SARM 69 - Mintek

SARM 69Certificate of Analysispage 1CERAMIC -1 SARM 69CERTIFIED REFERENCE MATERIALPrepared by and Distributed byMINTEKP/Bag X3015 Randburg 2125Republic of South AfricaDistributed byDepartment of GeologyUniversity of the Free StatePO Box 339Bloemfontein93001. STATUS OF CERTIFICATEThis is the first issue of the certificate.2. DATE OF ORIGINAL CERTIFICATIONNovember 20003. AVAILABILITY OF OTHER SIZES OF THE MATERIALOnly 100 g units of the powdered material are available.4. SOURCE OF THE MATERIALThe material was supplied by the Mc Gregor Museum.5. DESCRIPTION OF THE MATERIALClay potsherd material originating from an iron age site situated in the Orange Free State. There arethree mineral phases present, i.e. quartz (SiO 2 ), feldspar (CaAl 2 Si2O 8 ) and muscovite(KAl 2 (Si 3 Al)O 10 (OH).6. INTENDED USEAs a control sample in the analysis of samples of a similar type.Verification of analytical methods for ceramics.As a reference material for the calibration of equipment used for analysing similar materials.7. STABILITY, TRANSPORTATION AND STORAGE INSTRUCTIONSCare must be taken to avoid undue vibration, since this could cause segregation within the container.8. INSTRUCTIONS FOR THE CORRECT USE OF THE MATERIALThe material should be well mixed and dried at 110°C for over night (see label) before sub-samples aretaken. Sub-samples of 0,2 g mass were taken for homogeneity testing, therefore homogeneity cannot beguaranteed on smaller sub-samples.1

SARM 69page 29. METHOD OF PREPARATION OF THE REFERENCE MATERIALApproximately 80 kg of material was reduced in particle size until 95,7% was less than 83,4 µm.For full details of the comminution procedure see 17.10. STATE OF HOMOGENEITYThe material has been shown to be of sufficient homogeneity for its purpose (see 6). See 17 for a fulldescription of the tests carried out as a check on the homogeneity of the material.11. CERTIFIED PROPERTY VALUES AND CONFIDENCE LIMITSSARM 6995 % Confidence LimitsConstituentCertifiedvalue %LowHighSiO 2 66,6 66,1 67,1Al 2 O 3 14,4 14,2 14,5Total Fe as Fe 2 O 3 7,18 7,10 7,25CaO 2,37 2,33 2,41K 2 O 1,96 1,92 2,00MgO 1,85 1,83 1,88MnO 0,129 0,127 0,132TiO 2 0,777 0,769 0,785Certifiedvalue mg/kgBa 518 499 537Cr 223 215 230Zn 68 65 70Ni 53 51 54Cu 46 43 48Co 28 27 29Sc 20 19 21NOTES:1. All values (including uncertified values) relate to the dried (110°) material.2. The Certified Value is an estimate of the " true " value based upon the best available data at thetime of the certification.3. The 95% Confidence Interval for the Certified Value is the range of values having a 95% chanceof containing the certified value, should the certification program be repeated an infinite number oftimes.4. The precision of the user's proposed analytical method must be taken into account when using thisreference material.2

SARM 69page 312. TENTATIVE / PROVISIONAL PROPERTY VALUESDeterminant Tentative value %Loss on Ignition 3,6Na 2 O 0,79P 2 O 5 0,28Tentative value mg/kgZr 271Total V 157Sr 109Ce 67Rb 66Nd 30Y 29Pb 14Nb 9Th 913. VALUES OBTAINED BY INDIVIDUAL LABORATORIESNineteen laboratories in nine countries submitted analytical results on this material. See 17 for all theresults.14. MEASUREMENT TECHNIQUES USED FOR THE CERTIFICATIONAmong the techniques used by the contributing laboratories were the following:Atomic absorption spectrophotometryGravimetric analysisICP Mass spectrometryNeutron activation analysisOptical emission spectroscopy with ICP sourceVolumetric analysisX-ray fluorescence spectrometrySample dissolution was mainly by acid digestion or fusion.3

SARM 69page 4For further details of the techniques see 1715. TREATMENT OF THE NUMERICAL VALUESStatistical tests were used to identify outlying results which were then removed from the main population ofresults. Estimators of central tendency were then calculated and the most appropriate were assigned as thecertified value. For full details of the statistical treatment of the analytical data see 17.16. COLLABORATING LABORATORIESAustraliaAmdel Laboratories Limited……………………………..TorrensvilleGeneral Laboratories services Pty Ltd………………… GosnellsCANADASlow Poke Reactor Facility ……………………………..TorontoCzech RepublicGeological Survey Prague ……………………………...BarrandovFranceBureau de Recherches Geologiques & Minieres …….OrleansGermanyFreie University of Berlin ………………………………...BerlinGMBH ……………………………………………….…… Hohr - GrenzhausenUnited KingdomAlfred H Knight ………………………………………….. MersysideThe Open University ……………………………………...Milton KeynesUnited States of AmericaUniversity of Missouri …………………….……………....MissouriSouth AfricaCouncil for Geoscience ……………………………………PretoriaUniversity of Cape Town Geol. Sciences………………..Cape TownUniversity of Natal ………………………………………….NatalUnivesity of OFS Dept Geology …………………………. BloemfonteinMintek………………………………………………..………RandburgSetpoint (B&B Laboratories) ………………………………Bedfordview4

SARM 69page 517. REFERENCESMarsland S.A., Hansen R, Oosthuyzen J THE PREPARATION AND CERTIFICATION OF A CLAYCERTIFIED REFERENCE MATERIAL. Randburg, 2001.This report is available from MINTEK, Private Bag X3015, Randburg 2125, Republic of South Africa.18. NAME OF CERTIFYING OFFICERDr D Groot, Manager, Analytical Science Division, MINTEK.5