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Cellulose was first modified with thionyl chloride, giving 99% substitution at C6, and then reacted with ethylene-1,2-diamine to produce 6-(2'-aminoethylamino)-6-deoxy-cellulose. From the 8.5% of nitrogen incorporated in the polysaccharide backbone, the amount of ethylene-1,2-diamine anchored per gram of modified cellulose was determined to be 3.03+/-0.01mmol. This chemically immobilized surface was characterized by FTIR, TG, (13)C NMR, and SEM techniques. The available basic nitrogen centers covalently bonded to the biopolymer skeleton were studied for copper, cobalt, nickel, and zinc adsorption from aqueous solutions and the respective thermal adsorption effects were determined by calorimetric titration. The ability to adsorb cations gave a capacity order of Co(2+)>Cu(2+)>Zn(2+)>Ni(2+) with affinities of 1.91+/-0.07, 1.32+/-0.07, 1.31+/-0.02, and 1.08+/-0.04mmol/g, respectively. The net thermal effects obtained from calorimetric titration measurements were adjusted to a modified Langmuir equation and the enthalpy of the interaction was calculated to give the following exothermic values: -20.8+/-0.05, -11.72+/-0.03, -7.32+/-0.01, and -6.27+/-0.02kJ/mol for Co(2+), Cu(2+), Zn(2+), and Ni(2+), respectively. With the exception of the entropic value for copper, the other thermodynamic data for these systems are favorable for cation adsorption from aqueous solutions at the solid/liquid interface, suggesting the use of this anchored biopolymer for cation removal from the environment.
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PMID:Preparation of ethylenediamine-anchored cellulose and determination of thermochemical data for the interaction between cations and basic centers at the solid/liquid interface. 1702 56

MWNTs (multi-walled carbon nanotubes) were made by catalytic CVD process using iron-containing mesoporous silica, Fe-MCM-41, with 4 mol% Fe loading prepared by direct synthesis route. Uniform 5 nm size Fe2O3 nano-particles impregnated onto a mesoporous silica support, SBA-15 were also prepared for CNTs synthesis. The catalysts were characterized using XRD, SEM/TEM, N2 physisorption, UV-vis diffuse reflectance and FT-IR spectroscopies. Acetylene gas was introduced as a carbon source, and the gas mixture of Ar:H2:C2H2 = 14:5:1 pyrolyzed at 750 degrees C for 60 min was found to be the optimum synthesis condition. Fe-MCM-41 due to higher dispersion of nano-sized Fe-species was efficient as catalyst for MWNTs with more uniform size distribution. Cobalt-impregnated Fe-MCM-41 (Co/Fe = 1) produced a small fraction of SWNTs of ca. 2 nm diameter mixed with MWNTs.
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PMID:Synthesis of carbon nanotubes using mesoporous Fe-MCM-41 catalysts. 1725 85

A combination of pyro and hydrometallurgical process has been proposed to selectively recover molubdenum, cobalt and aluminium from the spent catalyst containing 12.3% Mo; 31.8% Al; 2.38% Co; 9.5% S and 2.9% C. Before a two-stage alkali-acid leaching process to selectively target Mo, Co and Al from the uncrushed sample, the spent catalyst was calcined at different temperatures. Characterization of different calcined samples was carried out by different instrumental analysis like XRD, TG/DTA, IR and SEM in order to understand the structural changes and dissolution behavior of spent catalyst. It was found that calcination at 500 degrees C preferred for spent catalyst roasting since the surface and pore structures obtained by roasting at this temperature facilitated dissolution of calcined spent catalyst in the leachant. Mo was selectively separated and recovered from the leach liquor by carbon adsorption method; whereas, Al and Co were separated by an organo-phosphinic-based extractant, Cyanex 272. In the whole process, 95.9% Mo, 89.6% Co and 39.8% Al was recovered from the spent catalyst. Finally, a complete process flowsheet has been presented.
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PMID:Selective recovery of Mo, Co and Al from spent Co/Mo/gamma-Al2O3 catalyst: effect of calcination temperature. 1736 21

