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Group Chemical Analysis

Micro and element analysis

Chemical Analysis at IAM-AWP uses a wide range of modern analytical instruments and methods to solve analytical questions in materials research within the Helmholtz-Programs Nano- and Microtechnology, Nuclear Fusion and Nuclear Safety Research as well as Efficient Energy Conversion and Use.

Established analytical methods are validated and developed for the continously newly developed materials. The reliability of the analyses is verified by the organisation and participation in ring analyses. Our expertise is also available for external clients and partners. The Chemical Analysis group is part of the Karlsruhe Nano Micro Facility (KNMF), the EUMINAfab and QNano, national and european infrastructures for the production, characterization and safety research of micro and nano materials. 

Analytical Methods

 

Auger electron spectrometry (AES)

 

Lateral high resolution Auger electron spectrometer
(Auger Nanoprobe 680 xi,
Physical Electronics)

Elements: Li to U

Detection limit: > 0.5 % - 5 % (depending on element);

Measurements and capabilities: Multipoint and area analysis, linescans, element maps ranging from ∅ > 24 nm to µm and depth analysis from  1 nm to 1 µm

Materials: electrically conducting and semiconducting solids and layers

Applications:

  • Surfaces and matrix, interfaces and in-situ fracture surfaces (in UHV fractures of different sample shapes are possible) 
  • Steels, alloys, hard materials, superconductors, multilayers (from 5 nm)
    Macro-, micro- to nano systems, e.g. moulds, sensors, stents, micro reactors, etc.  

 

ICP Mass spectrometry (ICP-MS)

 

 

Quadrupol mass spectrometer (Agilent 7500ce) with inductively coupled plasma ion source and reaction gas cell (He, H2)

Elements: Li to U except noble gases, C, N, O and F

Detection limit: 0.0001 to 10 µg/L (ppb), depending on element

Samples: aqueous solutions and dissolved solids

Special sample preparation: Microwave digestion system for solids, "subboiled" acids

Applications:

Ultratrace- und isotopic analysis in

  • water, waste water, eluates, aerosols, slag, ash, soil
  • metals and alloys such as tungsten, molybdenum, steel, special alloys etc
  • oxides, nitrides, carbides such as SiO2-, TiO2 nanopowder, C nanotubes

 

Laser ablation coupled to ICP mass spectrometer (LA-ICP-MS)

 

Laser Ablation System
(New Wave UP 193 FX) Excimer Laser coupled to ICP-MS (Agilent 7500ce)

 

Elements: Li to U except noble gases, C, N, O and F

Detection limit: < µg/g (depending on element)

Samples: anorganic and organic solids

Measurement capabilities: point analysis, linescans, with diameter and linewidth of 5 - 150 µm under normal pressure

Applications:

  • conductive and non-conductive materials
  • materials für Li-Ion-Batteries

Optical ICP emission spectrometry (ICP-OES)

 

Optical  emission spectrometer
(OPTIMA 4300DV, Perkin-Elmer) with inductively coupled plasma, an Echelle polychromator and a solid state detector (custom, two-dimensional CCD array)

Elements: Li to U except noble gases, halogenes, C, N and O

Detection limit: 0.05 to10 µg/L (ppb), depending on element

Samles: Solutions and dissolved solids

Special sample preparation: Microwave digestion system for solids with "sub boiled" acids; bead machine for solids

Anwendungen:

Trace analysis up to the determination of main components in

  • metalls and alloys, glass, concrete, ceramic, ore, superconductors, carbides, nitrides, materials for Li-ion batteries, nano materials, C-nano tubes etc.  
  • water, eluates, aerosols, slags

 

X-ray fluorescence spectrometry (RFA)

 

X-ray fluorescence spectrometer
(S4 PIONEER, Bruker-AXS) sequential wavelength dispersive spectrometer

Elements: B to U in solids, Na to U in solids and liquids

Detection limit: 0.0001 to 0.1 % depending on element and matrix


Samples: solids and liquids

Special sample preparation: automatic bead machine with Perl’X 3

Applications: Determination of main and minor components

  • oxides: silicate, titanate, zirconate, glass, concrete, bottom ash, soil, superconductors etc. 
  • metalls and alloys 
  • Further solids: aerosols, fly ash, etc.

 

C-S-Analysis

 

C/S-analyzer ((CS600, LECO),
Sample combustion in the high-frequency
furnace with oxygen to form CO2 and SO2 with subsequent IR detection.

Elements: C, S, differentiation of organically and inorganically bound C

Detection limit for C: 5 to 60000 µg

Detection limit for S: 2 to 4000 µg

Materials: all solids

Applications:

  • metalls and metallic alloys
  • oxidic and non-oxidic materials: silicate, aluminate, ceramic, etc.
  • hard materials: carbide, nitride, boride
  • ash, slag, dust
  • organic solids 

 

O-N-Analysis

 

Trägergasheißextraktion (TC 600, LECO):
Probenzersetzung im Metallbad in glühender Graphitkapsel im He-Gasstrom mit
anschließender IR-Detektion von CO bzw.
CO2 und Wärmeleitfähigkeitsmessung von N2

Elements: O, N

Detection limit for O: 0.1 to 50000 µg

Detection limit for N: 0.1 to 30000 µg

Materials: all solids, especially metals 

Applications:

  • metalls and metallic alloys
  • hard materials: carbide, nitride, boride
  • oxides and oxide mixtures: depending on CO-formation 
  • organic solids with high melting and decomposition temperatures