technical report itak rt-382-2020 pep...rt-382-2020 cgcre’s accredited abnt nbr iso/iec 17043:2011...

TECHNICAL REPORT ITAK

RT-382-2020 PEP

PROFICIENCY TEST FOR COPPER ORE AND

CONCENTRATE ANALYSIS

35th ROUND – JANUARY 2021

RT-382-2020 Cgcre’s accredited ABNT NBR ISO/IEC 17043:2011 Proficiency Testing Provider. Accreditation

nº PEP 0021. Contacts: email: [email protected]; Phone nº: +55 31 3851-3166 / +55 31 3851-6952 2 / 38

PROFICIENCY TEST PROGRAM IN COPPER ORE AND CONC. ANALYSIS – 35th ROUND

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1) Introduction

This Technical Report presents the obtained results, its evaluation and interpretation for

the participant laboratory.

The description of the statistical criteria and techniques used in the evaluation as well as

general information about this proficiency test is in a separate module and available to

each participant in the ITAK PTP Management System.

ITAK does not issue preliminary report. This current report is characterized as Final

Technical Report.

2) Preliminary Information

Tab. 1: Round information and participant laboratory identification

Round Identification: 35th Round – PTP in Copper Ore and Concentrate

Period of execution: November and December 2020

Laboratory Identification: Assarel Medet JSC

Unit/Site: Panagyurishte – Bulgaria

Laboratory Code: 12

Test Item Codes for this round: C69 and C70

Issue Data of this Report: January 12 of 2021

3) Participants of the Proficiency Testing

The participating laboratories of this inter-comparison PT are listed below:

Participating Laboratory Name Unit/Site

Alex Stewart Agriculture Supervisão e Análises Ltda Santos/SP - Brazil

Alex Stewart International Liverpool - England

AngloGold Ashanti Córrego do Sítio Mineração – SB Santa Bárbara/MG - Brazil

Assarel Medet JSC Panagyurishte - Bulgaria

Bureau Veritas Minerals Inspectorate Services - Constancia Lima - Perú

Bureau Veritas Minerals Inspectorate Services - Miller Miller - Perú

Ellatzite Med A.D. Mirkovo - Bulgaria

Magnesita Refratários S.A. Contagem/MG - Brazil

Mineração Caraíba S.A. Jaguarari/BA - Brazil

Mineração Maracá Indústria e Comércio S.A. Alto Horizonte/GO - Brazil

Paranapanema S.A. Dias D’Ávila/BA - Brazil

Vale – Centro de Desenvolvimento Mineral Santa Luzia/MG - Brazil

Vale – Salobo Marabá/PA - Brazil

4) Appeal

It is afforded to the participant of Proficiency Testing Programs - ITAK the right of appeal

as to the evaluation of its performance given in this Technical Report. For that, the

participating laboratory who have doubts or does not agree with the performance

evaluation should register an appeal on the ITAK PTP Management System. According to

a requirement of ISO/IEC 17043 – Conformity assessment - General requirements for




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Proficiency Testing, ITAK maintains a documented procedure governing all the systematic

including deadlines for appeal, analyses, and responses to participating clients.

5) Performance Commentary

Tab. 2: Performance evaluation of the participating laboratory – consolidated information.

Test

Item Analyzed

Parameter

Assigned

Value

obtained by

Standard

Deviation

obtained by

Reference

Tables Z Score

Performance Youden

Performance

C69 Ag Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2

5 Lab has not

participated

Lab has not

participated C70 Ag 6

C69 As Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2

8 Lab has not

participated

Insufficient

results C70 As 9

C69 Au Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2

11 Satisfactory Unsatisfactory

C70 Au 12 Satisfactory

C69 C Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2

14 Lab has not

participated

Insufficient

results C70 C 15

C69 Cl Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2

17 Lab has not

participated

Insufficient

results C70 Cl 18

C69 Cu Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2

20 Satisfactory Satisfactory

C70 Cu 21 Satisfactory

C69 F Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2

23 Lab has not

participated

Insufficient

results C70 F 24

C69 Fe Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2


C70 Fe 27 Satisfactory

C69 Ni Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2

29 Insufficient

results

Insufficient

results C70 Ni 30

C69 S Mean of data set means, Outliers

according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2


C70 S 33 Satisfactory

C69 SiO2 Mean of data set means, Outliers according

ISO 5725-2

Reproducibility

Standard

Deviation

ISO 5725-2

35 Lab has not

participated

Lab has not

participated C70 SiO2 36




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6) Summary of Assigned Values, EP Standard Deviations and Uncertainties

Tab. 3: Assigned Values, EP Standard Deviations and Standard Uncertainties – Summarized

Information.

Parameter Test

Item Unit

Assigned Value

(XD)

Standard

Deviation (S)

Standard

Uncertainty (U)

Ag C69 g/t 1.087 0.14 0.086 C70 g/t 39.5 3.7 2.0

As C69 g/t --- --- --- C70 g/t 10.2 3.9 4.0

Au C69 g/t 0.294 0.036 0.022 C70 g/t 13.79 0.92 0.57

C C69 % 0.0659 0.011 0.0076 C70 % 0.039 0.014 0.010

Cl C69 g/t 124 25 26 C70 g/t --- --- ---

Cu C69 % 0.3104 0.0026 0.0052 C70 % 24.26 0.086 0.34

F C69 g/t 1002 129 93 C70 g/t 70 54 48

Fe C69 % 4.90 0.55 0.29 C70 % 29.39 0.79 0.42

Ni C69 % 0.0030 0.0028 0.0029 C70 % 0.0030 0.0000 0.0000

S C69 % 2.281 0.059 0.030 C70 % 33.8 2.1 1.1

SiO2 C69 % 61.0 3.6 2.4 C70 % 7.24 0.74 0.50




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7) Mandel’s Graphs

Pic. 1: Graph with Mandel’s h statistics for sample C69 for all involved parameters.

