-score......................................................................................8
10.4.2 Combining z -scores: Distribution of absolute values............................................................8
10.4.3 Combining z-scores: Re-scaled Sum of z-Scores .................................................................9
10.4.4 Combining z-scores: Squared Sum of z-Scores....................................................................9
10.5 Withdrawal of sample................................................................................................................ 10
10.6 Example.................................................................................................................................... 10

PTP-MAL Guide version 13 Page iii of iii
10.7 Overall Assessment of Proficiency............................................................................................ 10
11.0 CERTIFICATE OF SUCCESSFUL PARTICIPATION IN PROFICIENCY TESTS.......................... 10
12.0 REFERENCES.............................................................................................................................. 11
13.0 APPENDICES............................................................................................................................... 11
APPENDIX A .......................................................................................................................................... 1
Abbreviations for Analytical Methods...................................................................................................1
APPENDIX B .......................................................................................................................................... 1
Fees....................................................................................................................................................1
Examples on how to calculate the fees per cycle.................................................................................3
Payment by using wire
transfert.7
APPENDIX C.......................................................................................................................................... 1
First Example of Assessment of Proficiency........................................................................................1
Second Example of Assessement of
proficiency.......3
Elements on the
Certificate....6

PTP-MAL Guide version 13 Page 1 of 11
1.0 CANADIAN CERTIFIED REFERENCE MATERIALS PROJECT (CCRMP)

CANMET Mining and Mineral Sciences Laboratories (MMSL) has offered reference materials and
spectroscopic standards since 1962. The Canadian Certified Reference Materials Project (CCRMP) was
created as a formal entity in 1973 to produce and distribute certified reference materials for use in the
analytical community associated with the mining industry in Canada and abroad. CCRMP provides
around 90 certified reference materials and distributes them to more than 65 countries. It offers the
largest selection of sulphide mineral and precious metal certified reference materials.

CCRMP was first certified to ISO 9002 in March 1997 for the production and distribution of certified
reference materials. In March 1998, ISO 9002 certification of the CCRMP quality system was extended
to include the operation of the Proficiency Testing Program for Mineral Analysis Laboratories (PTP-
MAL). In March 2002, the quality system of CCRMP was upgraded to ISO 9001:2000. In April 2008, the
quality system of CCRMP was upgraded to ISO 9001:2008.

In December 2001, PTP-MAL was accredited by the Standards Council of Canada to CAN-P- 1593
(which comprises CAN-P-43 (ISO/IEC Guide 43-1) and ILAC G13:2007). In February 2010, ILAC G13
and ISO/IEC Guide 43-1 were merged into ISO/IEC 17043. By this accreditation, PTP-MAL meets the
recognized international standards for proficiency testing providers. PTP-MAL is listed on the Asia
Pacific Laboratory Accreditation Cooperation website as a proficiency testing provider:

http://www.aplac.org/documents/pt/aplac_pt_003_issue_15.pdf

2.0 INTRODUCTION

CCRMP operates PTP-MAL in cooperation with the Task Group Laboratories (TG labs)-Mineral Analysis
Laboratories Working Group (MAWG) of the Standards Council of Canada (SCC). TG LABS-MAWG is
responsible for defining the metals of interest and the concentration range for each as well as
establishing the criteria and target values for assessing laboratory proficiency. Participation in PTP-MAL
is open to any laboratory for which the scope of testing is relevant. Participation is obligatory for
laboratories seeking or maintaining accreditation under CAN-P-1579 To maintain confidentiality,
participants are identified only by a code.

3.0 DESCRIPTION OF PTP-MAL

The operation of the proficiency testing program is in full accord with ISO/IEC 17043 (CAN-P-43)
Conformity assessment General requirements for proficiency testing and the proficiency testing
components of CAN-P-1579 Requirements for the Accreditation of Mineral Analysis Testing
Laboratories, while at the same time striving to respond to the needs of Canadian mineral analysis
laboratories.

The proficiency testing program has two functions. First, it is a vehicle to allow a mineral analysis
laboratory to assess its performance for one or more analytical methods independently of internal quality
control. Second, participation in the program is obligatory if a laboratory is to be accredited or is to retain
its accreditation for mineral analysis activities by SCC to CAN-P-1579 Requirements for the
Accreditation of Mineral Analysis Testing Laboratories, which includes meeting the requirements of
ISO/IEC 17025 General requirements for the competence of testing and calibration laboratories.

Given the wide variety of analytical demands, this proficiency testing program cannot cover all aspects
of mineral analysis testing but will instead be representative of this area of activity. The current focus,
which was selected in response to current market demand, is

Target Concentration Range
Metal
Lower Upper
Au 0.1 ppm 15 g/metric ton
Ag 1 ppm 1000 ppm
Cu 1 ppm 2%
Zn 1 ppm 3%
Pb 1 ppm 2%
Ni 1 ppm 2%
Co 1 ppm 0.1%
Pd 0.1 ppm 3 ppm
Pt 0.1 ppm 3 ppm

The materials used to prepare PTP-MAL samples are obtained from naturally occurring outcrops
deposits in Canada and worldwide including rocks, ores, mill feed and tailings.

