Analytical Services Division

Transcription

1 Analytical Services Division SCHEDULE OF SERVICES

2 Mintek s Analytical Services Division (ASD) is a wellestablished analytical chemistry laboratory that specialises in geochemical and general analytical chemistry. We provide analytical support to clients in the mineral, metallurgical and related industries, using state-of-the-art instrumentation for a variety of techniques. Our highly skilled scientists and analysts are backed-up by a top-quality consulting team, all operating according to ISO standards. We have a wide range of facilities that ensures a quality one-stop for exploration and general analytical services. About Mintek Mintek is an autonomous research and development (R&D) organisation specialising in all aspects of mineral processing, extractive metallurgy and related technology. Working closely with minerals and metal producers locally and internationally, Mintek develops and transfers innovative, new and improved technology to industry for processing, extracting, refining and utilising minerals and mineral products. Mintek offers R&D expertise, service testwork, and technologies for the gold, platinum-group metals (PGM), base metals, ferroalloys, and industrial minerals sectors. Extensive laboratory and pilot-plant facilities are available for investigations in the following fields: Analysis - characterisation of ores and other materials, analytical chemistry and mineralogical techniques; Mineral processing - comminution, flotation, gravity, electrostatic, magnetic, and dense-media separation; Hydrometallurgy - leaching, bacterial oxidation, adsorption (CIP and RIP), solvent extraction, and electrowinning; Pyrometallurgy pre-heating and pre-reduction, submerged-arc and DC transferred-arc smelting, converting, condensing, and process simulation; and, Other specialised technologies - metallurgical process control and optimisation, tank and heap bio-leaching of gold and base metals, alloy development, pollution studies, residue processing, and techno-economic studies. Mintek s activities range from initial investigations to complete process development and, in conjunction with engineering partners, the design, construction, and commissioning of plants.

3 Contents Quality assurance 2 sample submission, storage, and disposal 2 sample preparation 3 precious metals analysis 3 multi-element techniques 3 Geological and Metallurgical Materials 3 ICP-OES 4 ICP-MS 5 single element techniques 6 AAS 6 Wavelength-dispersive XrF 7 miscellaneous methods 8 Sulphur and carbon 8 Gases 8 Water analysis 8 Environmental analyses 9 Coal and graphite 9 Halides 10 Other analytes 10 sarm program 11 contact details Inside back cover

4 Quality assurance asd has been accredited to iso (testing and calibration laboratories) since Regular internal and external audits are held to maintain and improve the effectiveness of the Quality Management System, and the laboratory participates regularly in local and international proficiency testing programmes. A Laboratory Information Management System (LIMS) is used to track the status of samples from reception though every stage of the analytical process. Instruments are interfaced to the system to ensure accurate data transfer and archiving of results for quick retrieval. Quality controls and limits are incorporated to highlight results that need investigating. ASD has six methods on its schedule of accreditation: The spectrometric analysis of chromium bearing materials with particular reference to ferrochromium slags and chromite ores (chromium-bearing materials, ferrochromium slags and chromite ores - 24/11); The analysis by atomic absorption spectrometry of geological materials for sodium, potassium, lithium, calcium and magnesium (geological materials - 11/20); The determination of sulphur in various materials using a combustion technique (various materials - 16/26 revised); The determination of carbon in various materials using a combustion technique (various materials - 6/37); Direct titrimetric method for the determination of chromium in ores (chromium ores - 24/13); and, The determination of gold and of total platinum, palladium, rhodium and gold (PGM+Au) in ores and concentrates by the fusion technique with lead as the collector (ores and concentrates - 78/29). Mintek holds certifications for Quality (ISO 9001 and ISO 17025), Environment (ISO 14001), as well as Safety and Health (OHSAS 18001). The organisation is registered as a uranium testwork facility with the National Nuclear Regulator (NNR) and the Department of Minerals and Energy (DME). sample submission, storage, and disposal Solutions and solids must be packaged separately to avoid contamination and leakage; It is the submitter s responsibility to submit a sufficient amount of sample for analysis. If insufficient sample is submitted, the analysis request must be prioritised to minimise delays; The submitter must ensure that the samples are in a form suitable for chemical analysis. Solid samples must be submitted pulverised, homogenised, and dry. Preparation will be undertaken at Mintek only with prior consultation with the client. Solutions must be free of all solids, or entrained organics; Solution samples must be submitted in liquid-tight containers, preferably in a translucent polyethylene container with a screw cap. Solid samples should be submitted in plastic or glass vials, or bags that are spill-proof; and, Clients must ensure that samples are correctly labelled. Labels must be firmly fixed to the container and marked with permanent ink. The following details must accompany all samples: Name of the person to whom results should be sent by ; Date of submission and number of samples; Elements/method required; Client s order number; Client s telephone and fax number with the postal and physical addresses; Required turnaround time, sample type, and approximate concentrations of the analyte if known; and, Any other information pertaining to the sample that may be useful. Sample storage and disposal Unless expressly agreed otherwise, clients shall, upon conclusion of the project, be responsible for collection and/or disposal of any unused sample materials and products from the testwork from Mintek. Should the client fail to do so after notice to this effect from Mintek, Mintek may at its sole discretion return or dispose of any unused sample materials and testwork products at the client s risk and expense. 2