Pic. 2: Graph with Mandel’s h statistics for sample C70 for all involved parameters.




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Pic. 3: Graph with Mandel’s k statistics for sample C69 for all involved parameters.

Pic. 4: Graph with Mandel’s k statistics for sample C70 for all involved parameters.




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8) Results, Methods, Graphs and Interpretation.

Tab. 4 – Assigned Value, Standard Deviations and Standard Uncertainties for Ag.

Assigned Value

𝑿𝑫 (g/t)

Standard Deviation

𝒔 (g/t)

Standard Uncertainty

𝒖 (g/t) Sample

C69 1.087 0.14 0.086

C70 39.5 3.7 2.0

Tab. 5 – Reported Results, means and Z Scores of participating laboratories in the PT for Ag analysis in the sample C69.

Results for Ag – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Ag --- --- --- --- --- g/t --- --- --- Lab 02 Ag --- --- --- --- --- g/t --- --- --- Lab 03 Ag --- --- --- --- --- g/t --- --- --- Lab 04 Ag 3.000 3.000 3.000 3.000 3.000 g/t 3.000 13.979 DIGAC-AAS Lab 05 Ag 2.657 2.608 2.696 2.563 2.561 g/t 2.617 11.180 DIGAC-AAS Lab 06 Ag 1.380 1.300 1.260 1.380 1.200 g/t 1.304 1.585 DIGAC-AAS Lab 07 Ag --- --- --- --- --- g/t --- --- --- Lab 08 Ag 18.413 17.933 18.593 18.126 18.292 g/t 18.271 125.580 POP-XRF Lab 09 Ag 1.100 1.150 0.950 1.000 0.964 g/t 1.033 -0.397 DIGAC-AAS Lab 10 Ag 1.100 1.100 1.100 1.100 1.100 g/t 1.100 0.094 DIGAC-AAS Lab 11 Ag 1.000 0.995 0.975 0.975 0.990 g/t 0.987 -0.731 DIGAC-AAS Lab 12 Ag --- --- --- --- --- g/t --- --- --- Lab 13 Ag 1.002 1.003 1.003 1.025 1.025 g/t 1.012 -0.552 DIGAC-ICP

Tab. 6 – Reported Results, means and Z Scores of participating laboratories in the PT for Ag analysis in the sample C70.

Results for Ag – Sample C70 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Ag --- --- --- --- --- g/t --- --- --- Lab 02 Ag --- --- --- --- --- g/t --- --- --- Lab 03 Ag 43.000 40.000 40.000 42.000 41.000 g/t 41.200 0.470 FAAS Lab 04 Ag 51.000 52.000 51.000 52.000 52.000 g/t 51.600 3.318 DIGAC-AAS Lab 05 Ag 40.870 39.812 40.680 40.697 40.377 g/t 40.487 0.274 DIGAC-AAS Lab 06 Ag 45.681 46.500 44.911 49.377 44.799 g/t 46.254 1.854 DIGAC-AAS Lab 07 Ag 39.001 39.671 36.853 36.018 38.414 g/t 37.991 -0.409 DIGAC-AAS Lab 08 Ag 13.497 13.178 13.238 13.377 13.214 g/t 13.301 -7.173 POP-XRF Lab 09 Ag 41.200 42.000 40.000 41.200 39.100 g/t 40.700 0.333 DIGAC-AAS Lab 10 Ag 36.010 35.560 36.280 35.950 35.880 g/t 35.936 -0.972 DIGAC-AAS Lab 11 Ag 35.310 35.290 34.940 35.010 34.940 g/t 35.098 -1.202 DIGAC-AAS Lab 12 Ag --- --- --- --- --- g/t --- --- ---

Lab 13 Ag 38.125 38.126 38.265 38.298 38.296 g/t 38.222 -0.346 DIGAC-ICP

Legend:

DIGAC-AAS Acid dissolution / Atomic Absorption Spectromety – AAS

DIGAC-ICP Acid dissolution / Optical Emission Spectromety – ICP-OES

FAAS Fire Assay / Atomic Absorption Spectromety – AAS

POP-XRF Pressed Pellet / X-Ray Fluorescence

X,XX Satisfactory Result

X,XX Questionable Result

X,XX Unsatisfactory Result




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Pic. 5: Graph with Z Scores for samples C69 and C70 for Ag Analysis.

Laboratory 12 - Assarel Medet JSC has not participated of the PT for the parameter Ag.

Pic. 6: Youden Plot for Ag Analysis.

Performance Commentary – Confidence Ellipse:

Laboratory 12 - Assarel Medet JSC has not participated of the PT for the parameter Ag.




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Pic. 7: Ranking Graph according to the Mandel’s k statistic to sample C69 for Ag Analysis.

Pic. 8: Ranking Graph according to the Mandel’s k statistic to sample C70 for Ag Analysis.




