51 research outputs found

    Experimental methods in chemical engineering: X ‐ray absorption spectroscopy— XAS , XANES , EXAFS

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    Although X-ray absorption spectroscopy (XAS) was conceived in the early 20th century, it took 60 years after the advent of synchrotrons for researchers to exploit its tremendous potential. Counterintuitively, researchers are now developing bench type polychromatic X-ray sources that are less brilliant to measure catalyst stability and work with toxic substances. XAS measures the absorption spectra of electrons that X-rays eject from the tightly bound core electrons to the continuum. The spectrum from 10 to 150 eV (kinetic energy of the photoelectrons) above the chemical potential—binding energy of core electrons—identifies oxidation state and band occupancy (X-ray absorption near edge structure, XANES), while higher energies in the spectrum relate to local atomic structure like coordination number and distance, Debye-Waller factor, and inner potential correction (extended X-ray absorption fine structure, EXAFS). Combining XAS with complementary spectroscopic techniques like Raman, Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), and electron paramagnetic resonance (EPR) elucidates the nature of the chemical bonds at the catalyst surface to better understand reaction mechanisms and intermediates. Because synchrotrons continue to be the light source of choice for most researchers, the number of articles Web of Science indexes per year has grown from 1000 in 1991 to 1700 in 2020. Material scientists and physical chemists publish an order of magnitude articles more than chemical engineers. Based on a bibliometric analysis, the research comprises five clusters centred around: electronic and optical properties, oxidation and hydrogenation catalysis, complementary analytical techniques like FTIR, nanoparticles and electrocatalysis, and iron, metals, and complexes

    Experimental methods in chemical engineering: X-rayabsorption spectroscopy—XAS, XANES, EXAFS

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    Although X-ray absorption spectroscopy (XAS) was conceived in the early 20th century, it took 60 years after the advent of synchrotrons for researchers to exploit its tremendous potential. Counterintuitively, researchers are now developing bench type polychromatic X-ray sources that are less brilliant to measure catalyst stability and work with toxic substances. XAS measures the absorption spectra of electrons that X-rays eject from the tightly bound core electrons to the continuum. The spectrum from 10 to 150 eV (kinetic energy of the photoelectrons) above the chemical potential—binding energy of core electrons—identifies oxidation state and band occupancy (X-ray absorption near edge structure, XANES), while higher energies in the spectrum relate to local atomic structure like coordination number and distance, Debye-Waller factor, and inner potential correction (extended X-ray absorption fine structure, EXAFS). Combining XAS with complementary spectroscopic techniques like Raman, Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), and electron paramagnetic resonance (EPR) elucidates the nature of the chemical bonds at the catalyst surface to better understand reaction mechanisms and intermediates. Because synchrotrons continue to be the light source of choice for most researchers, the number of articles Web of Science indexes per year has grown from 1000 in 1991 to 1700 in 2020. Material scientists and physical chemists publish an order of magnitude articles more than chemical engineers. Based on a bibliometric analysis, the research comprises five clusters centred around: electronic and optical properties, oxidation and hydrogenation catalysis, complementary analytical techniques like FTIR, nanoparticles and electrocatalysis, and iron, metals, and complexes.The authors acknowledge travel support from the Eras-mus+KA107 (2018-1-ES01-KA107-049563) and funding for the open access charge from the Universidad deMÁlaga/CBUA. This work was undertaken, in part,thanks to funding from the Canada Research Chairs pro-gram (950-231476)

    Supported molybdenum carbide for higher alcohol synthesis from syngas

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    Molybdenum carbide supported on active carbon, carbon nanotubes, and titanium dioxide, and promoted by K2CO3, has been prepared and tested for methanol and higher alcohol synthesis from syngas. At optimal conditions, the activity and selectivity to alcohols (methanol and higher alcohols) over supported molybdenum carbide are significantly higher compared to the bulk carbide. The CO conversion reaches a maximum, when about 20 wt% Mo2C is loaded on active carbon. The selectivity to higher alcohols increases with increasing Mo2C loading on active carbon and reaches a maximum over bulk molybdenum carbide, while the selectivity to methanol follows the opposite trend. The effect of Mo2C loading on the alcohol selectivity at a fixed K/Mo molar ratio of 0.14 could be related to the amount of K2CO3 actually on the active Mo2C phase and the size, structure and composition of the supported carbide clusters. Unpromoted, active carbon supported Mo2C exhibits a high activity for CO conversion with hydrocarbons as the dominant products. The K 2CO3 promoter plays an essential role in directing the selectivity to alcohols rather than to hydrocarbons. The optimum selectivity toward higher alcohols and total alcohols is obtained at a K/Mo molar ratio of 0.21 over the active carbon supported Mo2C (20 wt%)

    Abdominal drainage after elective colorectal surgery: propensity score-matched retrospective analysis of an Italian cohort

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    background: In italy, surgeons continue to drain the abdominal cavity in more than 50 per cent of patients after colorectal resection. the aim of this study was to evaluate the impact of abdominal drain placement on early adverse events in patients undergoing elective colorectal surgery. methods: a database was retrospectively analysed through a 1:1 propensity score-matching model including 21 covariates. the primary endpoint was the postoperative duration of stay, and the secondary endpoints were surgical site infections, infectious morbidity rate defined as surgical site infections plus pulmonary infections plus urinary infections, anastomotic leakage, overall morbidity rate, major morbidity rate, reoperation and mortality rates. the results of multiple logistic regression analyses were presented as odds ratios (OR) and 95 per cent c.i. results: a total of 6157 patients were analysed to produce two well-balanced groups of 1802 patients: group (A), no abdominal drain(s) and group (B), abdominal drain(s). group a versus group B showed a significantly lower risk of postoperative duration of stay >6 days (OR 0.60; 95 per cent c.i. 0.51-0.70; P < 0.001). a mean postoperative duration of stay difference of 0.86 days was detected between groups. no difference was recorded between the two groups for all the other endpoints. conclusion: this study confirms that placement of abdominal drain(s) after elective colorectal surgery is associated with a non-clinically significant longer (0.86 days) postoperative duration of stay but has no impact on any other secondary outcomes, confirming that abdominal drains should not be used routinely in colorectal surgery
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