This technique is routinely used to determine the structure, orientation, lattice parameters and crystalline quality in crystalline materials (X-ray diffraction), and the thickness, density and roughness of thin films and multilayers (X-ray reflectivity). Two instruments are available at the LMA to perform these measurements.

Bruker’s D8 Advance diffractometer, with a configuration optimized for high-resolution X-ray diffraction (HR-XRD) and X-ray reflectivity (XRR) studies on thin films and nanostructured superlattices.

The PANalytical Empyrean diffractometer is a multi-platform diffractometer offering a wide range of diffraction geometries: reflection, transmission, capillary diffraction, Debye-Scherrer, grazing incidence diffraction (GIXRD), low angle and medium angle scattering (SAXS/WAXS). By combining the different optics and platforms available, it is capable of analyzing samples as diverse as powder samples, solid objects, dispersions or thin films. Also available as an accessory is an Anton Paar HTK 1200N high-temperature chamber designed for X-ray powder diffraction studies from room temperature up to 1200 ºC.

 More information: LMA 

SpINS is the acronym for Spanish Initiatives on Neutron Scattering. This name is intended to group together the different initiatives carried out in recent years by the Spanish administration to promote and encourage the use of neutron scattering techniques in the national scientific community.

 Contact person: Javier Campo (jcampo@unizar.es)

 More information: https://spins.unizar.es/

CEQMA’s Nuclear Magnetic Resonance service offers a set of non-destructive techniques that provide information about the structure and stereochemistry of organic compounds, organometallic compounds and biomolecules. Specifically, thanks to these techniques it is possible to perform:
– Structural characterization of small molecules, macromolecules and solids.
– Analysis of mixtures, quantification and identification of components.
– Study of chemical reaction mechanisms, characterization of reaction intermediates, obtaining kinetic and thermodynamic parameters of reactions.
– Study of molecular interactions, host-guest affinity, enzyme-substrate molecular recognition.

 More information: Servicios científicos del CEQMA

This facility allows the measurement of the longitudinal (T1) and transverse (T2) relaxation times of protons in an aqueous sample, by direct measurement of the time evolution of the respective components of their magnetic moment during the relaxation process following the application of a train of radiofrequency pulses. From the measurement of T1 and T2 the longitudinal (r1) and transverse (r2) relaxivity are determined, which are the parameters that characterize the effectiveness of the contrast agents used to improve the quality of the images obtained by nuclear magnetic resonance (MRI). Therefore, the main utility of the equipment is the in vitro characterization of magnetic nanoparticle suspensions as potential contrast agents for MRI. This avoids the use of MRI equipment for clinical use for patients or small animals, which is more complex and generally less available and more expensive to operate. In some cases qualitative information can also be obtained indirectly about the core-shell nanoparticle coating (e.g. existence of a hydration layer etc.).

The equipment is a Bruker Minispec mq60 (Figure 1), operating in a magnetic field of 1.5 T (like a large number of MRI equipment used in the clinic), which means working at a frequency of 60 MHz; the working temperature is 37 C (similar to human body temperature). Figure 2 shows a very simplified scheme of the same, except that in the Minispec mq60 the magnetic field is created by a permanent magnet, being a bench-top equipment. The measurement of relaxation times is fully automated, using for proton excitation pulse sequences pre-programmed in the Minispec mq60.

Contact person: Clara Marquina (clara@unizar.es)

Electron paramagnetic resonance (EPR) is the technique of choice for the characterization of paramagnetic systems. It allows describing the electronic structure of open-shell systems, paramagnetic rare earth ions and transition metals. It also provides information on the symmetry of paramagnetic compounds, which makes it a very useful structural technique in the fields of catalysis, magnetism or functional materials, among others. It can also be applied to the detection of short-lived transient chemical species through the use of spin traps, and allows characterization of the structure and dynamics of diamagnetic systems through the incorporation of spin labels.

The possibility of performing pulsed EPR experiments (currently the only laboratory with this capability in Spain) allows the fine structural characterization of paramagnetic systems through the detection of weak hyperfine interactions. Furthermore, it is the appropriate technique for the characterization and manipulation of electron spin qubits and other quantum systems.

Contact person: Jesús Ignacio Martínez Martínez (jimartin@unizar.es)

The mission of the elemental analysis service is to determine the percentage composition of carbon (C), hydrogen (H), nitrogen (N) and sulfur (S), simultaneously, of a sample or compound in solid or liquid state.

The analysis technique is based on the complete combustion of the same, under optimum conditions (1000-1300 ºC, pure O₂ atmosphere) to convert the elements to be determined (C, H, N and S) into CO₂, H₂O, N₂ and SO₂ respectively. These gases, after being separated by frontal chromatography, are detected, quantified and processed taking into account the weight of the sample itself and the data of a standard sample (used as a calibrator), thus obtaining the percentage content of each element in the sample.

 More information: Servicios científicos del CEQMA

The Chemical Analysis Service of the SAI offers the university community, other research centers and companies facilities equipped with the most modern spectrometric techniques, which allow the determination of majority, minority, trace and ultra-trace elements in samples from any scientific-technological area.

The existing infrastructure in the laboratory allows to carry out both semi-quantitative and quantitative determinations, with the following analytical techniques:
– Atomic Emission Spectrometry with Inductively Coupled Plasma (ICP-OES).
– Mass Spectrometry with Inductively Coupled Plasma (ICP MS)

 More information: SAI

The Agilent 4100 Microwave Plasma Atomic Emission Spectrometer (MP-AES) is a technique for multi-element determination by atomic emission. It uses an N2 plasma that is generated with microwaves. Detection limits can be up to 1ppm depending on the element and typically 10ppm for all elements.

Persona de contacto: Reyes Mallada (rmallada@unizar.es)

The equipment available to the CEQMA Mass Spectrometry Service allows obtaining information on the molecular mass of the compound analyzed as well as structural information. The service offers a set of techniques that allow qualitative and quantitative analysis of pure substances and complex mixtures.

 More information: Servicios científicos del CEQMA