The scope of the proficiency testing program may be modified and/or extended in the future depending
on market demand, and regulatory or other requirements. Furthermore CCRMP may, as samples
permit, provide an opportunity to laboratories to assess their proficiency in the analysis of other metals.

3.1 Operation of PTP-MAL

The proficiency testing program consists of two test cycles issued each year. Each cycle includes four or
more test samples to cover as best as possible the target concentration range of the metals specified
previously. Each participating laboratory is requested to perform one analysis for one or more of the
identified metals in each sample by a method of its choice in a manner identical, to the greatest extent
possible, to that applied to client samples.

A participant may request one (1) replacement specimen of a test sample that has been lost or destroyed
after receipt by the participant, in order to report analytical results for that sample. There is no cost for
such a replacement, which is limited to once in a three (3) year period. Test samples that have been lost
or destroyed during shipping are replaced at the request of the participant.

3.2 Extended Proficiency Testing Program

A participant may choose to extend the scope of its participation in the proficiency testing program by
submitting results for a metal using more than one analytical method, either on the same set of test
samples or on more than one set of the same test samples. The latter option is not available for
laboratories accredited by SCC to CAN-P-1579. There is a supplemental fee for extended participation.

3.3 Accreditation by SCC

Those laboratories accredited or seeking accreditation by SCC under the Program Specialty Area
Mineral Analysis Testing (CAN-P-1579) must follow Appendix A of CAN-P-1579 Requirements for the
Accreditation of Mineral Analysis Testing Laboratories. In particular, those laboratories must submit test
results for each of their accredited test methods where a relevant test sample is provided. For further
information, contact SCC.

Note: rules for accreditation by SCC are quite different from the criteria to obtain the PTP-MAL
certificates. Only the individual and absolute z scores value are used by SCC. The SCC MAWG has
requested the proficiency testing provider to continue to calculate and report the RSZ (Re-scaled Sum of
z-Scores) and SSZ (Square Sum of z-Scores) values and evaluate them in their reports. Please consult
SCC website at:

http://www.scc.ca

3.4 Submission of Results

Analytical results must be submitted to the PTP-MAL Coordinator no later than the identified due date,
usually five (5) weeks after the shipment date. Results must be reported to at least two (2) significant
figures. Laboratories must use the spreadsheet provided by PTP-MAL (input file.xls) and the submission
must be sent in electronic form to ptp@nrcan.gc.ca

A participant must report the analytical method (including both digestion and instrumental analysis) used
for a metal in a sample. Appendix A provides a list of method descriptors for use by the participant.
Other method descriptors will be added as necessary.

PTP-MAL sends an acknowledgment of receipt to each participant within three working days. Participants
not receiving an acknowledgment of receipt in this time frame should contact PTP-MAL.

Note: Values reported as less than <, for example values that are below the limits of detection of the
laboratory method, are neither evaluated nor considered in calculating the performance for multiple
samples by PTP-MAL. However, such values are reviewed by SCC to evaluate performance of
laboratories that are accredited under the CAN-P-1579/ISO 17025 standard.

3.5 Correction of results submitted

PTP-MAL uses the results as reported to perform its statistical calculation. Participants have up to three
working days after the deadline for submitting results to inform the PTP-MAL Coordinator of any
change in the results reported. No modification will be made on results after the three day period. No
modification will be made to the performance assessment after it is issued unless PTP-MAL has made
a mistake in the transcription of the results.


4.0 REPORTS TO PARTICIPANTS

4.1 Performance Report

A performance report is issued to each participant containing the assessment of proficiency for each
metal. This report will be issued to participants by the PTP-MAL Coordinator approximately 5 weeks
from the receipt of the analytical results.

For those laboratories accredited or seeking accreditation by SCC to CAN-P-1579, the performance
report will also be sent to SCC at the same time.

4.2 Comprehensive Report

A copy of the Comprehensive Cycle Report is issued to each participant approximately one month after
the delivery of the individual Performance Reports. It contains:

1. scope of Program and description of samples;
2. value reported by each participant for each metal in each sample;
3. method descriptor for each participant;
4. consensus/assigned value;
5. standard deviation of consensus/assigned value;
6. calculated values of statistical parameters described in Section 10.0 for each participant; and
7. assessment of proficiency for each statistical parameter for each participant.

4.3 Confidentiality

To maintain confidentiality, participants are identified only by a code.

