Solid samples are prepared prior to further analysis in a contamination-free and user-specific manner. Beside the classical comminution methods as well as grindings, specialized digestion procedure enable a complete or partial decomposition of pulverized solid samples. We offer mineralogical or petrographical methods for a comprehensive analysis of the mineral stock as well as a description of the microstructure or individual mineral grains. In our laboratories, solid samples can be comprehensively geochemically analysed in order to answer technical, geological and environmental questions.
Preparation
For a high-quality analysis, the samples must be prepared beforehand, i.e. sawn, crushed, pulverized and homogenized. In addition to the preparation of complete samples, we also offer the possibility of spatially resolved powder sampling (>30 µm). The mineralogy, geochemistry or isotopy of the solids can then be analysed on the pulverised material. Grinding vessels made of various materials are available for contamination-free sample preparation.
Grindings are the basis for microscopic mineral characterization (reflected light/transmitted light microscopy, SEM), as well as for high-resolution investigations of geochemistry (microprobe, synchrotron, LA-ICP-MS). Adapted to the respective examination method, we offer ground sections in various thicknesses and designs.
We will be pleased to advise you on the most suitable preparation and ground sections.
Grinding
Method |
Task |
Device/Material |
Rock crusher |
Crushing (hand pieces) |
Retsch |
Jaw crusher |
Crushing |
Retsch |
Vibrating Cup Mill |
Pulverization/ |
Sieving technology / agate, corundum, tungsten carbide |
Planetary micro mill |
Pulverization/ Homogenization |
Pulverisette 7, FRITSCH / corundum, tungsten carbide |
Micromill (locally dissolved) |
Pulverization |
Olympus SZ61, Dover |
Drying
Process |
Task |
Device |
Freeze drying |
Water content, preservation |
Christ Alpha 1-4, 100400 |
Drying |
Water content at 105 °C |
Drying ovens, Memmert |
Ashing |
Loss on ignition |
Muffle furnace, Nabertherm |
Ground joints (28x48 mm)
Type |
Thickness |
Variant |
Thin sections |
30 µm |
polished, capped, polished on both sides, removable |
Thick sections |
100 µm |
polished, capped, polished on both sides, removable |
Ground joint |
variable |
polished (cloth or lead plate) |
Acid digestion
Acid digestions allow complete or partial decomposition of pulverized solid samples (rock, ore, soil, dust filters, plants, materials, etc.). The type of digestion is specifically adapted to the elements to be analyzed and the sample matrix.
Among others, we offer (1) open and semi-open full digestions (HNO3(HCl)-HF-HClO4) for the subsequent analysis of major and trace elements, as well as rare earth elements; (2) microwave digestions for the subsequent analysis of volatile elements such as As, Se, etc. or (3) special digestions for the concentration of selected elements such as platinum group elements (tellurium co-precipitation). Specific leaching tests are used, for example, to extract readily soluble or acid-soluble components prior to their analysis. All digestion samples are measured by ICP-MS, ICP-OES or AAS depending on the element and the expected concentration.
Melt digestions also dissolve resistant minerals (e.g. heavy minerals), so that a complete decomposition of the rock matrix is possible. We analyse the fusion tablets with regard to the main element geochemistry by means of X-ray fluorescence analysis (XRF). However, melt tablets can also be further dissolved using acids and then analysed with ICP-MS or ICP-OES with regard to geochemistry.
We will be happy to advise you on the most suitable digestion and analysis method for your application.
Open/semi-open outcrops
DigiPRep, SPS Science, PFA vessels
Chemicals |
Sample material |
Elements |
HNO3(HCl)-HF-HClO4 |
Ore, soil, rock, concrete |
Major elements, trace elements, rare earth elements, technically critical elements (all as far as not volatile or radioactive) |
HNO3/H2O2 |
Plant material |
Main elements |
HNO3 |
Plant material |
Main/trace elements |
Microwave
Microwave, START 1500, MLS GmbH
Chemicals |
Sample material |
Elements |
HNO3/H2O2 |
Plants |
As, Se, Te, Cd, Sn |
HNO3/H2O2/HF |
Soil/rocks |
As, Se, Te |
HNO3/HCl |
Precious metals |
Trace elements |
HNO3/HCl/H2O2 + |
Soil, plants, road dust |
Platinum group elements |
Leaching
Leaching agent/process |
Sample material |
Elements |
Deionized water/ based on DIN EN 12457, DIN 19529 |
Solids (soils, wastes etc.) |
Main elements, selected trace elements, pH-value |
Ammonium nitrate / based on DIN ISO 19730 |
Soil |
Selected trace elements |
Aqua regia / based on DIN EN 13657 |
Solids (soils, wastes etc.) |
Selected trace elements |
Fusible solids
Melting agent |
Sample material |
Elements |
Li-borate (Sprektroflux 110) |
Rock, soil, ore |
Major elements, selected trace elements (if not volatile or radioactive) |
Mineralogy
Mineralogical or petrographical methods allow a comprehensive analysis of the mineral stock, as well as a description of the microstructure or individual mineral grains.
