Assaying and Analysis Choices in Practice
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1 Assaying and Analysis Choices in Practice Au assays at the GDL laboratories Dirk Hofmans Umicore UPMR Hoboken, Belgium March 2015 Agenda LBMA Good delivery rules for laboratories How to assay > 995 Gold? according to ASTM & ISO Fire assay vs instrumental Proficiency testing: extra information Conclusions 1
2 LBMA Good delivery rules for laboratories Every 3 years the GD Laboratories are audited for assaying fine gold. The lab receives 6 samples for the examination of its assaying capability. Au in range to Rod shaped samples LBMA referees normally use gravimetry or spectrometry for > Method selection is left open, but has to be reported with the results. LBMA criteria are very stringent: Au > should agree to +/ e.g certified Au should fall between & Au to should agree to +/ e.g certified Au should fall between to e.g. of an 0.05 error: 0.5 meter error on the height of Mt Everest. How assay Gold? 3 ASTM procedures: ASTM B (original 1972, reapproved 2005) Standard specifications for refined Gold Covers to Refers to ASTM E for chemical composition (concentrations of impurities) Adds classic fire assay cupellation method with gravimetry as appendix ASTM E (original 1992, reapproved 2013) Standard test method for chemical analysis of refined gold by direct current plasma atomic Emission spectrometry Instrumental method, but DCP no longer commercially available Recites only a limited number of elements (Cu, Fe, Pb, Pd, Ag) No instructions for other impurities, what to do with detection limits, no description how the DL is defined, ASTM E (original 1990, reapproved 2008) Standard test methods for determination of gold in bullion by fire assay cupellation analysis For Au in concentration range to Classic fire assay method with gravimetry 2
3 How assay Gold? 2 ISO procedures: ISO (2014) Jewellery determination of gold in gold jewellery alloys cupellation method (fire assay) Refers to ISO 9202 (Specifies a range of fineness of gold alloys (375, 585, 750, 916)) Is also applicable for > Au material ISO (2015) Jewellery determination of precious metals in 999 gold, platinum and palladium jewellery alloys Difference method using ICP-OES Covers > Au material Instrumental method by ICP OES (optical emission) Prescribes a 10g Au / l solution by using 500 mg per assay Impurities are determined and subtracted from 1000 Only impurities are counted when the concentration found is above detection limit A normative list of elements and wavelengths is given. With the remark These tables are not exhaustive. If other elements are present, they shall be analysed How assay Gold? Principle of fire assay cupellation method with Gravimetry: weigh Au sample with addition of Ag, Cu, Pb. Cupel, remove Ag with HNO 3. Dry, anneal gold and weigh. Gravimetry + - direct method extremely high precision required internationally accepted need for very experienced chemists fire assay equipment required expensive precision balances matrix interference lead time ASTM B (2005) ASTM E Standard specifications Fine Au Det of Au in bullion by FA maximum % allowed maximum % allowed 0.01% Pt Pd 0.01% Rh 0.01% 0.01% Ir 0.01% Ru 0.01% Os 0.01% Zn 5.00% Ni 2.00% 2.00% Fe 2.00% 2.00% Sn 2.00% W 0.50% 0.50% As 2.00% Sb 2.00% Bi 2.00% Se 2.00% Te 2.00% 3
4 How assay Gold? Principle of instrumental method with ICP: Weigh and dissolve the samples in Aqua Regia. Condition in e.g. 30% vol HCl solution. Impurities in solution are determined by ICP and the Au content is obtained by subtraction of the total content of impurities from ICP-OES + - Less precision required for the analyte No defined list of elements tbd Lead time No clear definition of detection limits Chemist skills All impurities have to dissolve Detection limits count for zero ICP instrument is required Less precision required for the analysis of the impurities as for the direct Au method: LBMA requirements for Good Delivery Labs: Au > should agree to +/ e.g = 0.16 impurities on 0.16 = 31% relative error on sum impurities Au to should agree to +/ e.g = 3.27 impurities on 3.27 = 5% relative error on sum impurities allowed. e.g = 5.00 impurities on 5.00 = 3% relative error on sum impurities allowed. Proficiency testing: extra information PT is performed by the GD Laboratories since 2012 (L0101 to L0104) PT benchmarks the labs performance against other GD labs Info Detail sample ID L0103 L0102 L0104 # participants # results Material impurities present Ag, Pt, Pd, Cu, Zn, Fe Ag, Pt, Pd, Cu Ag, Pt, Pd, Cu, Zn, Fe Statistical data assigned value xa from PT std dev σp for proficiency # scores z % scores z 2 88% 95% 94% # outliers Grubbs test * % outliers Grubbs test 0% 2.5% 14% # outliers Cochran test ** % outliers Cochran test 12.5% 5.0% 6.1% Technique applied # results by fire assay % results by fire assay 71% 73% 53% average by fire assay % st dev on fire assay results Remark # results by ICP % results by ICP 29% 25% 43% average by ICP st dev on ICP results All Cochran outliers on fire assay results All Cochran outliers on fire assay results All Cochran outliers and 6 o 7 Grubbs outliers on fire assay results * Grubbs test = compares simple mean of replicates to simple mean of all results ** Cochran test = check on the variances of the results 4
