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Cleaning is one of the most important, essential, and delicate operation which has to be handled by conservators before applying new materials to any substrates. In past decades, nanotechnology introduced new concepts and materials in the conservation field, which have been providing many advantageous performances, especially higher than older materials. As a result, the conservators have already started to use nanomaterials in the cleaning processes of artifacts. Taking into consideration this new approach, our study has focused on using nano-structured emulsions (NSE) as smart cleaning materials for removing polymer coatings (e.g., acrylic polymers). For this purpose, Paraloid B-72 was applied on three different substrates (glass, Lecce stone, and Arenaria stone) and cleaning was performed by a specific nano-structured emulsion (NSE) based on an eco-friendly surfactant (EcoSurf) and two organic solvents in different proportions. In order to better understand the interaction of surfactant and organic solvents with polymer coating, plain EcoSurf in water was also used for comparison. In this study, the decay process of the considered polymer was also deeply studied, because it directly affects the cleaning effectiveness. Coated specimens of the different substrates were artificially aged and examined by different techniques: chromatic variations and contact angle measurements, optical microscopy, FTIR, and SEM-EDS. This material characterization process is important to understand the colour, morphology, and micro-structural difference, and the changes of hydrophobic behaviour as well as chemical composition of Paraloid B-72 polymer due to different ageing processes. After that, substrates coated with both unaged and aged polymer were cleaned by NSE according to the direct-contact procedure and cellulose pulp method. Preliminary analyses suggested that the direct-contact cleaning performed by nano-emulsion (i.e., NSE) induced a complete removal of the acrylic polymer, despite that this method is not recommended for the artifacts and can be hardly applicable in real cases. On the other hand, experimental results showed that satisfactory cleaning of stone substrates can be obtained by using NSE/the cellulose pulp system.

The conversion-alloying compounds have been identified as promising anode materials for sodium ion batteries (SIBs). One of them, SnO2, with an enormous theoretical capacity of 1558 mAh g−1 is an interesting candidate, also due to its low cost, environmental friendliness and wide availability of tin. However, many drawbacks limit its application in commercial batteries. In this paper, SnO2 has been synthesized from cheap reagents by using simple and easily scalable coprecipitation synthesis routes obtaining nanoparticles with sizes between 2 and 14 nm with almost spherical morphologies. The reasons of the failure of the alloying/de-alloying process were investigated by combining the results obtained from common electrochemical techniques, providing useful examples for the investigation of every material with analogous electrochemical features. Thanks to cyclic voltammetry, different reaction paths were detected for the two samples. The first cycle irreversibility was well characterized with electrochemical impedance spectroscopy, showing interesting trends in the values of the resistance. Galvanostatic cycling with potential limitations was employed to quantify the irreversibility, finding out that the most crystalline sample reached the terminal phase in the Sn-Na system (Na15Sn4), while the least crystalline sample could not achieve such a result (Na3Sn). The crystallinity of SnO2 was determined to be a key parameter, often neglected, for the realization of satisfactory anode compounds.

Low-cost and simple methods are constantly chased in order to produce less expensive lithium-ion batteries (LIBs) while possibly increasing the energy and power density as well as the volumetric capacity in order to boost a rapid decarbonization of the transport sector. Li alloys and tin-carbon composites are promising candidates as anode materials for LIBs both in terms of capacity and cycle life. In the present paper, electrospinning was employed in the preparation of Sn/SnOx@C composites, where tin and tin oxides were homogeneously dispersed in a carbonaceous matrix of carbon nanofibers. The resulting self-standing and light electrode showed a greatly enhanced performance compared to a conventional electrode based on the same starting materials that are simply mixed to obtain a slurry then deposited on a Cu foil. Fast kinetics were achieved with more than 90% of the reaction that resulted being surface-controlled, and stable capacities of about 300 mAh/g over 500 cycles were obtained at a current density of 0.5 A/g.