We offer X-ray graphic analyses (XRD) on powder samples for the investigation of the mineralogical composition. You have the choice between a qualitative evaluation or a semi-quantitative mineral analysis using Rietveld modelling. For the determination of the proportion of swellable clay minerals, we prepare special texture preparations (swollen, burnt).
By means of polarization microscopic examinations of thin sections, we can determine minor constituents of your sample that are not detectable by XRD. Very small components can be detected by scanning electron microscopy (SEM) and clearly identified by coupled geochemical analysis. We estimate the mineral contents via a graphical evaluation from the microscopic images. A petrographic description provides additional information regarding grain size and shape, porosity, mineral association, alteration, etc.
By means of thermal analyses we can also determine specific weight loss as well as characteristic transformation or melting temperatures of minerals and mineral mixtures by means of thermogravimetry coupled with differential scanning calorimetry (TG/DSC) in the temperature range of 20-1400 °C.
We will be pleased to advise you in order to determine the appropriate analyses for your problem.
Radiographic analysis
D8 Discover, Brucker
Method |
Sample material |
Statement |
Powder diffraction (XRD) |
Pulverized ores, soils and rocks; amount > 10 mg - 2 g |
Qualitative, semi-quantitative mineral stock |
Texture preparations (unconditioned, glycolized, burnt) |
Gravimetrically separated clay constituents |
Specific characterization of clay minerals, identification of swellable clay minerals |
Microscopy on thin sections
Tesca Vega; resolution
Method |
Sample material |
Statement |
Polarization microscopy |
Thin section |
Mineral composition, grain size, grain shape, porosity, alteration, association |
Scanning electron microscope (SEM) coupled with X-ray fluorescence |
Thin section |
High resolution information |
Thermal analysis
STA 409 PC, Netzsch
Crucible |
Atmosphere |
Heating rate |
Sample quantity |
Platinum/Corundum |
air, N2 |
< 50K / min |
≤20-30 mg |
Determination of weight changes (>0.1%), identification of exo- and endothermic reactions, determination of reaction temperatures (outgassing, mineral transformation, melting temperature).
Geochemistry
Geochemical analyses enable a wide range of questions to be addressed. Rocks, for example, can be clearly assigned on the basis of their geochemistry and their formation can be understood. For raw material exploration, geochemical anomalies in soils or stream sediments are specifically searched for. For an economic evaluation, the content of the respective valuable elements must be determined in numerous samples. Concepts for the remediation of contaminated sites are based on an areal determination of the concentration of a contaminant element both as a whole and of the readily available fraction.
We analyse both major and trace element contents in solid samples (rock, ore, soil, materials, mineral or metallic waste) as a whole or after partial leaching. Alternatively, we determine geochemistry directly on powdered samples or on fused tablets using X-ray fluorescence analysis (XRF) or after acid digestion using ICP-MS/-OES. We can also analyse the Fe(II) content of your sample by titration. Carbon and sulphur content are also determined on the powder using an element analyser.
We will be pleased to advise you in order to determine the appropriate analyses for your problem.
Analyses
Method | Element spectrum | Device |
X-ray fluorescence (XRF), angle dispersive, melting tablet | main elements (Na, K, Ca, Mg, Al, Si, Fe, Mn, Ti, P), loss on ignition | S4 Explorer, Bruker AXS |
X-ray fluorescence (XRF), energy dispersive Melting tablet/powder bulk sample | main elements (Na, K, Ca, Mg, Al, Si, Fe, Mn, Ti, P) div. trace elements | Epsilon 5, PANanlytical; Epsilon 4, PANanlytical; EDX 8000; Shimadzu |
Carbon-sulfur analyzer (CSA) | TC, TOC, TS | CS-2000, ELTRA |
Titration (Manganometry) | Fe(II) | Dosimat 715, Metrohm |
div. digestions | Major and trace elements | ICP-MS (X-Series 2, Thermo Fisher); |