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Tab. 7 – Assigned Value, Standard Deviations and Standard Uncertainties for As.

Assigned Value

𝑿𝑫 (g/t)

Standard Deviation

𝒔 (g/t)


𝒖 (g/t) Sample

C69 --- --- ---

C70 10.2 3.9 4.0

Tab. 8 – Reported Results, means and Z Scores of participating laboratories in the PT for As analysis in the sample C69.

Results for As – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 As --- --- --- --- --- g/t --- --- --- Lab 02 As --- --- --- --- --- g/t --- --- --- Lab 03 As




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Pic. 9: Graph with Z Scores for the sample C70 for As Analysis.

Laboratory 12 - Assarel Medet JSC has not participated of the PT for the parameter As.

Assigned Value, EP Standard Deviation and Standard Uncertainty Calculations:

The valid results are not sufficient to calculate these parameters for the sample C69.

Z Scores:

The valid results are not sufficient to calculate the Z Scores for the parameter As for the sample

C69.

Confidence Ellipse:

The valid results are not sufficient to build the Confidence Ellipse for the parameter As.

Ranking Graphics:

The valid results are not sufficient to build the Ranking Graphics for the parameter As for the

sample C69.




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Pic. 10: Ranking Graph according to the Mandel’s k statistic to sample C70 for As Analysis.




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Tab. 10 – Assigned Value, Standard Deviations and Standard Uncertainties for Au.

Assigned Value

𝑿𝑫 (g/t)

Standard Deviation

𝒔 (g/t)


𝒖 (g/t) Sample

C69 0.294 0.036 0.022

C70 13.79 0.92 0.57

Tab. 11 – Reported Results, means and Z Scores of participating laboratories in the PT for Au analysis in the sample C69.

Results for Au – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Au --- --- --- --- --- g/t --- --- --- Lab 02 Au --- --- --- --- --- g/t --- --- --- Lab 03 Au --- --- --- --- --- g/t --- --- --- Lab 04 Au --- --- --- --- --- g/t --- --- --- Lab 05 Au --- --- --- --- --- g/t --- --- --- Lab 06 Au 0.279 0.216 0.242 0.250 0.217 g/t 0.241 -1.505 FAAS Lab 07 Au 0.295 0.310 0.283 0.297 0.306 g/t 0.298 0.109 FAAS Lab 08 Au 0.145 0.140 0.136 0.112 0.137 g/t 0.134 -4.506 POP-XRF Lab 09 Au 0.276 0.265 0.276 0.272 0.269 g/t 0.272 -0.639 FAAS Lab 10 Au 0.290 0.300 0.320 0.300 0.290 g/t 0.300 0.159 FA-GRAV Lab 11 Au 0.323 0.326 0.320 0.329 0.325 g/t 0.325 0.851 EXTR-AAS Lab 12 Au 0.328 0.334 0.330 0.330 0.332 g/t 0.331 1.025 FA-ICP Lab 13 Au 0.532 0.532 0.539 0.539 0.589 g/t 0.546 7.079 FAAS

Tab. 12 – Reported Results, means and Z Scores of participating laboratories in the PT for Au analysis in the sample C70.

Results for Au – Sample C70 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Au --- --- --- --- --- g/t --- --- --- Lab 02 Au --- --- --- --- --- g/t --- --- --- Lab 03 Au 14.000 13.800 13.900 13.850 14.000 g/t 13.910 0.126 FAAS Lab 04 Au --- --- --- --- --- g/t --- --- --- Lab 05 Au --- --- --- --- --- g/t --- --- --- Lab 06 Au 10.228 10.985 12.584 11.854 11.257 g/t 11.382 -2.636 FAAS Lab 07 Au 13.787 13.937 13.462 14.090 13.929 g/t 13.841 0.050 FAAS Lab 08 Au 0.011 0.155 0.344 0.204 0.605 g/t 0.264 -14.778 POP-XRF Lab 09 Au -- -- -- -- -- g/t --- --- --- Lab 10 Au 13.980 14.290 14.290 14.490 14.100 g/t 14.230 0.475 FAAS Lab 11 Au 13.220 13.100 13.240 13.240 13.310 g/t 13.222 -0.626 EXTR-AAS Lab 12 Au 12.470 12.460 12.435 12.456 12.405 g/t 12.445 -1.474 FA-ICP Lab 13 Au 15.148 15.265 15.078 15.042 15.072 g/t 15.121 1.448 FAAS

Legend:

FA-AAS Fire Assay / Atomic Absorption Spectromety – AAS

FA-GRAV Fire Assay / Gravimetric

EXTR-AAS DIBK Extraction / Atomic Absorption Spectromety – AAS

FA-ICP Fire Assay / Optical Emission Spectrometry – ICP-OES








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Pic. 11: Graph with Z Scores for samples C69 and C70 for Au Analysis.

Laboratory 12 - Assarel Medet JSC presented SATISFACTORY performance for Au analysis in the

samples C69 and C70, according to the criterion for Z Score evaluating.

Pic. 12: Youden Plot for Au Analysis.


The Confidence Ellipse obtained for Au analysis showed normal dispersion among the

participating laboratories. The laboratories 06, 08, 11, 12 and 13 were excluded from the

Confidence Ellipse.

