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Research Laboratory

The Research Laboratory of the Deutsches Bergbau-Museum Bochum is where we carry out chemical analyses and diverse evaluations of physical materials. To this end, we develop and adapt new procedures to meet the particular research demands. Our work delivers information regarding the characterisation of materials and material properties, as well as on questions concerning their origins.

The Research Laboratory can examine practically all kinds of inorganic materials to establish their chemical, structural and physical compositions. A suitable preparation process and method is selected, depending on the research issue and the qualities of the sample.

The Research Laboratory has a variety of equipment which is particularly important for the Materials Science, Mining Archaeology and Archaeometallurgy research departments. In the Research Laboratory we also conduct series of tests on behalf of the Materials Science department, to understand the way in which deterioration processes affect metals, plastics and natural stone. And we develop protective agents and measures for materials which are already damaged, in order to preserve them from further damage.

The entire spectrum of analytics carried out in the Research Laboratory, as well as our on-site sampling service, is also used by external clients, such as universities and non-university research institutions, companies and private individuals.

Publications
  • REICHMANN, CH./SIEPEN, M./BODE, M.: Der römische und frühmittelalterliche Hafen von Krefeld-Gellep, in: Mirschenz, Manuela/Gerlach, Renate/Bemman, Jan (Hrsg.): Der Rhein als europäische Verkehrsachse III, Bonner Beiträge zur Vor- und Frühgeschichte Archäologie 22, 2019, S. 215 – 232.
  • VAELSKE, V./BODE, M./LOEBEN, C. E.: Early Iron Age Copper Trail between Wadi Arabah and Egypt during the 21st dynasty: First Results from Tanis, ca. 1000 BC, in: Zeitschrift für Orient-Archäologie 12, 2019, S. 184 – 203.
  • VAELSKE, V./BODE, M./EL-MORR, Z.: Early Iron Age Copper Trails: The Case of Phoenica. First Results of a Pilotstudy, In: Bulletin d‘archéologie et d‘architecture libanaises, S. 267 – 279.

This method is used for the analysis of plastics, binders and for existing damage phenomena on museum objects. Through the interaction of matter with infrared radiation, information can be obtained about the structure of the substances present. FTIR is an excellent method for gaining conclusions about the main constituents of an unknown sample, whether organic or inorganic, without the need for time-consuming sample preparations. Excluded are metals and other infrared-transparent substances. A total of three infrared spectrometers are located in the research laboratory: these include a Thermo Fisher FTIR microscope, purchased in 2016, and an Agilent portable FTIR instrument, purchased in 2019 for in situ analysis. All are capable of operating in ATR (attenuated total reflection) mode, often eliminating the need for sampling.

A more detailed analysis of complex organic samples, for example fats, oils and resins, is conducted in the research laboratory using GC-MS. Our GC-instrument TRACE 1310 with coupled MS (ISQ 7000) (Thermo Fisher Scientific), purchased in 2019, allows analysis in EI and CI modes. Coupled with a pyrolysis unit from Frontier Labs. It further allows analysis of high molecular weight substances such as polymers, including Evolved Gas Analysis (EGA) mode. The unit is also capable of performing headspace analysis and derivatisation of samples prior to analysis.

Especially when assessing damages to rocks in buildings, it is necessary to obtain information about adherend water-soluble cations (Na+, K+ etc.) and anions (Cl-, NO3-, etc.), determined with ion chromatograph ICS 1600 (Dionex).

In our laboratory, standard tests such as the measurement of pH, conductivity, loss on ignition or the determination of carbon, carbonate and sulphur contents are verified.

For chemical element analysis, the research laboratory uses an Element XR, a high-resolution-sector field mass spectrometer (Thermo Fisher Scientific). It is currently one of the most powerful devices enabling elemental determinations down to the ultra-trace level.

We also offer e.g. highly precise determination of lead and copper isotopes with a Neptune XT (Thermo Fisher Scientific), purchased in 2020.

A disc mill and ball mills are used for the ultra-fine grinding of mineralogical materials and natural rocks, a sieving machine for grain size determination.
For sawing larger samples, the research laboratory has a water-cooled saw with a maximum cutting depth of 200 mm as well as cutting machines for finer cuts. It is possible to process both metallic and mineralogical samples.

Thin sections and mounts can be provided with precision surface grinding machines. In addition, modern semi-automatic water-cooled grinding and polishing machines are available for the preparation of metallic ground sections.

Polishing is performed on lead discs with oil-bonded diamond suspensions or on textile discs with water-bonded diamond suspensions.

The research laboratory's X-ray diffractometer provides an important tool for identifying minerals and phase mixtures. The PANalytical Xpert Pro diffractometer can be operated with either a 15-position sample changer for powdered samples or a universal sample table. The latter allows the non-destructive analysis of even larger samples up to 10 cm in length and width. Natural rocks, mortars, pigments, salts as well as weathering and corrosion products, ores, metals, slags, rocks or archaeological objects, can be analysed.

The research laboratory's portfolio includes a portable energy-dispersive X-ray fluorescence spectrometer Niton Xl3t GOLDD, which enables non-destructive surface analysis. The device allows semi-quantitative determination of the element distribution in metals as well as rocks, soils, ores, ceramics or plastics. Light elements up to sodium cannot be determined with this device.

To perform analyses in the ultra-trace range or isotope analyses, a clean room laboratory for sample preparation was set up in 2009. The clean room (ISO 8) and the benches (ISO 3) are classified and certified according to EN ISO 14644-1:1999.

In our simulation chambers, weathering and corrosion processes on treated and untreated as well as preserved natural rocks, metals, and plastics can be simulated over a short period of time. In addition to standardised tests that specifically check the influence of weathering factors, we carry out simulations with combined, nature-adapted influencing variables. The correlation of analyses of metal, platics, bricks or rocks and specific weathering simulations allows conclusions about the weathering and corrosion processes taking place, the further development of damage and possible damage prevention.

The field emission scanning electron microscope SUPRA 40 VP (Zeiss) allows measurements down to the nanometre scale. It is equipped with a variable vacuum mode, which is mainly used for samples that do not allow gold- or carbon-coating. Museum or archaeological objects that may not be coated can also be analysed in this way. This mode is also applicable for specimens that still have a certain moisture content or that may easily become charged. The large sample chamber without a limiting airlock allows examinations of larger objects up to 13 cm in length and width and 4 cm in height. Additional software enables the three-dimensional representation of surfaces and can be used for layer thickness measurement.
Our FE-SEM is equipped with a Noran System 7 energy dispersive X-ray spectrometer (Thermo Fisher Scientific) with a SDD detector, performing the non-destructive, qualitative, and semi-quantitative analysis of all sample components. Measurements can be taken at specific points, in profiles, or over a wider area. A two-dimensional element distribution is possible (mapping).

Polarisation light microscopy is widely used to examine thin sections and polished sections. On the one hand, it enables identifying mineral phases, and on the other hand, quantifying structures and microstructures by means of connected image analysis. Three-dimensional imaging of surfaces is possible by recording the sample layer by layer.


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