5 Feedback on the PT methodology remained limited: Only indication of the technique applied: gravimetry or ICP No detailed information for the ICP technique about What elements were determined What is done with detection limits No information if the method applied on the PT sample is the same as the in house method for routine samples in the GD laboratory. Questionnaire to evaluate What criteria are applied to select a method in a GD lab Is there a difference in the methods applied between the routine method and the one applied on the PT / GD samples? If a method by difference (e.g. ICP) is applied what elements are determined What is done with detection limits How not determined elements are accounted for We received feedback from 25 GD Laboratories ( 50%!) All feedback was anonymized by the LBMA What criteria are applied to select a method in a GD lab lab LG HG switch method grav ICP * grav ICP * permille 1 x x x x 3 x x x x x 5 x x 6 x x 7 x x x x 9 x x x x 10 x x x x 12 x x 13 x x x x 15 x x 16 x x x x x x 18 x x 19 x x x x 21 x x 22 x x 23 x x 24 x x 25 x x total of the 25 labs use a method by ICP (*) for all Au in the range (yellow). 5 labs use gravimetry only on 250mg to 500mg per replicate (blue) (*) 2 labs use gravimetry and ICP or equivalent over the whole concentration range (green). 7 labs switch from gravimetry to ICP for High Grade Au. The concentration where they change method is different (pink). 1 lab uses gravimetry over the whole range, but uses ICP in addition for the high grade material (brown). (*) 1 lab uses no ICP-OES but a combination of ICP-MS, Arc-OES and Flame AAS to determine the impurities in Au. 1 lab uses WD-XRF and Arc-OES as pre-assay, but reports by gravimetry 5
6 Is there a difference in the methods applied between the routine method and the one applied on the PT / GD samples? 4 of the 25 labs declare that their normal production quality is > Au their routine procedure for assaying production Au is Spark Source OES. SS-OES is a technique more performant for high grade Au quality SS-OES is not possible on the PT and GD samples, as the shape of the material is not suited. If a method by difference (e.g. ICP) is applied, what elements are determined Overview of the elements done for the High Grade Au material Elements suggested by the ISO method or LBMA list (GD Rules). Elements present in AuRM1 and AuRM2 (red). el # labs labs % ISO LBMA GDR LBMA GDR additional elements Ag x x Pd x x Pt x x Cu x x Zn x x Bi x x Cr x Fe x x Mg x Mn x x Pb x x Sn x x Cd x x Ni x x Sb x Si x Al x Ca x Co x x Rh x x As x In x Ir x x Se x Ti x x el # labs labs % ISO LBMA GDR LBMA GDR additional elements Be x Te x Ga x Ru x x Zr x Mo x Na x K x B 9 45 x Ge 9 45 x Li 9 45 x Os 9 45 x P 9 45 x Tl 9 45 x W 9 45 x Hg 7 35 x V 7 35 x Ba 5 25 Sr 4 20 Ta 4 20 Re is determined by 3 labs Ce, Hf, Nb by 2 labs Dy, Er, Gd, Ho, La, Lu, Pr, S, Sm, Tb, Th, Tm, U, Y, Yb by 1 lab 6
7 What is done with detection limits, how not-determined elements are accounted for? Only ISO (2015) gives a description how to deal with detection limits: Only impurities are counted when the concentration found is above detection limit for ICP-OES, one has to measure a 10 g Au / l solution However, the detection limit DL for the impurities in the Au is a function of Instrument selection and performance Instrument specific (Perkin Elmer, Spectro, Thermo Fisher, Agilent, ) Technique dependent (ICP-OES, ICP-MS, SS-OES, Arc-OES, FAAS ) Wavelength / mass of measurement Dilution factor The definition of the Detection Limit itself! What is done with detection limits, how not-determined elements are accounted for? Feedback from the Questionnaire: Each lab using a method by difference determines between 5 and 59 elements Mean value of elements checked is labs report that their detection limits is typical 1 or 2 ppm (0.001 or ) Although ISO describes that values below DL can be neglected, this is not what all labs do: 15 labs take < DL as 0 and take only the observed impurities above DL, in line with ISO lab sums the DL and adds this value to the observed impurities above DL 1 lab sums half of the DL and adds this value to the observed impurities above DL 1 lab sums the DL, takes the square root of this value, and adds this value to the observed impurities above DL 1 lab takes a default value as a safety margin and adds this value to the observed impurities above DL 7
8 Conclusions & Need for improved instructions? Both gravimetry and ICP are able to assay Au > 995 Precision of ICP is equivalent to classic fire assay + gravimetry at 995 level and is better than gravimetry at increasing purity of Au. There is a tendency at the Good Delivery Labs to move from gravimetry to ICP for the GD audit and PT, certainly for the high grade Au level. ICP gives additional info: impurities are identified and quantified However Present ISO and ASTM standards are not stringent enough about essential ICP parameters: A clear definition of detection limit is required and is to be used by all labs A minimum detection limit per element has to be defined A procedure to handle impurities below DL has to be defined (ISO OK?) A minimum list of impurities to be determined has to be defined Food for thought: One lab suggested to make 2 PT samples each year: one lower grade, one high grade As 4 labs use Spark OES, is it possible to produce samples of a suited shape? 15 Thank you & questions? Special thanks to all labs completing the questionnaire Special thanks to Varsha Peiris for the administrative support 8
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