Laboratory 12 - Assarel Medet JSC showed an UNSATISFACTORY performance for Au analysis

according to the criterion for Youden evaluation, because indicated possibility of random errors




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being excluded from the Ellipse. It is recommended to check the possible factors that may cause

random errors for Au analysis, such as calibration, operator, instruments, calculation and results

transcription.

Pic. 13: Ranking Graph according to the Mandel’s k statistic to sample C69 for Au Analysis.

Pic. 14: Ranking Graph according to the Mandel’s k statistic to sample C70 for Au Analysis.




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Tab. 13 – Assigned Value, Standard Deviations and Standard Uncertainties for C.

Assigned Value

𝑿𝑫 (%)

Standard Deviation

𝒔 (%)


𝒖 (%) Sample

C69 0.0659 0.011 0.0076

C70 0.039 0.014 0.010

Tab. 14 – Reported Results, means and Z Scores of participating laboratories in the PT for C analysis in the sample C69.

Results for C – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 C 0.051 0.049 0.049 0.049 0.050 % 0.050 -1.445 IR Lab 02 C 0.062 0.057 0.049 0.063 0.055 % 0.057 -0.770 IR Lab 03 C --- --- --- --- --- % --- --- --- Lab 04 C --- --- --- --- --- % --- --- --- Lab 05 C 0.060 0.060 0.060 0.064 0.061 % 0.061 -0.435 IR Lab 06 C 0.077 0.073 0.075 0.076 0.076 % 0.075 0.834 IR Lab 07 C --- --- --- --- --- % --- --- --- Lab 08 C --- --- --- --- --- % --- --- --- Lab 09 C 0.069 0.070 0.068 0.069 0.074 % 0.070 0.358 IR Lab 10 C 0.080 0.080 0.080 0.080 0.080 % 0.080 1.240 IR Lab 11 C --- --- --- --- --- % --- --- --- Lab 12 C --- --- --- --- --- % --- --- --- Lab 13 C 0.059 0.060 0.061 0.060 0.058 % 0.060 -0.558 IR

Tab. 15 – Reported Results, means and Z Scores of participating laboratories in the PT for C analysis in the sample C70.

Results for C – Sample C70 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 C 0.028 0.030 0.031 0.030 0.030 % 0.030 -0.662 IR Lab 02 C 0.088 0.084 0.147 0.107 0.089 % 0.103 4.431 IR Lab 03 C --- --- --- --- --- % --- --- --- Lab 04 C --- --- --- --- --- % --- --- --- Lab 05 C 0.038 0.040 0.037 0.037 0.040 % 0.038 -0.073 IR Lab 06 C 0.069 0.061 0.066 0.066 0.060 % 0.064 1.740 IR Lab 07 C --- --- --- --- --- % --- --- --- Lab 08 C --- --- --- --- --- % --- --- --- Lab 09 C -- -- -- -- -- % --- --- --- Lab 10 C 0.060 0.060 0.060 0.060 0.060 % 0.060 1.433 IR Lab 11 C --- --- --- --- --- % --- --- --- Lab 12 C --- --- --- --- --- % --- --- --- Lab 13 C 0.032 0.030 0.029 0.028 0.029 % 0.030 -0.687 IR

Legend:

IR Infrared Analyzer







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Pic. 15: Graph with Z Scores for samples C69 and C70 for C Analysis.

Laboratory 12 - Assarel Medet JSC has not participated of the PT for the parameter C.


The valid results are not sufficient to build the Confidence Ellipse for the parameter C.




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Pic. 16: Ranking Graph according to the Mandel’s k statistic to sample C69 for C Analysis.

Pic. 17: Ranking Graph according to the Mandel’s k statistic to sample C70 for C Analysis.




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Tab. 16 – Assigned Value, Standard Deviations and Standard Uncertainties for Cl.

Assigned Value

𝑿𝑫 (g/t)

Standard Deviation

𝒔 (g/t)


𝒖 (g/t) Sample

C69 124 25 26

C70 --- --- ---

Tab. 17 – Reported Results, means and Z Scores of participating laboratories in the PT for Cl analysis in the sample C69.

Results for Cl – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Cl --- --- --- --- --- g/t --- --- --- Lab 02 Cl --- --- --- --- --- g/t --- --- --- Lab 03 Cl --- --- --- --- --- g/t --- --- --- Lab 04 Cl --- --- --- --- --- g/t --- --- --- Lab 05 Cl 228 215 289 284 247 g/t 253 5.076 FUSALK-TIT Lab 06 Cl 111 111 85 108 119 g/t 107 -0.673 FUS-POT Lab 07 Cl --- --- --- --- --- g/t --- --- --- Lab 08 Cl --- --- --- --- --- g/t --- --- --- Lab 09 Cl -- -- -- -- -- g/t --- --- --- Lab 10 Cl -- -- -- -- -- g/t --- --- --- Lab 11 Cl --- --- --- --- --- g/t --- --- --- Lab 12 Cl --- --- --- --- --- g/t --- --- --- Lab 13 Cl 142 141 140 140 141 g/t 141 0.670 DIGAC-IC

Tab. 18 – Reported Results, means and Z Scores of participating laboratories in the PT for Cl analysis in the sample C70.

Results for Cl – Sample C70 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Cl --- --- --- --- --- g/t --- --- --- Lab 02 Cl --- --- --- --- --- g/t --- --- --- Lab 03 Cl --- --- --- --- --- g/t --- --- --- Lab 04 Cl --- --- --- --- --- g/t --- --- --- Lab 05 Cl




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Pic. 18: Graph with Z Scores for the sample C69 for Cl Analysis.

