technician working in a glovebox


Wet chemical element analysis and spectrometry

Our working group support material research by methods of bulk and species analysis especially to lithium battery research, titanium based alloys for biotechnical applications, metallic glasses, steel and magnetic materials. Common tasks are quality controls of precursors, semi-finished materials and the final products.
We have special experiences and technical possibilities in

  • digestion methods
  • semi-quantitative survey analysis of traces up to major components
  • quantitative analysis of major, minor and trace elements
  • high-precision analysis of main components
  • trace element analysis
  • layer analysis

Methods

ICP OES - Inductively Coupled Plasma with Optical Emission Spectrometry

Principle:
The analyte solution is sprayed as an aerosol into an argon plasma. At temperatures of 6500 K the elements are atomized and/or ionized. The temperature is high enough to excite atoms and ions electronically so that they emit light. The resulting spectrum consisting of many emission lines is split up by an Echelle optics. The intensity of the emission lines is proportional to the concentration of the analyte.

Application:Simultaneous determination of main, minor and trace elements
Determination limit:0,01 - 1 µg/L  (depends on element)
Accuracy:0,2 - 1 % relative standard deviation
Instruments:iCAP6500 DUO (Thermo Fisher Scientific GmbH), ARCOS II MV (SPECTRO Analytical Instruments GmbH)

 

Titrimetry

Principle:
In a titrimetry increments of a reagent solution -the titrant- are added to the analyte until their reaction is completed. From the quantity of titrant required, the quantity of analyte in the unknown sample can be calculated. The  requirements for a titrimetry reaction are to have a large constant equilibrium and to proceed rapidly. The most common titrations are based on acid-base, oxidation-reduction, complex formation or precipitation reactions. The equivalence point occurs when the quantity of added titrant comes  to the exact amount necessary for stoichiometric reaction with the analyte. Actually measured is the end point, which is marked by a sudden change of a physical property, e.g. the electrochemical potential, conductivity, pH, the color of an indicator (spectrophotometric titrimetry) etc. Determination of fluoride is possible.

Application:Precise main component analysis of metals (except alkali metals), precise determination of stoichiometries and oxidation numbers, determination of concentrations of acids and alkali.
Determination limit:about 0.5 mg
Accuracy:about 0.1 - 1 %
Instruments:Automatic titration system DL 77 (Mettler Toledo) with several electrodes and phototrodes

UV/VIS-Spectrophotometry

Principle:
The analyte forms a colored complex by a reaction with an organic agent . The light absorption of the colored solution is measured  at a certain wavelength in the visible or UV spectral range. The absorption is proportional to the concentration of the analyte.
Intermolecular interactions can be detected between 200 and 1100 nm. Ulbricht sphere is available.

Application:Wide application range from main and minor component analysis and also trace analysis of numerous transition metals, e.g. Fe, Co, Ni, Ti, e.g. Determination of Fe in numerous alloys e.g. hard magnetic alloys (Fe-Nd-B based) and soft magnetic alloys (Fe-Si-B), in steel, and numerous intermetallic compounds, molecul spectroscopy (investigation of bondings and interactions)
Determination limit:between 5 and 50 µg/g
Accuracy:about 0.5 - 2 %
Instruments:UV-VIS spectrophotometer Specord 250 (Analytik Jena AG)

Contact

Andrea Voss
Room B2E.15
Phone: +49 351 4659 708
E-mail: a.voss(at)ifw-dresden.de

Anne Voidel
Room B2E.18
Phone: +49 351 4659 704
E-mail: a.voidel(at)ifw-dresden.de