The X-ray Diffraction Service of the ICTJA-CSIC is an analytical facility focused on the qualitative and quantitative characterization of the crystalline phases of materials. The XRD Service, with more than 30 years of experience in the field, offers support to ICTJA researchers and also to external users from public and private universities and companies.
One of the main objectives of the XRD Service at ICTJA is to support the ongoing investigations carried out by ICTJA researchers on Earth Sciences topics, including studies of volcanology, petrology and sedimentology. The XRD Service offers also support to external researchers working in geology, materials science, environment, chemistry, pharmacy, archaeology, etc. A large number of companies and organizations from the public or private sectors make use of the XRD Service at ICTJA-CSIC for their industrial applications, quality control, environmental studies, forensics, etc.
Samples and service request
For XRD measurements, powdered samples with particle size lower than 60 microns are required (sizes around 5 microns are optimal). Samples can be grinded at ICTJA-CSIC. The minimum amount of material that can be analysed by XRD is determined by the size of the sample holders (the approximate sample volume that we require is similar to that of a two-euro coin). Clay analysis and identification are also routinely carried out. Besides the X-ray measurement of the powdered sample, the clay analyses include i) X-ray measurement of the oriented aggregate; ii) X-ray measurement of the ethylene glycol solvated sample; iii) X-ray pattern of the sample heated at 550 °C.
- Bruker-AXS D5005: it is set up in Bragg-Brentano geometry (theta-2theta), with a Cu X-ray tube of up to 2.2 kW (with point/line focus). Detection is performed with a scintillation detector (linear up to 2 million cps). This diffractometer is equipped with a secondary monochromator and Soller slits, and it has an automatic sample loader for up to 40 samples.
- Bruker-AXS D8-A25 Advance: this state-of-the-art diffractometer can work in Bragg-Brentano geometry (theta-theta) or in parallel optics geometry (Göbel mirror). It is equipped with a Cu X-ray tube of up to 3 kW with point/line focus, large diameter goniometer (560 mm), and ultra-fast PSD detector (0D and 1D modes). It has an automatic sample loader for 30 samples. Micro-diffraction measurements can be performed by using appropriate pin-holes and a XYZ sample stage. Project CSIC10-4E-141 co-funded by the European Regional Development Fund (ERDF).
- DIFFRACplus Evaluation Package (together with the PDF-2 and COD databases): for phase identification and semi-quantitative analyses
- TOPAS v4.2: for quantitative and structural Rietveld analyses
- Particle size analyses by means of a MALVERN Mastersizer 2000 laser diffraction system are also offered. The particle size distribution of a sample (dry or in aqueous solution) can be determined within the 0.1 - 1000 µm range.
- We also offer the possibility to perform elemental analyses in situ by X-ray fluorescence spectrometry using a Bruker Tracer-IV Geo handheld spectrometer. This equippment is ideally suited for field work, cultural heritage materials and industrial applications.
- Identification of crystalline phases
- Crystal-quality assessment, composition determination and microstructural analyses
- Semi-quantitative and quantitative analysis of crystalline phases and amorphous content
- Application of the Rietveld method for profile adjustment, structure refinement and quantitative phase analyses
- Investigation of small or inhomogeneous samples with micro-diffraction
- Determination of crystalline structures
- Phase identification and quantification of geological samples. Identification and analysis of clay minerals
- Analysis of mineral phases in building materials: cement, concrete, aggregates, etc.
- Study of degraded calcium aluminate cements, identification of fibre cements, etc.
- Determination of the amorphous content in ashes and synthetic mixtures
- Study of corrosion products
- Determination of crystalline silica in respirable airborne dusts by direct-on-filter methods