Laboratory 12 - Assarel Medet JSC has not participated of the PT for the parameter Cl.


The valid results are not sufficient to calculate these parameters for the sample C70.

Z Scores:

The valid results are not sufficient to calculate the Z Scores for the parameter Cl for the sample

C70.

Confidence Ellipse:

The valid results are not sufficient to build the Confidence Ellipse for the parameter Cl.

Ranking Graphics:

The valid results are not sufficient to build the Ranking Graphics for the parameter Cl for the

sample C70.




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Pic. 19: Ranking Graph according to the Mandel’s k statistic to sample C69 for Cl Analysis.




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Tab. 19 – Assigned Value, Standard Deviations and Standard Uncertainties for Cu.

Assigned Value

𝑿𝑫 (%)

Standard Deviation

𝒔 (%)


𝒖 (%) Sample

C69 0.3104 0.0026 0.0052

C70 24.26 0.086 0.34

Tab. 20 – Reported Results, means and Z Scores of participating laboratories in the PT for Cu analysis in the sample C69.

Results for Cu – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Cu --- --- --- --- --- % --- --- --- Lab 02 Cu --- --- --- --- --- % --- --- --- Lab 03 Cu 0.239 0.230 0.236 0.241 0.239 % 0.237 -28.166 DIGAC-TIT Lab 04 Cu 0.310 0.310 0.310 0.310 0.310 % 0.310 -0.165 DIGAC-AAS Lab 05 Cu 0.313 0.306 0.305 0.313 0.308 % 0.309 -0.548 DIGAC-ICP Lab 06 Cu 0.310 0.310 0.310 0.310 0.310 % 0.310 -0.165 DIGAC-AAS Lab 07 Cu 0.315 0.311 0.314 0.316 0.312 % 0.314 1.216 DIGAC-AAS Lab 08 Cu 0.407 0.403 0.383 0.339 0.386 % 0.384 28.131 POP-XRF Lab 09 Cu 0.352 0.363 0.350 0.347 0.344 % 0.351 15.639 DIGAC-AAS Lab 10 Cu 0.312 0.311 0.314 0.313 0.312 % 0.312 0.756 DIGAC-AAS Lab 11 Cu 0.308 0.307 0.311 0.311 0.310 % 0.309 -0.395 DIGAC-AAS Lab 12 Cu 0.306 0.306 0.310 0.311 0.310 % 0.309 -0.702 DIGAC-TIT Lab 13 Cu 0.292 0.296 0.292 0.285 0.296 % 0.292 -6.992 DIGAC-ICP

Tab. 21 – Reported Results, means and Z Scores of participating laboratories in the PT for Cu analysis in the sample C70.

Results for Cu – Sample C70 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Cu --- --- --- --- --- % --- --- --- Lab 02 Cu --- --- --- --- --- % --- --- --- Lab 03 Cu 24.270 24.380 24.260 24.360 24.270 % 24.308 0.506 DIGAC-TIT Lab 04 Cu 24.240 24.260 24.250 24.260 24.270 % 24.256 -0.101 DIGAC-TIT Lab 05 Cu 24.447 24.626 24.650 24.594 24.579 % 24.579 3.674 DIGAC-ICP Lab 06 Cu 24.280 24.310 24.360 24.410 24.360 % 24.344 0.927 DIGAC-TIT Lab 07 Cu 24.086 24.097 24.150 24.140 24.119 % 24.118 -1.709 DIGAC-TIT Lab 08 Cu 13.139 13.182 13.111 13.174 13.299 % 13.181 -129.482 POP-XRF Lab 09 Cu 24.815 24.433 24.688 24.419 24.419 % 24.555 3.389 DIGAC-TIT Lab 10 Cu 24.341 24.313 24.344 24.325 24.340 % 24.333 0.793 DIGAC-TIT Lab 11 Cu 24.340 24.240 24.200 24.340 24.260 % 24.276 0.132 DIGAC-TIT Lab 12 Cu 24.212 24.216 24.219 24.230 24.212 % 24.218 -0.548 DIGAC-TIT Lab 13 Cu 28.782 28.792 28.790 28.796 28.789 % 28.790 52.863 DIGAC-TIT

Legend:

DIGAC-TIT Acid dissolution / Titrimetric method

DIGAC-ICP Acid dissolution / Optical Emission Spectromety – ICP-OES

DIGAC-AAS Acid dissolution / Atomic Absorption Spectromety – AAS








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Pic. 20: Graph with Z Scores for samples C69 and C70 for Cu Analysis.

Laboratory 12 - Assarel Medet JSC presented SATISFACTORY performance for Cu analysis in the


Pic. 21: Youden Plot for Cu Analysis.


The Confidence Ellipse obtained for Cu analysis showed high dispersion among the participating

laboratories. The laboratories 03, 05, 08, 09 and 13 were excluded from the Confidence Ellipse.

Laboratory 12 - Assarel Medet JSC showed a SATISFACTORY performance for Cu analysis

according to the criterion for Youden evaluation.




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Pic. 22: Ranking Graph according to the Mandel’s k statistic to sample C69 for Cu Analysis.

Pic. 23: Ranking Graph according to the Mandel’s k statistic to sample C70 for Cu Analysis.




