2026-10-14T15:58:03Z https://www.scidb.cn/oai

10.57760/sciencedb.41593 2026-07-06T14:36:33Z

2026-07-06 Undergraduate Comprehensive Experiment: Construction of a New Dispersion Solid Phase Extraction Method Based on Halogen Bond Organic Framework Materials and Its Application in Analysis of Brominated Flame retardants doi:10.57760/sciencedb.41593 en This dataset systematically records the entire process of adsorbent XOF-1 development and trace bromobisphenol A (TBr BPA) detection method research conducted by the Drug Analysis Laboratory of Southwest Medical University, covering spatial, temporal, and multidimensional experimental data. The experiment will be conducted in the academic year 2024-2025, with a total of 16 class hours (pre class 2+in class 12+post class 2). The synthesis of XOF-1, infrared characterization, development of dispersion solid-phase extraction (DSPE) method, and HPLC detection will all be completed in the Drug Analysis Laboratory of Southwest Medical University. The material microstructure characterization (SEM, TEM) will be carried out in the Baice Laboratory of Zhongke; Actual water samples were collected from three typical substrates - tap water from Southwest Medical University, campus pond water, and Tuojiang water from the upper reaches of the Yangtze River (Luzhou section, Sichuan), and the reliability of the method was verified through spiked recovery experiments. The dataset contains 6 types of core data: ① XOF-1 synthesis data, with detailed records of raw material dosage (AgOTf 15.42mg, TPy 12.36mg), reaction conditions (room temperature stirring for 1 hour, 130 ℃ N ₂ protection for 5 hours), centrifugation parameters (7600r/min × 5 minutes), and product processing flow, supporting the validation of synthesis reproducibility; ② Material characterization data were integrated, including PXRD crystal plane diffraction peaks (2 θ=5.05 °, 6.52 °), FT-IR functional group shifts, ¹ H NMR proton signals, TGA thermal stability (weight loss of 4.30% before 360 ° C), Zeta potential (isoelectric point pH ≈ 11.36), and water contact angle (29.30 °), to clarify the material structure and physicochemical properties; ③ The adsorption isotherm data covers the adsorption capacities of TBr BPA, TCl BPA, and HBB at initial concentrations of 0-800 μ g/mL (calculated as Q=(C ₀ - C ₑ) V/m), revealing a saturated adsorption capacity of approximately 21mg/g for TBr BPA; ④ Adsorption kinetics data, tracking the adsorption dynamics of the target substance at 400 μ g/mL within 0-300min, showed an equilibrium time of approximately 150min for TBr BPA/TCl BPA and 120min for HBB; ⑤ DSPE condition optimization data, system investigation of adsorbent dosage (0.5-2.5mg), pH (3-11), salt concentration (0-10mmol/L), and desorption parameters to determine the optimal pretreatment plan (1.5mg adsorbent pH=7、 Methanol desorption for 15 minutes x 3 times); ⑥ The actual water sample spiked recovery data (Table 1) includes 9 independent experiments (3 types of water samples x 3 spiked concentrations: 10, 25, 50 μ g/L), recording the spiked amount, measured value, recovery rate (60%~90%), and RSD (<5.3%, n=3), confirming the reliability of the method in actual matrices, and matrix effects are the main cause of differences in recovery rates. All data are recorded in experiments and instrument raw outputs (chromatograms, spectra), and plotted using Orign software. All physical units are standardized, and data errors are mainly caused by operational randomness. The overall range is controllable, with RSD values below 5.3%. The difference in recovery rates between different water samples is mainly due to matrix effects, which is in line with the conventional characteristics of teaching experiments and trace analysis. It can provide complete data support for the development of adsorption materials, validation of environmental water sample pretreatment methods, and analytical chemistry teaching.  comprehensive experiment; pharmaceutical analysis; halogen-bonded organic frameworks; dispersive solid phase extraction; brominated flame retardants Die Gao PUBLIC https://creativecommons.org/licenses/by-nc-nd/4.0/ dataset Science Data Bank