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Some ambiguity is still involved in the interpretation of the growth mechanism of monodispersed hematite (alpha-Fe2O3) particles in dilute FeCl3 solutions. Namely, there are two entirely different proposals on this issue, viz. aggregation of preformed primary particles of alpha-Fe2O3 itself and reprecipitation of the ionic species through dissolution of the preformed beta-FeOOH particles. In order to resolve this problem, the formation process was followed in detail through TEM, Electron Diffraction, XRD, FT-IR, and ICP spectrometry along with quantitative analyses on seed effects. As a result, it has been concluded that the nuclei of the hematite particles are initially generated with the formation of beta-FeOOH particles and that they are grown by deposition of the solute originally present in the solution phase and indirectly furnished from the beta-FeOOH by dissolution. As the concentration of the solute is lowered by the growth of the hematite particles, they continue to grow with the solute provided mainly from the beta-FeOOH in a steady-state of the dissolution of beta-FeOOH and growth of alpha-Fe2O3. The basic formation mechanism is common to the ellipsoidal particles grown in the presence of phosphate ions and spherical particles in their absence.
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PMID:Formation Mechanism of Monodispersed alpha-Fe2O3 Particles in Dilute FeCl3 Solutions 897 68

By mixing an aqueous solution of CuCl2 with an NaDC aqueous solution of various concentration and initial molar ratio, seven coordinated samples with distinct appearances and characters were obtained. Their structures and components were investigated by FT-IR spectroscopy, EXAFS (the extended X-ray absorption fine structure), thermal analysis, X-ray diffraction, laser light scattering, TEM (transmission electron micrograph), element analysis and ICP (inductively coupled plasma) analysis. The following conclusions were given: (1) The complexes of Cu2+-NaDC with distinct appearances and properties were synthesized. (2) After Cu(DC)2 dissolved in NaDC aqueous solution, larger micelles (30-90 nm diameter) formed in the supernate, it is a mixed micelle with Cu(DC)2 and NaDC. So these micelles are a new kind of micelle containing two kinds of metal ions. This is a new result using metal ions as bridges to form micelle. (3) According to the different concentration of Cu2+ to NaDC, the complexes formed as gel or poly-crystals. Both the composition of gel complexes and the coordination structure of carboxyl groups with metal ions varied with the initial molar ratio of Cu2+ to Na+. The gel complexes exhibits the non-stoichiometric character. (4) These results are in agreement with physiological condition. All the different states such as gel, precipitate, micelles of various structures are present in bile of gallbladder. We can suggest an ideal model of the interaction between Cu2+ and bile salts in vivo.
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PMID:The interaction of Cu2 + ions and NaDC micelles. 1208 72

We report here, for the first time, synthesis of anchored Pd complexes in mesoporous supports such as MCM-41 and MCM-48 as true heterogeneous catalysts for hydrocarboxylation of aryl olefins and alcohols to give excellent conversion ( approximately 100%) and regioselectivity ( approximately 99%) for 2-arylpropionic acids. The catalysts were characterized by powder-XRD, 31P CP-MAS NMR, FT-IR, TEM, XPS and ICP-AES. Recycle studies with these anchored Pd mesoporous catalysts were performed to confirm true heterogeneity.
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PMID:Anchored Pd complex in MCM-41 and MCM-48: novel heterogeneous catalysts for hydrocarboxylation of aryl olefins and alcohols. 1217 12

Results from aromatic aminations and Kumada couplings, together with spectroscopic analyses (TEM, EDX, ICP-AES, React-IR), reveal that catalysis using nickel-on-charcoal (Ni/C) is most likely of a homogeneous rather than heterogeneous nature. In the course of a reaction with Ni/C, nickel bleed from the support was calculated to be as high as 78%. However, the existence of an equilibrium for this homogeneous species between nickel located inside vs outside the pore system of charcoal strongly favors the former, thus leaving only traces of metal detectable in solution. This accounts for virtually complete recovery of nickel on the charcoal following filtration of a reaction mixture and allows for recycling of the catalyst. TEM and EDX data were used to explain different reactivity profiles of Ni/C, which depended upon the method of reduction used to convert Ni(II)/C to Ni(0) as well as the level of nickel loading on the support.
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PMID:On the nature of the 'heterogeneous' catalyst: nickel-on-charcoal. 1258 54

Star polymers containing ruthenium complex in the core were prepared by ruthenium-catalyzed living radical polymerization, where the metal catalysts were directly encapsulated on linking reactions of living poly(MMA) in the presence of ethylene glycol dimethacrylate as a linker and diphenyl-4-styrylphosphine as a ligand incorporated in the core. The products were characterized by SEC/MALLS, UV-vis, NMR, AFM, TEM, and ICP-AES and were employed as polymer catalysts for the oxidation reaction of alcohol.
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PMID:Polymer catalysts from polymerization catalysts: direct encapsulation of metal catalyst into star polymer core during metal-catalyzed living radical polymerization. 1272 Apr 36

Pd(0) nanoparticles with approximately 2 nm diameter, immobilized in 1-n-butyl-3-methylimidazolium hexafluorophosphate ionic liquid, are efficient catalyst precursors for coupling of aryl halides with n-butylacrylate. In situ TEM analysis of the ionic liquid catalytic solution after the catalytic reaction shows the formation of larger nanoparticles ( approximately 6 nm). The palladium content in the organic phase during the arylation reaction was checked by ICP-AS and shows significant metal leaching (up 34%) from the ionic phase to the organic phase at low substrate conversions and drops to 5-8% leaching at higher conversions. These results strongly suggest that the Pd(0) nanoparticles serve as a reservoir of "homogeneous" catalytic active species.
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PMID:The role of Pd nanoparticles in ionic liquid in the Heck reaction. 1575 45