5.0 PARTICIPATION IN PTP-MAL

5.1 New participants

A laboratory wishing to participate in cycle of the proficiency testing program cycle should contact:

PTP-MAL Coordinator
CANMET-MMSL
555 Booth Street
Ottawa, Ontario K1A 0G1, Canada
Tel: 613-995-4738, Fax: 613-943-0573, e-mail: ptp@nrcan.gc.ca
Or fill the registration form for new participants on our website at: www.ccrmp.ca and click on the lab
proficiency testing program link.

Your company name and coordinates will be added to our databases and will be used only to send
you the letter of invitation, an Order Form and other communications related to PTP-MAL
participation.


5.2 Previous participants

5.2.1 A letter of invitation with an Order Form will be sent before each cycle to each laboratory listed
in our database. The participating laboratory indicates the number of sets of samples and if
necessary, the additional method(s) to be evaluated. The completed Order Form is returned to
ptp@nrcan.ca or sent by facsimile to 613-943-0573.

5.2.2 A laboratory is considered to be a participant for a cycle only if pre-payment has been received
or special arrangements have been made, by the date specified for the cycle.

A laboratory wishing to extend the scope of its participation in PTP-MAL should contact the PTP-
MAL Coordinator.

6.0 FEE

Examples on how to fill the Order Form and instructions on payment by wire transfer for participation in
PTP-MAL are given in Appendix B.

7.0 UNSATISFACTORY LABORATORY PERFORMANCE

First option: A laboratory that fails a set of samples in a test cycle may request another set of the same
samples to assist in undertaking the required corrective action for the analytical method. There is a fee
associated with the set of remedial samples. No assessment of performance, no certificate and
comprehensive report will be provided.

Second option: Laboratories accredited or seeking accreditation, to CAN-P-1579 by SCC may require a
set of remedial samples completely different than the cycle set to independently demonstrate to a third
party (e.g. SCC) that measurement deficiencies of a cycle have been corrected. Refer to Appendix A of
CAN-P-1579 for the Corrective Actions required by the SCC. A set of remedial of samples is also
available for any participating laboratory. There is a fee associated with the set of remedial samples. An
assessment of performance will be performed and, if successful, a certificate will be delivered. The
certificate will say has been assessed Satisfactory for remedial samples for cycle Month 2XXX for
only the element(s) reassessed. No comprehensive report will be provided.

Fees are payable as indicated in Appendix B.

Any questions concerning CAN-P-1579 proficiency testing performance requirements should be
addressed to SCC and not to PTP-MAL.

8.0 FEEDBACK AND PARTICIPANT COMPLAINTS

PTP-MAL welcomes feedback from participants at any time.

If a participant has feedback or a complaint with regard to PTP-MAL, he or she should contact the PTP-
MAL Coordinator directly by telephone, post, e-mail or fax.


9.0 SCC-ACCREDITED LABORATORIES AND ACTION REQUIREMENTS

SCC and CCRMP have a Cooperation Agreement to define mutual responsibilities in PTP-MAL wherein:

- SCC will provide the PTP-MAL Coordinator with a list of the laboratories that are accredited or
seeking to be accredited by SCC in the Program Specialty Area Mineral Analysis Testing
(CAN-P-1579); and

- PTP-MAL Coordinator will submit to SCC and the Convener, TG-Labs MA-WG, a copy of the
performance report of these laboratories in each cycle of test samples, as stated in CAN-P-1579
Clause 6.1.11.

A laboratory that is accredited or seeking accreditation by SCC should consult CAN-P-1579
"Requirements for the Accreditation of Mineral Analysis Testing Laboratories for a description of
requirements regarding method validation, frequency of participation, and unsatisfactory performance in
PTP-MAL, as well as non-compliance with the conditions of participation in PTP-MAL.

Note that it is the responsibility of SCC-accredited participants to ensure compliance with SCC
requirements. Laboratories are directed to contact SCC for any clarification of these requirements.
PTP-MAL does not perform this role.

10.0 ASSESSMENT OF PROFICIENCY

10.1 Rules
For the assessment of Ag, Co, Cu, Ni, Pb, and Zn, the results of at least three samples analysed by the
same method (including both digestion and instrumental analysis) must be reported. Only these results
will be used for calculation of the distribution of z, SSZ and RSZ and the overall rating. The element will
qualify to be on the certificate if an overall "Satisfactory" rating is achieved. If the result for a fourth
sample by a different method is submitted, its z-value will be ignored for the calculation of distribution of
z, SSZ and RSZ and overall rating.
For these six elements, if results for fewer than three samples by the same method (including both
digestion and instrumental analysis) are submitted, only the z-values will be calculated. The distribution
of z, SSZ, RSZ and the overall rating will not be calculated (n.c. will appear in the tables) and the
element will not qualify for inclusion in the certificate.
For Pt and Pd assessment, where only two samples are provided, the same method (including both
digestion and instrumental analysis) must be used for both samples. A Satisfactory overall assessment
will be given if both z-scores are satisfactory.
Gold will be assessed by either single-method or multi-method.
For gold single-method assessment, there must be results for at least three samples analysed by the
same method (including both digestion and instrumental analysis) and only these results will be used for
calculation of the distribution of z, SSZ and RSZ and overall rating. If the overall rating is Satisfactory,
Gold will appear on the certificate.

