Go to IR-35 Go to Laboratorios Convencionales
Radioactive laboratories IR-30: Laboratories to manipulate long life radionuclides, which include two associated radioactive facilities.
IR- 30-(S1.26) Experimental lab.
It is a laboratory equipped and authorized for running experiments with a large variety of radioisotopes. Solubility, oxidation and leaching tests can be carried out at a long-term scale in final geological conditions, fabrication of new model systems based in different solid matrix and studies for the improvement or development of nuclear fuel reprocessing processes, such as studies of radionuclide complexation, liquid–liquid extraction, mass transference and stability to hydrolysis and radiolysis.
This laboratory is equipped with: 3 anoxic gloveboxes (Ar atmosphere for tests under controlled atmospheric conditions), 5 fume-hood, uniaxial press (25Tn), furnace (1700°C); mixer mill, polisher and metallographic surface preparation, ultracentrifugation, titrators, viscometer, colorimetry & chemiluminescence, electrodeposition for alpha samples analysis, UV-Vis spectroscopy, climatic chamber, thermal treatments, etc.
IR- 30-(S1.21) Analysis lab
This laboratory is equipped for the qualitative and quantitative analysis of the composition of aqueous and organics samples by ICP-MS, HPLC-MS, beta-gamma and alpha spectrometry.
Supervisors of the Radioactive Facilities IR30/IR35:
Gamma and alpha spectrometry
At the HLWU, we generally evaluate the variation in the extraction capacity of a metal (or family of metals) between two phases, an aqueous and an organic one, throughout different separation processes and under conditions of extreme acidity and radiation. For this, it is necessary to evaluate how much metal passes from one phase to another by varying these conditions. The concentration of each of the isotopes is determined in the organic and aqueous phases using different techniques depending on the characteristics of the element/radionuclide/isotope in question.
In the IR-30 facility (Building 12 S1. d21) of CIEMAT (Madrid, Spain) we have two GeHP semiconductor detectors with 20% intrinsic efficiency, associated with an electronic chain and a DSA-1000 multichannel analyzer (AMC) (Canberra Industries Inc., Meriden, USA). Spectral analyzes are performed with Genie-2000 software (Canberra Industries Inc., Meriden, USA). For example, the determination of the concentration of 241Am and 152Eu in organic and aqueous solutions is carried out, using their characteristic energies of 59.5 keV (35.9%) and 122 keV (28.4%), respectively. Calibrations in energies and efficiencies were performed using the QCY-48 gamma emitter cocktail (Amersham, U.K.). The elements we usually work with are (mainly 241Am and 152Eu, and rarely 238Pu, 237Np, 233-235U, 230-232Th). The activity concentration of certain isotopes, such as 238U, is determined by gamma spectrometry from the analysis of the gamma emissions of their descendants. Although gamma spectrometry is not the best technique for uranium quantification (as ICP-MS is), it does allow us a good estimate to be made in a very short time, in addition to not being a destructive technique.
We also have a Canberra Alpha Analyst unit with four independent alpha emitter measurement chambers, each with a PIPS-type semiconductor detector inside. These detectors are of the A450-18AM model, with an active surface of 450 mm2 and a certified energy resolution of 18 keV for the 5486 keV emission of 241Am. The energy calibration is carried out using a standard source of 233U, 239Pu and 241Am. And the methodology normally used, given the concentration of activity present in our samples, is the deposition of the sample (after radiochemical separation) on the plate and/or evaporation under an IR lamp. This technique allows us to determine the concentration of 241Am 244Cm, 233-235U and, eventually, 237Np, 239Pu, among others.
Technicians:
HPLC-MS
In the IR-30 facility (Edificio 12 S1. d21) of the CIEMAT (Madrid, Spain) we have a Bruker LCMS Triple Quadrupole EVOQ QUBE unit with HPLC Advance. This equipment can be divided into three well-differentiated modules, which are the Bruker Advance high-performance liquid chromatography (HPLC) system, the Bruker PAL-xt robotic automatic injector, and finally the Bruker EVOQ QUBE triple quadrupole detector.
Liquid chromatography (LC) combined with mass spectroscopy (MS) is an analytical technique that allows us the qualitative and quantitative analysis of different organic compounds with which we have been working for years within the line of separation of radionuclides from nuclear fuel.
Technicians:
ICP-MS
In the IR-30 facility (Edificio 12 S1. d21) of the CIEMAT (Madrid, Spain) we have a mass spectrometer with an induced coupling plasma source (ICP-MS) (Thermo Scientific ™ iCAP ™ Q ICP-MS), with Collision Cell Mode (CCT). And a nitric acid purifier for sample preparation (Milestone Sub-DuoPUR).
Conventional radiochemical methods at low concentration levels require careful chemical separation of the analyte to achieve low detection limits and this is often time consuming. The development of analytical methods for the determination of long-lived radionuclides at ultratrace concentration levels in radioactive samples focuses on reducing sample volume and improving detection limits, precision and accuracy of measurements.
The main advantages of this technique lie in its high precision, low detection limits and low economic cost, analyzing most of the elements and isotopes present in the periodic table simultaneously in no more than a couple of minutes. It is therefore, an ideal technique for analyzing water, rock and mineral leachates, etc. And there are numerous examples where the precise and accurate determination of the isotopic ratios of long-lived radionuclides is required in the characterization of nuclear materials, for which the ICP technique is valid. For example, in the characterization of radioactive waste it is necessary especially with regard to long-lived transuranids (237Np , 239Pu, 240Pu, 242Pu, 241Am, 243Am) and fission and activation products (79Se, 93Zr, 99Tc, 107Pd, 126Sn, 129I and 135Cs).
Technician:
Uranium purification
To date, the unit had a large number of uranium samples from a wide variety of sources that were stored in the IR30 to be treated as waste. A large part of these samples come from different pellet preparation processes and are made up of different residual particles generated as friction wear between the materials used, as well as different dopants and the uranium oxide itself. Taking into account the experience in the HLWUin the separation processes, it was proposed to purify the uranium from the other impurities that may exist.
A search for uranium purification methods was carried out through hydrometallurgical separation processes and the one that showed a higher extraction yield, a lower generation of final residues and lower cost was achieved when the liquid-liquid extraction technique was used using the extracting agent TBP (Tributylphosphate). In recent years, more than 100 grams of uranium have been purified, which in previous years would have been considered waste.
Technicians:
Autoclaves
At the IR-30 facility (Building12 S1. d21) of CIEMAT (Madrid, Spain) we have an autoclave system for carrying out different experiments simulating storage conditions for irradiated fuel, both temporary (dry) and final (wet) storage. ). The autoclaves consist of tubular stainless steel reactors that are coupled to an aluminum isothermal block, which is connected to a temperature controller to establish the experimental conditions. Each autoclave has two auxiliary tubes for gas inlet and outlet, so the atmosphere inside each reactor is controlled according to the needs of the experiment.
Technicians:
