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Mineralogy & Geochemistry Laboratories Structural analysis Xpert Pro

Diffractometer X'Pert Pro diffractometer (Malvern-Panalytical)

Goniometer mit Basisausstattung © AG MinGeO

Goniometer mit Basisausstattung © AG MinGeO

  • Tube: Cu ceramic tube (2.2kW), line and point focus Sample changer: 15x sample changer
  • Angular resolution: 0.001°2Theta (at 240mm goniometer radius) Detector: X’Celerator RTMS detector, Proportional detector Measurement settings: 45KV, 40mA
  • Sample holder: – Sample spinner (powder samples, rotation, reflection mode) – Sample holder for narrow solid samples (reflection mode)
  • Capillary (powder or wet samples, rotation, transmission mode) – Heating chamber HTK16 Anton Paar GmbH (RT-1600°C, air/inert gas)

  • Qualitative analysis of crystalline phase mixtures (cement, secondary raw materials)
  • Qualitative analysis of very small quantities (approx. 1 mg)
  • Quantitative phase analysis using the Rietveld method (cement (CEM I), composite cements (CEM II) and determination of the amorphous content)
  • Investigation of the hydration kinetics of cement pastes at variable temperatures using capillary film preparations and prim. Multilayer mirror
  • Qualitative analysis of pure phases:
  • Determination of metric parameters
  • Characterisation / determination of metric parameters at variable relative humidities and temperatures (LDH, AFt (ettringite structures), AFm (calcium aluminate hydrate) phases)
  • Structure refinement using the Rietveld method, also in combination with synchrotron or neutron diffraction data

Transmission geometry Transmission measurements with films 

By using different PreFix modules, the X'Pert diffractometer can be easily changed from reflection geometry to transmission geometry.
‍Sample carriers ‍with ‍reflectance-free ‍Kapton foil ‍from ‍PANalytical ‍are available for ‍transmittance measurement ‍. ‍The ‍sample material ‍can be ‍supplied as ‍suspension ‍or ‍dry ‍powder ‍between ‍two ‍Folien ‍eingespannt ‍werden. ‍This ‍prevents ‍exchange ‍with ‍the ‍atmosphere ‍. ‍By ‍preparation ‍in ‍an ‍artificial ‍atmosphere ‍(N2, Ar) ‍a ‍XRD measurement can ‍be made ‍bei ‍konstanten ‍Bedingungen ‍unter ‍Ausschluss ‍von‍O2 ‍oder‍CO2 ‍und ‍bei ‍konstanter ‍Luftfeuchtigkeit ‍erfolgen.

Transmission_Foil

Goniometer in Transmissionsgeometrie

Transmissionsprobenträger mit Mylar-Folie

  • Investigations on the hydration kinetics of cement pastes of latent hydraulic and pozzolanic reactions
  • Transmission measurements on organic metal sulphonate hydrates and metal carboxylates
  • Measurement ‍of ‍moist ‍or ‍reactive ‍samples ‍by means of ‍transmission ‍or ‍reflection
  • ‍ ‍‍‍Prevention ‍of: ‍hydration/dehydration reactions, ‍carbonation reactions, ‍oxidation

Transmission - focussing mirror Capillary spinner with variable rotation speed and focussing mirror for Cu radiation 

The combination of focusing mirrors with capillary spinners opens up the possibility of analysing rotating capillary tubes using high-energy (focusing) and parallelised X-rays.

  • X’Pert ‍Pro ‍Theta ‍- ‍PreFix ‍- ‍Module ‍Capillary spinner ‍in ‍combination ‍with ‍focussing ‍mirrors
  • ‍ ‍‍Präzise ‍Measurements of ‍smaller ‍sample quantities, ‍which ‍are due to ‍the ‍influence ‍of the ‍ambient atmosphere ‍verändert ‍oder ‍zerstört ‍werden
  • ‍ ‍‍Durch ‍die ‍Rotation ‍of the ‍sample ‍more ‍crystals ‍(mesh planes) ‍are brought into ‍reflection ‍position, ‍so ‍dass ‍die ‍Partikelstatistik ‍verbessert ‍wird.
  • ‍ ‍‍Textureffekte ‍are ‍except ‍for ‍minerals ‍with ‍stalked ‍habitus ‍significantly ‍reduced.

Hydration sample carrier Hydration sample carrier Dr Ecker GmbH 

The ‍cement paste ‍is filled ‍into ‍metal sample holders ‍and ‍tensioned ‍through ‍die ‍a ‍Capton foil ‍(polyimide) ‍über ‍die ‍Probenoberfläche ‍mittels ‍zweier ‍Kunstoffringe ‍abgedichtet. ‍The ‍reaction temperature ‍is kept ‍constant ‍by ‍setting ‍der ambient temperature ‍in ‍der ‍device software ‍. ‍Heat developments, ‍which ‍durch ‍exothermic ‍processes ‍in ‍der ‍probe ‍are created, ‍werden ‍durch ‍an ‍automatic ‍adjustment ‍der ‍control unit ‍abgeführt ‍und ‍können ‍aus ‍der ‍Leistungskurve ‍(blue ‍Kurve) ‍in ‍der ‍Software ‍"Maetre ‍3.1" ‍bestimmt ‍werden. ‍The ‍measurement parameters ‍for ‍the ‍kinetic ‍phase analysis ‍are ‍set ‍in ‍the ‍control software ‍des ‍Diffraktometers ‍eingestellt.

  • ‍‍Studies ‍on the ‍hydration kinetics ‍of ‍cement pastes ‍latent hydraulic ‍and ‍puzzolanic ‍reactions
  • ‍Quantification ‍der ‍Phase development ‍( ‍crystalline ‍und ‍amorphous ‍components) ‍in ‍dependence ‍der ‍reaction time ‍und ‍temperature ‍mittels ‍der ‍Rietveldmethode

  • ‍ ‍‍Application range: ‍10 ‍- ‍50°C
  • ‍ ‍‍Temperature stability: ‍approx. ‍0, ‍2°C

Dome sample carrier Dome sample carrier 

The dome sample carrier is a closed sample carrier for powder and wet samples and can be used in combination with a PANalytical Empyrean, X'Pert Pro or X'Pert Powder X-ray diffractometer. The sample carrier can be sealed with a plastic dome to prevent exchange with the atmosphere. By preparing the sample in an artificial atmosphere (), an XRD measurement can be carried out under constant conditions, excluding or and at constant humidity.

  • Measurement of moist or reactive samples under specific atmosphere (N2, Ar)
  • Prevention of: Hydration/dehydration reactions, carbonation reactions, oxidation

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