Background: Macroaggregated human serum albumin (MAA) properties are widely used in nuclear medicine, labelled with 99mTc. The aim of this study is to improve the knowledge about the morphology, size, dimension and physical–chemical characteristics of MAA and their bond with 99mTc and 68Ga. Methods: Commercial kits of MAA (Pulmocis®) were used. Characterisation through experiments based on SEM, DLS and Stokes’ Law were carried out. In vitro experiments for Langmuir isotherms and pH studies on radiolabelling were performed and the stability of the radiometal complex was verified through competition reactions. Results: The study settles the MAA dimension within the range 43–51 μm. The Langmuir isotherm reveals for [99mTc]MAA: Bmax (46.32), h (2.36); for [68Ga]MAA: Bmax (44.54), h (0.893). Dual labelling reveals that MAA does not discriminate different radioisotopes. Experiments on pH placed the optimal pH for labelling with 99mTc at 6. Conclusion: Radiolabelling of MAA is possible with high efficiency. The nondiscriminatory MAA bonds make this drug suitable for radiolabelling with different radioisotopes or for dual labelling. This finding illustrates the need to continue investigating MAA chemical and physical characteristics to allow for secure labelling with different isotopes.

The present work is a concrete example of how physico-chemical studies, if performed in depth, are crucial to understand the behavior of pharmaceutical solids and constitute a solid basis for the control of the reproducibility of the industrial batches. In particular, a deep study of the thermal behavior of glipizide, a hypoglycemic drug, was carried out with the aim of clarifying whether the recognition of its polymorphic forms can really be done on the basis of the endothermic peak that the literature studies attribute to the melting of the compound. A number of analytical techniques were used: thermal techniques (DSC, TGA), X-ray powder diffraction (XRPD), FT-IR spectroscopy and scanning electron microscopy (SEM). Great attention was paid to the experimental design and to the interpretation of the combined results obtained by all these techniques. We proved that the attribution of the endothermic peak shown by glipizide to its melting was actually wrong. The DSC peak is no doubt triggered by a decomposition process that involves gas evolution (cyclohexanamine and carbon dioxide) and formation of 5-methyl-N-[2-(4-sulphamoylphenyl) ethyl] pyrazine-2-carboxamide, which remains as decomposition residue. Thermal treatments properly designed and the combined use of DSC with FT-IR and XRPD led to identifying a new polymorphic form of 5-methyl-N-[2-(4-sulphamoylphenyl) ethyl] pyrazine-2-carboxamide, which is obtained by crystallization from the melt. Hence, our results put into evidence that the check of the polymorphic form of glipizide cannot be based on the temperature values of the DSC peak, since such a peak is due to a decomposition process whose Tonset value is strongly affected by the particle size. Kinetic studies of the decomposition process show the high stability of solid glipizide at room temperature.

The addition of transition metals to alkali intercalated fullerides proved to enhance their already good hydrogen absorption properties. Herein we present a study based on two different synthetic strategies, allowing the addition of nickel as aggregates with different size to the lithium fulleride Li6C60: the former is based on the metathesis of nickel chloride, while the latter on the thermal decomposition of nickel carbonyl clusters. The hydrogen-storage properties of the obtained materials have been investigated with manometric and calorimetric measurements, which indicated a clear enhancement of the final absorption value and kinetics with respect to pristine Li6C60, as a consequence of nickel surface catalytic activity towards hydrogen molecules dissociation. We found up to 10 % increase of the total H2 weight % absorbed (5.5 wt% H2) in presence of Ni aggregates. Furthermore, the control of the transition metal particles size distribution allowed reducing the hydrogen desorption enthalpy of the systems.

The use of peptides in paper-based analytics is a highly appealing field, yet it suffers from severe limitations. This is mostly due to the loss of effective target recognition properties of this relatively small bioprobes upon nonspecific adsorption onto cellulose substrates. Here, we address this issue by introducing a simple polymer-based strategy to obtain clickable cellulosic surfaces, that we exploited for the chemoselective bioconjugation of peptide bioprobes. Our method largely outperformed standard adsorption-based immobilization strategy in a challenging, real-case immunoassay, namely the diagnostic discrimination of Zika+ individuals from healthy controls. Of note, the clickable polymeric coating not only allows efficient peptides bioconjugation, but it provides favorable anti-fouling properties to the cellulosic support. We envisage our strategy to broaden the repertoire of cellulosic materials manipulation and promote a renewed interest in peptide-based paper bioassays.

