Tel: +2711 923 7000 Fax: +2711 923 7027 e-mail: [email protected] web: www.amis.co.za A division of the Set Point Group, 30 Electron Avenue, Isando, 1600. P.O. Box 856, Isando, 1600, South Africa. AMIS0156 Certified Reference Material Uraniferous Alaskite Ore, Rössing Uranium Mine, Namibia Certificate of Analysis Recommended Concentrations and Limits1. (at two Standard Deviations) Certified Concentrations2. U XRF (or U3O8 XRF) Ca M/ICP ppm Specific Gravity 210 248 2.42 2.69 ± ± ± ± 23 27 0.21 0.18 ppm ppm % Provisional Concentrations U M/ICP (or U3O8 M/ICP) Nb M/ICP Ta M/ICP 195 230 17.50 2.14 ± ± ± ± 34 40 2.80 0.30 ppm ppm ppm ppm 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, 9 and 12. 2. 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), SJ Ingram, MC Louw, K Gerber, N Robinson, MJ Smith, MH Snelling, J Vassiloudis, D Williams Major Element Recommended Concentrations and Limits (at two Standard Deviations) Certified Concentrations Al2O3 CaO Fe2O3 K2O MgO MnO Na2O P2O5 SiO2 TiO2 12.82 3.45 3.01 4.46 1.92 0.06 3.44 0.14 68.47 0.30 ± ± ± ± ± ± ± ± ± ± 0.20 0.10 0.08 0.12 0.06 0.01 0.12 0.01 0.60 0.01 % % % % % % % % % % Provisional Concentrations Cr2O3 LOI 0.064 1.77 ± ± 0.010 0.46 % % 1. Intended Use: AMIS0156 can be used to check analysis of samples of uraniferous alaskite ores with a similar grade and matrix. 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: AMIS0156 was supplied by Rio Tinto Limited from the Rössing Uranium Mine situated 70km north-east of Swakopmund in Namibia. The uranium mineralisation is associated with Neoproterozoic Damara Orogen syntactic alaskitic granites that display concordant, discordant and replacement relationships to the heavily folded host gniesses, marbles and limestones of the Khan and Rössing Formations. 3. Mineral and Chemical Composition: The uranium bearing minerals are mainly uraninite and its alteration products, and minor betafite. 4. Appearance: The material is a very fine Light Grey powder (Corstor colour chart – 5Y 7/1). 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. 2 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 into 1kg 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 consensus test results were carried out by an independent statistician. 7. Methods of Analysis requested: 1. Multi-acid digest, including HF, ICP- OES or ICP-MS. Multi element scan to include U, Ca, Ta, Nb. 2. U, Ca, Ta, Nb. XRF. 3. Majors ( Al2O3, CaO, Cr2O3, Fe2O3, K2O, MgO, MnO, Na2O, SiO2, TiO2. LOI. ) XRF fusion. 4. SG ( gas pycnometer ). 8. Information requested: 1. 2. 3. 4. 5. 6. State and provide brief description of analytical techniques used. State aliquots used for all determinations. Results for individual analyses to be reported ( not averages ) All results for multi-element scans to be reported in ppm. All results for major elements to be reported in %. Report all QC data, to include replicates, blanks and certified reference materials used. 9. Method of Certification: Twenty one laboratories were each given eight packages, comprising eight samples scientifically selected from throughout the batch. Nineteen laboratories reported results in time for certification of the economic elements. Eight of these laboratories reported results for the major elements. 