For gold multi-method (MM) assessment, the results of at least three samples must be reported. A
maximum of 2 different methods (digestion and instrumental analysis) must be submitted regardless of
the number of samples tested. Only results that fulfill these requirements will be used for calculation of
the distribution of z, SSZ and RSZ and the overall rating. If the overall rating is Satisfactory, "Gold MM"
will appear on the certificate.

10.2 Estimation of Statistical Parameters

Note: When a participant reports an analytical result for an element as less than [value], the reported
result is not used in the statistical assessment of results but may be considered by the MAWG of SCC for
overall proficiency.

10.2.1 Consensus value

After the removal of outliers as determined by the Grubbs test (also known as the T-test) or the
Tietjen-Moore test, both described in ASTM E-178:2008, the mean value of the results from all
accepted laboratories for a metal in a sample is used as the consensus value as:

k
x
x
k
i
i
M
=
=
1

where:
X
M
=the consensus value;
X
i
=the result reported by laboratory i; and
k =the number of accepted results (laboratories).

10.2.2 The standard deviation of the consensus value, S
M
, is estimated by:

1
1
2
=

=
k
) x x (
s
k
i
i M
M

10.2.3 Calculation of z-score for an analysis

A z-score is calculated for each analysis by:

M
M
s
x x
z

=
i
i


10.3 Scope of Assessment of Proficiency

The two test cycles in the year are treated as independent assessments of proficiency by PTP-MAL.

10.4 Tests for Assessment of Proficiency

TG LABS MAWG sets targets for four statistical tests to assess proficiency:
- the individual z-score to assess a single analysis;
- the behaviour of the absolute values of a set of z-scores to assess a series of analysis for the
same metal;
- the Re-scaled Sum of z-Scores (RSZ) to detect consistent bias in an analytical system; and
- the Squared Sum of z-Scores (SSZ) to detect abnormally high deviation in the overall
performance of a laboratory.

10.4.1 Assessment of proficiency: z-score

z-score Range Rating
l z
i
l s 2 Satisfactory
2 < l z
i
l < 3 Questionable
l z
i
l > 3 Unsatisfactory

10.4.2 Combining z -scores: Distribution of absolute values

The distribution of the absolute value of z-scores is calculated when there are three or more
samples analysed by the same method (digestion and instrumental analysis) for a metal. The
distribution of the absolute value of z-scores is assessed as:

Absolute z-scores Rating
All z-scores < 2 Good
All z-scores < 3 Satisfactory
Only one z-score > 3 Questionable
Two or more z-scores > 3 Unsatisfactory

The combined z-scores is used to assign an assessment of performance based on the analyses for a
given analyte in a series of test samples.

For gold, platinum and palladium see Section 10.0 for details.


10.4.3 Combining z-scores: Re-scaled Sum of z-Scores

The Re-scaled Sum of z-Scores (RSZ) is calculated by E zi / \ n when there are three or more
samples analysed by the same method (digestion and instrumental analysis) for a metal. RSZ uses
the signs of the z-scores to detect consistent bias in an analytical system.

In order to avoid undue emphasis on an isolated poor result, z-scores greater than +3 or less than 3
are assigned the value of 3 and -3, respectively.

l RSZ l Range Rating
l RSZ l s 2 Good
2 < l RSZ l s 3 Satisfactory
3 < l RSZ l < 4 Questionable
l RSZ l > 4 Unsatisfactory


10.4.4 Combining z-scores: Squared Sum of z-Scores

The Squared Sum of z-Scores (SSZ) is calculated by E zi
2
when there are three or more samples
analysed by the same method (digestion and instrumental analysis) for a metal. SSZ does not take
into account the signs of the z-scores and is used to detect abnormally high deviations between
values from the same population.

SSZ is compared with the value in the _
2
(chi-squared) distribution table at the agreed confidence
levels with n degrees of freedom, where n =the number of analyses for a metal.

