Analysis Technology: Methods and Devices

About Analysis
In our laboratory, we use classical wet chemical methods such as gravimetry, volumetry, electrogravimetry, instrumental analytical methods and melt extractions for the main and minor group elements, especially for the precious metals Ag (silver), Au (gold), Pd (palladium), Pt (platinum) and Rh (rhodium).
Extraction of Precious Metals:
For precious metal analysis, we prefer to work with the methods established under the term docimasy (fire assay). These include the melting (1000 – 1200°C) and collection of the precious metals gold (Au), silver (Ag), platinum (Pt), palladium (Pd) with lead (Pb). The Pb can be partially or completely expelled. The remaining precious metal grain is either analysed for its components Au, Pd and Pt using ICP-OES, titrated (Ag), or the Au is determined gravimetrically (roll sample).
Other collectors such as copper (Cu) or nickel sulphide (NiS) are often used specifically for the platinum group metals platinum (Pt), palladium (Pd), rhodium (Rh), iridium (Ir) and ruthenium (Ru). The docimastic methods separate the often interfering and therefore disturbing matrix of the sample material and, with simultaneous enrichment of the precious metals Ag, Au, Pd, Pt, Rh, Ir, Ru, enable instrumental analysis with a constant matrix of Cu or Pb. We have a large number of chamber furnaces for melting and driving work, so that there are no bottlenecks in the collective melting of Ag, Au, Pd, Pt, Rh, Ir, Ru.
Analysis Technology with Inductively Coupled Optical Emission Spectrometry (ICP-OES):
Using ICP-OES technology, we are able to analyse almost all elements of the periodic table of elements. We have two ICP-OES spectrometers at our disposal: ThermoFisher iCap 6300 (radial and axial observation of the plasma) and Spectro Arcos (radial observation). We also use the Analytik Jena Plasma Quant ICP-MS for trace levels. The working range is between 0.001 and 200 mg/L.
Certified or validated standard solutions with metrological traceability are a prerequisite for reliable results.
For stable measurements, we use the bracketing method, among other things.

Analysis Technology with Wavelength Dispersive X-ray Fluorescence Spectrometer (WD-XRF):
With this measuring method, all precious metals Ag, Au, Pd, Pt, Rh, Ir, Ru collected with Cu-docimania are measured in the copper king/copper regulus using specially calibrated methods. Accuracy is verified using natural reference material and synthetically produced comparisons made from pure metals, the purity of which is checked prior to use using GDMS (glow discharge mass spectrometry). The WD-XRF can analyse concentration ranges from 1 – 2 ppm up to 100% depending on the sample weight and the elements to be determined. We use the Axios (MalvernPanalytical) with a 4 KW molybdenum tube.

GDMS Analytics
Glow discharge mass spectrometry (GDMS) enables the reliable determination of trace and ultratrace elements in solids. With very low detection limits, the method is particularly suitable for purity analyses of metals, alloys, and semiconductor materials.

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Analysis of trace elements in a wide variety of sample material.
Myint Myint Sein, Wolfgang van Leeuwen and Peter Glörfeld (2017) Combination of fire assay and modern instrumental techniques for precious metal analysis, In: Production and recycling of non-ferrous metals: Saving resources for a sustainable future, European Metallurgical Conference EMC 2017, Vol. 4, 1785 – 1796.
Frequently Asked Questions (FAQ)
Which analysis methods are used in your laboratory?
We use classical wet chemical methods such as gravimetry, volumetry and electrogravimetry as well as modern techniques such as ICP-OES, ICP-MS, GD-MS and WD-XRF.
How does precious metal analysis work in your laboratory?
To analyse precious metals, we use docimacies methods. This involves enriching precious metals such as gold, silver, platinum and palladium by melting and collecting them with lead, copper or nickel sulphide and then analysing them.
Which devices are available for the analysis technology?
Our laboratory is equipped with three ICP spectrometers (Spectro Modula, Spectro Arcos, ICAP 6300 DUO), one wavelength dispersive X-ray fluorescence spectrometer (WD-XRF), two GD-MS (Thermo Fisher) and several chamber furnaces for melting and refining work.
Welche Geräte gibt es für die Analysetechnik?
Our methods cover concentrations from 0.1 mg/L to 100%, depending on the method and sample weight.
How is the accuracy of the analyses ensured?
Our results are checked with natural reference material and synthetic reference samples. We also use pure metals whose purity is carefully checked before use.
Can trace elements be analysed?
Yes, with our ICP-MS system we can precisely analyse trace elements in a wide variety of sample materials.