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 them 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. 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: (Not in same order as in the table of assays): 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. Activation Laboratories Pty Ltd (ActLabs) CA ALS Chemex Laboratory Group Brisbane Australia ALS Chemex Laboratory Group Johannesburg SA ALS Chemex Laboratory Group Lima (Peru) ALS Chemex Laboratory Group Perth WA ALS Chemex Laboratory Group Vancouver CA Anglo Gold Ashanti - Vaal River Laboratory SA Anglo Research (Crown Campus) Genalysis Laboratory Services (South Africa) Pty Genalysis Laboratory Services WA Performance Labs (Welkom) Reptile Uranium Namibia Rossing Uranium Limited Set Point Laboratories (Isando) SA 3 15. 16. 17. 18. 19. SGS Australia Pty Ltd (Newburn) WA SGS Geosol Laboratories Ltda (Brazil) SGS Mineral Services Lakefield (Canada) SGS South Africa (Pty) Ltd - Booysens Ultra Trace (Pty) Ltd WA 11. Assay Data: Data as received from the laboratories for the important certified elements listed on p1 is set out below. A proficiency report has been sent to the managers of the participating laboratories. Additional digital data from this round robin is available on request. Lab Code A A A A A A A A B B B B B B B B C C C C C C C C D D D D D D D D E E E E E E E E F F F F F F F F G G G G G G G G H H H H H H H H I I I I I I I I J J J J J J J J K K K K K K K K U M/ICP ppm 209 207 207 208 205 211 202 208 170 168 172 175 169 172 169 179 194 191 192 187 187 180 189 191 192 180 183 185 183 184 185 186 179 185 180 185 179 187 189 183 185 174 171 164 174 179 159 164 201 199 202 201 199 209 197 210 225 221 218 221 216 221 227 219 211 197 194 202 190 192 197 193 U XRF ppm 221 217 211 215 225 226 219 211 275 261 246 265 252 266 248 240 226 225 222 224 226 220 221 220 209 210 212 210 213 209 211 210 210 200 210 200 210 200 210 200 200 200 190 200 190 200 190 200 200 200 200 200 200 200 200 200 220 240 230 230 240 220 230 230 Ca M/ICP ppm 23100 23300 24000 24700 24800 24300 23500 23700 22719 22274 22845 23057 21873 23128 23089 23907 21600 23500 22600 21700 23800 21100 24000 21500 23700 23800 23200 23600 22900 22600 23400 23400 25100 26100 23800 24000 23600 23800 24100 23900 24500 23900 23300 24200 23300 23800 24000 23600 25500 25300 25300 24300 24200 24500 23900 24700 22900 22700 22600 22400 22800 24100 23000 23600 27500 27600 26300 27600 26200 26300 27100 26300 24900 24900 24900 24700 24900 25100 25000 24900 Nb M/ICP ppm 20.10 19.90 19.90 20.00 20.20 20.10 19.70 20.00 12.50 11.70 12.20 11.80 13.00 13.20 13.30 13.50 18.30 18.30 18.30 18.50 18.30 