5 sample preparation good sample preparation practice is essential for obtaining meaningful and reliable data. this involves technologically advanced equipment to process different sample types. asd s sample preparation section is a specialised and centralised sample preparation, dissolution area for metallurgical and geological samples. To ensure that your samples are prepared correctly we recommend that you discuss your requirements with our consultant for the best possible option for your sample type before starting any analysis. Sample Preparation Crushing, pulverising of geochemical samples 15 g min. 1.5 kg max. Particle size analysis Sympatech Saturn Digisizer 100 g max. SG/RD Specific gravity/relative density 100 g max precious metals analysis this classical fire assay technique is still preferred for precious metals analysis, as it allows high-precision analysis of low concentrations of precious elements in a variety of sample types. excellent facilities are available for lead collection (mainly for au, pt, pd, and rh, either as individual elements or as a gravimetric finish), and for nickel sulphide collection (au, pt, pd, rh, ru, ir and os). a gravimetric finish is generally used, but analysis for individual precious metals requires an icp-oes or icp-ms finish, as per client preference. no. description analyte list FA1 Standard fire assay with high-temperature cupellation followed by gravimetric finish Total PGM+Au mass/ vol determination limit 0.28 g/t FA2 FA3 FA4 Standard fire assay with no high-temperature cupellation, followed by the dissolution of the silver prill in aqua-regia and analysis using ICP-OES Standard fire assay with no high-temperature cupellation, followed by pressure dissolution of the prills using sealed glass tubes and analysis using ICP-OES Standard fire assay with nickel sulphide collector, followed by crushing, leaching and dissolution of the nickel sulphide button in aqua-regia and analysis using ICP-OES Pt, Pd, Au (3E) Pt, Pd, Rh, Au (4E) Pt, Pd, Rh, Au, Ru, Ir (6E) Depends on sample grade 0.1 ppm 0.1 ppm 0.1 ppm FA5 Standard fire assay with low-temperature cupellation of the silver prill, parting and annealing, followed by gravimetric finish Total Au 0.08 g/t 3