Several different milling parameters (additive content, rotation velocity, ball-to-powder ratio, degree of filling, and time) affect the hydrogen absorption and desorption properties of a reactive hydride composite (RHC). In this paper, these effects were thoroughly tested and analyzed. The milling process investigated in such detail was performed on the 2LiH-MgB2 system doped with TiCl3. Applying an upgraded empirical model, the transfer of energy to the material during the milling process was determined. In this way, it is possible to compare the obtained experimental results with those from processes at different scales. In addition, the different milling parameters were evaluated independently according to their individual effect on the transferred energy. Their influence on the reaction kinetics and hydrogen capacity was discussed and the results were correlated to characteristics like particle and crystallite size, specific surface area, presence of nucleation sites and contaminants. Finally, an optimal value for the transferred energy was determined, above which the powder characteristics do not change and therefore the RHC system properties do not further improve. Fil: Jepsen, Julian. Helmholtz zentrum Geesthacht; Alemania. Helmut Schmidt University; Alemania Fil: Capurso, Giovanni. Helmholtz zentrum Geesthacht; Alemania Fil: Puszkiel, Julián Atilio. Helmholtz zentrum Geesthacht; Alemania. Comisión Nacional de Energía Atómica. Centro Atómico Bariloche; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Patagonia Norte; Argentina Fil: Busch, Nina. Helmholtz zentrum Geesthacht; Alemania Fil: Werner, Tobias. Helmholtz zentrum Geesthacht; Alemania Fil: Milanese, Chiara. Universita Degli Studi Di Pavia; Italia Fil: Girella, Alessandro. Universita Degli Studi Di Pavia; Italia Fil: Von Colbe, José Bellosta. Helmholtz zentrum Geesthacht; Alemania Fil: Dornheim, Martin. Helmholtz zentrum Geesthacht; Alemania Fil: Klassen, Thomas. Helmholtz zentrum Geesthacht; Alemania. Helmut Schmidt University; Alemania

New insights into the reaction pathways of different potassium/magnesium amide-hydride based systems are discussed. In situ SR-PXD experiments were for the first time performed in order to reveal the evolution of the phases connected with the hydrogen releasing processes. Evidence of a new K-N-H intermediate is shown and discussed with particular focus on structural modification. Based on these results, a new reaction mechanism of amide-hydride anionic exchange is proposed.

Reaction kinetic behaviour and cycling stability of the 2LiBH4-MgH2 reactive hydride composite (Li-RHC) are experimentally determined and analysed as a basis for the design and development of hydrogen storage tanks. In addition to the determination and discussion about the properties; different measurement methods are applied and compared. The activation energies for both hydrogenation and dehydrogenation are determined by the Kissinger method and via the fitting of solid-state reaction kinetic models to isothermal volumetric measurements. Furthermore, the hydrogen absorption-desorption cycling stability is assessed by titration measurements. Finally, the kinetic behaviour and the reversible hydrogen storage capacity of the Li-RHC are discussed. Fil: Jepsen, Julian. Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung; Alemania Fil: Milanese, Chiara. Università degli Studi di Pavia; Italia Fil: Puszkiel, Julián Atilio. Comisión Nacional de Energía Atómica. Centro Atómico Bariloche; Argentina. Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung; Alemania. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Patagonia Norte; Argentina Fil: Girella, Alessandro. Università degli Studi di Pavia; Italia Fil: Schiavo, Benedetto. Università degli Studi di Palermo; Italia Fil: Lozano, Gustavo A.. Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung; Alemania Fil: Capurso, Giovanni. Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung; Alemania Fil: Von Colbe, José M. Bellosta. Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung; Alemania Fil: Marini, Amedeo. Comisión Nacional de Energía Atómica. Centro Atómico Bariloche; Argentina Fil: Kabelac, Stephan. Leibniz Universität Hannover; Alemania Fil: Dornheim, Martin. Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung; Alemania Fil: Klassen, Thomas. Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung; Alemania