17.90 18.10 18.70 19.10 18.50 17.80 19.20 18.60 18.90 18.30 18.40 18.50 18.20 17.60 17.80 17.90 17.90 18.50 18.00 17.90 17.60 17.50 16.50 17.00 17.30 17.40 16.40 17.40 17.00 17.30 17.00 17.00 18.40 17.00 17.70 15.70 17.10 18.50 17.00 16.40 17.20 15.10 15.40 25.00 25.00 20.00 25.00 25.00 25.00 25.00 25.00 Ta M/ICP ppm 2.68 2.46 2.35 2.30 2.31 2.46 2.31 2.44 2.12 2.04 2.02 2.08 1.97 1.96 1.98 2.08 2.42 2.31 2.20 2.37 2.33 2.33 2.32 2.30 2.04 2.03 1.95 1.98 1.96 1.96 2.05 1.99 2.16 2.23 2.23 2.10 2.14 2.13 2.24 2.11 2.09 2.07 2.06 2.03 2.00 2.21 2.05 2.15 1.60 1.60 1.60 1.50 1.40 1.30 1.20 1.30 1.60 1.60 1.70 1.60 1.40 1.50 1.60 1.50 Al2O3 XRF % 12.80 12.80 12.80 12.90 12.80 12.70 12.80 12.80 12.42 12.40 12.23 12.14 12.35 12.31 12.10 12.11 12.90 12.90 12.90 12.90 12.80 12.80 13.00 13.00 12.80 12.80 12.80 13.00 12.70 12.80 12.70 12.90 12.70 12.70 12.65 12.75 12.70 12.70 12.65 12.65 12.70 12.75 12.70 12.75 12.70 12.70 12.65 12.75 13.06 13.03 13.01 13.08 13.08 13.07 13.10 13.03 12.75 12.70 12.65 12.65 12.75 12.75 12.70 12.80 CaO XRF % 3.43 3.42 3.43 3.41 3.42 3.44 3.44 3.45 3.35 3.37 3.37 3.37 3.39 3.37 3.41 3.37 3.50 3.52 3.49 3.53 3.45 3.52 3.50 3.52 3.41 3.42 3.43 3.44 3.40 3.41 3.40 3.44 3.43 3.42 3.43 3.45 3.44 3.44 3.43 3.43 3.50 3.51 3.50 3.50 3.49 3.50 3.47 3.51 3.42 3.41 3.43 3.45 3.44 3.45 3.44 3.45 3.43 3.41 3.42 3.40 3.42 3.44 3.43 3.46 Cr2O3 XRF % 0.07 0.06 0.07 0.07 0.07 0.07 0.07 0.06 0.07 0.07 0.07 0.07 0.06 0.07 0.06 0.07 0.06 0.07 0.07 0.07 0.07 0.07 0.07 0.07 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.07 0.07 0.07 0.07 0.07 0.07 0.07 0.07 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.05 0.04 0.05 0.04 0.05 0.05 0.05 0.05 0.06 0.06 0.06 0.06 0.06 0.07 0.07 0.06 Fe2O3 XRF % 3.06 3.07 3.06 3.07 3.06 3.05 3.07 3.07 3.15 3.14 3.18 3.15 3.14 3.18 3.16 3.17 3.04 2.91 3.05 3.06 3.03 3.13 3.06 3.08 2.99 2.95 2.95 3.06 2.90 3.05 3.06 3.16 3.01 3.00 3.00 3.01 2.99 3.00 3.00 2.99 2.99 2.98 2.94 2.99 2.94 2.96 3.01 2.95 2.99 3.01 2.98 3.01 3.00 3.01 3.01 3.00 3.02 3.00 2.99 2.98 3.00 3.01 3.01 3.04 K2O XRF % 4.47 4.47 4.47 4.48 4.48 4.47 4.49 4.49 4.48 4.51 4.52 4.47 4.50 4.50 4.52 4.51 4.43 4.43 4.43 4.47 4.44 4.44 4.50 4.49 4.37 4.37 4.40 4.42 4.37 4.40 4.40 4.42 4.41 4.43 4.43 4.46 4.43 4.47 4.46 4.47 4.45 4.46 4.45 4.46 4.45 4.45 4.48 4.45 4.33 4.31 4.32 4.35 4.34 4.35 4.35 4.36 4.35 4.32 4.34 4.32 4.35 4.34 4.33 4.37 MgO XRF % 1.91 1.90 1.91 1.90 1.91 1.90 1.91 1.92 1.91 1.88 1.87 1.85 1.90 1.88 1.92 1.89 1.93 1.93 1.93 1.94 1.93 1.92 1.95 1.95 1.86 1.85 1.84 1.90 1.83 1.91 1.86 1.88 1.91 1.93 1.94 1.92 1.91 1.95 1.90 1.88 1.96 1.96 1.96 1.96 1.96 1.96 1.98 1.96 1.93 1.91 1.92 1.93 1.92 1.91 1.91 1.92 1.90 1.88 1.88 1.88 1.88 1.90 1.90 1.90 MnO XRF % 0.06 0.06 0.06 0.07 0.06 0.06 0.06 0.06 0.07 0.06 0.07 0.07 0.07 0.07 0.07 0.07 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.07 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.07 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 