AMIS0318. Certified Reference Material. Certificate of Analysis

Transcription

1 Tel: +27 (0) , Fax: +27 (0) , web: 11 Gewel Street (off Hulley Road), D1 Isando Business Park, Kempton Park, 1609 P.O. Box 856, Isando, 1600, Gauteng, South Africa, a division of the Set Point Group AMIS0318 Nickel, Copper, PGM Sulphide Ore Nkomati Mine South Africa Certified Reference Material Certificate of Analysis Recommended Concentrations and Limits (at two Standard Deviations) Certified Concentrations Pt Pb Collection 0.17 ± 0.02 g/t Pd Pb Collection 0.30 ± 0.02 g/t Co P 98 ± 7 ppm Cu M/ICP 1566 ± 108 ppm Cu P 1552 ± 81 ppm Cu XRF 1495 ± 168 ppm Ni P 1529 ± 121 ppm Ni XRF 1653 ± 196 ppm Specific Gravity Provisional Concentration Au Pb Collection 0.06 ± 0.01 g/t Co M/ICP 107 ± 14 ppm Co XRF 107 ± 29 ppm Ni M/ICP 1686 ± 216 ppm PGM 3E= 0.53g/t 1. Manufacturers recommended limits for use of the material as control samples, based on two standard deviations, calculated using Between Laboratory statistics for treatment of the data for trivial, non-trivial and technically invalid results. See sections 1, 10and There is additional certified major element data presented on p2 and uncertified trace element data presented as an appendix. Directors: GJ Horsfield (CEO), MD Evers (CFO)(British), A Buddingh, W Erasmus, Gerber, SJ Ingram M McWha, N Robinson, V Singh (Alt), MH Snelling, D Steenkamp (Alt), J Vassiloudis

2 Major Element Recommended Concentrations and Limits (at two Standard Deviations) Certified Concentrations Al 2 O ± 0.12 % CaO 6.63 ± 0.10 % Fe 2 O ± 0.30 % K2O 0.98 ± 0.02 % MgO 9.31 ± 0.20 % MnO 0.16 ± 0.01 % Na 2 O 1.10 ± 0.10 % SiO ± 0.58 % TiO ± 0.02 % S Combustion / LECO 1.51 ± 0.08 % Provisional Concentrations Cr 2 O ± 0.03 % LOI 5.51 ± 0.80 % 1. Intended Use: AMIS0318 is a certified reference material which may be used to demonstrate the validity of measurement results of a single analysis of nickel-copper-pgm sulphide ores hosted by mafic-ultramafic rocks. It is a matrix matched Certified Reference Material, fit for use as control samples in routine assay laboratory quality control when inserted within runs of samples and measured in parallel to the unknown. Its purpose is to monitor inter-laboratory or instrument bias and within lab precision. It can be used, indirectly, to establish the traceability of results to an SI system of units. The recommended concentrations and limits for this material are property values based on a measurement campaign (round robin) and reflect consensus results from the laboratories that participated in the round robin. Slight variations in analytical procedures between laboratories will reflect as slight biases to the recommended concentrations (see 19). Good laboratories will report results within the two standard deviation levels with a failure rate of <10 %. The material can also be used for method development and for the calibration of equipment. 2. Origin of Material: The material for AMIS0318 was provided by the Nkomati Nickel Mine, joint venture between ARM Platinum and Norilsk Nickel Africa (Pty) Ltd. The mine is situated in the Machadodorp area, Mpumalanga, approximately 300 km east of Johannesburg in South Africa. 3. Mineral and Chemical Composition: Mineralisation at Nkomati occurs in a number of distinct zones within the Uitkomst Complex, a layered mafic-ultramafic intrusion exposed in a broad valley dissecting the Transvaal Sequence. Economic sulphide mineralization occurs as disseminations, blebs and stringers in three zones, namely the Basal Mineralised Zone (BMZ), in the Basal Gabbro; the Main Mineralised Zone (MMZ), in the Lower Pyroxenite, and the Chromititic Peridotite Mineralised Zone (PCMZ), in the Chromititic Peridotite. The Massive Sulphide Body 2

