Raw material prescription with hydrophile ion interchange and inphase opposition ion interchange separation mode chromatographic column and preparation
A technology of ion exchange and reversed-phase ions, applied in the field of electrochromatography, can solve the problems of brittle columns, high column packing skills, and low sample capacity, and achieve a wide range of separation objects, high space utilization, and fast mass transfer. Effect
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[0021] Example 1
[0022] 1. Pretreatment of capillary
[0023] Rinse the capillary empty column with 0.1 mol / L HCl solution for 30 minutes, then rinse with deionized water for 10 minutes, then rinse with 0.1 mol / L NaOH for 4 hours, then rinse with methanol for 15 minutes, and dry it with nitrogen until use;
[0024] 2. Silanization of the capillary wall
[0025] Inject a mixture of methanol and methacryloxypropyltrimethoxysilane in a volume ratio of 1:1 into the capillary treated in step 1, and react at 60°C for 24 hours to bond a layer with alkenyl groups on the capillary wall. The silanized substance; then rinse with methanol for 15 minutes; dry the capillary with nitrogen at 70°C;
[0026] 3. In-column synthesis
[0027] Glycidyl methacrylate, ethylene glycol dimethacrylate, propyl sulfonate methacrylate, N,N-dimethylformamide and 1,4-butanediol are respectively 29.6% by weight , 10.0%, 0.4%, 12.0%, 48.0%, the amount of initiator azobisisobutyronitrile (AIBN) added is 0.3% of ...
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[0029] Example 2
[0030]Combine glycidyl methacrylate, ethylene glycol dimethacrylate, methacryloxyethyl trimethylammonium chloride, N,N-dimethylformamide and 1,4-butanediol by weight The ratios are respectively 22.2%, 7.5%, 0.3%, 14.0%, and 56.0%. The amount of initiator azobisisobutyronitrile (AIBN) added is 0.3% of the total amount of the matrix monomer and ionic monomer. The raw materials are mixed according to the above formula, the resulting mixture is ultrasonically oscillated for 15 minutes, and nitrogen is blown for 10 minutes to remove the dissolved oxygen in the mixture, and then the mixture is injected into the silanized capillary, and the length of the capillary is controlled. After the reaction is completed, the capillary column is rinsed with methanol to remove the residual reagents in the column; then, the capillary column is filled with 1mol / L hydrochloric acid solution and heated in a 60℃ water bath for 4 hours. After hours, rinse the capillary column with water...
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