Na2O XRF % 3.54 3.51 3.50 3.52 3.54 3.51 3.55 3.52 3.34 3.36 3.35 3.39 3.36 3.32 3.34 3.40 3.50 3.52 3.49 3.53 3.51 3.49 3.53 3.55 3.63 3.61 3.58 3.64 3.55 3.71 3.61 3.67 3.26 3.27 3.27 3.26 3.26 3.27 3.44 3.27 3.42 3.42 3.43 3.42 3.43 3.43 3.43 3.42 3.43 3.39 3.42 3.40 3.42 3.43 3.43 3.44 12.81 12.79 12.86 12.85 12.85 12.90 12.91 12.81 12.80 12.87 12.86 12.83 12.89 12.84 12.86 12.86 3.38 3.39 3.41 3.40 3.41 3.39 3.38 3.40 3.47 3.48 3.49 3.48 3.49 3.47 3.48 3.49 0.06 0.07 0.06 0.06 0.06 0.06 0.06 0.06 0.07 0.07 0.07 0.07 0.07 0.07 0.07 0.07 3.04 3.05 3.06 3.06 3.06 3.06 3.06 3.05 3.03 3.05 3.05 3.04 3.05 3.03 3.04 3.05 4.49 4.47 4.47 4.47 4.47 4.50 4.48 4.48 4.48 4.50 4.50 4.50 4.50 4.49 4.49 4.51 1.93 1.93 1.95 1.92 1.96 1.94 1.96 1.95 1.98 1.99 1.99 1.98 1.98 1.99 1.99 1.99 0.06 0.07 0.07 0.07 0.06 0.07 0.06 0.07 0.06 0.07 0.06 0.06 0.07 0.06 0.06 0.06 3.46 3.44 3.44 3.43 3.48 3.46 3.44 3.45 3.45 3.46 3.47 3.46 3.47 3.44 3.46 3.46 4 P2O5 XRF % 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 SiO2 XRF % 68.6 68.6 68.6 68.6 68.6 68.7 68.6 68.6 69.0 69.0 69.5 69.4 68.9 69.4 69.7 69.6 68.4 68.4 68.1 68.5 67.3 68.5 68.4 68.7 68.5 68.2 68.6 68.9 68.1 68.3 68.2 68.4 68.1 68.1 68.1 68.3 68.1 68.2 68.0 68.0 68.8 68.9 69.0 69.0 68.9 68.9 68.7 68.9 68.0 68.2 68.1 68.2 68.0 68.2 68.2 68.0 69.3 68.7 68.9 68.6 69.2 69.1 68.8 69.5 TiO2 XRF % 0.31 0.30 0.30 0.30 0.30 0.30 0.30 0.30 0.31 0.30 0.31 0.30 0.31 0.32 0.29 0.31 0.30 0.31 0.31 0.31 0.30 0.31 0.30 0.30 0.31 0.31 0.31 0.31 0.30 0.34 0.31 0.30 0.30 0.30 0.30 0.30 0.30 0.30 0.30 0.30 0.30 0.29 0.30 0.31 0.31 0.30 0.31 0.29 0.31 0.30 0.30 0.30 0.30 0.31 0.30 0.30 0.30 0.30 0.30 0.30 0.30 0.30 0.30 0.30 1.31 1.16 1.18 0.96 1.31 1.19 1.20 1.18 1.98 1.99 2.04 2.02 1.96 2.00 2.02 2.13 1.53 1.60 1.62 1.55 1.54 1.58 1.42 1.63 0.14 0.15 0.14 0.15 0.15 0.14 0.14 0.14 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15 67.2 67.2 67.6 67.2 67.5 67.6 67.7 67.4 68.5 68.6 68.7 68.6 68.6 68.5 68.6 68.7 0.30 0.30 0.30 0.30 0.31 0.30 0.30 0.30 0.31 0.31 0.31 0.31 0.31 0.31 0.31 0.31 1.96 1.95 1.97 1.97 2.06 2.00 1.98 2.02 1.42 1.44 1.44 1.43 1.44 1.45 1.41 1.41 0.14 0.14 0.14 0.14 0.15 0.15 0.15 0.14 0.14 0.15 0.14 0.15 0.14 0.13 0.14 0.15 LOI % 1.55 1.52 1.52 1.56 1.59 1.50 1.46 1.50 1.67 1.63 1.68 1.68 1.69 1.69 1.76 1.72 2.00 1.98 2.00 1.95 2.01 1.98 1.98 2.15 2.01 2.02 2.07 2.07 2.03 2.05 1.93 2.01 SG Pyc 2.54 2.45 2.56 2.42 2.57 2.61 2.58 2.43 2.70 2.68 2.71 2.68 2.69 2.70 2.71 2.69 2.70 2.69 2.71 2.71 2.71 2.68 2.70 2.70 2.53 2.56 2.50 2.57 2.55 2.55 2.54 2.58 2.81 2.74 2.82 2.81 2.81 2.65 2.84 2.65 2.60 2.56 2.52 2.53 2.53 2.52 2.53 2.55 2.78 2.78 2.74 2.81 2.86 2.79 2.86 2.85 2.66 2.66 2.66 2.70 2.73 2.71 2.70 2.70 2.71 2.71 2.71 2.71 2.74 2.74 2.74 2.73 Assay data (cont) Lab Code 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 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 M/ICP ppm U XRF ppm Ca M/ICP ppm Nb M/ICP ppm Ta M/ICP ppm Al2O3 XRF % 12.80 12.80 12.80 