16 research outputs found

    Non-isovalent substitution in a Zintl phase with the TiNiSi type structure, CaMg1–xAgxGe [x = 0.13 (3)]

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    Single crystals of the title Ag-substituted calcium magnesium germanide, CaMg1–xAgxGe [x = 0.13 (3)] were obtained from the reaction of the corresponding elements at high temperature. The compound crystallizes with the TiNiSi structure type (Pearson code oP12) and represents an Ag-substituted derivative of the Zintl phase CaMgGe in which a small fraction of the divalent Mg atoms have been replaced by monovalent Ag atoms. All three atoms in the asymmetric unit (Ca, Mg/Ag, Ge) occupy special positions with the same site symmetry (.m.). Although the end member CaAgGe has been reported in an isomorphic superstructure of the same TiNiSi type, higher Ag content in solid solutions could not be achieved due to competitive formation of other, perhaps more stable, phases

    Assessment of the Nutrients in the Leachate and the Groundwater Quality for Drinking and Farming around the Nkolfoulou Landfill in Yaoundé, Cameroon

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    This study focuses on the assessment of the nutrients in the leachate and the groundwater quality around the Nkolfoulou landfill in Yaoundé known in French as “Centre de Traitement de Déchets (CTD).” Landfilling generates leachate that can pollute groundwater. Leachate along with groundwater samples (n=1+13) was collected in January (long dry season) and May (long wet season) 2014 and explored for various parameters including pH, temperature, EC, turbidity, TDS, TA, TSS, TH, BOD5, COD, Na+, K+, Mg2+, Ca2+, NH4+, NO3−, Cl−, F−, SO42−, PO43−, HCO3−, and colour using standard methods. In the leachate samples, values of TSS (700.2 and 130.2 mg/L), BOD5 (140 mg/L), COD (1350 and 1750 mg/L), NH4+ (82.50 and 39.51 mg/L), NO3− (159.32 and 74.82 mg/L), and Cl− (702.69 and 345.50 mg/L) exceeded the Cameroonian standards for effluent discharge. All the values of pH and some values of turbidity (4.55 and 4.50 NTU) and NH4+ (0.51 and 0.73 mg/L) in the groundwater samples violated the Cameroonian standards for drinking water. Based on the water quality index (WQI), an average of 11.53% of groundwater samples was improper for drinking in both seasons. Based on the parameters assessed, all the samples complied with the standard set for irrigation, poultry, and livestock. The hazard quotient (HQ) and the hazard index (HI) of NO3− and F− for children and adults were <1, and hence, the increased non-cancer risks due to these ions through the drinking of groundwater was low. From the statistical analysis, the Nkolfoulou landfill may not be the main source of major ions to the nearby groundwater

    Synthesis, characterization and gas sensing properties of Ni1-xZnxO nanoparticles and Ni1-xZnxO/ZnO nanocomposites

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    The selectivity of oxide based resistive gas sensors remains a challenging issue as they suffer from low selectivity. Researchers have suggested various ways to overcome this problem of cross-sensitivity. Thus it was established that a significant improvement can be reached by using mixed metal oxide system [1], by microstructural modification and by the use of dopants and catalysts [2] or by controlling the size and the shape of the oxide grains. Among mixed metal oxides, the nanocomposite materials and the doped materials are very promising for gas sensor applications. Indeed, various authors have reported sensitive and selective gas sensing characteristics of composite oxide materials made by different methods [3]. According to our knowledge, reports on the NiO-ZnO systems are limited [4] and the literature on Zn doped NiO used as gas sensor is very scarce. In this work we report for the first time, the synthesis of Ni1-xZnxO nanoparticles and Ni1-xZnxO/ZnO nanocomposites at relatively low temperature using corresponding metal malonate as single batch precursors. These materials were obtained by thermal decomposition (~ 360°C) of the corresponding metal malonate presynthesized by coprecipitation in aqueous solution. All the precursors were characterized by ICP-AES, FTIR, and TGA and these analyses confirm the structure of the precursors as Ni1-xZnx(OOCCH2COO).2H2O. The presence of mixed phase nanoparticles after thermal decomposition of the precursor was confirmed by a combination of characterization techniques (SEM, XRD, XPS and ToF-SIMS). The gas sensing properties of the synthesized materials were examined using some reducing and oxidant gases showing significant changes in behavior in function of the doping

    A new heteroleptic oxalate-based compound: poly[[2-(aminomethyl)pyridine]di-μ 6 -oxalato-chromium(III)potassium(I)]

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    International audienceThe title compound, [KCr(C2O2)2(C6H8N2)]n, was obtained from aqueous solution and analyzed with single-crystal X-ray diffraction at 100 K. It crystallizes in the monoclinic space group C2/c and displays a three-dimensional polymeric architecture built up by bimetallic oxalate-bridged CrIII-K helical chains linked through centrosymmetric K2O2 units to yield a sheet-like alternating P/M arrangement which looks like that of the previously described two-dimensional [NaCr(ox)2(pyim)(H2O)]·2H2O [pyim is 2-(pyridin-2-yl)imidazole; Lei et al. (2006). Inorg. Chem. Commun. 9, 486-488]. The CrIII ions in each helix have the same chirality. The infinite neutral sheets are eclipsed with respect to each other and are held together by a hy­dro­gen-bonding network involving 2-(amino­meth­yl)pyridine H atoms and oxalate O atoms. Each sheet gives rise to channels of Cr4K4 octanuclear rings and each resultant hole is occupied by a pair of 2-(amino­meth­yl)pyridine ligands with partial overlap. The shortest Cr...Cr distance [5.593 (4) Å] is shorter than usually observed in the K-MIII-oxalate family