6 multi-element techniques - Geological and Metallurgical Materials icp-oes icp-optical emission spectrometry (icp-oes) is a multi-element analytical technique that can analyse more than 10 elements simultaneously. icp-oes instruments have a long dynamic range, meaning that they can be used to analyse high concentrations without the need for further intermediate dilutions. ASD has six ICP-OES instruments, including three of the latest models, which are fully automated for improved turnaround time. no. description analyte list ICP1 ICP2 ICP3 ICP4 ICP5 Ores and Slags. Fusion followed by acid dissolution in HCl/HN Beach sands and Ti-bearing minerals, Fusion in Pt/Au crucibles followed by acid dissolution Impurities in high-purity metals eg. impurities in pig iron Ferrochromium metal. Acid digestion Resins or activated carbon. Acid digestion Mg, Al, Si, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Pb Mg, Al, Si, Ca, Ti, V, Cr, Mn, Fe, Zr Per 5 elements, eg. Ca, Ti, V, Cr, Mn. Mg, Al, Si, Ca, Ti, V, Cr, Mn, Fe, Co, Ni Na, Mg, Al, Si, Ca, Fe, Co, Ni, Cu, Zn, Ag, Au, Pb mass/vol. ICP6 Andalusite. Fusion followed by acid dissolution Al 2, Fe 2, SiO 2. 1 g ICP7 ICP8 ICP9 ICP10 Ferrosilicon metal. Acid digestion PGM concentrates and matte samples, Fusion followed by acid dissolution Tin and tungsten ores. Fusion followed by acid dissolution Tantalite samples. Fusion followed by acid dissolution. Mg, Al, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Mo, Pb Si, Cr, Fe, Cu, Ru, Rh, Pd, Ag, Zr, Pt, Au, Ni, Co Mg, Al, Si, Ca, Mn, Fe, Zn, Sn, W Sn, Nb, Ta, W determination limit 1 g 0.05% 1 g 1 g 1 g 2 g Depends on matrix and analyte Depends on matrix and analyte Mg, Al, Ca 0.05% Ti, V, Mn, Co, Ni 0.01% Si 0.2% Cr 1% Fe 0.5% 50 ppm except for Si (100 ppm) Al 2 15% SiO 2 0.5% Fe 2 0.1% 1 g 20 ppm 1 g 1 g 1 g Si, Cr, Fe, Cu, Rh, Ag 0.05% Ru 0.06% Pt and Pd 0.2% Au 0.5 % Zr 0.1% Mg, Ca, Fe, Mn, Zn 0.05% Sn 0.02% W 0.05% Al 0.07% Si 0.05% Si, Fe, Ca, 0.05% Mn, Sn, Ti Ta, W 0.5% Al 0.1% Nb 0.2% 4

7 ICP 15 Cr 2 1 g 0.70% ICP16 Acid digestion Co, Ni, Fe, Cu 1 g <10 ppm ICP19 ICP21 ICP11 ICP12 ICP13 ICP22 Ores and slags. Fusion followed by acid dissolution Determination of low-concentration base metals in solids by acid digestion Water samples after required dilution PGM solutions after required dilution Multi-element solutions after required dilution Low-concentration base metals in water samples MgO, Al 2, SiO 2, CaO, TiO 2, Cr 2, MnO, FeO Mg, Cr, Si, Fe, Ca, Ti, Mn, Cu, V, Ni, Co, Al Mg, Al, Si, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Pb, Li, Be, Na, K, Ag, Cd, Sn Mg, Al, Cr, Mn, Fe, Co, Ni, Cu, Pb, Ru, Rh, Pd, Os, Ir, Pt, Au Mg, Al, Si, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Pb, Mo, SO 4, As Mg, Cr, Si, Fe, Ca, Ti, Mn, Cu, V, Ni, Co, Al, Zn, Pb, Li, Be, Ag, Cd, Sn 1 g MgO 0.1% Al 2, SiO 2, Cr 2 0.2% CaO 0.3% TiO % MnO 0.03% FeO 0.06% 2 g 0.1 ppm 5 ml 5 ml 5ml 10ml Ti, V, Cr, Mn, Fe, Cu, Li Co, Zn, Ag, Cd, Be Mg, Si, Ni, Pb, Sn Al, Ca Na, K 2 ppm except for Ru Rh 2 ppm except for SO ppm 0.05 ppm 0.1 ppm 0.2 ppm 0.5 ppm 6 ppm 4 ppm 15 ppm 0.02 ppm ICP23 Low-concentration PGMs in solutions Au, Pt, Pd, Rh, Ru, Ir, Os 10 ml 0.1 ppm ICP24 icp-ms Low-concentration base metals in solutions Mg, Cr, Si, Fe, Ca, Ti, Mn, Cu, V, Ni, Co, Al, Zn, Pb, Li, Be, Na, K, Ag, Cd, Mo, SO 4, As 10ml 0.02 ppm icp-mass spectrometery (icp-ms) is a trace technique that analyses in the low parts-per-billion (ppb) range. icp-ms is especially suited for environmental and water analyses, impurities in high-purity end-products of two- to fivenines quality, and soils or ores for trace and ultra-trace elements. Very low detection limits of 0.01 ppm in solutions and 0.1ppm in solids can be attained. Quick semi-quantitative scans can be obtained for solid and solution samples containing trace levels of dissolved solids. The section has three ICP-MS instruments. no. description analyte list determination limit MS2 MS3 Fusion Semi-quantitative scan All elements, excluding Na, C, S, P, Si, K, Ca and gases. Radioactive material - only U and Th All elements, excluding Na, C, S, P, Si, K, Ca and gases. Radioactive material - only U and Th 0.1 ppm 0.1 ppm MS4 Special dissolutions B or Hg or Os 0.1 ppm MS5 Filter analysis As for MS2, excluding volatiles 0.1 ppm 5