Confidence Limit Rating
95% Satisfactory
99% Questionable
>99% Unsatisfactory

Table of
2
versus confidence interval

2

Confidence
Interval
n = 2 n = 3 n = 4 n = 5 n = 6
95% s 5.99 s 7.82 s 9.49 s 11.07 s 12.59

99%
>5.99
s 9.21
>7.82
s 11.34
>9.49
s 13.28
>11.07
s 15.09
>12.59
s 16.81
>99% >9.21 >11.34 >13.28 >15.09 >16.81


10.5 Withdrawal of sample
If, after investigation, the level of homogeneity is found to be unsatisfactory, the sample will be
withdrawn and the participants notified. The proficiency calculations are carried out as described
previously. Note that if one of the samples containing Pt or Pd is withdrawn then no certificate will be
issued for Pt or Pd in that cycle. The results of the findings will be discussed in the Comprehensive
Report.

10.6 Example

Examples of the assessment of the proficiency of a participating laboratory are given in Appendix C.

10.7 Overall Assessment of Proficiency

PTP-MAL applies a fifth assessment test that is not part of ISO/IEC 17043 (CAN-P-43) or the SCC
MAWG assessment. The Overall Assessment of Proficiency is given by the lowest rating achieved by
a laboratory for Distribution of Absolute Values of z -scores, Re-scaled Sum of z-Scores or Squared Sum
of z-Score. There must be at least three samples analysed by the same method (digestion and
instrumental analysis) and only these will be used to get an overall assessment of proficiency for Cu, Ni,
Pb, Co, Zn, Ag.

For platinum and palladium where only two results have been submitted, a Satisfactory overall
assessment is given if both z-scores are satisfactory.

Gold is assessed by either single method or multi-method.
For gold single-method, there must be at least three samples analysed by the same method (including
both digestion and instrumental analysis) and only these (results) will be used to get an overall
assessment of proficiency. If Satisfactory, gold will appear on the certificate.
For gold multi-method (MM), there must be results from at least three samples submitted. A maximum of
2 different methods (digestion and instrumental analysis) should be submitted regardless the number of
samples tested. If Satisfactory, "gold
MM
" will appear on the certificate.

11.0 CERTIFICATE OF SUCCESSFUL PARTICIPATION IN PROFICIENCY TESTS

For each cycle, PTP-MAL issues a Certificate of Successful Participation in Proficiency Tests to each
participating laboratory for the metals for which the laboratory achieved a Satisfactory rating overall for
that cycle. [Note that this is independent of SCC accreditation.]

Note: The certificate for the test samples of a cycle will state has been assessed "Satisfactory" for test
samples in Cycle Month 2XXX. A certificate for a set of remedial samples will state "has been assessed
"Satisfactory" for remedial samples for Cycle Month 2XXX

12.0 REFERENCES

CAN-P-43 Proficiency Testing by Inter-laboratory Comparison - Part 1: Development and
Operation of Proficiency Testing Schemes
ISO 17043 Conformity assessment General requirements for proficiency testing
CAN-P-1579 Requirements for the Accreditation of Mineral Analysis Testing Laboratories
ISO/IEC 17025 General requirements for the competence of calibration and testing laboratories
CAN-P-1570 Program for the Accreditation of Laboratories Canada (PALCAN), PALCAN
Handbook
ASTM E 178 Standard Practice for Dealing with Outlying Observations

13.0 APPENDICES

- Appendix A: Acronym for Analytical Methods
- Appendix B: Fees, examples, Fax Form for Intent to Participate in PTP-MAL
- Appendix C: Two examples of Assessment of Proficiency

Appendix A

Abbreviations for Analytical Methods

Method Descriptor = Code 1 - Code 2 (For example, the method descriptor for analyzing a sample
for copper (1) by sodium peroxide fusion followed by measurement by graphite furnace atomic
absorption is FSP-GAA and (2) by X-ray fluorescence with pressed powder pellets is PPP-XRF).

Code 1 Procedure for Decomposition/Preparation of Solid Samples
ADN Acid Decomposition, where N =the number of different acids used
FLM Fusion with Lithium Metaborate
FSP Fusion with Sodium Peroxide
FSC Fusion with Sodium Carbonate
FPP Fusion with Potassium Pyrosulphate
FAL Fire Assay with Lead Button Collection
FAN Fire Assay with Nickel Sulphide Collection
FAT Fire Assay with Tin Button Collection
PPP Pressed Powder Pellet
FP Fused Pellet
Code 2 Procedure for Measurement
VOL Volumetry or Titrimetry
GRV Gravimetry
COU Couloumetry
OPT Visible and UV Spectrometry
FAA Flame Atomic Absorption Spectrometry
GAA Graphite Furnace Atomic Absorption Spectrometry
HAA Hydride Generation Atomic Absorption Spectrometry
ICPE Inductively Coupled Plasma Optical Emission Spectrometry
ICPM Inductively Coupled Plasma Mass Emission Spectrometry
XRF X-Ray Fluorescence Spectrometry
IC Ion Chromatography
INAA
Instrumental Neutron Activation Analysis (sample analyzed without
decomposition)
NAA Neutron Activation Analysis (measurement of a decomposed sample)

Appendix B

Fees

The Proficiency Testing Program for Mineral Analysis Laboratories (PTP-MAL) consists of two test cycles
issued each year. For each cycle, participating laboratories receive 4 to 5 test samples. Each sample
can be analyzed for up to nine metals: gold, silver, copper, zinc, lead, nickel, cobalt, platinum and
palladium. Participants submit their results, and PTP-MAL assesses their laboratory performance as
described in Section 10.0.
The fee for participating in PTP-MAL includes the laboratory performance report, the comprehensive
report of a regular cycle and the certificate (if applicable). For a set of remedial samples, only the
laboratory performance report and the certificate (if applicable) are provided.