Thermodynamic and heat transfer properties of the 2LiBH4-MgH2 composite (Li-RHC) system are experimentally determined and studied as a basis for the design and development of hydrogen storage tanks. Besides the determination and discussion of the properties, different measurement methods are applied and compared to each other. Regarding thermodynamics, reaction enthalpy and entropy are determined by pressure-concentration-isotherms and coupled manometric-calorimetric measurements. For thermal diffusivity calculation, the specific heat capacity is measured by high-pressure differential scanning calorimetry and the effective thermal conductivity is determined by the transient plane source technique and in situ thermocell. Based on the results obtained from the thermodynamics and the assessment of the heat transfer properties, the reaction mechanism of the Li-RHC and the issues related to the scale-up for larger hydrogen storage systems are discussed in detail. Fil: Jepsen, Julian. Helmholtz-Zentrum Geesthacht; Alemania Fil: Milanese, Chiara. University of Pavia; Italia Fil: Puszkiel, Julián Atilio. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Comisión Nacional de Energía Atómica. Centro Atómico Bariloche; Argentina. Helmholtz-Zentrum Geesthacht; Alemania Fil: Girella, Alessandro. University of Pavia; Italia Fil: Schiavo, Benedetto. Universidad de Palermo; Argentina. Istituto per le Tecnologie Avanzate; Italia Fil: Lozano, Gustavo A.. Helmholtz-Zentrum Geesthacht; Alemania. BASF; Alemania Fil: Capurso, Giovanni. Helmholtz-Zentrum Geesthacht; Alemania Fil: Von Colbe, José M. Bellosta. Helmholtz-Zentrum Geesthacht; Alemania Fil: Marini, Amedeo. University of Pavia; Italia Fil: Kabelac, Stephan. Leibniz Universität Hannover; Alemania Fil: Dornheim, Martin. Helmholtz-Zentrum Geesthacht; Alemania Fil: Klassen, Thomas. Helmholtz-Zentrum Geesthacht; Alemania

We herein report on the synthesis of mixed alkali cluster intercalated fullerides NaxLiy−xC60 (y = 12; x = 1–6) by a two-steps mechanochemical reaction of fullerene with sodium and lithium. These compounds crystallize in the cubic lattice of C60 displaying a contracted lattice parameter with respect to the Na6C60 parent structure. The analysis of the hydrogen sorption behaviour shows a slight decrease in the dehydrogenation enthalpy for y = 12 with respect to the sodium free member. Raman spectroscopy highlighted a partial electron transfer from alkali metals to C60, suggesting the presence of charged sodium/lithium clusters. Finally, we applied muon spectroscopy to understand the different hydrogenation mechanisms in NaxLi6−xC60 and NaxLi12−xC60 and explain their different performance.

Magnesium has been studied as a potential hydrogen storage material for several decades because of its relatively high hydrogen storage capacity, fast sorption kinetics (when doped with transition metal based additives), and abundance. This research aims to study the possibility to use waste magnesium alloys to produce good quality MgH2. The production costs of hydrogen storage materials is still one of the major barriers disabling scale up for mobile or stationary application. The recycling of magnesium-based waste to produce magnesium hydride will significantly contribute to the cost reduction of this material. This study focuses on the effect of different parameters such as the addition of graphite and/or Nb2O5 as well as the effect of milling time on the material hydrogenation/de-hydrogenation performances. In addition, morphology and microstructural features are also evaluated for all the investigated materials.

The work deals with the synthesis of multiferroic BiFeO3 starting from mixture of Bi citrate and Fe(II) oxalate dihydrate. By combined TG-DSC and XRPD experiments it is put into evidence that the mechanically activated mixture absorbs an extra enthalpy (+235 kJ) that is due to the reaction between the forming oxides. Furthermore it is shown that mechanical activation of the starting mixture sensibly enhances the formation of Bi ferrite. Indeed BiFeO3 is obtained by annealing the activated mixture at temperatures as low as 750 °C while this does not happen by annealing the physical mixture at temperatures up to 800 °C. Finally by MTDSC (Modulated Temperature Differential Scanning Calorimetry) we measured the thermal capacity of BiFeO3 obtained from the annealed activated mixture.

Lithium and hydrogen dynamics in Li12C60 and Li12C60Hy are investigated by means of 7Li and 1H solid state Nuclear Magnetic Resonance (NMR) in the temperature range 80–550 K. Differential scanning calorimetry characterization on the hydrogen sorption and X-rays structural analysis are also reported. In the pure phase, the 7Li results show a thermally activated dynamics that can be associated to Li motions within the crystal interstices. Upon hydrogenation, Li ionic motion is considerably hindered by the presence of hydrofullerene molecules. The 1H measurements show that C–H bonds are stable on the local scale up to 400–450 K. The NMR results at higher temperatures are compatible with a H diffusion mechanism which anticipates the H desorption process.