    Coprecipitation of nickel zinc malonate: A facile and reproducible synthesis route for Ni1-xZnxO nanoparticles and Ni1-xZnxO/ZnO nanocomposites via pyrolysis

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    Nanoparticles of Ni1-xZnxO and Ni1-xZnxO/ZnO, which can be good candidates for selective gas sensors, were successfully obtained via a two-step synthetic route, in which the nickel zinc malonate precursor was first synthesized by co-precipitation from an aqueous solution, followed by pyrolysis in air at a relatively low temperature (~500 °C). The precursor was characterized by ICP-AES, FTIR and TG and the results indicate the molecular structure of the precursor to be compatible with Ni1-xZnx(OOCCH2COO).2H2O. The decomposition product, characterized using various techniques (FTIR, XRD, ToF-SIMS, SEM, TEM and XPS), was established to be a doped nickel oxide (Ni1-xZnxO for 0.01≤ x ≤0.1) and a composite material (Ni1-xZnxO/ZnO for 0.2≤ x≤0.5). To elucidate the form in which the Zn is present in the NiO structure, three analytical techniques were employed: ToF-SIMS, XRD and XPS. While ToF SIMS provided a direct evidence of the presence of Zn in the NiO crystal structure, XRD showed that Zn actually substitutes Ni in the structure and XPS is a bit more specific by indicating that the Zn is present in the form of Zn2+ ions

    Two-dimensionally stacked heterometallic layers hosting a discrete chair dodecameric ring of water clusters: synthesis and structural study

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    International audienceThe stacked two-dimensional supramolecular compound catena-{Co(amp)3Cr(ox)3·6H2O} (amp = 2-picolylamine, ox = oxalate) has been synthesized from the bimolecular approach using hydrogen bonds. It is built from layers in which both Co(amp)(3+) (D) and Cr(ox)(3-) (A) ions are bonded in a repeating DADADA… pattern along the a and c axes by multiple hydrogen bonds. These layers host a well resolved R12 dodecameric discrete ring of water clusters built by six independent molecules located around the 2c centrosymmetric Wyckoff positions of the P21/n space group in which the compound crystallizes. These clusters are ranged along the [001] direction, occupy 733.5 Å(3) (22.0%) of the unit cell and have a chair conformation via 12 hydrogen bonds. The water molecules of the cluster are linked with stronger hydrogen bonds than those between the cluster and its host, which explains the single continuous step of the dehydration process of the compound

    Structural Characterization and Magnetic Properties of Undoped and Ti-Doped ZnO Nanoparticles Prepared by Modified Oxalate Route

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    Ti-doped zinc oxide and pure zinc oxide nanoparticles were synthesized by a modified oxalate route using Averrhoa carambola fruit juice as a natural source of oxalate. The characteristics of the precursors have been investigated by FTIR, TGA, and XRD. The results from the investigation revealed that the precursors are zinc oxalate and Ti-doped zinc oxalate which readily decompose at 450°C. The as-prepared precursors were calcined at 450°C for 4 hours, and the decomposition products have been characterized by XRD, SEM, EDX, and VSM. XRD results revealed crystallinity with hexagonal wurtzite structure, while the average grain size was found to be 26 nm for Ti-doped ZnO and 29 nm for ZnO, using calculations based on Debye-Scherrer equation. Furthermore, the morphological studies by SEM showed particle agglomeration, while the presence of Ti3+ in the zinc oxide lattice is indicated by EDS analysis. Finally the hysteresis loop from VSM results shows that Ti-doped ZnO exhibits ferromagnetism

    Structural characterization and magnetic properties of undoped and copper-doped cobalt ferrite nanoparticles prepared by the octanoate coprecipitation route at very low dopant concentrations

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    Nanoparticles of undoped and copper-doped cobalt ferrite Co1−xCuxFe2O4 at very low dopant concentrations (x = 0; 0.02; 0.04; 0.06; 0.08) were successfully synthesized by pyrolysis of the corresponding hetero metal octanoate precursors obtained via coprecipitation using the octanoate ligand as precipitating agent. The precursors were then characterized by FTIR, ICP-AES and TG-DTA analyses and the results reveal the formation of a copper-cobalt-iron hydroxooctanoate represented by the formula [Co1−xCuxFe2(C8H15O2)6(OH)2·2H2O]. The decomposition products obtained upon pyrolysis in air at 400 °C for 3 h were characterized by FTIR, XRD, SEM, TEM, XPS and VSM analyses. FTIR and XRD analyses showed the formation of a single phase mixed spinel ferrite while TEM analysis showed that the particles have a spherical shape with a mean size of 20 nm and form spherical agglomerates with sizes reaching 500 nm in some cases as the SEM images show. The chemical states of the metallic species in the samples were revealed by XPS to be Cu2+, Co2+ and Fe3+. These results combined with XRD confirmed the mixed spinel structure, Co1−xCuxFe2O4 in which Cu2+ ions substitute Co2+ ions in tetrahedral sites for x lower than 0.06 and in octahedral sites for x between 0.06 and 0.08. Magnetic parameters such as saturation magnetization (Ms), coercivity (Hc), remanent magnetization (Mr), magnetocrystalline anisotropy constant (K) and reduced magnetization (Mr/Ms), obtained from magnetic hysteresis loops measured at room temperature, are in agreement with this mixed spinel structure and also indicate that these materials are ferromagnetic and could be good candidates for applications in biomedicine and in microwave devices
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