3 (MSB), which was situated mainly in the granite basement below the Uitkomst Complex, has been mined out. 4. Appearance: The material is a very fine powder. It is colored amedium light Grey (Corstor 10Y6/2). 5. Handling instructions: The material is packaged in Laboratory Packs and Explorer Packs that must be shaken or otherwise agitated before use. Normal safety precautions for handling fine particulate matter are suggested, such as the use of safety glasses, breathing protection, gloves and a laboratory coat. 6. Method of Preparation: The material was crushed, dry-milled and air-classified to <54um. Wet sieve particle size analysis of random samples confirmed the material was 98.5% <54um. It was then blended in a bi-conical mixer, systematically divided and then sealed into1kg Laboratory Packs. Explorer Packs are subdivided from the Laboratory packs as required. Samples were randomly selected for homogeneity testing and third party analysis. Statistical analysis of both homogeneity and the consensus test results were carried out by independent statisticians. 7. Methods of Analysis requested: 1. Pt, Pd and Au. Pb collection with Ag as a co-collector, ICP-OES or ICP-MS. 2. Multi element scan to include Co, Cu and Ni. Multi-acid total digestion, including HF, ICP- OES or ICP-MS. 3. Co, Cu and Ni. Aqua regia digestion with ICP-OES or ICP-MS. 4. Co, Cu and Ni. Pressed Pellet, XRF. 5. Majors (Al2O3, CaO, Cr2O3, Fe2O3, K2O, MgO, MnO, Na2O, SiO2, TiO2. LOI. ) XRF fusion. 6. SG, gas pycnometer. 8. Information requested: 1. State aliquots used for all determinations. 2. All results for major elements to be reported as oxides in percentages. 3. All results for multi-element scans to be reported in ppm. 4. Report all QC data, to include replicates, blanks and certified reference materials used. 5. State and provide brief description of analytical techniques used. 9. Method of Certification: Twenty Five laboratories were each given eight randomly selected packages of sample. Twenty one of the laboratories submitted results in time for certification. Final limits were calculated after first determining if all data was compatible within a spread normally expected for similar analytical methods done by reputable laboratories. Data from any one laboratory was then removed from further calculations when the mean of all analyses from that laboratory failed a t test of the global means of the other laboratories. The means and standard deviations were then re-calculated using all remaining data. Any analysis that fell outside of the new two standard deviations was removed from the ensuing data base. The mean and standard deviations were again calculated using the remaining data. The between-laboratory standard deviation is used in the calculation to eliminate technically and statistically invalid data. Upper and lower limits are based on the standard deviation of the remaining data, which reflect individual analyses and can be used to monitor accuracy in routine laboratory quality control. This is different to limits based on standard deviations derived from grouped set of analyses (see 12), which provide important measures for precision and trueness, but which are less useful for routine QC. 3

4 Standards with an RSD of near or less than 5 % are termed Certified, RSD s of between near 5 % and 15 % are termed Provisional, and RSD s over 15 % are termed Informational. 10. Participating Laboratories: The 21 out of 25 laboratories that provided results timeously were (not in same order as in the table of assays): 1. ACME Analytical Laboratories Ltd CA 2. Activation Laboratories Pty Ltd (ActLabs) CA 3. ALS Chemex Laboratory Group Brisbane Australia 4. ALS Chemex Laboratory Group Johannesburg SA 5. ALS Chemex Laboratory Group Perth WA 6. ALS Chemex Laboratory Group Vancouver CA 7. ALS OMAC 8. Bureau Veritas (USA) 9. Genalysis Laboratory Services (W Australia P) 10. Intertek Utama Services (Indonesia) 11. Labtium Inc Finland 12. Set Point Laboratories (Isando) SA 13. SGS Australia Pty Ltd (Newburn) WA 14. SGS Geosol Laboratories Ltda (Brazil) 15. SGS Mineral Services Callao (Peru) 16. SGS Mineral Services Lakefield (Canada) 17. SGS South Africa (Pty) Ltd - Booysens JHB 18. SGS Toronto (Canada) 19. SGS Townsville (Australia) 20. SGS Vancouver (Canada) 21. Ultra Trace (Pty) Ltd WA 11. Assay Data: Data as received from the laboratories for the important certified elements listed on p1 are set out below. Assay data: Economic Elements Lab Pt Pd Au Co Co Co Cu Cu Cu Ni Ni Ni Code PbColl PbColl PbColl M/ICP P XRF M/ICP P XRF M/ICP P XRF g/t g/t g/t ppm ppm ppm ppm ppm ppm ppm ppm ppm A A A A A A A A B B B B B B B B C C C C C C C C