12.80 12.90 12.90 12.90 12.90 CaO XRF % 3.52 3.53 3.51 3.51 3.55 3.54 3.51 3.53 Cr2O3 XRF % Fe2O3 XRF % 3.03 3.01 3.02 3.02 3.03 3.04 3.02 3.03 K2O XRF % 4.47 4.48 4.48 4.48 4.49 4.51 4.47 4.49 MgO XRF % 1.91 1.92 1.90 1.94 1.93 1.95 1.91 1.93 MnO XRF % 0.07 0.07 0.07 0.07 0.07 0.07 0.07 0.07 Na2O XRF % 3.34 3.34 3.33 3.33 3.36 3.36 3.32 3.34 P2O5 XRF % 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15 SiO2 XRF % 68.4 68.3 68.2 68.3 68.7 68.7 68.1 68.6 TiO2 XRF % 0.31 0.31 0.30 0.30 0.30 0.31 0.31 0.30 % 1.23 1.23 1.26 1.23 1.22 1.22 1.22 1.27 182 203 212 187 203 215 187 176 238 229 231 230 233 233 216 230 205 205 205 203 206 206 206 205 25467 25556 25449 25665 25831 26365 25498 25419 15.35 15.09 15.20 15.24 15.74 15.55 15.44 15.64 2.09 1.99 2.01 2.01 2.03 2.00 1.98 2.02 12.75 12.77 12.75 12.84 12.80 12.73 12.83 12.83 3.50 3.50 3.49 3.49 3.48 3.48 3.50 3.48 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 2.98 2.97 2.99 2.99 2.98 3.00 2.98 2.98 4.53 4.51 4.54 4.53 4.55 4.54 4.53 4.53 1.93 1.90 1.90 1.92 1.91 1.93 1.89 1.89 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 3.47 3.43 3.47 3.45 3.44 3.44 3.45 3.40 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 68.2 68.2 68.4 68.5 68.5 68.3 68.4 68.5 0.32 0.31 0.31 0.31 0.31 0.31 0.31 0.31 1.57 1.57 1.55 1.57 1.56 1.56 1.56 1.55 220 220 221 219 219 222 217 225 209 213 210 215 214 217 212 211 192 186 187 184 200 186 193 177 196 203 202 201 200 203 203 200 217 218 218 216 213 213 216 218 2.16 2.02 2.16 2.02 2.02 2.16 2.02 2.16 12.88 12.90 12.90 13.03 12.96 12.91 13.02 12.42 1.89 1.75 1.75 1.75 1.75 1.75 1.89 1.89 3.50 3.48 3.48 3.48 3.52 3.45 3.51 3.52 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 2.29 2.16 2.16 2.16 2.16 2.29 2.29 2.29 2.91 2.93 2.89 2.91 2.92 2.92 2.92 2.93 1.21 1.21 1.21 1.21 1.21 1.21 1.21 1.21 4.23 4.23 4.23 4.23 4.21 4.21 4.22 4.22 0.94 0.94 0.94 0.94 0.94 0.94 1.08 0.94 1.49 1.49 1.50 1.49 1.51 1.47 1.51 1.53 0.05 0.06 0.05 0.06 0.06 0.06 0.06 0.08 0.94 0.67 0.81 0.67 0.81 0.81 1.08 0.81 3.46 3.47 3.51 3.50 3.46 3.40 3.44 3.50 0.15 0.16 0.15 0.15 0.15 0.15 0.15 0.11 68.2 68.9 68.9 68.0 68.8 68.9 68.3 68.8 0.29 0.29 0.30 0.30 0.31 0.31 0.31 0.31 1.90 1.89 1.89 1.88 1.88 1.88 1.92 1.91 26100 26200 26026 25710 25159 24900 24857 25739 16.67 15.83 16.57 16.75 17.22 15.67 16.01 16.87 LOI SG Pyc 2.69 2.67 2.76 2.75 2.73 2.72 2.69 2.77 2.76 2.80 2.78 2.77 2.77 2.75 2.79 2.70 2.69 2.68 2.69 2.68 2.69 2.69 2.68 12. Measurement of Uncertainty: The samples used in the certification process were 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. 5 Analyte U U Ca Nb Ta SG Al2O3 CaO Fe2O3 K2O MgO MnO Na2O P2O5 SiO2 TiO2 LOI Method M/ICP XRF M/ICP M/ICP M/ICP pyc P M/ICP P M/ICP P M/ICP P M/ICP P M/ICP M/ICP Unit ppm ppm ppm ppm ppm % % % % % % % % % % % S ' 17.1 11.6 1056 1.386 0.151 0.087 0.102 0.046 0.040 0.056 0.033 0.004 0.058 0.005 0.295 0.005 0.232 σ L ² 14.1 8.7 850 1.271 0.158 0.067 0.070 0.035 0.029 0.045 0.024 0.002 0.051 0.003 0.199 0.002 0.214 SW ³ CSU ⁴ 6.1 3.87 530 0.532 0.058 0.032 0.055 0.016 0.019 0.016 0.014 0.002 0.021 0.003 0.186 0.004 0.042 4.30 2.44 275 0.428 0.060 0.020 0.021 0.010 0.009 0.013 0.007 0.001 0.016 0.001 0.063 0.001 0.068 1. 