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3 protocols using d max 2500 5 x ray diffractometer

1

Comprehensive Characterization of Material Properties

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X-ray powder diffraction (XRPD) patterns were recorded using a Rigaku-D/max 2500 V X-ray diffractometer equipped with a source of Cu-Kα radiation (λ = 1.54178 Å) (Rigaku, Tokyo, Japan). Scanning electron micrographs (SEM) were obtained using a Sigma-300 scanning electron microscope (Zeiss, Jena, Germany). Infrared spectroscopy (IR) and thermogravimetric analysis (TGA) were carried out using an EQUINOX 55 spectrometer (Bruker, Germany) and STA449C apparatus (NETZSCH, Selb, Germany), respectively. The BET surface areas and pore distributions were tested based on N2 adsorption using GEMINI VII 2390 apparatus (Micromeritics, Georgia, USA) at 77 K. Before BET testing, the powder was degassed at 200 °C for 8 h. The sample extracts were flowed through SPE columns using a vacuum pump (Yiheng, Shanghai, China). The chromatographic separation and detection of SAs were carried out using a Waters Acquity UHPLC system coupled to a Waters Xevo G2 QTOF mass spectrometer (Waters, USA) equipped with an ACQUITY UHPLC® BEH C18 column (2.1 mm × 50 mm, 1.7 μm).
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2

Multimodal Analysis of Material Characterization

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X-ray powder diffraction (XRPD) patterns were recorded on a Rigaku-D/max 2500 V X-ray diffractometer equipped with a source of Cu-Kα radiation (λ = 1.54178 Å) (Rigaku, Tokyo, Japan). The scanning electron micrographs (SEM) were obtained from a model S-3700 scanning electron microscope (Hitachi, Kyoto, Japan). The infrared spectrum (IR) and thermogravimetric analysis (TGA) were measured by using an EQUINOX 55 spectrometer (Bruker, Germany) and STA449C (NETZSCH, Selb, Germany), respectively. The BET surface area and pore distribution were tested by N2 adsorption on GEMINI VII 2390 (Micromeritics, Georgia, USA) under 77 K. Water samples flowed the SPE column by a vacuum pump (Yiheng, Shanghai, China).
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3

Characterization of Porous Calcium Carbonate

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The X-ray diffraction (XRD) patterns were recorded on a Rigaku D/MAX 2500 V X-ray diffractometer (Rigaku, Tokyo, Japan) with Cu Kα radiation used for phase detection. The microstructure of the samples was obtained by a Hitachi SU8220 scanning electron microscope (Hitachi Limited, Tokyo, Japan). Fourier transform infrared (FT-IR) spectra were obtained by a Tensor II FT-IR spectrometer (Bruker, Mannheim, Germany) using KBr pellets in the range of 4000–400 cm−1 to investigate the chemical nature of the particles. The pore volume, BET-specific surface area, and BJH pore size of the porous calcium carbonate were determined by N2 adsorption–desorption measurements using an ASAP 2020 (Micrometrics, Norcross, GA, USA). The X-ray photoelectron spectroscopy (XPS) profiles were recorded on a Thermo Scientific K-Alpha (Thermo Fisher Scientific, Waltham, MA, USA). Thermogravimetric (TG-DTG) analysis was performed on a Thermo Plus EVO2 thermogravimetric analyzer (Rigaku, Japan) under a N2 atmosphere at 10 °C/min from 30 °C to 800 °C. The PCC/PAA sample saturated with water absorption was cut into cuboid shapes (the length, width, and height were 3 cm, 3 cm, and 2 cm, respectively, and the weight was approximately 18 g), and the compressive test of samples was performed using a universal electronic material testing machine (Instron, Norwood, MA, USA) at a compression rate of 5 mm/min.
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