Synthetic method for high-performance liquid-phase chromatography column packing materials
A technology of high performance liquid chromatography and synthesis method, which is applied in the field of synthesis of high performance liquid chromatography column packing material TiO2/MWCNTs, can solve the problems of limited application of metal oxide packing, complex surface properties, tailing of chromatographic peaks, etc. The effect of short cycle, low cost and simple process flow
Inactive Publication Date: 2013-07-17
SHANGHAI UNIV
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Problems solved by technology
However, due to the complex surface properties of metal oxides and the existence of various active sites, metal oxide fillers can specifically adsorb certain samples, resulting in severe tailing or even dead adsorption of chromatographic peaks. These problems also limit the use of metal oxides. Application of Packing in Chromatography
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Embodiment 1
[0023] Concrete preparation steps:
[0024] a. Weigh 0.025 g MWCNTs with an electronic balance and add to 40 mL 0.08 mol / L TiF 4 aqueous solution, and ultrasonic for 30 min to make it evenly mixed;
[0025] b. Transfer the above solution into a self-made sealed bag, and place it in the irradiation area under the electron accelerator for irradiation, with an irradiation dose of 280 kGy;
[0026] c. Transfer the irradiated solution into a 200 mL beaker, seal it with parafilm and put it in an oven at 60 °C for 20 h;
[0027] d. wash the reaction product with water and ethanol successively;
[0028] e. Put the washed product in a vacuum oven at 60 °C for 6 h to obtain TiO 2 / MWCNTs composite filling material.
Embodiment 2
[0030] The steps in this embodiment are exactly the same as those in Embodiment 1 above. The difference is: weigh 0.050 g MWCNTs.
Embodiment 3
[0032] The steps in this embodiment are exactly the same as those in Embodiment 1 above. The difference is: weigh 0.075 g MWCNTs.
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The invention relates to a synthetic method for high-performance liquid-phase chromatography column packing materials. The synthetic method includes 1, buying market-sold multi-walled carbon nanotubes (MWCNTs) and taking 0.1g of the MWCNTs, adding 15ml thick HNO3 (Nitric acid) and 45ml thick H2SO4 (sulfuric acid) sequentially, performing ultrasonic processing for a period of time respectively, washing the mixture repeatedly with deionized water to be neutral, drying the mixture at the temperature of 100 DEG C for 12 hours, weighting proper processed MWCNTs and adding the MWCNTs into a titanium fluoride (TiF4) solution with certain concentration, and performing the ultrasonic processing on the mixed solution for 30 minutes to mix the mixed solution evenly; 2, pouring the prepared solution into a self-sealed bag, and placing the solution under a 2.5MeV (million electron volt) and 40mA (milliampere) electronic accelerator to be irradiated; 3, transferring the solution into a 200ml beaker, sealing the beaker with a sealing film, and putting the beaker in a baking oven at the temperature of 60 DEG C for 20 hours; and 4, washing the reacted products with water and ethanol sequentially, putting the washed products into a vacuum drying oven at the temperature of 60 DEG C for 6 hours, and then obtaining TiO2 (titanium dioxide)/ MWCNTs. TiO2/MWCNTs high-performance liquid-phase chromatography column packing materials prepared by the synthetic method have good separating efficiency, and separating detection effects of organic pollutants can be effectively improved.
Description
technical field [0001] The invention relates to a high performance liquid chromatography column packing material TiO 2 The invention discloses a method for synthesizing MWCNTs, belonging to the technical fields of material synthesis and radiation chemistry. Background technique [0002] High-performance liquid chromatography has become one of the indispensable methods in modern scientific research, and plays an important role in industry, agriculture, medicine, medicine, life science, environmental science, material science and other fields. At the same time, with the development of science and technology, the types and complexity of samples faced by HPLC have increased, and the requirements for separation effects have increased. In order to meet the requirements of different fields, new technologies and methods of liquid chromatography are also developing rapidly. As the "heart" of liquid chromatography, column packing materials are the focus of liquid chromatography resea...
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IPC IPC(8): B01J20/286B01J20/30
Inventor 潘赟程伶俐刘强
Owner SHANGHAI UNIV
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