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Tab. 22 – Assigned Value, Standard Deviations and Standard Uncertainties for F.

Assigned Value

𝑿𝑫 (g/t)

Standard Deviation

𝒔 (g/t)


𝒖 (g/t) Sample

C69 1002 129 93

C70 70 54 48

Tab. 23 – Reported Results, means and Z Scores of participating laboratories in the PT for F analysis in the sample C69.

Results for F – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 F --- --- --- --- --- g/t --- --- ---

Lab 02 F --- --- --- --- --- g/t --- --- ---

Lab 03 F 1000 995 928 950 948 g/t 964 -0.292 COMB-POT

Lab 04 F --- --- --- --- --- g/t --- --- --- Lab 05 F 1194 1199 1209 1186 1212 g/t 1200 1.533 FUS-ISE Lab 06 F 1041 1060 1037 1071 1022 g/t 1046 0.342 FUS-ISE Lab 07 F --- --- --- --- --- g/t --- --- --- Lab 08 F 1139 1095 1402 1082 1178 g/t 1179 1.372 POP-XRF Lab 09 F -- -- -- -- -- g/t --- --- --- Lab 10 F 859 879 876 860 860 g/t 867 -1.047 FUS-ISE Lab 11 F --- --- --- --- --- g/t --- --- --- Lab 12 F --- --- --- --- --- g/t --- --- --- Lab 13 F 930 927 935 935 936 g/t 933 -0.537 DIGAC-IC

Tab. 24 – Reported Results, means and Z Scores of participating laboratories in the PT for F analysis in the sample C70.

Results for F – Sample C70 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 F --- --- --- --- --- g/t --- --- ---

Lab 02 F --- --- --- --- --- g/t --- --- ---

Lab 03 F 112 111 105 111 111 g/t 110 0.743 COMB-POT

Lab 04 F --- --- --- --- --- g/t --- --- ---

Lab 05 F




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Pic. 24: Graph with Z Scores for samples C69 and C70 for F Analysis.

Laboratory 12 - Assarel Medet JSC has not participated of the PT for the parameter F.


The valid results are not sufficient to build the Confidence Ellipse for the parameter F.




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Pic. 25: Ranking Graph according to the Mandel’s k statistic to sample C69 for F Analysis.

Pic. 26: Ranking Graph according to the Mandel’s k statistic to sample C70 for F Analysis.




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Tab. 25 – Assigned Value, Standard Deviations and Standard Uncertainties for Fe.

Assigned Value

𝑿𝑫 (%)

Standard Deviation

𝒔 (%)


𝒖 (%) Sample

C69 4.90 0.55 0.29

C70 29.39 0.79 0.42

Tab. 26 – Reported Results, means and Z Scores of participating laboratories in the PT for Fe analysis in the sample C69.

Results for Fe – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Fe --- --- --- --- --- % --- --- --- Lab 02 Fe --- --- --- --- --- % --- --- --- Lab 03 Fe 5.658 5.514 5.562 5.653 5.644 % 5.606 1.294 DIGAC-ICP Lab 04 Fe 5.550 5.490 5.490 5.490 5.550 % 5.514 1.125 DIGAC-TIT Lab 05 Fe 5.088 5.099 5.019 4.984 5.096 % 5.057 0.287 FUSALK-ICP Lab 06 Fe 7.732 7.800 8.453 7.562 7.994 % 7.908 5.515 DIGAC-AAS Lab 07 Fe 4.246 4.178 4.235 4.433 4.084 % 4.235 -1.220 DIGAC-AAS Lab 08 Fe 3.215 3.193 3.183 3.067 3.199 % 3.171 -3.171 POP-XRF Lab 09 Fe 4.113 3.856 3.924 3.788 4.008 % 3.938 -1.766 DIGAC-AAS Lab 10 Fe 4.690 4.710 4.720 4.700 4.730 % 4.710 -0.350 DIGAC-AAS Lab 11 Fe 4.950 5.000 4.990 5.000 4.930 % 4.974 0.134 DIGAC-ICP Lab 12 Fe 5.000 5.020 5.130 5.020 5.000 % 5.034 0.244 DIGAC-ICP Lab 13 Fe 5.055 5.056 5.026 5.029 5.026 % 5.038 0.252 DIGAC-ICP

Tab. 27 – Reported Results, means and Z Scores of participating laboratories in the PT for Fe analysis in the sample C70.

Results for Fe – Sample C70 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Fe --- --- --- --- --- % --- --- --- Lab 02 Fe --- --- --- --- --- % --- --- --- Lab 03 Fe 29.346 29.682 29.346 29.522 29.550 % 29.489 0.129 DIGAC-ICP Lab 04 Fe 30.710 30.650 30.710 30.770 30.650 % 30.698 1.649 DIGAC-TIT Lab 05 Fe 28.738 29.241 29.089 28.484 28.698 % 28.850 -0.676 FUSALK-ICP Lab 06 Fe 25.475 25.500 25.725 25.149 25.299 % 25.430 -4.979 DIGAC-AAS Lab 07 Fe 29.349 29.877 29.621 30.131 29.213 % 29.638 0.316 DIGAC-AAS Lab 08 Fe 14.467 14.452 14.466 14.454 14.424 % 14.453 -18.788 POP-XRF Lab 09 Fe 28.026 28.153 29.138 29.588 28.476 % 28.676 -0.894 DIGAC-AAS Lab 10 Fe 28.390 28.400 28.390 28.370 28.380 % 28.386 -1.259 DIGAC-AAS Lab 11 Fe 29.050 28.900 28.950 28.950 29.070 % 28.984 -0.507 DIGAC-ICP Lab 12 Fe 30.120 30.090 30.240 30.160 30.140 % 30.150 0.960 DIGAC-ICP Lab 13 Fe 28.789 28.765 28.764 28.800 27.768 % 28.577 -1.019 DIGAC-TIT

