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Laboratory for Environmental and Raw Materials Analysis (LERA)
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Laboratory for Environmental and Raw Materials Analysis (LERA)

 

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  • Orders
  • Solids

 

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    • Solids
    • Water
    • Plants
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    • Sensor systems
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  • Solids
    • Preparation
    • Digestions
    • Mineralogy
    • Geochemistry

Solids

  • Start
  • Preparation
  • Acid digestion
  • Mineralogy
  • Geochemistry

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
(cm-mm)

Retsch

Vibrating Cup Mill

Pulverization/
Homogenisation

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 +
Te, SnCl2 (tellurium co-precipitation)

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
(nm to µm) on mineral composition,
grain shape,
surface properties etc.
 

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);
ICP-OES (Varian 715ES)

last change: 2022-08-01
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