Basic fee

Participants have the option to register for one or two cycles at the same time. The basic fees per cycle
are in Canadian dollars (Can) and include one assessment for up to nine elements at a cost of $750.
Registration for two cycles is only offered during September cycle and has to be paid in full at the time of
the first cycle (September cycle). The deadline for payment of two cycles is the same as for one cycle
registration.

Note: Basic fees include the assessment of only one method per element. Supplemental fees are
applicable for the assessment of additional analytical methods.

Note: There is no discount for doing fewer than the nine elements offered.

Note: Payments for your participation in PTP-MAL can now be made in Canadian or US dollars.

Canadian Destination
The fee for each cycle is Can $750 for one set of samples and is collected by prepayment before the
samples are shipped. Participants must add applicable taxes (G.S.T. / H.S.T.).
Foreign Destination
The fee for each cycle is Can $750 for one set of samples and is collected by prepayment before the
samples are shipped. There is a Can $150 surcharge for shipping and handling for destinations outside
of Canada. No tax is charged.


Supplemental Fees per Cycle

Laboratories may choose to submit data for a metal using two or more different analytical methods.
There is a supplemental fee of Can $40 for each additional analytical method for which data are
submitted per metal.
Additional sets of samples can be requested at a supplementary fee of Can $375 each (plus applicable
taxes for Canadian participants).
Fee for a set of remedial samples
First option: A laboratory may request the same set of samples of the most recent cycle to assist in
undertaking the required corrective action for the analytical method. Costs will be Can $375 per set. No
assessment of performance will be provided. No comprehensive report and certificate will be
provided.
Second option: A remedial sample set, completely different than the most recent cycle set, may be
required by a laboratory to independently demonstrate to a third party (e.g. SCC) that measurement
deficiencies of a cycle have been corrected. Such sets and specific re-assessments may be provided by
PTP-MAL on a custom basis if requested by the laboratory. Costs will be Can $600 per set plus Can
$100 for each element or method re-assessed (plus applicable taxes for Canadian destinations.). A Can
$150 shipping and handling surcharge will apply to destinations outside of Canada. An assessment of
performance and a certificate (if applicable) will be provided. No comprehensive report will be
provided.

Examples on how to calculate the fees per cycle

Participating laboratory located in Canada who want be assessed for:

- Gold by method A
- Silver, Copper, Lead, Zinc, Nickel, and Cobalt by method B
- Platinum and Palladium by method C.

DESCRIPTION No. units Unit Cost TOTAL
1. Basic Fee: Includes 1 set of test samples
70g each. Includes assessments of one
method per metal.
1 Can $ 750 Can $750
2. Add $375 for each additional set of
samples. (Includes material only).
Can $375
3. Add $40 for each additional method to be
assessed (per metal).
Can $40
4. Non-Canadian participants: add $150 for
extra S&H of foreign shipments, or provide
name and account number for shipping
collect.

Can $150
or courier name
and account #

Sub-Total
5. Canadian participants:
Please add applicable taxes.

G.S.T. / H.S.T.
or exemption #
+G.S.T./H.S.T.
6. Payment by Wire Transfer Can$30
Total
Can $750
+G.S.T.

Participating laboratory located outside Canada who want be assessed for:
- Gold only by method D.

method per metal.
1 Can $750 Can $750
Can $375
Can $40
collect.

Can $150
or courier name
and account #
Can $150
Sub-Total

G.S.T. / H.S.T.
or exemption #

Total Can $900


- Gold by method A *
- Gold by method P
- Silver, Copper, Lead, Zinc, Nickel, and Cobalt by method B *
- Copper, Lead, Nickel and Cobalt by method D
- Platinum and Palladium by method C *.

method per metal.
1 Can $750 Can $750
Can $375
5 Can $40 Can $200
collect.

Can 150
or courier name
and account #

Sub-Total

G.S.T. / H.S.T.
or exemption #
+G.S.T./H.S.T.
Total
Can $950
+G.S.T.
* Methods are covered in the basic fee (1 method for each of 9 elements ($750))
There are 5 additional metal/method assessments at $40 each =($200).


