The method of modifying the surface of a solid carrier for chromatography

 

(57) Abstract:

Usage: as a modified surface of solid media for distribution chromatography. The inventive method of modifying the surface of a solid carrier, which consists in processing the surface of a solid carrier modifier, which is used as aliphatic hydrocarbons with double bonds in the molecule and not containing a polar functional group, for example, squalene, by polymerization in suspension in the presence of initiator and solvent extraction nesupykit.vasara residues modifier. Modification made in this way can reduce the adsorption activity of the solid carrier, to improve the separation capacity of the sorbent and to obtain symmetrical chromatographic zone of the analyzed substances. 1 Il.

The invention relates to the field distribution chromatography, and in particular to a method of modifying the surface of a solid carrier.

The main purpose of solid media in the chromatographic column to provide the most efficient use of the static fluid. One of the most important properties of a solid carrier must b is, prepared on the basis of various lands, are not completely inert and therefore require additional modification to eliminate the harmful effects of active centers. There are several ways to reduce the adsorption activity of media, such as washing with acid or alkali treatment of a small number of the polarity of the fluid, chemical decontamination [1]

The disadvantage of all these methods is that they do not allow to completely block the active centers on the surface of the media.

Closest to the present invention is a method of inoculation, using the application of the stationary phase with its polymerization directly on the media. So, on the surface of the medium conducting the curing of polyester resins [2] the Resin M-3 dissolved in a volatile solvent (acetone), the resulting solution is injected solid media, to initiate polymerization of 100 wt.h. the resin was added 1 of 6 o'clock ethyl ketone peroxide or cumene hydroperoxide, heated to the boiling point of the solvent is evaporated and dried his sorbent with mechanical pomeshivanii smell removal of the solvent. Download the sorbent in the column mortar which strengthens and stabilizes imerikasina remnants of the resin. The resulting sorbent or covered with a layer of the desired stationary phase, or use directly.

The disadvantage of the prototype is that the modifier contains polar functional groups and, therefore, is not sufficiently inert with respect to a number of substances may be non-linear sorption isotherm, which causes the asymmetry of the peaks and the deterioration of their separation.

The objective of the invention is the reduction of the adsorption activity of the solid carrier and, consequently, improve the separation ability of the sorbent and obtaining symmetrical chromatographic zones of the analyzed substances.

This task is solved in that in the method of modifying the surface of a solid carrier, which consists in processing the surface of a solid carrier modifier by polymerization in the presence of initiator and solvent extraction nesupykit.vasara residues modifier, the polymerization is carried out in suspension, and as a modifier use aliphatic hydrocarbons with double bonds in the molecule.

And aliphatic hydrocarbons with double bonds in the molecule is squalene C30H50(2, 4, 10, 15, 19, 23-hexamethyltetracosane is unknown its use for modifying the surface of a solid medium aliphatic hydrocarbons with double bonds in the molecule. This new set of essential features enables you to achieve new technical result consists in the formation on the surface of the carrier nonpolar solid layer, which contributes to ravnopravnosti stationary phase and prevents contact with the active centers of the media.

The figure shows the chromatogram obtained for columns with

a) a sorbent prepared from unmodified media;

b) a sorbent prepared according to the proposed method the solutes: 1 - ethanol, 2 propanol-1,3-butanol 1,4-pentanol-1.

The method is illustrated by the following example.

Example. Sample of squalene (10% by weight of solid carrier) and the polymerization initiator benzoyl peroxide (5 parts per 100 mass. parts squalene) is dissolved in acetone and applied to the calculated number of zithroma IK (4, particle size 0,125 0,160 mm) in the usual way when the decomposition temperature of the initiator 70oC) avoid premature start of the polymerization reaction. This is followed by a polymerization reaction by heating the sorbent in distilled water (50 ml) in a flask under reflux with constant stirring at 80oC for 3 hours, the Obtained sorbent is loaded into capicator extracted by passing acetone through a column (to establish the absence of the modifier in the resulting acetone) and dried sorbent. On the sorbent in the usual way a layer of immobile liquid phase polymethylsiloxane PMS 1000 (5% wt.).

Chromatographic analysis is performed on the chromatograph COLOR 100 when the temperature of the column 100oC. Column length 100 cm of the carrier gas nitrogen, rate 15 ml/min Detector flame ionization.

The choice of the sorbent with the best performance by comparing the properties of the sorbent derived from unmodified media and media modified as described in the prototype, according to the method developed based on the known chemistry of polymers, methods of polymerization in emulsion [4] and the method proposed in the invention.

Evaluation of the adsorption activity of zithroma IK before and after modification of its surface by squalene is the coefficient of asymmetry of chromatographic peaks standards of Arsagera and some alcohols. For example, for butanone 2 the asymmetry parameters of the chromatographic peaks have the following values: for a sorbent prepared from unmodified zithroma IK, 2, 15 0,33; for sorbent obtained by the method described in the prototype, 1,89 0,61 and 1,70 0,20 (5% and 20% of the mass. mod the NTA, obtained by the method of suspension polymerization, 1,05 0,05. Determination of the coefficients of asymmetry of the chromatographic peaks for other standards of Arsagera and some alcohols shows that in all cases the best results are obtained by the method of modifying the surface of a solid carrier, based on the polymerization in suspension. The asymmetry coefficients close to unity.

Evaluation of the separation ability of the sorbent, prepared on the basis of modified media was conducted by the values of efficiency speakers. Efficiency speakers with sorbents prepared from unmodified zithroma IK, and sorbents based on solid medium, modified in three different ways, is evaluated by the number of theoretical plates by standard substance (n) and the maximum number of theoretical plates, corresponding to the hypothetical sorbate with retention time tending to infinity (n). As standards when calculating n used n-nonan and n-pentanol-1, and a value of ncalculated on a homologous series of n-alkanes and n-alkanols-1. The highest of the efficiency values have columns with sorbent-based solid media, modificy theC5H11OHdiacronic with sorbents obtained in other ways, fluctuate within 692 1170, n(n-alkanols-1) within 1229 2206. This is because the modification of the media by the method of suspension polymerization can inflict on the surface of solid media the largest number modifier (about 3.2% of the initial mass), while according to the method described in the prototype and method of polymerization in emulsion is applied to only about 1% and 2.7% of the initial mass) modifier, respectively.

Illustration improve the separation capacity of the column are also shown in the figure chromatogram obtained on columns with sorbents on the basis of the original and modified according to the method of polymerization in suspension of solid media.

Use of the method of modifying the surface of a solid carrier, based on the polymerization in suspension of aliphatic hydrocarbons with double bonds in the molecule, allows to reduce the adsorption activity of the media, to improve the separation capacity of the sorbent and to obtain a more symmetric peaks of the analyzed substances.

1. The method of modifying the surface of a solid carrier for chromatography, solicitor and extraction nesupykit.vasara residues modifier, characterized in that the polymerization is carried out in suspension, and as a modifier use aliphatic hydrocarbons with double bonds in the molecule and not containing a polar functional group.

2. Method p. 1, characterized in that as a modifier use squalene.

 

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