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Contact (User Office)

 

Karlsruhe Nano Micro Facility
KIT-Campus North

Building 440

H.-von-Helmholtz-Platz 1

76344 Eggenstein-Leopoldshafen, Germany

 

phone: +49(721)608-23123

fax: +49(721)608-26273

knmf-userofficeQyp1∂kit edu

User Office

KNMF Profile

Bulk and Trace Analysis (BTA) of Nanomaterials

KNMF Laboratory for Microscopy and Spectroscopy

For the chemical characterization of the bulk material for micro and nano materials five different analytical instruments are operated for the KNMF by the analytical group of the Institute of Applied Materials - Applied Material Physics (IAM-AWP):

Download technology description (PDF)

Contact

Dr. Thomas Bergfeldt

Phone +49 721 608-22914
Fax +49 721 608-27715
Email thomas bergfeldtJds3∂kit edu
Institute for Applied Materials (IAM-AWP) - www.iam.kit.edu/awp/english

 

Equipment

X-Ray Fluorescence Spectrometry, XRF
(S4 Pioneer, Bruker-AXS) 

Specification

  • Sequential wavelength dispersive X-ray spectrometer
  • Detectable elements: (B) F to U in the concentration range from ppm to 100%
  • Non-destructive analysis for qualitative and semi-quantitative determinations
  • Sample forms like powder, solid, paste, film, liquid with size of 10 to 50000 μm
  • Precise quantitative determination of samples prepared in fused borate beads or with polished surface

Accessories

  • Grinding, pelletizing, fusion machines

Typical samples

  • Precise determination of main compounds like Si, Ti, Al and other minor elements in nano powders of SiO2, TiO2, Al2O3, glass, other nano oxides/carbides/nitrides

Figure 1

Fig. 1: S KA1. Analysis from a filter cake on a paper filter. Concentration range 0.01 – 3.0 mass %.

 

Atomic Emission Spectrometry by Inductively Coupled Plasma, ICP-AES
(OPTIMA 4300 DV, Perkin-Elmer)

Specification

  • Echelle grating optical system combined with prisms and two segmented charge coupled device (SCD) detectors enables simultaneous measurement of all elements except noble gas, halogens, hydrogen, oxygen and nitrogen
  • Element concentrations ranging from below 1 μg/g (depending on sensitivity) to 50% in solids and < 0.001 to 100 mg/L in liquids

Accessories

  • For solid samples all kind of dissolution techniques, i.e. microwave assisted digestion

Typical samples

  • Widely used, one of the most versatile methods of inorganic and organic analysis: liquids, electrolytes, dissolved solids of metals, oxides, nitrides, carbides

Figure 2

Fig. 2: Au with the ICP-OES by 242.795 nm. Chemical digestion from a mixture of Au and TiO2 NM with aqua regia. Concentration range 0.005 – 0.20 mg/l

 

Mass Spectrometry by Inductively Coupled Plasma, ICP-MS
(7500ce, Agilent)

Specification

  • Quadrupole mass spectrometer with off-axis Omega lenses and Octopole
  • Reaction System (ORS) to eliminate polyatomic interferences
  • Mass range: 6–260 amu, He–U
  • Ultra trace analysis ranging from below 1 ng/g (depending on sensitivity) to 1000 μg/g in solids and < 0.001 to 100 μg/L in liquids

Accessories

  • For ultra-trace analysis: sub boiling point distillation, laminar flow bench

Figure 3

Fig. 3: Consistent interference reduction in a variable, complex matrix using He mode. Comparison plots showing Std mode (no cell gas - red) and He mode (green) spike recovery data for 5 ppb Cr in a variable matrix (up to 1% each of HCl, H2, SO4 and Butanol). Potential interferences on 52 Cr include ArC, ClOH and SO.

 

Carrier Gas Heat Extraction, CGHE
(TC 600, LECO)

Specification

  • Simultaneous Nitrogen and Oxygen determination using IR and thermal conductivity by melting the sample in a graphite crucible in a metal bath at 2600°C with He as carrier gas
  • Analysis range: < 0.00001 to 50%

Typical samples

Solids: metals, inorganic materials like oxides, nitrides etc.

Figure 4

Fig. 4: Different kind of oxygen bonds in steel

 

Carbon-Sulfur-Analyzer
(CS 600, LECO)

Specification

  • Simultaneous Carbon and Sulfur determination by combustion in a high frequency furnace in oxygen flow using IR-detection of CO2 and SO2
  • Analysis range: < 0.0005 to 100%

Typical samples

  • Solids: metals, inorganic and organic materials

Figure 5

Fig. 5: C in WC