Lead ion imprinting integral column and preparation method thereof

A lead ion, monolithic column technology, applied in the field of lead ion imprinted monolithic column and preparation, to achieve the effect of high adsorption capacity and selective identification

Inactive Publication Date: 2011-05-25
DALIAN OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Lead ion imprinting integral column and preparation method thereof
  • Lead ion imprinting integral column and preparation method thereof
  • Lead ion imprinting integral column and preparation method thereof

Examples

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experiment example 1

[0021] Experimental example 1: the embodiment of the present invention is connected on the pump of high performance liquid chromatography (HPLC) as chromatographic column, and preparation lead ion concentration is 3.3784 * 10 -7 mol / L solution as the mobile phase, measure 300mL and pass through the embodiment of the present invention at a flow rate of 0.4mL / min, then wash the column with pure water at a flow rate of 0.4mL / min to wash away the remaining unadsorbed lead ions. Finally, change the nitric acid of 0.5mol / L to elute the lead ion adsorbed by the chromatographic column at a flow rate of 0.2mL / min, collect the eluent 10mL, and pass through 4-sulfonic acid phenylporphyrin C 44 h 34 N 4 o 20 S 6 (TPPS4) adopts HPLC analysis after derivatization, and its chromatogram is as follows figure 2 It is shown in spectrum a.

[0022] Control experiment: replace the chromatographic column with a non-imprinted monolithic column (no template was added during synthesis), collect...

experiment example 2

[0024] Experimental example 2: selectivity experiment, connect the embodiment of the present invention on the HPLC pump, and prepare three kinds of ions of Pb(II), Cu(II), and Cd(II) whose concentration is 3.3784×10-7mol / L The mixed solution is used as the mobile phase, measure 300mL and pass it through the chromatographic column at a flow rate of 0.4mL / min, and then wash the chromatographic column with pure water at a flow rate of 0.4mL / min for 1h to wash away the residue in the chromatographic column that is not adsorbed by the chromatographic column. Ions, and finally change to 0.5mol / L nitric acid for elution, and collect 10mL of the eluent solution. 4-sulfophenylporphyrin C 44 h 34 N 4 o 20 S 6 (TPPS4) was derivatized and analyzed by HPLC, and the elution concentration of Pb(Ⅱ) was 4.63×10 -6 mol / L, copper ions and cadmium ions were not detected, indicating that the embodiment of the present invention has strong selective adsorption, and can be used for the enrichmen...

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Abstract

The invention discloses a lead ion imprinting integral column and a preparation method thereof. An imprinting polymer is the lead ion imprinting integral column which is prepared by an in-situ polymer molecular imprinting technique and comprises the following raw materials: lead ions serving as templates, methanol serving as a solvent, 4-vinylpyridine serving as a monomer, ethylene glycol dimethacrylate serving as a cross-linking agent, azobisisobutyronitrile serving as an initiator and dodecanol serving as a porogenic agent, wherein the mole ratio of the template to the monomer is 1:3, the volume fraction of the cross-linking agent is 25.0-30.0%, the concentration of the initiator is 0.9-1.1 mg/mL, and the volume fraction of the porogenic agent is 15.0-20.0%. Even though other competitive ions exist, the lead ion imprinting integral column has high absorption capability and selective recognition on free ions, the lead ions can be enriched from a solution containing trace lead ions, thereby achieving the purpose of concentrating the free ions. The lead ion imprinting integral column is suitable for high performance liquid chromatography and is in favor of further rapidly analyzing the lead ions.

Description

Technical field: [0001] The invention relates to a chromatographic column and a preparation method, in particular to a chromatographic column with high selectivity for adsorbing free lead ions (Pb ++ ) effect, the lead ion imprinted monolithic column and preparation method that can enrich the trace or trace free lead ions in the solution. Background technique: [0002] Molecularly imprinted technique (MIT) is a method of synthesizing a polymer with specific recognition for a certain molecule by simulating the molecular recognition principle of antibodies and antigens, enzymes and substrates. The polymer is called molecularly imprinted polymer (MIP). In the synthesis, imprinted molecules (templates), functional monomers and cross-linking agents are copolymerized, because there are generally covalent or non-covalent (hydrogen bonds, metal coordination bonds, electrostatic attraction, etc.) between imprinted molecules and functional monomers. ) function, the functional monome...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/30B01D15/22
Inventor 孔亮吴曦罗碧容李伟
Owner DALIAN OCEAN UNIV
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