Through the substitution of Li with Na in Li6C60, we synthesized a series of mixed alkali cluster intercalated fullerides, NaxLi6−xC60. These compounds share lattices of Na6C60 and Li6C60 with a cubic parameter linearly dependent on x. H2 absorption and desorption were studied by means of charge/discharge kinetic measurements and coupled calorimetric–manometric evaluation. By varying the stoichiometry, we found the best compromise among the absorption rate, temperature and amount of hydrogen for x = 0.5 and 1. Small concentrations of Na substituted to Li significantly lower the absorption temperature of Li6C60, improving the hydrogenation capacity, the kinetics, and the dehydrogenation enthalpy, the latter being 43.8 kJ mol−1 H2 for x = 1. This study moves further toward the utilization of intercalated fullerides for hydrogen storage applications.

Among different Reactive Hydride Composites (RHCs), the combination of LiBH4 and MgH2 is a promising one for hydrogen storage, providing a high reversible storage capacity. During desorption of both LiBH4 and MgH2, the formation of MgB2 lowers the overall reaction enthalpy. In this work, the material was compacted to pellets for further improvement of the volumetric hydrogen capacity. The influence of compaction pressure on the apparent density, thermal conductivity and sorption behaviour for the Li-based RHC during cycling was investigated for the first time. Although LiBH4 melts during cycling, decrepitation or disaggregation of the pellets is not observed for any of the investigated compaction pressures. However, a strong influence of the compaction pressure on the apparent hydrogen storage capacity is detected. The influence on the reaction kinetics is rather low. To provide explanations for the observed correlations, SEM analysis before and after each sorption step was performed for different compaction pressures. Thus, the low hydrogen sorption in the first cycles and the continuously improving sorption for low pressure compacted pellets with cycling may be explained by some surface observations, along with the form stability of the pellets.

Magnesium borohydride Mg(BH4)2 is a promising hydrogen storage material as it releases high hydrogen storage capacity at mild desorption temperatures, but it is still limited by slow hydrogen release kinetics and by the harsh conditions required to re-hydrogenate this compound. In this work, composites made of commercial Mg(BH4)2 and synthesized silica aerogel microparticles were prepared by thermal treatment in hydrogen under 120 bar and 200ºC. As a result, the sorption properties of the hydride are improved: calorimetric measurements show that decomposition temperature is reduced by 60ºC, and the typical 3-step decomposition mechanism of Mg(BH4)2 changes to a single-step mechanism in range of 220-400°C. The kinetics of the first dehydrogenation at 300ºC was two times faster in Mg(BH4)2-SiO2 composites than in the case of bulk γ-Mg(BH4)2. Additionally, the re-hydrogenation of this material at comparatively moderate conditions of 390ºC and 110 bar is presented for the first time, achieving cyclability with a reversible release of hydrogen up to 6wt%. Different amounts of hydrogen were exchanged depending on the temperature of desorption (300ºC or 400ºC) and the presence or absence of silica aerogel. This result indicates that silica aerogel chemically interacts with Mg(BH4)2, acting as an additive, which can result in different hydrogenation-dehydrogenation routes in which different amounts and types of intermediates are formed, influencing the kinetics and the cyclability., 2018-07-27, Spanish Ministry of Economy and Competitiveness project ENE2014-53459-R

The synthesis of barium metastannate, BaSnO3, by heating mixtures of metal oxalates, either physically mixed or subjected to a phase of mechanical activation, up to temperatures in the range 750- 1200 °C has been studied. Simultaneous thermogravimetric-differential scanning calorimetric (TGDSC) analyses and powder X-ray diffractometry have been applied to check the advancement of the reactions. BaSnO3, though slightly contaminated by BaCO3, can be obtained by heating the activated mixture up to T ≥ 1000 °C while heating a sample of a physical mixture at temperature as high as 1200 °C resulted in a mixture of BaSnO3, SnO2 and Ba2SnO4. The heat capacities of BaSnO3 samples prepared at temperatures between 1000 and 1200 °C have been measured by modulated temperature differential scanning calorimetry (MTDSC) in the temperature range 50-400 °C.

