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Preparation method of weakly-acidic cation chromatography column packing

A technology for cation chromatography and column packing is applied in the field of preparation of weakly acidic cationic chromatography column packing resin, which can solve the problems of complexity and time-consuming, and achieve the effects of low detection limit, easy operation and short time.

Active Publication Date: 2019-05-03
QINGDAO PUREN INSTR
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention firstly solves the problems existing in base material pretreatment, such as surface quaternization, preparation of microspheres and the problems of complex operation and long time-consuming pretreatment process of film attachment; Polymerization eliminates the problems of constant temperature, uniform stirring and continuous reflux in the reaction solution that must be maintained for a long time in the wet grafting polymerization reaction

Method used

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  • Preparation method of weakly-acidic cation chromatography column packing
  • Preparation method of weakly-acidic cation chromatography column packing
  • Preparation method of weakly-acidic cation chromatography column packing

Examples

Experimental program
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Embodiment 1

[0027] (1) Pretreatment of polymer microspheres:

[0028] Take 1.0g maleic anhydride (MAH) as a functional monomer, 1.0ml divinylbenzene (DVB) as a crosslinking agent and 0.1ml dicumyl peroxide (DCP) as an initiator and put it into 10.0ml acetone organic solvent, After stirring and dissolving in a 100ml beaker, add 5.0g of PS-DVB polymer microspheres that have been swollen completely with dichloromethane (DCM), and treat them in an ultrasonic or water bath (35°C) for 15 minutes to evaporate most of the solvent and the microspheres After the surface is micro-dried and solidified, the above-mentioned materials are attached to the surface of the microsphere and the surface of the pores inside the microsphere, and then placed in an oven at a constant temperature of 40° C. for 1 hour until the PS-DVB polymer microsphere is dry.

[0029] (2) Graft polymerization of polymer microspheres:

[0030] Place the pretreated polymeric microspheres in an oven, raise the temperature to 170°C,...

Embodiment 2

[0053] The difference from the step (1) of Example 1 is that 1.2g of PBDMAN (polybutadiene-g-maleic anhydride) was used instead of MAH (maleic anhydride) to be dissolved in 10ml of acetone organic solvent, and the others were the same.

[0054] The difference from step (2) of Example 1 is that the temperature is kept at 180° C. for 6 hours in an oven, and the others are the same.

[0055] The difference from step (3) of Example 1 is that 200ml of 0.5mol / M NaOH solution is added, hydrolyzed at 60°C for 2 hours, soaked in 1.0mol / M hydrochloric acid overnight, and then washed with deionized water to obtain Weakly acidic cation column packing.

[0056] Other steps are with embodiment 1.

[0057] The separation column made with the weakly acidic cation chromatographic column filler prepared in Example 2, adopts the same sample and test conditions as in Example 1, and simultaneously separates and detects alkali metals, ammonium and alkaline earth metals in the sample, and the data ...

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Abstract

The invention discloses a preparation method of a weakly-acidic cation chromatography column packing. The preparation method comprises the following steps: adding a functional monomer, a crosslinkingagent and an initiator into an organic solvent, performing stirring to achieve complete dissolving, adding a completely-swollen polystyrene-divinylbenzene microspheres, performing ultrasonic treatmentor heating to volatilize the solvent, raising the temperature to 120-200 DEG C after the surfaces of the microspheres are slightly dry and solidified, and carrying out a dry graft polymerization reaction at a constant temperature of the 120-200 DEG C to obtain a weakly-acidic cation chromatography column packing resin; and hydrolyzing the prepared packing resin by an acid or an alkali to obtain the weakly-acidic cation chromatography column packing. The preparation method has the advantages of simplicity, easiness in operation, realization under routine production conditions, a routine pressure and a constant and high temperature (120-200 DEG C), no special care, and completion after a period of treatment. A weakly-acidic cation chromatography column made from the packing has the advantages of high detection response value, low detection limit, increased resolution, increased column efficiency and shortened retention time.

Description

technical field [0001] The invention relates to a preparation method of an ion chromatographic column filler, in particular to a preparation method of a weakly acidic cationic chromatographic column filler resin. Background technique [0002] The publication number is CN 1412554 A Chinese invention patent application discloses a new preparation method of a surface thin-shell high-efficiency cationic chromatographic column filler, using 10 μm monodisperse PS-DVB (polystyrene-divinylbenzene) microspheres as the base ball , firstly carry out quaternization on its surface, and then uniformly agglomerate a layer of sulfonated cationic latex to obtain a cationic chromatographic stationary phase, but it can only be used for the determination of alkali metals and alkaline earth metals respectively. [0003] "Journal of Analytical Testing" in May 2005, No. 3 "Development and Performance Evaluation of Weak Acid Cationic Chromatographic Packing" published a method for making functional...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F257/02C08F222/06C08F212/36C08F299/02B01J39/26B01J39/20B01D15/36
Inventor 曲新聪郭文轩
Owner QINGDAO PUREN INSTR
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