- Gold by 30g lead fire-assay with FAA measurement and ICPE measurement
- Gold by a second 30g lead fire-assay with gravimetric finish
- Platinum and palladium by 25g nickel fire assay (FAN) with ICPM finish
- Silver, Copper, Lead, Zinc, Nickel, and Cobalt by method B

(Lab needs at least 90g to do these measurements and therefore a second set of samples.)

method per metal.
1 Can $750 Can $750
1 Can $375 Can $375
2 Can $40 Can $80
collect.

Can $150
or courier name
and account #

Sub-Total

G.S.T. / H.S.T.
or exemption #
+G.S.T./H.S.T.
Total
Can $1205
+G.S.T.

There are two additional method assessments (in total there are three methods to be assessed for gold).

Payment by using wire transfer

BANKING DETAILS
To get banking details, please contact us at ptp@nrcan.gc.ca or at 613-995-4738
VERY IMPORTANT: on wire transfer forms, ALWAYS ADD PT in front of your invoice number. This
accelerates receipt of the payment.
Example: Write PT44893 instead of 44893

Fa x : PTP- M AL
D a te :
N umber of pa ges including cover sheet :
Ema il ptp@ nrcan.gc.ca
Telephone (6 1 3 ) 9 4 3 - 0 2 3 3
Fa x (6 1 3 ) 9 4 3 - 0 5 7 3
To

PTP- M AL C oordina tor
M M SL- C AN M ET
5 5 5 , Booth Street
O tta wa , O nta rio
K1 A 0 G 1
C a na da

N a me
O rga niza tion
Address
Telephone
Fa x
From
Ema il

Appendix C

First Example of Assessment of Proficiency

Analysis for Gold (single-method) in a Cycle of Four Test Samples for the Assessment of Proficiency.

Results for All Laboratories:

Analytical Results for Gold (g/g)
Sample 1 Sample 2 Sample 3 Sample 4
Number Labs. 35 35 35 34
Mean Value 26.20 3.10 8.67 0.28
Stand. Dev. 1.11 0.98 1.11 0.074

Results for Laboratory 5 (same method used for all 4 samples):

Analytical Results for Gold (g/g)

Result 27.71 3.55 8.50 0.47

Assessment of Proficiency of Laboratory 5:

(1) z-score

z-score 1.36 0.46 -0.15 2.57
Rating Satisfactory Satisfactory Satisfactory Questionable

(2) Distribution of absolute values

Absolute z-scores Rating
All z-scores < 3 Satisfactory

(3) Re-scaled Sum of z-Scores

l RSZ l Rating
l RSZ l = 2.37 Satisfactory

(4) Squared Sum of z-Scores

SSZ =8.68

_
2
Table at n =4

2

n = 4 Conf. Int. Rating
s 9.49 95% Satisfactory
>9.49 s 13.28 99%
>13.28 >99%

(5) Overall assessment is Satisfactory
Certificate awarded for Au single method.

Second Example of Assessment of Proficiency

Results for laboratory XY of: z-score, individual z-score, distribution of z, Re-scaled Sum of z-Scores (RSZ) and Squared Sum of z-Scores (SSZ).
An individual z-score rating is given to each corresponding z-score value according to Section 10.4.1.

DC: decomposition FC: Analytical method nc: not calculated
1
G: good, S: satisfactory, Q: Questionable, U: unsatisfactory
2
z-scores greater than +3 or less than 3 are assigned the value of 3 and -3, respectively
z score samples
Element
1 2 3 4
RSZ SSZ
Individual
z score
dist z
RSZ
rating
SSZ
rating
Overall DC-1 DC-2 DC-3 DC-4 FC-1 FC-2 FC-3 FC-4
Element on
certificate
Ag 0.42 0.45 0.45 0.92 1.13 1.44 SSSS G G S S AD2 AD2 AD2 AD2 FAA FAA FAA FAA Yes
Co 2.33 1.95 0.94 0.26 2.75 10.2 QSSS S S Q Q FSP FSP FSP FSP FAA FAA FAA FAA No
Ni -1.80 -2.24 -0.84 -1.18 -3.03 10.3 SQSS S Q Q Q AD4 AD4 AD4 AD4 ICPM ICPM ICPM ICPM No
Pb -1.84 -3
2
-0.67 0.87 -2.30 13.5 SUSS Q S U U AD3 AD3 AD3 AD3 FAA FAA FAA FAA No
Ag 1.35 1.50 0.0050 -1.03 1.05 5.15 SSSS G G S S AD4 AD4 AD4 AD4 ICPE ICPE FAA ICPE Yes
Cu 1.88 2.11 0.59 0.60 nc nc SQSS nc nc nc nc AD4 AD4 AD4 AD4 ICPE ICPE FAA FAA No
Pt -1.61 -1.68 nc nc SS S nc nc S FAL FAL ICPE ICPE Yes
Pd -2.82 -0.58 nc nc QS Q nc nc Q FAL FAL FAA FAA No

PTP-MAL applies a fifth assessment: Overall assessment. The overall rating is given by the lowest
rating achieved by a laboratory for distribution of z, RSZ and SSZ. There must be at least three samples
tested by the same method (digestion and instrumental analysis) to get an overall assessment of
proficiency for Ag, Co, Cu, Ni, Pb, Zn.

