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A carboxylated organic-inorganic hybrid monolithic column and its preparation method and application

A carboxylated monolithic column technology, applied in the detection field, can solve the problems of poor stability of the carboxylated monolithic column, cumbersome preparation process, low reproducibility, etc., and achieves cheap and easy-to-obtain reagents, good repeatability, and low column pressure. Effect

Active Publication Date: 2021-09-28
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In view of the poor stability, low reproducibility, cumbersome and time-consuming preparation process of the carboxylated monolithic column in the prior art, the present invention provides a carboxylated organic-inorganic hybrid monolithic column and its preparation method and application

Method used

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  • A carboxylated organic-inorganic hybrid monolithic column and its preparation method and application
  • A carboxylated organic-inorganic hybrid monolithic column and its preparation method and application
  • A carboxylated organic-inorganic hybrid monolithic column and its preparation method and application

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preparation example Construction

[0045] like figure 1 As shown in A of the present invention are carboxylated organic - inorganic hybrid monolith preparation of, comprising the steps of:

[0046] SlO, activation of the capillary, capillary 5-10cm taken, washed with 1.5mol L -1 NaOH solution (12h), water (30min), 1.5mol L -1 Hydrochloric acid (12h), water (for 30 min), methanol (for 30 min) rinsing, then blown dry with nitrogen for later use;

[0047] S20, and the starting material to provide carboxyl DMSA mercapto functional group with the initiator, porogen, pH adjusting agent are mixed in a centrifuge tube, a mixed solution of mercaptosuccinic acid, wherein the pH adjusting agent is ammonia and urea mixture, the initiator is 2,2'-azobisisobutyronitrile hydrochloride; porogen -20,000 polyethylene glycol, polyethylene glycol-8000, cetyltrimethylammonium bromide one or more ammonium, preferably the porogen is polyethylene glycol -20000;

[0048] S30, γ- added tetramethoxysilane and methyl methacrylate mercaptosucc...

Embodiment 1

[0060] The actual environmental water samples at three Case RIVER water, river water and Jiuxiang sheep mountain lakes, were collected from Nanjing, over 0.45μm filter, wherein the measured concentration of the inorganic forms of chromium.

[0061] A carboxylated embodiment of the present organic - inorganic hybrid monolith separation application of inorganic chromium enrichment, including the following steps:

[0062] 1, carboxylated organic - inorganic hybrid monolithic column of Preparation

[0063] The specific steps are:

[0064] S10, the 42.6mg mercaptosuccinic acid (MSA), 1.5mg 2,2'- azobisisobutyronitrile hydrochloride (V 50 ), 0.225mL mass fraction of 2.5% aqueous ammonia (NH 3 · H 2 O), 0.4mL H 2 O, 60mg of polyethylene glycol -20000 (PEG-20000), 75mg of urea were mixed in 1.5mL centrifuge tube, a mixed solution of DMSA;

[0065] S20, tetramethoxysilane was added 0.2mL (of TMOS) the tube to the mixed solution of mercaptosuccinic acid and methyl methacrylate 0.1mLγ- - tri...

Embodiment 2

[0078] The basic content of the present embodiment is in the same embodiment, and the molar ratio of MSA and γ-MAPs in this embodiment is 1: 1, TMOS and γ-MAPs are 1: 2.7, ammonia water and gamma- The mass ratio of MAPs is 2: 1, the mass ratio of urea and MSA is 1.5: 1, V 50 The amount of the total mass of MSA and γ-MAPs, and the amount of PEG-20000 is 1.5 times the mass of MSA. The resulting carboxylated organic-inorganic hybrid monolithic column has good permeability and stability.

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Abstract

The invention discloses a carboxylated organic-inorganic hybrid monolithic column as well as a preparation method and application thereof, belonging to the technical field of detection. The present invention uses the "mercapto-ene" click reaction to use the cheap functional monomer mercaptosuccinic acid containing mercapto and carboxyl groups and the readily available alkenyl silylating agent γ-methyl methacrylate-trimethoxysilane "one pot" Synthesized carboxylated organic-inorganic hybrid monolithic column, which has good permeability, stability and selectivity to Cr(III), and can be used for the separation and analysis of trivalent chromium and hexavalent chromium in environmental water samples , and the preparation reagents are cheap and easy to obtain, the synthesis process is simple, and the reaction efficiency is high.

Description

Technical field [0001] The present invention belongs to the field of detection, and more particularly to a carboxylated organic-inorganic hybrid integral column and preparation method thereof. Background technique [0002] In environmental and organisms, the presence of elements is closely related to their effectiveness, biological activity and toxicity. In ambient water body, there are two main forms of chromium: trivalent chromium and hexavalent chromium. Trivalent chromium is a trace element necessary for the human body, play an important role in glucose metabolism with insulin. Hexavalent chromium is carcinogens, long-term exposure to six-vagrer chromium is easily caused by a variety of diseases such as skin allergies, inflammation, necrosis and other issues. Differentiated chromium forms are of great significance for studying the activity and (or) toxicity of chrome, but general metal element assay such as inductively coupled plasma mass spectrometry, inductive coupling plas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/22B01J20/22B01J20/30G01N1/34G01N1/40G01N21/31G01N21/73G01N27/626
CPCB01D15/22B01J20/22B01J2220/4812G01N1/34G01N1/405G01N21/3103G01N21/73G01N27/62
Inventor 练鸿振孙悦伦赵灵瑜
Owner NANJING UNIV
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