Legend:

DIGAC-TIT Acid dissolution / Titrimetric method DIGAC-AAS Acid dissolution / Atomic Absorption Spectromety – AAS

DIGAC-ICP Acid dissolution / Optical Emission Spectrometry – ICP-OES

FUSALK-ICP Alkaline fusion / Optical Emission Spectrometry – ICP-OES








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Pic. 27: Graph with Z Scores for samples C69 and C70 for Fe Analysis.

Laboratory 12 - Assarel Medet JSC presented SATISFACTORY performance for Fe analysis in the


Pic. 28: Youden Plot for Fe Analysis.


The Confidence Ellipse obtained for Fe analysis showed normal dispersion among the

participating laboratories. The laboratories 06 and 08 were excluded from the Confidence

Ellipse.

Laboratory 12 - Assarel Medet JSC showed a SATISFACTORY performance for Fe analysis





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Pic. 29: Ranking Graph according to the Mandel’s k statistic to sample C69 for Fe Analysis.

Pic. 30: Ranking Graph according to the Mandel’s k statistic to sample C70 for Fe Analysis.




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Tab. 28 – Assigned Value, Standard Deviations and Standard Uncertainties for Ni.

Assigned Value

𝑿𝑫 (%)

Standard Deviation

𝒔 (%)


𝒖 (%) Sample

C69 --- --- ---

C70 --- --- ---

Tab. 29 – Reported Results, means and Z Scores of participating laboratories in the PT for Ni analysis in the sample C69.

Results for Ni – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 Ni --- --- --- --- --- % --- --- --- Lab 02 Ni --- --- --- --- --- % --- --- --- Lab 03 Ni




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The valid results are not sufficient to calculate these parameters.

Z Scores:

The valid results are not sufficient to calculate the Z Scores for the parameter Ni.

Confidence Ellipse:

The valid results are not sufficient to build the Confidence Ellipse for the parameter Ni.

Ranking Graphics:

The valid results are not sufficient to build the Ranking Graphics for the parameter Ni.




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Tab. 31 – Assigned Value, Standard Deviations and Standard Uncertainties for S.

Assigned Value

𝑿𝑫 (%)

Standard Deviation

𝒔 (%)


𝒖 (%) Sample

C69 2.281 0.059 0.030

C70 33.8 2.1 1.1

Tab. 32 – Reported Results, means and Z Scores of participating laboratories in the PT for S analysis in the sample C69.

Results for S – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 S --- --- --- --- --- % --- --- --- Lab 02 S 1.960 1.950 1.960 1.950 1.950 % 1.954 -5.569 IR Lab 03 S 2.340 2.300 2.280 2.270 2.260 % 2.290 0.161 COMB-TIT Lab 04 S 2.220 2.160 2.210 2.200 2.300 % 2.218 -1.067 GRAV Lab 05 S 2.310 2.365 2.350 2.320 2.325 % 2.334 0.912 IR Lab 06 S 2.368 2.318 2.354 2.334 2.377 % 2.350 1.188 IR Lab 07 S 2.280 2.355 2.350 2.250 2.335 % 2.314 0.571 IR Lab 08 S 0.511 0.517 0.501 0.459 0.575 % 0.513 -30.152 POP-XRF Lab 09 S 2.300 2.330 2.310 2.330 2.325 % 2.319 0.656 IR Lab 10 S 2.200 2.240 2.230 2.220 2.190 % 2.216 -1.101 IR Lab 11 S 1.530 1.530 1.540 1.540 1.530 % 1.534 -12.733 FUS-XRF Lab 12 S 2.255 2.273 2.237 2.220 2.204 % 2.238 -0.729 IR Lab 13 S 2.245 2.235 2.268 2.236 2.245 % 2.246 -0.592 GRAV

Tab. 33 – Reported Results, means and Z Scores of participating laboratories in the PT for S analysis in the sample C70.

Results for S – Sample C70 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 S --- --- --- --- --- % --- --- --- Lab 02 S 37.700 37.700 37.800 37.800 37.200 % 37.640 1.868 IR Lab 03 S 33.860 33.840 33.900 34.040 34.100 % 33.948 0.073 COMB-TIT Lab 04 S 32.350 32.210 32.490 32.060 32.090 % 32.240 -0.757 GRAV Lab 05 S 33.784 33.746 33.793 33.775 33.777 % 33.775 -0.011 IR Lab 06 S 35.660 35.630 35.840 35.350 35.650 % 35.626 0.889 IR Lab 07 S 34.780 32.350 33.725 34.015 33.405 % 33.655 -0.069 IR Lab 08 S 8.235 8.284 8.351 8.292 8.289 % 8.290 -12.396 POP-XRF Lab 09 S -- -- -- -- -- % --- --- --- Lab 10 S 34.900 34.880 34.900 34.980 34.980 % 34.928 0.550 IR Lab 11 S 30.980 30.950 31.000 30.880 30.920 % 30.946 -1.385 FUS-XRF Lab 12 S 32.040 32.032 31.827 31.920 32.112 % 31.986 -0.880 IR Lab 13 S 33.096 33.095 33.125 33.090 33.005 % 33.082 -0.347 GRAV

Legend:

IR Infrared Analyzer

COMB-TIT Combustion / Titrimetric method

GRAV Gravimetric Method

FUS-XRF Fusion / X-Ray Fluorescence








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Pic. 31: Graph with Z Scores for samples C69 and C70 for S Analysis.