BACKGROUND: It is estimated that over 80% of respirable particulate matter (PM10) in cities comes from road transport and that tire and brake wear are responsible for the 3-7% emission of it. Data on the indicators of environmental impact of tire debris (TD), originated from the tire abrasion on roads, are extremely scarce, even though TD contains chemicals (zinc and organic compounds) which can be released in the environment. METHODS: TD particle morphology was analysed with SEM, TEM and FIB instruments. TD eluates and TD organic extracts were tested at dilution series on human cell lines and Xenopus laevis embryos. 50 and 100 g/L TD were used for the eluates obtained after 24 h at pH 3 and the quantity of zinc present was measured with a ICP-AES. Eluates diluted to 1%, 10%, 50% in culture media and undiluted were used on X. laevis embryos in the FETAX test. HepG2 cells were exposed for 24 h to 0.05 - 50 mug/ml of zinc salt while A549 cells were exposed for 24, 48 and 72 h to 10, 50, 60, or 75 mug/ml of TD extract. X. laevis embryos were exposed to 50, 80, 100, or 120 mug/ml TD extract. RESULTS: The solution of undiluted 50 g/L TD produced 80.2% mortality (p < 0.01) in X. laevis embryos and this toxic effect was three times greater than that produced by 100 g/L TD. Zn accumulation in HepG2 cells was evident after 4 h exposure. A549 cells exposed to TD organic extract for 72 h presented a modified morphology, a decrease in cell proliferation and an increase in DNA damage as shown by comet assay. The dose 80 mug/ml of TD extract produced 14.6% mortality in X. laevis embryos and 15.9% mortality at 120 mug/ml. Treatment with 80, 100, or 120 mug/ml TD organic extract increased from 14.8% to 37.8% malformed larvae percentages compared to 5.6% in the control. CONCLUSION: Since the amount of Zn leached from TD is related to pH, aggregation of particles and elution process, the quantity of TD present in the environment has to be taken into account. Moreover the atmospheric conditions, which may deeply influence the particle properties, have to be considered. The TD organic fraction was toxic for cells and organisms. Thus, because of its chemical components, TD may have a potential environmental impact and has to be further investigated.
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PMID:Impact of tire debris on in vitro and in vivo systems. 1581 62

Self-assembly of BaF2 nanoparticles was described. BaF2 nanoparticles were prepared by microemulsion technology. The self-assembly of the particles is spontaneous without coating reagent on the surface or external force being applied during the procedure of sample preparation. XRD examination and ICP data showed the phase purity of the final product; FTIR spectroscopy confirmed that there was no organic species leaved in the product. By depositing one drop of colloid solution containing BaF2 particles on the TEM grid directly, we can get the ring-like self-assembly with larger particles dispersing peripherally to form a ring and smaller particles inside this ring forming circles.
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PMID:Spontaneous ring-like self-assembly of BaF2 nanoparticles. 1591 44

Copper-chromite oxide and TiO2-supported copper-chromite oxide catalysts are prepared by various methods. They are characterized with ICP, BET, XRD, XPS, SEM, and TEM, etc. Their catalytic performance for liquid phase hydrogenation of furfural to furfuryl alcohol is also valuated. The catalysts prepared by ultrasound exhibit good performance. Catalytic activity of TiO2-supported catalysts is higher than that of catalyst without TiO2, notwithstanding they are all prepared by ultrasound. It is worth stressing that after reduced the TiO2-supported catalysts, which are X-ray amorphous, display good performance at 140 degrees C, while the catalysts without TiO2 show no activity under the same condition. Obtained results indicate that the catalytic performance of catalysts depends upon the amount of reducible copper ions and the activity decay is related to the loss of metal elements on the surface of catalyst.
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PMID:Selective hydrogenation of furfural to furfuryl alcohol over catalysts prepared via sonochemistry. 1669 Mar 43

Biphasic beta-rhenanite (beta-NaCaPO(4))-hydroxyapatite (Ca(10)(PO(4))(6)(OH)(2)) biomaterials were prepared by using a one-pot, solution-based synthesis procedure at the physiological pH of 7.4, followed by low-temperature (300-600 degrees C) calcination in air for 6 h. Calcination was for the sole purpose of crystallization. An aqueous solution of Ca(NO(3))(2). 4H(2)O was rapidly added to a solution of Na(2)HPO(4) and NaHCO(3), followed by immediate removal of gel-like, poorly-crystallized precursor precipitates from the mother liquors of pH 7.4. Freeze-dried precursors were found to be nanosize with an average particle size of 45 nm and a surface area of 128 m(2)/g. Upon calcination in air, precursor powders crystallized into biphasic (60% HA-40% rhenanite) biomaterials, while retaining their submicron particle sizes and high surface areas. beta-rhenanite is a high solubility sodium calcium phosphate phase. Samples were characterized by XRD, FTIR, SEM, TEM, ICP-AES, TG, DTA, DSC, and surface area measurements.
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PMID:A new rhenanite (beta-NaCaPO(4)) and hydroxyapatite biphasic biomaterial for skeletal repair. 1676 21


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