The prepared mild steel samples were immersed in a test solution of 0.1 M HCl (100 mL) with and without 1 mM concentration of L1 and L2 inhibitors in their respective beakers at 303 K and were subjected to an exposure period of 3 h in a thermostat water bath and afterwards removed from the solution and rinsed using distilled water and acetone respectively. It was allowed to dry and stored in a desiccator before the analysis of the surface morphology. The scanning electron microscope on (SEM, Quanta 450 FEI, voltage 10 kv, spot size 9 mm and magnification range 2228–2382 with 10 μm scale bar model: Σigma HD, Zeiss, Germany).
σigma hd
Manufactured by Zeiss
Sourced in Germany
The ΣIGMA-HD is a high-performance laboratory equipment designed for precision measurements and analysis. It features advanced optics and sophisticated digital processing capabilities to provide accurate and reliable data. The core function of the ΣIGMA-HD is to enable precise quantitative assessments of various samples and materials.
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6 protocols using σigma hd
1
Inhibitor Evaluation on Mild Steel
2
Mineral Morphology and Electrochemical Analysis
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The morphology of the minerals was observed using the field-emission scanning electron microscope (FE-SEM) (ΣIGMA-HD, ZEISS). The chemical components of pyrite and chalcopyrite were obtained using an X-ray fluorescence analyzer EDX 8300 manufactured by Suzhou Precision Instrument Co., Ltd. Electrochemical measurements were performed with a CHI 750D workstation (Shanghai Chenhua, China). A conventional three electrode system with pyrite or chalcopyrite as working electrode, a thin Pt wire as counter electrode and Ag/AgCl (sat. KCl) as reference electrode was employed in this study. All measurements were performed in air at room temperature of approximately 20 °C.
3
Electrochemical Characterization of Modified Electrodes
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The X-ray diffraction (XRD) pattern was taken from 5° to 60° (2θ value) with Cu-Kα radiation (λ = 1.541 Å) by an X’ Pert Powder X-ray diffractometer (X’Pert PRO, PANalytical, Almelo, The Netherlands). Fourier transform infrared spectrometry (FT-IR) spectra were measured using a Nicolet IS 10 (Thermo Scientific, Madison, WI, USA) equipped in the range of 500–4000 cm−1, the average scanning frequency of the instrument was 16 times. The synthesized monomer and polyimide were analyzed by proton nuclear magnetic resonance (1H-NMR) spectra on a Bruker Advance-AV 500 MHz instrument (Bruker, Karlsruhe, Germany) in deuterated dimethyl sulfoxide. The morphologies of the modified electrode surfaces were observed using the field emission scanning electron microscope (FE-SEM, ΣIGMA-HD, ZEISS, Oberkochen, Germany). Electrochemical measurements were performed with a CHI 750D workstation (Shanghai Chenhua, Shanghai, China). A conventional three electrode system with PI modified GCE as working electrode, a 1.0 mm diameter of Pt wire as counter electrode, and Ag/AgCl (sat. KCl) as reference electrode was employed in this study. All measurements were performed in air at room temperature of approximately 20 °C.
4
Multimodal Characterization of Electrode Surfaces
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X-ray diffraction (XRD)
measurements were
performed with a Bruker D8 Advance diffractometer. X-ray fluorescence
(XRF) experiments were carried out with an S8TLGER (Bruker). The morphologies
of the modified electrode surfaces were observed using field emission
scanning electron microscopy (FE-SEM, ΣIGMA-HD, ZEISS, Germany).
Raman spectroscopy was performed using a laser micro-Raman spectrometer
(JASCO NRS-4100, Japan) with an excitation wavelength of 532.0 nm
laser with a working distance on a ×100 lens. The Raman spectra
of MLN, MLN/TYR, and MLN/AO/TYR were recorded by depositing the samples
on a GCE rod (3 mm in diameter and 5 mm in length). All electrochemical
measurements such as cyclic voltammetry (CV), constant-potential amperometry,
and electrochemical impedance spectroscopy (EIS) were performed with
a CHI 660E workstation (Shanghai Chenhua, China). Quartz crystal microbalance
with dissipation (QCM-D) measurements were performed with a Q-Sense
analyzer (Biolin Scientific) equipped with a MoS2-coated
sensor tip.
measurements were
performed with a Bruker D8 Advance diffractometer. X-ray fluorescence
(XRF) experiments were carried out with an S8TLGER (Bruker). The morphologies
of the modified electrode surfaces were observed using field emission
scanning electron microscopy (FE-SEM, ΣIGMA-HD, ZEISS, Germany).
Raman spectroscopy was performed using a laser micro-Raman spectrometer
(JASCO NRS-4100, Japan) with an excitation wavelength of 532.0 nm
laser with a working distance on a ×100 lens. The Raman spectra
of MLN, MLN/TYR, and MLN/AO/TYR were recorded by depositing the samples
on a GCE rod (3 mm in diameter and 5 mm in length). All electrochemical
measurements such as cyclic voltammetry (CV), constant-potential amperometry,
and electrochemical impedance spectroscopy (EIS) were performed with
a CHI 660E workstation (Shanghai Chenhua, China). Quartz crystal microbalance
with dissipation (QCM-D) measurements were performed with a Q-Sense
analyzer (Biolin Scientific) equipped with a MoS2-coated
sensor tip.
5
Hydrogel Structure Analysis via SEM
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To investigate the structure and surface morphology of the hydrogel, samples were frozen with liquid nitrogen and then freeze-dried. For the anisotropic hydrogel samples, after freezing with liquid nitrogen, they were cut along the directions parallel and perpendicular to the hydrogel fibers to reveal the internal structure. The lyophilized hydrogels were sputtered with gold and observed using SEM (ΣIGMA-HD, ZEISS) at an acceleration voltage of 8 kV.
6
Characterizing Modified Surface Morphology
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A scanning electron microscopy (SEM, ΣIGMA-HD, ZEISS) was used to evaluate the morphology of a modified surface. A laser confocal high-temperature scanning microscope (LCSM, VL2000DX, Yonekura MFG Co., Ltd.) was used to understand the surface roughness. X-ray diffraction (XRD, X'Pert Powder, PANalytical) patterns were collected using Cu Kα radiation. X-ray fluorescence (XRF, S8TLGER, Bruker) was carried out to quantify the components of MLN. Cyclic voltammogram (CV) analysis, electrochemical impedance spectroscopy (EIS), and amperometric i-t curve were performed on a CHI 750E electrochemical workstation (Shanghai, China). A conventional three-electrode system was used for electrochemical experiments, which consisted of a platinum wire as counter electrode, and Ag/AgCl (saturated in 3.0 M of KCl) as a reference electrode, and a modified GCE as a working electrode. All experiments were performed at room temperature.
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