Herein, novel, loose, and porous graphite phase carbon nitride/porous carbon (g-C₃N₄@PC) composites were prepared by decorating cellulose nanocrystals (CNCs). The characterization results demonstrate that the as-prepared composites presented high specific surface areas, porous structures, and abundant chemical groups, with the modification of CNCs. In view of the unique advantages, g-C₃N₄@PC was used as the coating material for the solid-phase microextraction (SPME) of organochlorine pesticides (OCPs) in water and juice samples. The g-C₃N₄@PC-coated fibers showed better extraction efficiencies than commercial fibers (100/7 μm PDMS and PA) toward the OCPs, with the enrichment factors of the g-C₃N₄@PC-coated fibers 5–30 times higher than the latter. Using a gas chromatography–mass spectrometry (GC-MS) instrument, the g-C₃N₄@PC-coated fibers exhibited a gratifying analytical performance for determining low concentrations of OCPs, with a wide linear range (0.1–1600 ng L⁻¹ for water; 0.1–1000 ng L⁻¹ for juice), low limits of detection (0.0141–0.0942 ng L⁻¹ for water; 0.0245–0.0777 ng L⁻¹ for juice), and good reproducibility and repeatability in optimal conditions. The established method showed good sensitivity and recovery in the determination of OCPs in the water and fruit juice samples, which displayed broad prospects for analyzing organic pollutants from environmental samples.

To remove the pollutant methylene blue (MB) from water, a sheet-like skeleton carbon derived from shaddock peels (SPACs) was prepared by NaOH activation followed by a calcination procedure under nitrogen protection in this study. Characterization results demonstrated that the as-prepared SPACs displayed a hierarchically porous structure assembled with a thin sheet-like carbon layer, and the surface area of SPAC-8 (activated by 8 g NaOH) was up to 782.2 m²/g. The as-prepared carbon material presented an ultra-fast and efficient adsorption capacity towards MB due to its macro-mesoporous structure, high surface area, and abundant functional groups. SPAC-8 showed ultrafast and efficient removal capacity for MB dye. Adsorption equilibrium was reached within 1 min with a removal efficiency of 99.6% at an initial concentration of 100 mg/g under batch adsorption model conditions. The maximum adsorption capacity for MB was up to 432.5 mg/g. A pseudo-second-order kinetic model and a Langmuir isotherm model described the adsorption process well, which suggested that adsorption rate depended on chemisorption and the adsorption process was controlled by a monolayer adsorption, respectively. Furthermore, column adsorption experiments showed that 96.58% of MB was removed after passing through a SPAC-8 packed column with a flow rate of 20 mL/min, initial concentration of 50 mg/L, and adsorbent dosage of 5 mg. The as-prepared adsorbent displays potential value in practical applications for dye removal due to its ultrafast and efficient adsorption capacity.