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. Uncertified values: The Certified, Provisional and Informational values listed on p1 and p2 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, who have maintained measurement traceability during the analytical process. 15. Certification: AMIS0156 is a new material. 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 www.amis.co.za 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 and Explorer Packs containing custom weights (from 50g to 250g) of material. The Laboratory Packs are sealed bottles delivered in sealed foil pouches. The Explorer Packs contain material in standard geochem envelopes, 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 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. 6 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. 26 January 2010 Certifying Officers: African Mineral Standards:_______________________________________ Mike McWha BSc (Hons), FGSSA, MAusIMM, Pr.Sci.Nat Geochemist:____________________________________________________ Barry W. Smee BSc, PhD, P.Geo, (B.C.) 7 Appendix 1. – Uncertified trace element statistics Twelve of the laboratories reported multi-element scan data. The iterated data is presented below for informational use. Analyte Ag Al As Ba Be Bi Cd Ce Co Cr Cs Cu Dy Er Eu Fe Ga Gd Ge Hf Ho In K La Li Lu Mg Mn Mo Na Nd Ni P Pb Pr Rb S Sb Sc Se Si Sm Sn Sr Tb Te Th Ti Tl Tm V W Y Yb Zn Zr Method M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP M/ICP Unit ppm % ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm % ppm ppm ppm ppm ppm ppm % ppm ppm ppm % ppm ppm % ppm ppm ppm ppm ppm ppm % ppm ppm ppm % ppm ppm ppm ppm ppm ppm % ppm ppm ppm ppm ppm ppm ppm ppm Mean 0.041 6.67 2.26 226 3.07 0.312 0.200 46.3 89.8 331 4.07 104 6.33 4.44 0.592 2.10 18.3 4.21 0.145 2.01 1.36 0.031 3.47 24.3 26.5 0.735 1.06 462 3.75 2.41 17.4 38.6 633 37.6 5.16 274 0.119 8.55 5.43 1.43 46.6 4.14 5.90 144 0.871 0.200 30.7 0.178 0.935 0.753 45.5 12.3 33.0 4.97 108 53.0 8 2SD 0.026 0.41 0.94 18 0.43 0.034 0.022 2.4 10.2 73 0.35 11 0.43 0.25 0.057 0.21 1.0 0.37 0.063 0.25 0.16 0.008 0.34 2.4 4.4 0.091 0.12 53 0.40 0.26 1.7 3.1 62 6.2 1.06 22 0.011 1.67 1.41 0.93 29.7 0.42 0.48 10 0.101 RSD% 32.0 3.1 20.8 3.9 7.0 5.4 5.5 2.6 5.7 11.0 4.3 5.3 3.4 2.8 4.8 4.9 2.7 4.3 21.7 6.3 5.9 12.0 4.9 4.9 8.2 6.2 5.5 5.7 5.4 5.4 4.8 4.0 4.9 8.2 10.3 4.1 4.8 9.8 13.0 32.5 31.8 5.0 4.1 3.6 5.8 2.7 0.013 0.142 0.084 4.2 2.8 4.1 0.78 7 12.5 4.4 3.6 7.6 5.6 4.6 11.2 6.3 7.8 3.1 11.8 n 28 53 49 93 69 61 53 51 85 78 54 86 23 23 22 95 46 22 39 48 24 50 77 55 68 23 79 93 59 88 23 70 84 79 23 53 72 70 31 48 16 23 58 93 22 8 69 69 64 23 71 61 77 30 86 63
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