5 Assay data (cont): Economic Elements Lab Pt Pd Au Co Co Co Cu Cu Cu Ni Ni Ni Code PbColl PbColl PbColl M/ICP P XRF M/ICP P XRF M/ICP P XRF g/t g/t g/t ppm ppm ppm ppm ppm ppm ppm ppm ppm E E E E E E E E G G G G G G G G H H H H H H H H J J J J J J J J K K K K K K K K L L L L L L L L M M M M M M M M N N N N N N N N O O O O O O O O

6 Assay data (cont): Economic Elements Lab Pt Pd Au Co Co Co Cu Cu Cu Ni Ni Ni Code PbColl PbColl PbColl M/ICP P XRF M/ICP P XRF M/ICP P XRF g/t g/t g/t ppm ppm ppm ppm ppm ppm ppm ppm ppm P P P P P P P P Q Q Q Q Q Q Q Q R R R R R R R R S S S S S S S S T T T T T T T T U U U U U U U U W W W W W W W W X X X X X X X X Y Y Y Y Y Y Y Y

7 Assay data: Major Oxides Lab Al2O3 CaO Cr2O3 Fe2O3 K2O MgO MnO Na2O SiO2 TiO2 LOI S SG Code XRF XRF XRF XRF XRF XRF XRF XRF XRF XRF Comb/LECO pyc % % % % % % % % % % % % A 1.51 A 1.49 A 1.49 A 1.49 A 1.50 A 1.48 A 1.51 A 1.48 B B B B B B B B C C C C C C C C E 1.50 E 1.49 E 1.58 E 1.58 E 1.57 E 1.53 E 1.56 E 1.56 G G G G G G G G H H H H H H H H J J J J J J J J K 1.45 K 1.44 K 1.44 K 1.48 K 1.45 K 1.38 K 1.41 K 1.44 L L L L L L L L M M M M M M M M N N N N N N N N

8 Assay data (cont): Major Oxides Lab Al2O3 CaO Cr2O3 Fe2O3 K2O MgO MnO Na2O SiO2 TiO2 LOI S SG Code XRF XRF XRF XRF XRF XRF XRF XRF XRF XRF Comb/LECO pyc % % % % % % % % % % % % O O O O O O O O P 2.91 P 2.94 P 2.90 P 2.95 P 2.98 P 2.87 P 2.90 P 2.88 Q Q Q Q Q Q Q Q R R R R R R R R S 2.82 S 2.93 S 3.00 S 2.92 S 3.01 S 2.98 S 2.83 S 3.06 T T T T T T T T U 2.98 U 2.89 U 2.93 U 2.95 U 2.95 U 2.98 U 2.97 U 2.97 W W W W W W W W X X X X X X X X Y Y Y Y Y Y Y Y

9 12. Measurement of Uncertainty :(ref Dr Hugh Bartlett, Hugh Bartlett Consulting CC.) The samples used in this certification process have been selected in such a way as to represent the entire batch of material and were taken from the final packaged units; therefore all possible sources of uncertainty (sample uncertainty and measurement uncertainty) are included in the final combined standard uncertainty determination. The uncertainty measurement takes into consideration the between lab and the within lab variances and is calculated from the square roots of the variances of these components using the formula: Combined standard uncertainty=sqrt((between lab.var/no of labs) + ( mean square within lab.var /no of assays)) These uncertainty measurements may be used, by laboratories, as a component for calculating the total uncertainty for method validation according to the relevant ISO guidelines. Analyte Method unit S ' σl ² SW ³ CSU ⁴ Pt PbColl g/t Pd PbColl g/t Au PbColl g/t Co M/ICP ppm Co P ppm Co XRF ppm Cu M/ICP ppm Cu P ppm Cu XRF ppm Ni M/ICP ppm Ni P ppm Ni XRF ppm Al 2 O 3 XRF % CaO XRF % Cr 2 O 3 XRF % Fe 2 O 3 XRF % K 2 O XRF % MgO XRF % MnO XRF % Na 2 O XRF % SiO 2 XRF % TiO 2 XRF % LOI % S Comb/LECO % SG pycnometer S - Std Dev for use on control charts. 2. σ L - Betw Lab Std Dev, for use to calculate a measure of accuracy. 3. S W - Within Lab Stc Dev, for use to calculate a measure of precision. 4. CSU - Combined Standard Uncertainty, a component for use to calculate the total uncertainty in method validation. 13. Certified values: The Certified, Provisional and Indicated values listed on p1 of this certificate fulfill the AMIS statistical criteria regarding agreement for certification and have been independently validated by Dr Barry Smee. 14. Metrological Traceability: The values quoted herein are based on the consensus values derived from statistical analysis of the data from an inter laboratory measurement program. Traceability to SI units is via the standards used by the individual laboratories the majority of which are accredited and who have maintained measurement traceability during the analytical process. 15. Certification: AMIS0318 is a new material. 9