The electrochemical detection of H2O2 was investigated on a cobalt oxide nanoparticles modified glassy carbon electrode in phosphate buffer solution (pH 7). Cyclic voltammetry at potential range -1.1 to 1.1 V from CoCl2 natural aqueous solution produced well defined cobalt oxide nanoparticles deposited on the surface of glassy carbon electrode. The surface of resulting electrode was characterized with SEM. The formation of cobalt oxyhydroxide film was investigated by cyclic voltammetry in alkaline and natural aqueous solution. The modified electrode showed well defined and stable redox couples in both alkaline and natural aqueous solution. The modified electrode showed excellent electrocatalytic activity for oxidation of hydrogen peroxide. The response to H2O2 on the modified electrode was examined using cyclic voltammetry and amperometry. The amperometric detection of hydrogen peroxide is carried out at 0.75 V versus Ag/AgCl reference electrode in phosphate buffer solution with pH 7.4. The detection limit (S/N=3) was 0.4 nM with linearity up to 6 orders of magnitude and sensitivity of 4.86 microA microM(-1) cm(-2). The response time of the electrode to achieve 95% of the steady-state current is <2 s. No measurable reduction in analytical performance of the modified electrode was found by storing the electrode in ambient conditions for 20 days. This modified electrode recedes many advantages such as remarkable catalytic activity, good reproducibility, simple preparation procedure and long term stability of signal response during hydrogen peroxide oxidation. The immobilization of cobalt oxide nanoparticles on the surface of GC electrode appears to be a highly efficient method for the development of a new class of sensitive, stable and reproducible hydrogen peroxide electrochemical sensor.
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PMID:Nanomolar detection of hydrogen peroxide on glassy carbon electrode modified with electrodeposited cobalt oxide nanoparticles. 1756 Mar 81

The hydrothermal synthesis and structural characterization of a number of complex compounds containing the divalent tris(oxalato-O,O')germanate anion, [Ge(C2O4)3]2-, or the neutral bis(oxalate-O,O')germanium fragment, [Ge(C2O4)2], with transition-metal (M) cationic complexes of 1,10'-phenanthroline (phen) is reported: [M(phen)3][Ge(C2O4)3].xH2O [where M2+ = Cu2+ (1a and 1b), Fe2+ (2a and 2b), Ni2+ (3), Co2+ (4); x = 0.2 for 2b], [MGe(phen)2(mu2-OH)2(C2O4)2] [where M2+ = Cd2+ (5) and Cu2+ (6)]. The isolation of two polymorphs with Cu2+ (1a and 1b) and other pseudo-polymorphs for Fe2+ (2a and 2b) was rationalized based on slightly different molar ratios for the starting materials. All compounds have been characterized using EDS, SEM, vibrational spectroscopy (FT-IR and FT-Raman), thermogravimetry, and CHN elemental composition and their structure determined on the basis of single-crystal X-ray diffraction studies. The crystal packing of the different chemical moieties for each series of compounds was discussed on the basis of the various intermolecular interactions present (strong C-H...pi and weak C-H...O hydrogen-bonding interactions, C-H...pi and pi-pi contacts).
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PMID:Heterodimetallic germanium(IV) complex structures with transition metals. 1762 37

This work reports the synthesis of multiwalled carbon nanotubes (MWCNTs) on nanoporous titanium dioxide (TiO2) templates. TiO2 nanotubular templates for MWCNTs are produced by anodization of titanium followed by pulsed electrodeposition (PED) of cobalt inside the TiO2 nanotubes. Cobalt acts as a catalyst for the growth of MWCNTs using chemical vapor deposition (CVD) technique. The cobalt catalyst initiates the growth of well graphitized MWCNTs inside the titania pores as well as beyond the titania pores. These materials have been characterized by SEM, EDS, GXRD, XPS, TEM, and ED techniques. The MWCNTs were about 10 mu in length and 80-120 nm in diameter.
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PMID:Growth of carbon nanotubes on nanoporous titania templates. 1768 78

Cyclic voltammetry at potential range -1.1 to 0.5 V from aqueous buffer solution (pH 7) containing CoCl(2) produced a well defined cobalt oxide (CoOx) nanoparticles deposited on the surface of glassy carbon electrode. The morphology of the modified surface and cobalt oxide formation was examined with SEM and cyclic voltammetry techniques. Hemoglobin (Hb) was successfully immobilized in cobalt-oxide nanoparticles modified glassy carbon electrode. Immobilization of hemoglobin onto cobalt oxide nanoparticles have been investigated by cyclic voltammetry and UV-visible spectroscopy. The entrapped protein can take direct electron transfer in cobalt-oxide film. A pair of well defined, quasi-reversible cyclic voltammetric peaks at about -0.08 V vs. SCE (pH 7), characteristic of heme redox couple (Fe(III)/Fe(II)) of hemoglobin, and the response showed surface controlled electrode process. The dependence of formal potential (E(0')) on the solution pH (56 mV pH(-1)) indicated that the direct electron transfer reaction of hemoglobin was a one-electron transfer coupled with a one proton transfer reaction process. The average surface coverage of Hb immobilized on the cobalt oxide nanoparticles was about 5.2536x10(-11) mol cm(-2), indicating high loading ability of nanoparticles for hemoglobin entrapment. The heterogeneous electron transfer rate constant (k(s)) was 1.43 s(-1), indicating great of facilitation of the electron transfer between Hb and electrodeposited cobalt oxide nanoparticles. Modified electrode exhibits a remarkable electrocatalytic activity for the reduction of hydrogen peroxide and oxygen. The Michaels-Menten constant K(m) of 0.38 mM, indicating that the Hb immobilized onto cobalt oxide film retained its peroxidases activity. The biosensor exhibited a fast amperometric response <5 s, a linear response over a wide concentration range 5 microM to 700 microM and a low detection limit 0.5 microM. According to the direct electron transfer property and enhanced activity of Hb in cobalt oxide film, a third generation reagentless biosensor without using any electron transfer mediator or specific reagent can be constructed for determination of hydrogen peroxide in anaerobic solutions.
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PMID:Immobilization of hemoglobin on electrodeposited cobalt-oxide nanoparticles: direct voltammetry and electrocatalytic activity. 1782 77

