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Radiochemical analysis

Radioanalitik
Fig. 1: ionising radiation

At INE a wide experience in chemical and radiochemical analytical methods is available. The main tasks of the INE analytical group are:

-     Chemical and radiochemical analysis for INE R&D work
-     Chemical analysis for waste conditioning and dismantling of nuclear facilities
-     Chemical analysis for vitrification processes of high active waste
-     Analytical services
 

A main task of the analytical group is routine analysis for INE R&D work including development and optimization of speciation methods. Members of the analytical group supervise practical student courses and the education of chemical laboratory technicians.

At INE samples from waste conditioning facilities (e.g., digested ash samples, evaporator concentrates from KTE) or from dismantling of nuclear facilities are analyzed. Important nuclides are 55Fe, 63Ni, 90Sr as well as U and Pu isotopes (including quantitative analysis and determination of isotope ratios).

Analytical services for companies are provided in several fields: radio pharmaceutical products containing alpha emitting nuclides (needed in tumor therapy) are analyzed as well as resins for radiochemical separations. Both examples serve for the product quality control.

 
Nuclear chemical methods:
 

-     radiochemical separations

-     α-spectrometry

-     liquid scintillation spectrometry (standard and low-level)

-     γ-spectrometry
 

For the analysis of radioactive samples see also elemental analysis and other methods.

 

 

Contact:

Marcus Plaschke     

    +49 721 608 24747


Elemental Analysis

Sec4_2_fig1
Fig. 1: Box-adapted Thermo Element XR sector field ICP-MS
Boxenadaptierte Thermo Element XR Sektorfeld ICP-MS
Fig. 2: Box-adapted Thermo Element XR sector field ICP-MS

At INE a wide experience in chemical and radiochemical analytical methods is available. For the main tasks of the INE analytical group see radiochemical analysis.

New ways in element and isotope analysis for actinide speciation by high resolution sector field mass spectrometry adapted at a glove box

Element and isotope analysis by high resolution sector field mass spectroscopy (SF-ICP-MS, type Element XR) is now available at INE. Improved detection limits (down to the sub-ppq range) and high mass resolution allow for extremely precise determination of actinides or long-lived fission products at very low concentrations. This analytical tool is applied for the analysis of natural samples (e.g., groundwater or surface water) and ambitious lab experiments. By coupling of methods multi-dimensional analytical systems are developed. Coupling with laser ablation (LA-SF-ICP-MS) delivers information about the spatial distribution of actinides and fission products in solids (e.g., interaction of actinides with mineral phases acting as natural or geotechnical barriers). Advanced speciation methods are developed by coupling separation techniques with mass spectroscopy. As an example capillary electrophoresis coupled to sector field mass spectroscopy (CE-SF-ICP-MS) is developed to study actinide speciation at very low concentrations (10-11 bis 10-12 Mol/l).

 

Methods:

-     ICP-MS quadrupole (inactive and adapted at a glove box)

-     ICP-MS sector field (adapted at a glove box)                          

-     ICP-OES (inactive and adapted at a glove box)

-     Flame-AES/AAS (only non-radioactive samples)

-     WDXRF (only weak radioactive samples)                   

 

For the analysis of radioactive samples see also radiochemical analysis and other methods.

 

 

Contact:

Marcus Plaschke     

    +49 721 608 24747


Other methods

At INE a wide experience in chemical and radiochemical analytical methods is available. For the main tasks of the INE analytical group see radiochemical analysis.

 

Other methods:

-     ion chromatography (cations and anions, radioactive and inactive samples)

-     gas chromatography (only inactive samples)

-     organic and inorganic carbon (TOC, DOC, NPOC)

-     surface determination after BET (inactive)

-     column separations

-     digestions (conventional or microwave)

-     volumetric analysis

-     gravimetric analysis

 

For the analysis of radioactive samples see also radiochemical analysis and elemental analysis.

 

 

Ansprechpartner:

Marcus Plaschke     

    +49 721 608 24747


Hyphenated fractionation-based methods as tools for the actinide speciation in solution

AsFFFF
Fig. 1: Schematic view of the AsFlFFF principle: the colloids/nanoparticles are separated according to their size and eluted towards different detectors coupled on-line like UV-Vis., LLS, LIBD or ICP-MS.
CE
Fig. 2: CE coupled to SF(sectorfield)-ICP-MS (Element XR adapted at a glovebox).

Actinides speciation in solution is necessary to elucidate their environmental behaviour. Speciation information can be obtained by sample fractionation and subsequent sensitive detections. The coupling of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) with separation procedures like the Asymmetric Flow Field-Flow Fractionation (AsFlFFF) or the Capillary Electrophoresis (CE) allows sample fractionation and detection of a variety of elements at low concentrations relevant for environmental purposes.

AsFFFF offers the possibility to separate colloidal matter ranging from <1 nm up to 100 µm. Colloid size fractionation takes place in a thin ribbon-like flow channel by applying a cross flow perpendicular to the channel flow (Scheme 1). At INE, the AsFlFFF is coupled on-line with a UV-Visible spectrophotometer, a Laser Light Scattering (LLS) detector and a Laser-Induced Breakdown Detection system (LIBD) or an ICP-MS. The LIBD is characterized by its particularly high sensitivity while the coupling with ICP-MS allows to gain insight into the elemental composition of colloids and notably the elucidation of trace metal interactions with colloids. The results obtained provide semi quantitative view into the trace elements distribution in colloidal systems. This flexible colloid characterization method has already been applied successfully at INE to the examination of inorganic particles (e.g. clays, iron oxide/hydroxides), humic substances, hydrocolloids in general and synthetic nanoparticles like quantum dots.

CE-ICP-MS (Figure 2) use for actinide speciation at low concentration is a well established technique which does not disturb the redox species ratio during the measurement. It has been recently applied at INE (picture) to study the Pu(IV) hydrolysis, the redox speciation of arsenic (As(III)/(V)) and selenium (Se(IV)/(VI)) and to the separation of uranium species (U(IV)/(VI)).

Complementary informations are obtained by using additional spectroscopic (EXAFS, TRLFS) or imaging (AFM, SEM, TEM, STXM) techniques.

 

 

Contact:

Muriel Bouby    

   +49 721 608 24939


x-ray diffraction

Diffractometer D8
Diffraktometer D8 Brucker

X-ray diffraction (XRD) is a non-destructive analytical technique used to identify and characterize solid samples. Information on the crystallographic structure can be obtained without complex sample preparation and with low amount of sample. For any given crystalline material, both the position and the intensity of the lines on the diffractogram are indicative of a particular phase (“fingerprint”). Quantitative information on a sample can be obtained by applying a full pattern analysis technique, such as the Rietveld method for example.

Powder X-ray diffractograms are collected in reflection mode using a D8 ADVANCE (Bruker) diffractometer located in the controlled area of INE. X-rays are produced from a Cu anode and the intensity of the scattered radiation is detected with an energy dispersive detector (SOL-X). The sample stage concept allows analyses of powders, oriented or textured samples (such as sheet silicates), air-sensitive and/or active samples (closed and airtight sample holder).

Information provided by XRD is of key importance in various areas of the research activities at INE. Besides determining the mineralogical composition of natural samples, XRD is used to characterize samples after corrosion experiments (nuclear waste glass, cement waste form…), the purity of synthetic samples from (co)precipitation experiments (retention of radionuclides in solid phases, identification of precipitates).

 

 

Contact:

Nicolas Finck     

   +49 721 608 24321