Note: If a laboratory received a Questionable rating for any of distribution of z, SSZ or RSZ, the overall
rating will be either a Questionable or Unsatisfactory which means that the laboratory did not pass the
element for that cycle.

For platinum and palladium where only two results have been submitted, a Satisfactory overall
assessment is given if both z-scores are satisfactory.

Interpretation of the results showed in the table above:

For Ag: Both sets got a Satisfactory overall. Silver by AD2+FAA and AD4+ICPE will appear on the
certificate.

For Co: distribution z: S RSZ: S and SSZ: Q The lowest rating is Q then the overall assessment
will be Questionable.

For Ni: distribution z: S RSZ: Q and SSZ: Q. The lowest rating is Q then the overall assessment
will be Questionable.

For Pb: distribution z: Q RSZ: S and SSZ: U. The lowest rating is U then the overall assessment
will be Unsatisfactory.

For Cu: not calculated because less than three results used the same method (decomposition+
instrumental analysis). Only z-score are calculated.

For Pt: A Satisfactory overall is given because both z-scores are satisfactory.

For Pd: A Questionable overall is given because the lowest rating of the z-scores is Q (Questionable)

Gold can be assessed on either single-methodor multi-method. In both cases, results for at least three samples must be submitted. To be assessed single-method, three or more samples must have
been analyzed using the same method. To be assessed multi-method, the results of at least three samples must be reported and a maximum of 2 different methods (digestion and instrumental analysis)
should be submitted regardless the number of samples tested. Looking at the table below, Gold #1 to 4 is rated for single-method. Gold #5 is rated for multi-method. Gold #6 is not rated because less
than three results have been submitted.

PTP-MAL issues a certificate when a laboratory achieves a Satisfactoryrating overall. In the tables above, only silver, platinum, gold #1, 4 and 5 would appear on the certificate.

z score samples
Gold
1 2 3 4
RSZ SSZ
Individual
z score
dist z
RSZ
rating
SSZ
rating
Overall DC-1 DC-2 DC-3 DC-4 FC-1 FC-2 FC-3 FC-4 Single-method Multi-method
1 -1.85 -1.71 0.23 -1.17 -2.25 7.83 SSSS G S S S FAL FAL FAL FAL ICPE ICPE ICPE ICPE Satisfactory
2 -0.91 2.00 -1.76 -1.30 -0.91 9.66 SQSS S G Q Q FAL FAL FAL FAL FAA FAA FAA FAA Questionable
3 -2.22 0.18 -1.50 -2.92 -3.23 15.8 QSSQ S Q U U FAL FAL FAL FAL FAA FAA FAA FAA Unsatisfactory
4 1.68 1.82 -0.35 0.11 1.82 6.29 SSSS G G S S FAL FAL FAL FAL FAA FAA FAA GRV Satisfactory
5 0.67 0.36 -0.13 0.55 0.72 0.91 SSSS G G S S FAL FAL FAL FAL ICPE ICPE FAA FAA Satisfactory
6

2.46 -0.13 nc nc --QS nc nc nc nc FAL FAL GRV GRV

Elements on the Certificate

This protocol determines if an element (Ag, Cu, Co, Ni, Pb, Zn) qualifies to be on a certificate.

Note that this protocol is valid only for Ag, Cu, Co, Ni, Pb, Zn. For platinum and palladium, where only
two samples are provided, a Satisfactory overall assessment will be given if both z-scores are
satisfactory. Gold is assessed by either single-method or multi-method. For more details see section
10.1.

Protocol for Determining Certifiability of Element
Is the method 'constant'?
(Same method for all samples?)

Yes No
Are there 3 results?

Element does NOT
qualify to be on
certificate
Is the Overall
rating satisfactory?

Are there 3 results
by the SAME method
Using only results by the same
method, recalculate:
RSZ value and SSZ value
Using only results by the same
method, and the new
RSZ and SSZ values, use the
PTP rules to determine:
Distribution of z rating
RSZ rating,
SSZ rating
The lowest of these three
becomes the " overall rating"
Is the new Overall rating
satisfactory?

Element does
NOT qualify to
be on
certificate
Element does
qualify to be
on certificate

Yes No
Yes No
Yes No
Element does
NOT qualify to
be on
certificate
Yes No
Element does
qualify to be
on certificate

Element does
NOT qualify to
be on
certificate

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