8 MS6 Quantitative Analysis after appropriate dilution All elements, excluding Na, C, S, P, Si, K, Ca and gases. Radioactive material - only U and Th 0.01 ppm MS7 Semi-quantitative scan All elements, excluding Na, C, S, P, Si, K, Ca and gases. Radioactive material - only U and Th 0.01 ppm single element techniques aas atomic absorption spectroscopy (aas) is a single-element technique, used as an alternative technique for troublesome elements like na and K in complicated matrices. it is also used when icp-oes is unable to do the analysis for a particular element, owing to interference. For some elements, aas has lower detection limits than icp-oes. ASD has three AA instruments, one of which is a Graphite Furnace instrument that allows detection limits down to ppm for Au in solutions. no. description analyte list mass/ vol. determination limit AA1 Acid digestion Na, K, Mg, Ca, Li 2 ppm Ca 10 ppm Ag, Cu 5 ppm Ni, Pb, Zn 15 ppm AA2 Acid digestion Ag, As, Au, Cd, Co, Cu, Fe, Mn, Mo, Cd, Co, Fe, Mn 25 ppm Ni, Pb, Zn Mo 50 ppm As 80 ppm Au 100 ppm Al 150 ppm Ba, Sb, Sr 50 ppm AA3 Fusion Bi 10 ppm Cr 200 ppm Sn 1000 ppm V 70 ppm AA4 Sequential Cu analysis Oxide, cyanide and residual 1 g 20 ppm AA5 After appropriate dilution Co, Cr, Mn Mo, Al, As, Sn, Bi Na, K, Ag Mg, Li, Cu Ca, Cd, Pb, Sr, Zn 0.1 ppm 0.2 ppm 0.5 ppm 1.0 ppm 5 ppm Ba, Fe, Ni, Sb 2 ppm V Au on flame AA Au in cyanide solutions by ETA 2.5 ppm 0.6 ppm ppm 6