10 16. Period of validity: The certified values are valid for this product, while still sealed in its original packaging, until notification to the contrary. The stability of the material will be subject to continuous testing for the duration of the inventory. Should product stability become an issue, all customers will be notified and notification to that effect will be placed on the website. 17. Minimum sample size: The majority of laboratories reporting used a 0.5g sample size for the ICP and a 30g sample size for the fire assay. These are the recommended minimum sample sizes for the use of this material. 18. Availability: This product is available in Laboratory Packs containing 1kg of material or Explorer Packs containing custom weights (from 50 to 250g) of material. Laboratory Packs are sealed bottles delivered in sealed foil pouches. Explorer Packs contain material in standard geochem envelopes, nitrogen flushed and vacuum sealed in foil pouches. 19. Recommended use: The data used to characterize this CRM has been scrutinized using outlier treatment techniques. This, together with the number of participating laboratories, should overcome any inter-laboratory issues and should lead to a very accurate measure for the given methods; notwithstanding the underlying assumption that what the good inter-laboratory labs reported was accurate. However an amount of bad data might have had an effect, resulting in limits which in some situations might be too broad for the effective monitoring of a single analytical method, laboratory or production process. Users should therefore set their own limits based on their own data quality objectives and control measurements, after determining the performance characteristics of their own particular method, using a minimum of 20 analyses using this CRM. User set limits should normally be within the limits recommended on p1 and 2 of this certificate. 20. Legal Notice: This certificate and the reference material described in it have been prepared with due care and attention. However AMIS, Set Point Technology (Pty) Ltd, Mike McWha, Dr Barry Smee and Smee and Associates Ltd; accept no liability for any decisions or actions taken following the use of the reference material. 22 September 2012 Certifying Officers: African Mineral Standards: Mike McWha BSc (Hons), FGSSA, MAusIMM, Pr.Sci.Nat Geochemist: Barry W. Smee BSc, PhD, P.Geo, (B.C.) 10

11 Appendix uncertified trace element statistics Analyte Method Unit Mean 2SD RSD% n Ag M/ICP ppm Al M/ICP % As M/ICP ppm Ba M/ICP ppm Be M/ICP ppm Bi M/ICP ppm Ca M/ICP % Cd M/ICP ppm Ce M/ICP ppm Cr M/ICP ppm Cs M/ICP ppm Dy M/ICP ppm Eu M/ICP ppm Fe M/ICP % Ga M/ICP ppm Gd M/ICP ppm Ge M/ICP ppm Hf M/ICP ppm Ho M/ICP ppm In M/ICP ppm K M/ICP % La M/ICP ppm Li M/ICP ppm Lu M/ICP ppm Mg M/ICP % Mn M/ICP ppm Mo M/ICP ppm Na M/ICP % Nb M/ICP ppm Nd M/ICP ppm P M/ICP ppm Pb M/ICP ppm Pr M/ICP ppm Rb M/ICP ppm Re M/ICP ppm S M/ICP % Sb M/ICP ppm Sc M/ICP ppm Se M/ICP ppm Sm M/ICP ppm Sn M/ICP ppm Sr M/ICP ppm Ta M/ICP ppm Tb M/ICP ppm Te M/ICP ppm Th M/ICP ppm Ti M/ICP % Tl M/ICP ppm Tm M/ICP ppm U M/ICP ppm V M/ICP ppm W M/ICP ppm Y M/ICP ppm Yb M/ICP ppm Zn M/ICP ppm Zr M/ICP ppm