Laboratory 12 - Assarel Medet JSC presented SATISFACTORY performance for S analysis in the


Pic. 32: Youden Plot for S Analysis.


The Confidence Ellipse obtained for S analysis showed normal dispersion among the

participating laboratories. The laboratories 02, 08 and 11 were excluded from the Confidence

Ellipse.

Laboratory 12 - Assarel Medet JSC showed a SATISFACTORY performance for S analysis





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Pic. 33: Ranking Graph according to the Mandel’s k statistic to sample C69 for S Analysis.

Pic. 34: Ranking Graph according to the Mandel’s k statistic to sample C70 for S Analysis.




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Tab. 34 – Assigned Value, Standard Deviations and Standard Uncertainties for SiO2.

Assigned Value

𝑿𝑫 (%)

Standard Deviation

𝒔 (%)


𝒖 (%) Sample

C69 61.0 3.6 2.4

C70 7.24 0.74 0.50

Tab. 35 – Reported Results, means and Z Scores of participating laboratories in the PT for SiO2 analysis in the sample C69.

Results for SiO2 – Sample C69 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 SiO2 --- --- --- --- --- % --- --- --- Lab 02 SiO2 --- --- --- --- --- % --- --- --- Lab 03 SiO2 59.100 59.360 59.480 59.370 59.320 % 59.326 -0.456 GRAV Lab 04 SiO2 66.880 66.920 66.200 67.720 67.720 % 67.088 1.702 GRAV Lab 05 SiO2 61.080 61.528 60.885 60.347 61.285 % 61.025 0.016 FUSALK-ICP Lab 06 SiO2 --- --- --- --- --- % --- --- --- Lab 07 SiO2 --- --- --- --- --- % --- --- --- Lab 08 SiO2 50.107 50.203 49.316 44.631 49.560 % 48.763 -3.393 POP-XRF Lab 09 SiO2 -- -- -- -- -- % --- --- --- Lab 10 SiO2 59.060 59.220 59.590 59.100 59.650 % 59.324 -0.457 FUSALK-ICP Lab 11 SiO2 73.960 74.020 73.850 73.990 74.050 % 73.974 3.617 FUS-XRF Lab 12 SiO2 --- --- --- --- --- % --- --- --- Lab 13 SiO2 58.040 58.158 58.002 58.015 58.125 % 58.068 -0.806 GRAV

Tab. 36 – Reported Results, means and Z Scores of participating laboratories in the PT for SiO2 analysis in the sample C70.

Results for SiO2 – Sample C70 Code Parameter 1 2 3 4 5 Unit Average Z Score Method

Lab 01 SiO2 --- --- --- --- --- % --- --- --- Lab 02 SiO2 --- --- --- --- --- % --- --- --- Lab 03 SiO2 6.108 6.078 5.878 5.915 5.892 % 5.974 -1.712 GRAV Lab 04 SiO2 7.620 7.640 7.500 7.700 7.620 % 7.616 0.501 GRAV Lab 05 SiO2 7.772 7.810 7.769 7.894 7.830 % 7.815 0.769 FUSALK-ICP Lab 06 SiO2 --- --- --- --- --- % --- --- --- Lab 07 SiO2 --- --- --- --- --- % --- --- --- Lab 08 SiO2 4.972 4.801 4.781 4.782 4.840 % 4.835 -3.247 POP-XRF Lab 09 SiO2 -- -- -- -- -- % --- --- --- Lab 10 SiO2 7.630 7.630 7.560 7.520 7.530 % 7.574 0.444 FUSALK-ICP Lab 11 SiO2 9.550 9.460 9.520 9.600 9.590 % 9.544 3.099 FUS-XRF Lab 12 SiO2 --- --- --- --- --- % --- --- --- Lab 13 SiO2 7.289 7.275 7.269 7.198 7.185 % 7.243 -0.002 GRAV

Legend:

FUSALK-ICP Alkaline fusion / Optical Emission Spectromety – ICP-OES

FUS-XRF Fusion / X-Ray Fluorescence

GRAV Gravimetric Method








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Pic. 35: Graph with Z Scores for samples C69 and C70 for SiO2 Analysis.

Laboratory 12 - Assarel Medet JSC has not participated of the PT for the parameter SiO2.

Pic. 36: Youden Plot for SiO2 Analysis.


Laboratory 12 - Assarel Medet JSC has not participated of the PT for the parameter SiO2.




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Pic. 37: Ranking Graph according to the Mandel’s k statistic to sample C69 for SiO2 Analysis.

Pic. 38: Ranking Graph according to the Mandel’s k statistic to sample C70 for SiO2 Analysis.

technical report itak rt-382-2020 pep...rt-382-2020 cgcre’s accredited abnt nbr iso/iec 17043:2011...

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