9 Wavelength-dispersive XrF X-ray Fluorescence (XrF) is well known for its accuracy and reliability. this technique is universally accepted as industry s standard and preferred technique for solid analysis. sample types analysed by XrF range from geological to metallurgical process materials for the determination of major, minor and minor to trace elements. Environmental analysis of filters by a quick semi-quantitative scan has been particularly useful in determining volatile elements associated with acid digestion. Samples for analysis are prepared as either powder briquettes or fused beads, depending on matrix and the client s request. The section has 3 XRF instruments: An energy dispersive X-ray instrument (EDX) For quick semi-quantitative scans of solids and solutions; A wavelength dispersive instrument (WDX) Ideal for U analysis and R&D work. Instrument also has mapping capability; and, A multi-channel instrument (MXF) Has the capability of 36 elements analysed simultaneously with the added option of a scanning channel from Ti to U. The instrument has a 100 autosampler. Especially, purchased to provide quick turn around times. Methods are also developed to clients specifications, provided the request is within acceptable limits. no. description analyte list mass/vol. XRF1 Andalusite samples on a pressed pellet Al 2, Fe 2, SiO 2 8 g XRF2 Mn ore samples on a pressed pellet 8 g XRF3 Merensky/UG2 ores on a pressed pellet 8 g determination limit Al ppm SiO 2 35 ppm Fe 2 25 ppm Mg, Al, Si, 100 ppm Ca, Mn 20 ppm Fe 15 ppm Cu & Ni 1ppm Mg 100 ppm Cr 15ppm XRF4 Semi-quantitative scan on pressed pellet (under vacuum) All elements excluding: Those with Z<13 Sc and PGMs Rare Earth Elements except La, Ce, Hf Radioactive elements except U, Th 8 g N/A XRF5 Qualitative/semi-quantitative powder scan All elements excluding: Those with Z<13 Sc and PGMs Rare Earth Elements except La, Ce, Hf Radioactive elements except U, Th 5 g N/A XRF6 Alloy scan to 100% totals Depending on the alloy Smooth surface disc <32 mm diameter N/A XRF7 Apatite P, Fe, Ca, Al 8 g XRF8 Fe ore Fe, Si, Al, P 8 g 7

10 miscellaneous methods many types of classical analysis are done by volumetric, gravimetric and spectrophotometric determination. these techniques are useful for high-precision work, as well as for some difficult analyses and in particular speciation of elements. sulphur and carbon description method analyte list mass/vol. determination limit Total S Combustion (LECO) g 0.01 ppm Elemental S Gravimetric, after extraction g 0.2 ppm Sulphate S Gravimetric, after extraction g 0.2 ppm Sulphide S Combustion, after SO4 removal g 0.1 ppm SO 4 or total S Gravimetric 10 g Sulphide in solution Iodometric titration 10 g Total C Combustion g 0.01 ppm Organic C Combustion after extraction g 0.1 ppm Carbonate C Total C - Organic C g 0.5 ppm gases description method analyte list mass/vol. determination limit Oxygen* Combustion 20 ppm** Nitrogen* Combustion g 20 ppm** * Method calibrated for steel **Depends on matrix Water analysis description method analyte list mass/vol. determination limit ph ph electrode n/a n/a Conductivity Electrode n/a n/a TDS (Evaporation) Gravimetric n/a n/a TSS Gravimetric n/a n/a Total hardness Titration n/a n/a Alkalinity Titration n/a n/a Acidity Titration n/a n/a Dissolved oxygen Electrode n/a n/a 8

11 environmental analyses description method analyte list mass/vol. determination limit TCLP Leach procedure according to EPA 105 g n/a Acid rain Leach procedure according to EPA 105 g n/a Acid rain By ICP-MS after acid rain leach Li, Be, B, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, As, Se, Sr, Zr, Mo, Ag, Cd, Sn, Sb, Ba, Hg,Pb, Bi n/a n/a By ICP-MSOES after acid rain leach Na, Mg, Al, Si, P, S, K, Ca, Fe n/a n/a TCLP By ICP-MS after acid rain leach By ICP- MSOES after acid rain leach Li, Be, B, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, As, Se, Sr, Zr, Mo, Ag, Cd, Sn, Sb, Ba, Hg,Pb, Bi n/a n/a Na, Mg, Al, Si, P, S, K, Ca, Fe n/a n/a Metallics leached from solid samples By instrumental technique e.g. ICP-OES Fe, Al, or by request g coal and graphite description method analyte list mass/vol. determination limit LOI Loss on ignition at 950ºC or (other temperatures) 2 g Moisture Moisture at ºC 2 g Ash Ashing at 950ºC 2 g Proximate analysis of coal Graphite Moisture, ash, volatiles and fixed carbon Moisture, ash, volatiles and fixed carbon 10 g 10 g 9

