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2.1. Materials Palygorskite (PAL) powder was provided by the Mingguang Colloidal Co. Ltd., (Anhui, China), and was dried to constant weight at 105 °C before use. Methylene blue (MB) was purchased from Alfa Aesar, Ward Hill, MA, U.S.A., used without further purification. The solution was prepared with distilled water. 2.2. Methods 1.0 kg of raw PAL was put in the helical disc stone miller with diameter of 22 cm (Xinkun Stone machinery Factory, Shandong, China) at 10 rpm and grinded for 0–10 times with each times of 60 min, then the samples were sieved through a screen with diameter of 75 μm. The samples were denoted as PAL-0 to PAL-10 according to the grinding times, respectively. FTIR spectra of the samples were recorded with a Nicolet Nexus TM spectrophotometer (Thermo, Madison, USA) in the range of 4000–400 cm−1 using KBr pellets. FESEM observations were carried out employing a JSM-6701F field emission scanning electron microscope (JEOL) after coating the sample with gold. XRD analysis was performed using an X-ray powder diffractometer with Cu anode (PAN analytical Co. X'pert PRO), running at 40 kV and 30 mA. The specific surface area and pore structure were analyzed with an Accelerated Surface Area and Porosimetry System (Micromeritics, ASAP 2020, Atlanta, USA) using N2 as an adsorbate at −196 °C. The BET specific surface area (SBET) [19] was examined using the data in the relative pressure range of 0.1–0.3 and the micropore volume (Vmicro), micropore area (Smicro) and external surface area (Sext) were determined by t-plot method. The mesopore volume (Vmeso) was determined by subtracting the micropore volume from the volume of N2 adsorbed at a relative pressure of 0.95. The pore-size distribution was estimated by the Barrett–Joyner–Halenda (BJH) method [20,21]. The microstructural parameters of PAL samples were analyzed in triplicate and the standard deviation was lower than 1%. The adsorption properties of treated PAL samples toward MB were investigated. The experimental conditions were 0.025 g of grinded PAL sample mixed with 50 mL of 500 mg/L MB solution (pH=7.0) in 100 mL flask, and shaken on a thermostatic shaker (THZ–98) with a constant speed of 120 rpm at 30 °C for 660 min to reach the adsorption equilibrium. The residual concentration of MB solution after adsorption was measured with a Specord 200 UV/visible spectrophotometer (Germany) by monitoring the absorbance at a wavelength of maximum absorbance (670 nm). |
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