Currently, the rapid diagnosis of mesenteric ischemia is problematic because of the nonspecificity of most laboratory assays and the unreliability of physical examinations. The evaluation of the cobalt-albumin binding assay (CABA) as a diagnostic marker for short-term risk stratification of emergency department patients presenting with symptoms of intestinal ischemia is reported. This preliminary study includes patients scheduled for exploratory laparotomy with symptoms of ischemic bowel and/or bowel obstruction. Approximately 10 mL of blood was drawn from each patient 1 hour preoperatively into a serum separator gel tube. After 30 minutes of clotting time, serum was collected and frozen at -80 degrees C. The CABA test was performed on the samples by an investigator blinded to the patient's condition, and values were compared with the clinical and pathologic diagnosis of ischemic bowel postoperatively. CABA test values are reported as absorbance units (ABSU) at 470 nm. Of the 26 patients enrolled in the study, 12 were clinically diagnosed with intestinal ischemia. These patients had significantly higher CABA test values (0.52 ABSU +/- 0.04 SEM) than patients without intestinal ischemia (0.31 ABSU +/- 0.02 SEM, p = 0.00023). Only two false-positives and no false-negatives were recorded. This resulted in a sensitivity of 100% and a specificity of 85.7% for the CABA test for these particular samples. The CABA test could be a useful tool for clinicians in the risk stratification of intestinal ischemia.
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PMID:Clinical utility of the cobalt-albumin binding assay in the diagnosis of intestinal ischemia. 1818 97

Depleted fullerene soot (DFS) with fullerene residue content of about 2.2-3.2% are investigated in order to elucidate the possibility for their use as support of catalysts in low-temperature reduction of NO with CO. Bimetalic copper-cobalt and copper-manganese oxides supported on DFS are prepared. All samples are characterized by chemical analysis, XRD, SEM, IR spectroscopy, XPS, nitrogen adsorption measurements. The two DFS supported bimetallic catalysts manifest a high activity towards the reduction of NO with CO at temperatures below 150 degrees C, the CuCo/DFS being the more active one. The peculiarity of the support DFS predetermines the porous texture of the catalysts. The occurrence of a specific metal-support interaction favors the formation of the mixed oxide spinels CuCo2O4 and Cu1.5 Mn1.5 O4 that are responsible for the enhanced activity.
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PMID:Novel application of depleted fullerene soot (DFS) as support of catalysts for low-temperature reduction of NO with CO. 1819 47

Inhalation of cobalt (Co) and tungsten carbide (WC) particles, but not Co or WC alone, may cause hard metal disease, risk of which does not appear to be uniform across cemented tungsten carbide (CTC) production processes. Inhalation of Co alone or in the presence of WC may cause asthma. Hypothesizing that aerosol size, chemical content, heterogeneity, and constituent compaction may be important exposure factors, we characterized aerosols from representative CTC manufacturing processes. Six work areas were sampled to characterize aerosol size distributions (dust, Co) and 12 work areas were sampled to characterize physicochemical properties (using scanning electron microscopy with energy dispersive x-ray spectrometry [SEM-EDX]). Bulk feedstock and process-generated powders were characterized with SEM-EDX and x-ray diffraction. The dust mass median diameter was respirable and the cobalt respirable mass fraction was highest (37%) in grinding. Morphology of particles changed with processing: individual, agglomerate, or aggregates (pre-sintered materials), then mostly compacted particles (subsequent to sintering). Elemental composition of particles became increasingly heterogeneous: mostly discrete Co or W particles (prior to spray drying), then heterogeneous W/Co particles (subsequent work areas). Variability in aerosol respirability and chemical heterogeneity could translate into differences in toxicity and support detailed characterization of physicochemical properties during exposure assessments.
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PMID:Characteristics of dusts encountered during the production of cemented tungsten carbides. 1821 75


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