Urban mining by flash Joule heating

Precious metal recovery from electronic waste, termed urban mining, is important for a circular economy. Present methods for urban mining, mainly smelting and leaching, suffer from lengthy purification processes and negative environmental impacts. Here, a solvent-free and sustainable process by flash Joule heating is disclosed to recover precious metals and remove hazardous heavy metals in electronic waste within one second. The sample temperature ramps to ~3400 K in milliseconds by the ultrafast electrical thermal process. Such a high temperature enables the evaporative separation of precious metals from the supporting matrices, with the recovery yields >80% for Rh, Pd, Ag, and >60% for Au. The heavy metals in electronic waste, some of which are highly toxic including Cr, As, Cd, Hg, and Pb, are also removed, leaving a final waste with minimal metal content, acceptable even for agriculture soil levels. Urban mining by flash Joule heating would be 80× to 500× less energy consumptive than using traditional smelting furnaces for metal-component recovery and more environmentally friendly.

Accurate Determination of the Cold Detection Threshold with High-Speed Cooling of the Skin

Objective This study used high-speed cooling of the skin and exact control of stimulus duration to measure the cold detection threshold in healthy participants. The objective was to compare the method of limits, in which the temperature is slowly and gradually increased/decreased until the subject perceives the stimulation, and the method of levels, in which the subject must detect brief thermal stimulations close to the threshold of perception. Methods Twenty healthy volunteers (nine women, 11 men) aged 20–30 years participated in the study. The method of limits and method of levels were performed in all subjects in a counterbalanced order. Four cold detection thresholds were measured with the method of levels, with a temperature ramp of 300°C/sec and stimulus durations of 50 ms, 100 ms, 300 ms, and 500 ms. Three thresholds were measured with the method of limits, with temperature ramps of 1°C/sec, 2°C/sec, and 4°C/sec. Results On average, the cold detection thresholds were −0.47°C below skin temperature with the method of levels and −1.67°C the method of limits. Interindividual variability was significantly lower with the method of levels than with the method of limits. Conclusions These results suggest that the method of levels is more accurate than the method of limits for measuring cold detection threshold. The improvement of cold detection threshold measurement may provide new perspectives to more precisely assess the function of A-delta fibers and the spino-thalamic pathway.

Use of Temperature Controlled Stage Confocal Raman Microscopy to Study Phase Transition of Lead Dioxide (Plattnerite)

The present work concerns the study of the phase transition of plattnerite [β-PbO2 lead (IV) oxide]-based samples when they are analysed by Raman spectroscopy. The laser-induced degradation process was carried out either on historical painting samples, where plattnerite was present as a degradation product of lead-based pigments, or commercial plattnerite samples as powder and pellets. The Raman spectra of plattnerite taken at low excitation power, to avoid phase transformations, are reported up to low wavenumbers, and they were characterized by the features at 159, 380, 515 and 653 cm−1 and a shoulder at 540 cm−1. The degradation of plattnerite was induced by increasing the laser power on the sample, and the formation of its secondary products red lead (Pb3O4), litharge (α-PbO) and massicot (β-PbO), when varying the laser power, is discussed. The analyses were performed in a controlled condition by coupling the Raman spectrometer to a temperature-controlled stage (Linkam THMS600- Renishaw), which allows for varying the sample temperature (from room temperature up to 600 °C) and keeping it constant inside the stage during the analysis. In this way, commercial plattnerite samples were heated by increasing the cell temperature to verify the temperature range at which the phase transitions of lead dioxide occur. In addition, thanks to the construction of temperature ramps, all the degradation pathways were shown, and other lead compounds were identified, generated by the laser power contribution. A different behaviour was found between pigments from historical painting samples and commercial samples under the effect of the laser. This information could be useful in order to recognize their nature when they are found in cultural heritage materials.

Differential scanning calorimetry on micro hotplates for temperature calibration and mass quantification

In this work a novel calibration method for micro hotplates is developed and tested. The method is based on phase change processes of applied testing materials, which can be identified due to their phase change enthalpy in the power needed for the hotplate to linearly heat up. For traceability and reproducibility tests a ceramic heating element (Umweltsensortechnik GmbH, Geschwenda, Germany) including a Pt100 sensing element was used. Using the melting process of Hexatriacontane and different temperature ramps the feasibility of the method was tested, and the onset point of the phase change was identified as the best feature for temperature calibration. On this substrate we achieved an absolute deviation of 5 °C to literature values and a relative uncertainty of 0.3 °C. Pyrazine, which can be removed more easily, showed an absolute deviation of 2.5 °C to literature values and a relative uncertainty of again 0.3 °C for temperature calibration. The sublimation process of Hexamethylenetetramine was also tested but did not yield stable results. The two materials successfully tested on the ceramic heater were then transferred to MEMS membrane heaters (AS-MLV-P2 and AS-MLV, both metal oxide semiconductor gas sensors, ams AG, Premstätten, Austria) showing the applicability of the method for MEMS device calibration and yielding relative uncertainties for the calibrated heater resistance of 0.17 Ω (corresponding to 0.39 °C). For Hexatriacontane on the ceramic hotplate we also show the possibility of mass quantification through evaluating the phase change enthalpy.

Bonding States of Hydrogen in Plasma-Deposited Hydrocarbon Films

We applied temperature-programmed desorption (TPD) spectroscopy to study the bonding of hydrogen in amorphous hydrogenated carbon (a–C:H) films. Typical hard plasma-deposited a–C:H films with an initial hydrogen content (H/(H+C)) of about 30% were used as samples. About 85% of the initial hydrogen content is released in the form of H2, the rest in the form of hydrocarbons. Using a temperature ramp of 15 K/min, release of hydrogen starts at about 600 K with a first peak at about 875 K and a broad shoulder around 1050 K. The peak positions depend on the temperature ramp. This fact was exploited to determine the pre-exponential factor for an analytic analysis of the release spectra. This analysis revealed a pre-exponential factor of ν = 1 × 10 16 1/s, which deviates significantly from the frequently assumed prefactor 1 × 10 13 1/s. This higher prefactor leads to a shift in the determined binding energies by about +0.5 eV. Standard TPD measurements with linear temperature ramps up to 1275 K were complemented by so-called “ramp and hold” experiments with linear ramps up to certain intermediate temperatures and holding the samples for different times at these temperatures. Such experiments provide valuable additional data for investigation of the thermal behavior of the investigated films. Our experiments prove that the width of the hydrogen release spectrum is determined by a distribution of binding energies rather than release kinetics or diffusive effects. This binding energy distribution has a peak at about 3.1 eV and a shoulder at higher energies extending from about 3.6 to 3.9 eV.

Thermal Transitions of Cocoa Butter: A Novel Characterization Method by Temperature Modulation

For the first time, the novel experimental technique Temperature Modulated Optical Refractometry (TMOR) was employed for cocoa butter thermal transitions characterization. The average refractive index (NMEAN), the volume (v) change, and the volumetric expansion coefficient ( β q ) as well as the dynamic quantities β ′ and β ″ (real and imaginary volumetric expansion coefficient, respectively) were monitored during cooling and heating and compared to the heat flow curves obtained via the standard technique dynamic scanning calorimetry (DSC). The investigation of these quantities showed that TMOR analysis can yield not only thermal transitions temperatures that are comparable to DSC results, but also some new thermal events that are not detected by DSC. This outcome suggests that TMOR might provide some additional insights on cocoa butter melting and crystallization by means of frequency-dependent measurements due to temperature modulation. This new information that can be accessed during temperature ramps might provide a deeper insight into thermal behavior of fat-based foods, evidencing TMOR value as a tool for thermal transitions investigation.