Mg-based ternary mixtures (40 ≤ Mg wt% ≤ 80) containing increasing amount (up to 30 wt %) of Ni and Cu were prepared by ball milling (BM) under Ar for 16 h and subsequently activated at high temperature (623 K) by charging/discharging cycles at H 2 pressure of 50 bar/0.7 bar. The work aims to analyze the influence of the mixtures' composition on the storage properties (H 2 intake and sorption kinetics) and to describe the role played by an ad-hoc activation in reaching these same properties. The storage capacity of the mixtures decreases by decreasing the Mg starting content, the H 2 active phases being “free Mg” and the “bonded Mg” intermetallic compounds Mg 2 Ni and Mg 2 Cu. After full activation (3 charging/discharging runs), “free Mg” hydrogenates 10 times quicker than the “bonded Mg phases”, while the discharging of both “free” and “bonded” Mg hydrides takes place simultaneously with similar kinetics. The best kinetic performance is shown by the samples with Mg = 60 wt% and 70 wt% and the highest Ni content (30% and 20% respectively), with sorption rates up to 7 times higher than those of the pure Mg/MgH 2 system.

The sorption capacity and kinetics of mechanically activated binary mixtures of Mg with nine different metals (Al, Cu, Fe, Mn, Mo, Sn, Ti, Zn, Zr) have been studied to determine whether these metals act as catalyzing/destabilizing agents in formation/decomposition of Mg hydrides. Identification of crystalline phases before and after the absorption/desorption processes assists our understanding of the different behaviors displayed by the studied compounds. Cu, Al and Zn take active part in Mg hydrogenation/dehydrogenation, but only the addition of Cu is actually effective in MgH 2 destabilization, leading to a substantial decrease of the desorption temperature of this phase (down to 270 °C), and to an improved desorption kinetics. With the other metals, the hydrogen release usually occurs at a significant rate only above 320 °C and the kinetics of the absorption/desorption processes are slower than in the Mg/MgH 2 system.

Molecular cocrystals are of growing interest in pharmaceutics for their improved physicochemical properties. Their mechanochemical synthesis is very promising, being easy, cheap, and “green”. Here, for the first time, we report on cocrystallization of bumetanide, a diuretic and natriuretic active principle, and 4-aminobenzoic acid. The synthesis is performed both by wet and dry grinding. The cocrystal formation was investigated with a wide range of techniques, including solid- state NMR, IR, XRD, microscopy, and thermal analysis. Wet and dry grinding procedures led to different cocrystal polymorphs. In particular, the dry method gave a cocrystal by powder amorphization and subsequent crystallization. DFT calculations at the B3LYP/6-31+G(d,p) level of theory shed light on the H-bond scheme at the basis of cocrystal formation. The cocrystals showed improved solubility and dissolution rate with respect to the drug alone. This could guarantee a faster absorption and a better bioavailability of the active principle.

Correction for ‘Rational design of functionalized polyacrylate-based high internal phase emulsion materials for analytical and biomedical uses’ by Gloria Brusotti et al., Polym. Chem., 2016, DOI: 10.1039/c6py01992g.

Cobalt ferrite (CoFe2O4) has been synthesized by a solid-state mechanothermal process, and its molar heat capacity has been determined. A stoichiometric mixture of CoC2O4 ・ 2H2O and FeC2O4 ・ 2H2O was subjected to a combination of mechanical activation (by high-energy milling) and thermal activation (by annealing at temperatures between 300 and 700 °C). The process was followed by thermogravimetric analysis and high-temperature X-ray powder diffraction. It has been shown that CoFe2O4 forms at all temperatures, though with different degrees of crystallization, while Co3O4 and Fe2O3 are the only products formed when starting from unmilled mixtures. The molar heat capacity of CoFe2O4 has been determined in the temperature range 60 - 400 °C by MTDSC. It has been shown that the molar CP values of CoFe2O4 samples produced at T ≥ 500 °C are close to each other while those of the samples produced at 300 and 400 °C are lower. Furthermore the CoFe2O4 samples prepared at T ≥ 500 °C show very similar microstructures.