12 halides description method analyte list mass/vol. determination limit Cl in solids Gravimetric, potentiometric or turbimetric (depends on level) Fusion Acid dissolution 5 g 0.03% 60 ppm Cl in solution Potentiometric Fusion Acid dissolution 5g F in solids Ion-selective electrode Fusion Acid dissolution 5 g 0.1% 200 ppm F in solutions Ion-selective electrode 20 g 10 ppm other analytes description method analyte list mass/vol determination limit P (or P 2 O 5 ) in solids Colourimetric after fusion 2 g 10 ppm P (or PO 4 ) in solutions Colourimetric 20 g NH 4 in solutions Colourimetric 20 g NH 4 Distillation/back-titration 5 g Cr 6+ in solids Matrix-dependent 5 g Cr 6+ in solution Colourimetric 5 g 0.02 ppm Fe 2+ in chromites Titration after fusion 10 g Fe 2+ in solids Titration after fusion 10 g Fe 2+ in solutions Titration 10 g 0.1 g/l Ti 3+ Titration (total Fe must be subtracted) 20 g SiO 2 Gravimetric 5 g CO 2 /C Distillation/gravimetric 5 g ** By agreement only Other analyses are available on request and after discussion/consultation. 10

13 sarm program mintek is a producer of metallurgical and geological certified reference materials (the south african reference materials or sarms series). these materials are made according to iso guides 30 to 35 which describe the best practices for manufacturing and certification. there are over 70 reference materials available (ores, heavy minerals, soils, sediments, coal and rocks), and these are continually being added to in an ongoing programme. type description sarm number unit of packing Granite SARM 1 NIM-G 100 g Syenite SARM 2 NIM-S 100 g Lujavrite SARM 3 NIM-L 100 g Norite SARM 4 NIM-N 100 g Pyroxenite SARM 5 NIM-P 100 g Dunite SARM 6 NIM-D 100 g Kimberlite SARM g Carbonatite SARM g Carbonaceous shale SARM g rocks and minerals Soil SARM g Magnesite SARM g Sillimanite schist SARM g Kinzingite SARM g Stream sediment SARM g Serpentinite SARM g Fluorspar granite SARM g Quartz SARM g Dolerite SARM g Stream sediment SARM g Stream sediment SARM g 11

14 Titanium slag (RBM) SARM g Titanium slag (AAC) SARM g heavy minerals Ilmenite (RBM) SARM g Rutile (RBM) SARM g Zircon (RBM) SARM g Ferrosilicon SARM g Ferro-alloys Ferrochromium SARM g Ferrochromium slag SARM g Gold tailings SARM g, 2 kg Gold calcine SARM g PGM ore UG2 low SARM 70 3 kg Precious metals PGM ore UG2 high SARM 72 3 kg PGM ore Merensky SARM 73 3 kg PGM ore Sheba s Ridge SARM 75 3 kg PGM ore Merensky SARM 76 3 kg Coal (Witbank) SARM g coal Coal (OFS) SARM g Coal (Sasolburg) SARM g Uranium, acid leach residue SARM 21 UREM g Uranium, pyrite concentrate SARM 23 UREM g Uranium, slimes dam material SARM 24 UREM g uranium Uranium, pyrite concentrate SARM 25 UREM g Uranium, pyrite concentrate SARM 26 UREM g Uranium, acid leach residue SARM 27 UREM g Uranium, Witwatersrand ore SARM 29 UREM g Phosphate rock SARM g Andalusite SARM g Vanadium pentoxide SARM g ores and semi-processed materials Fluorspar (Zeerust) SARM g Manganese ore (Wessels) SARM g Manganese ore (Mamatwan) SARM g Pot shard (archaeological ceramic) SARM g 12

15 Contact details The Manager Analytical Services Division, Mintek Phone: Fax: The Customer Services Consultant Phone: The Sales and Marketing Consultant Phone:

16 Mintek 200 Malibongwe Drive, Randburg, South Africa Private Bag X3015, Randburg, 2125 South Africa Phone: Fax: