Search results for "powder"
showing 10 items of 437 documents
The crystal structure of 3,5-diisopropyl-4-nitropyrazole from X-ray powder diffraction data
2001
The crystal structure of 3,5-diisopropyl-4-nitropyrazole, 3c, has been determined by a Patterson Search method from laboratory X-ray powder diffraction data. The crystal data are: monoclinic symmetry with the unit-cell parameters aa 19:530O5U; ba 6:485O1U and ca 17:937O3U A; ba 100:32O1U8; space group I2/a ,C 9H15N3O2, Za 8, 293 K. After indexing the powder pattern by two methods, the unit-cell parameters found were refined by a least-squares technique. A whole pattern- fitting program was used to extract the integrated intensities. The structure was solved taking a related compound as a search model and the final Rietveld refinement converged to Rwpa 0.1971 and Rpa 0.1437. The structure pr…
Crystal structure of a new polytype in the V–P–O system: is ω-VOPO4 a dynamically stabilised metastable network?
2001
Abstract ω-VOPO 4 has been prepared by thermal decomposition of different oxovanadium hydrogen phosphates, namely VO(HPO 4 ) n H 2 O ( n =2( α ), 2(β) and 4) and β-NH 4 (VO 2 )(HPO 4 ). The ω-VOPO 4 phase only remains well crystallised at relatively high temperatures. Its crystal structure has been determined ab initio from X-ray powder diffraction data collected at 475°C. The cell is tetragonal (space group P4 2 /mmc) with a =4.8552(3) A and c =8.4301(6) A. Starting positional parameters were obtained by direct methods, and the structure was refined using Rietveld profile refinement principles. Disorder of two oxygen sublattices is observed. To rationalise some features of the crystal stru…
Metallic lead recovery from lead-acid battery paste by urea acetate dissolution and cementation on iron
2009
Abstract A suitable hydrometallurgical and environmentally friendly process was studied to replace the currently used practices for recycling lead-acid batteries via smelting. Metallic lead was recovered by cementation from industrial lead sludge solutions of urea acetate (200 to 500 g/L) using different types of metallic iron substrates (nails, shaving or powder) as reducing agents. Under specific operating conditions, up to 99.7% of lead acid battery paste, mainly composed of PbSO4, PbO2 and PbO·PbSO4 species, was converted to metallic lead.. The conversion of the metallic lead and rate of the cementation reaction were strictly dependent on the type of iron substrate used as the reductant…
Protective effect of mesoporous silica particles on encapsulated folates.
2016
Mesoporous silica particles (MSPs) are considered suitable supports to design gated materials for the encapsulation of bioactive molecules. Folates are essential micronutrients which are sensitive to external agents that provoke nutritional deficiencies. Folates encapsulation in MSPs to prevent degradation and to allow their controlled delivery is a promising strategy. Nevertheless, no information exists about the protective effect of MSPs encapsulation to prevent their degradation. In this work, 5-formyltetrahydrofolate (FO) and folic acid (FA) were entrapped in MSPs functionalized with polyamines, which acted as pH-dependent molecular gates. The stability of free and entrapped vitamins af…
NanoSr - A New Carbonate Microanalytical Reference Material for In Situ Strontium Isotope Analysis
2019
The in situ measurement of Sr isotopes in carbonates by MC‐ICP‐MS is limited by the availability of suitable microanalytical reference materials (RMs), which match the samples of interest. Whereas several well‐characterised carbonate reference materials for Sr mass fractions > 1000 µg g−1 are available, there is a lack of well‐characterised carbonate microanalytical RMs with lower Sr mass fractions. Here, we present a new synthetic carbonate nanopowder RM with a Sr mass fraction of ca. 500 µg g−1 suitable for microanalytical Sr isotope research (‘NanoSr’). NanoSr was analysed by both solution‐based and in situ techniques. Element mass fractions were determined using EPMA (Ca mass fraction),…
Affinity scale between a carrier and a drug in DPI studied by atomic force microscopy.
2002
The dry powder inhalers (DPIs) consist, in the most cases, of ordered mixture where the particles adhesion results of interactions between the drug and the carrier. Generally, one step of production process is the micronization of the drug particles in order to reduce the size for ordered mixing optimization. But this operation is known to partially create an amorphous surface. In this case, surrounding storage conditions, like relative humidity (RH), are able to modify the percentage of amorphous drug surface. The aim of this study was to investigate surface reactivity, surface energy and direct force measurements by atomic force microscopy (AFM) between lactose (carrier) and zanamivir (dr…
Coordination polymer flexibility leads to polymorphism and enables a crystalline solid-vapour reaction: a multi-technique mechanistic study.
2015
Despite an absence of conventional porosity, the 1D coordination polymer [Ag4 (O2 C(CF2 )2 CF3 )4 (TMP)3 ] (1; TMP=tetramethylpyrazine) can absorb small alcohols from the vapour phase, which insert into AgO bonds to yield coordination polymers [Ag4 (O2 C(CF2 )2 CF3 )4 (TMP)3 (ROH)2 ] (1-ROH; R=Me, Et, iPr). The reactions are reversible single-crystal-to-single-crystal transformations. Vapour-solid equilibria have been examined by gas-phase IR spectroscopy (K=5.68(9)×10(-5) (MeOH), 9.5(3)×10(-6) (EtOH), 6.14(5)×10(-5) (iPrOH) at 295 K, 1 bar). Thermal analyses (TGA, DSC) have enabled quantitative comparison of two-step reactions 1-ROH→1→2, in which 2 is the 2D coordination polymer [Ag4 (O2 …
The structural versatility of proton sponge bismuth halides
2022
Hybrid halometalates containing lead, tin, bismuth and antimony and organic cations have recently shown a bevy of interesting photophysical properties. Aiming at finding chemically stable and thermally inert species, three halobismutate species of this class, crystallized with proton sponge-derived cations (PRSH), have been isolated as microcrystalline powders by mixing 1,8-bis(dimethylamino)-naphthalene (proton sponge, or PRS) and bismuth oxide in concentrated HX acids (X = Cl, Br and I). The two isomorphous (PRSH)3Bi2X9 (X = Br, I) species, containing isolated [Bi2X9]3- anions, are triclinic at room temperature and convert upon heating into a monoclinic structure through a displacive …
From nitrides to carbides: topotactic synthesis of the η-carbides Fe3Mo3C and Co3Mo3C
2004
The molybdenum bimetallic interstitial carbides Fe(3)Mo(3)C and Co(3)Mo(3)C have been synthesized by temperature-programmed reaction (TPR) between the molybdenum bimetallic interstitial nitrides Fe(3)Mo(3)N and Co(3)Mo(3)N and a flowing mixture of CH(4) and H(2) diluted in Ar. These compounds have been characterized by X-ray diffraction, laser Raman spectroscopy, elemental analysis, energy dispersive analysis of X rays, thermal analysis (in air) and scanning electron microscopy (field emission). Their structures have been refined from X-ray powder diffraction data. These carbides crystallize in the cubic system, space group Fd3m[a= 11.11376(6) and 11.0697(3)[Angstrom] for Fe and Co compound…
Structural and magnetic studies of mononuclear lanthanide complexes derived from Ν-rich chiral Schiff bases.
2021
Zn(II) complexes containing N, N,N and N,N,N pyridine (dPy) ligands tend to display improved fluorescence efficiencies in comparison with their starting ligands benefiting from the chelation enhanced effect (CHEF) and preventing photoinduced electron transfer (PET) mechanisms by the coordination of their lone pair electrons. Nevertheless, the size of Zn(II) makes steric crowding an important factor to be considered, since it can promote the elongation of the coordination bonds that weakens their strength and favors the reduction of fluorescence efficiencies through PET processes. For that reason, in this contribution we have performed a systematic study of Zn(II) compounds based on α-acetam…