The pH value of muskeg soils was characterized by using a digital pH meter (HQ411d Benchtop pH/mV Meter) equipped with a glass electrode probe. A standard procedure for calibrating pH meters was implemented by plotting the measured potential as a function of pH. The morphological characteristics of the muskeg specimens before and after modification were evaluated using a Leica EZ4 stereomicroscope equipped with KL 1500 LCD and a FEI Quanta 600 field emission scanning electron microscope (FE-SEM) equipped with a conventional Everhart-Thornley detector, back-scattered electron detector, and IR-CCD chamber camera. An accelerating voltage of 10–20 kV was used to image the muskeg. The chemical composition of muskeg was evaluated by energy-dispersive X-ray spectroscopy (EDS) using an Oxford Instruments silicon drift detector. Fourier transform infrared (FT-IR) spectra were obtained using a Bruker VERTEX 70 instrument in the range of 4000–500 cm−1 with a spectral resolution of 4 cm−1.
Silicon drift detector
Manufactured by Oxford Instruments
Sourced in United Kingdom
A silicon drift detector (SDD) is an x-ray detector used in various analytical techniques, such as energy-dispersive X-ray spectroscopy (EDS) and X-ray fluorescence (XRF) analysis. The core function of an SDD is to detect and measure the energy of X-ray photons emitted from a sample, enabling the identification and quantification of the elements present in the sample.
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4 protocols using silicon drift detector
1
Characterization of Muskeg Soil Properties
2
Elemental Analysis using SEM-EDS
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Element analysis is a technique used to analyze the chemical makeup of a sample. To enable qualitative and quantitative microanalyses, an energy-dispersive X-ray spectrometer (silicon drift detector; Oxford Instruments, Oxford, UK) was attached to the SEM. As a type of spectroscopy, this approach investigates a sample based on interactions between electromagnetic radiation and matter and analyzes X-rays emitted by that matter in response to bombardment with charged particles.
3
Morphological Characterization of Electrodes using FE-SEM and EDX
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Field Emission Scanning Electron Microscopy (FE-SEM) coupled with energy-dispersive X-ray spectroscopy (EDX) was performed with a ΣIGMA high-resolution scanning electron microscope (Carl Zeiss Microscopy GmbH, Germany). The electrodes' morphological characterization was assessed on the uncoated working electrode surface, using an acceleration potential of 2 kV at a working distance of about 4 mm. Energy-dispersive X-ray analysis (EDX) was performed using a silicon drift detector (Oxford Instruments) coupled with SEM using a working distance of about 8.5 mm and an accelerating potential of 15 kV, analyzing a sampling area ranging from 0.06 to 0.09 mm 2 .
4
Comprehensive Surface Analysis via SEM Photomosaics
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For each of the exposed surfaces of the sample (top surface and 4 lateral surfaces), a grid 12 of SEM images was acquired to compose a photomosaic of the entire surface. The 13 analysis was performed on a JEOL 5310--LV system, equipped with a secondary and 14 backscattered electron detector and an Oxford Instruments silicon--drift detector for EDS 15 analysis. A total of 300 backscattered SEM images were acquired at each plane, resulting 16 in a total of 1500 images, which had to be taken manually since the JEOL 5310 is not 17 equipped with automated stage control. The SEM was operated at 20 kV with a spot size 18 of 13 nm and a working distance of 20 mm. Images were stitched together using the 19 Microsoft Image Composite Editor (ICE; http://research.microsoft.com), which has 20 algorithms for automatic grid--based registration of images. Next, EDS mappings were 21 obtained, at 24 to 28 images per side. Due to time restrictions, only half of the surface of 22 the SEM photomosaics was covered, at half the magnification. This resulted in 125 23 separate acquisitions, taking over 40 hours to acquire the data. 24
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