Empyrean series 2

The FTIR spectra were obtained by using Bruker–Vertex 60. The various surface functional groups present in the adsorbents that may aid in the adsorption process were identified using the FTIR analysis. This was observed within a wavelength of 4000 to 400 cm^-1 (Fig. 1). The X-ray diffractometer (Panalytical Empyrean Series 2) was employed to study the structure of the adsorbents. Copper K alpha served as the radiation source and Nickel was used as the filter medium for the analysis. The K radiation was maintained at 1.54 Å and using a current and voltage of 40 mA and 45 kV respectively. The diffraction pattern is presented in Fig. 2.Figure 1

FTIR spectra of (A1) as-prepared alumina (A2) modified alumina with ratio of 1:0.5 and (A3) modified alumina with ratio of 1:1.

Figure 2

XRD patterns for (A1) as-prepared alumina (A2) modified alumina with ratio 1:0.5 and (A3) modified alumina with ratio 1:1.

16 samples of sediment were selected for analysis. These samples are all dark in color and were distinguished from the soft tissues as they were collected from regions usually beyond the body outline. The samples are from 11 resin slabs, representing four stratigraphic intervals (nine anuran sites). For each sample, a small amount (0.1–2 g) of sediment was powdered manually with a sterile agate pestle and mortar. XRD analysis was performed using a PANalytical Empyrean Series 2 microprobe with a Co X-ray tube, a PIXcel1D detector and a single crystal Si substrate.

The powder diffraction patterns were recorded in a PANalytical Empyrean Series 2 diffractometer with Cu Kα radiation, a step size of 0.0167°, a scanning time of 15 s per step, and 2θ range of 5 to 90° at ambient temperature. The single-crystal X-ray diffraction data were collected at 193(2) K using a Bruker-AXS D8 VENTURE diffractometer equipped with a PHOTON-100/CMOS detector (GaKα, λ = 1.3414 Å). The indexing was performed using APEX2, while data integration and reduction were completed using SaintPlus 6.01. Absorption correction was conducted using the multi-scan method implemented in SADABS. The space group was determined using XPREP implemented in APEX2.1. The structures were solved by direct methods and refined by nonlinear least-squares on F2 using SHELXL-97, OLEX2 v1.1.5, and WinGX v1.70.01 program packages. All non-hydrogen atoms were refined anisotropically. The contribution of disordered solvent molecules was treated using the Squeeze routine implemented in Platon.

XRD was conducted on
a PANalytical Empyrean Series 2 instrument using Cu Kα irradiation.

PXRD patterns were collected using a PANalytical Empyrean Series 2 diffractometer with Cu─Ka radiation, at room temperature, with a step size of 0.0167°, a scan time of 15 s per step, and 2θ ranging from 5° to 50°. The contents of Cu and Ti were measured by ICP-OES (Agilent 5110, USA). The ultimate element analysis was conducted using a CHNS elemental analyzer (Vario MICRO). The N₂ adsorption-desorption isotherms at 77 K were measured on a Micromeritics ASAP 2460 volumetric adsorption apparatus. The apparent BET-specific surface area was calculated using the adsorption branch with the relative pressure P/P₀ in the range of 0.005 to 0.3. The total pore volume (V_tot) was calculated on the basis of the adsorbed amount of nitrogen at the P/P₀ of 0.99. The PSD was calculated using the NLDFT methodology with nitrogen adsorption isotherm data and assuming a slit pore model. The time-dependent gas uptake profiles were recorded on an Intelligent Gravimetric Analyzer (IGA-100, HIDEN). The pressure was raised at a rate of 100 mbar min⁻¹ and kept for 60 min to reach full adsorption equilibriums.

TEM was conducted on a Thermo
Scientific (FEI) Talos F200X G2 TEM. All samples were dropcast on
carbon-coated Cu grids (300 mesh). X-ray powder diffractometry was
conducted on a PANalytical Empyrean Series 2 instrument using Cu Kα
irradiation.