JPS5841351A - Filler for liquid chromatography column - Google Patents

Abstract

PURPOSE:To obtain a high speed liquid chromatography filler especially with high mechanical strength and with excellent heat-resistance, chemical resistance, small swell and contracting by alkylating the surface of an optically anisotropic small spheric body that is obtained by treating a pitch groups under a specified heating condition. CONSTITUTION:Petroleum pitch or coal pitch is treated by heating it to 350 deg.C- 500 deg.C to produce optically anisotropic beads. After they are separated and washed, using quinoline, bezene, etc., and the surface is hydrogen ated at 100 deg.C for 20min. Next, alkylchloride is made to conduct Friedel-Crafts reaction to alkylate the surface of small spherical bodies. The C number of alkyl is preferably 10-30. The small spherical bodies thus obtained is filled in a chromatography column. In this way a filler with high mechanical strength and uniform surface and especially suitable for high speed chromatograph without variation in activity due to moisture can be obtained.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention is a novel column packing material Kl! do. 41K high-speed liquid chromatinous filler Kll with 41 properties for use in spinach flies. Ru.

The inventor! C using iKmen carbon microbeads as a column packing material for liquid clotfish
I would like to propose that
As a result of their subsequent research, they found that by modifying the surface of the Metsu★-Pon microbeads O! It was discovered that a product with excellent properties could be obtained as a column packing material for high-speed filtrate tarmadography.

In other words, zero origin WA? ! Grain length obtained by heating i pitches/
-iepwgo optically anisotropic spherules, - so-called memechan! Italobies 01! The present invention relates to a column packing material for liquid lithography obtained by multiple modification by introducing an alkyl group.

Hereinafter, five aspects of the present invention will be explained in detail.

The filler from zero is petroleum-based or coal-based O-pitch.
Optically anisotropic spherules are produced by heating to o-zoo°C, separated and washed using quinoline, bene, acetone, etc., and then usually classified to sharpen the particle size distribution. This can be obtained by surface modification treatment. Table iii #c. Surface alkylation occurs through 7 reactions. K causes surface hydrogenation.
It is usually carried out by contacting with hydrogen gas under high temperature conditions of around 10 OOC.For alkylation, a corresponding alkyl halide is used and introduced (by 1-delta lac reaction) in the presence of a Lewis acid catalyst @0. . The alkyl base line to be introduced may have carbon atoms of 10 to JO, preferably Id, /4 to Jo@degree 0, which may be a linear or circular branched group. Examples of variants include tetradecyl chloride, hex-ffcyclochloride, and octadecyl chloride, but in addition to these, many other types of alkyl halides are used. When i is small, the separation characteristics are generally not good.

The packing material of the present invention can be used in the same manner as a typical column packing material for liquid chromatography. I! #
It has great mechanical strength and heat resistance.

In addition to chemical resistance, there is little swelling and shrinkage, and it is resistant to severe heat.
1. It has a homogeneous surface and its activity does not change due to moisture, so it has desirable properties as a column packing material for high-performance liquid clotgelography. Furthermore, the type of alkyl group to be introduced must be selected (K). Various O fillers can be prepared with characteristics depending on the purpose. 9. Comparing the filler made of carbon microbeads themselves with the filler of the present invention, the former adsorbs acidic substances and basic substances, so these substances do not adhere to each other or other substances. In contrast, in many cases, it is impossible to separate the O-filled rigid wire of the present invention from the O-filled rigid wire, whereas such a phenomenon does not occur with the O-filled rigid wire of the present invention, and separation is possible.

Hereinafter, the present invention will be explained in a different manner by giving examples.

Example/Memcarbon Mitaropeas 01111 and 7 satalbits were produced by heat-treating them at 30°C for 60 minutes and K! Ik r beast was treated with s J capacity of quinoline at 5°C, centrifuged to remove the supernatant, quinoline was added and the same procedure was repeated, and finally benzene and acetone were added. Wash and dry with
The men carbon mita beads obtained in the above were classified using a backflow classifier, and the particle poles were classified into tr, o~/da,
I got 4pm IC.

Heating and surface hydrogenation treatment The obtained mesocarbon microbeads.

It still contains some low molecular weight substances such as quinoline that are eluted from the dissolved fsK. Therefore, in order to obtain a uniform surface by polymerizing them and removing the oxygen-containing functional groups present on the surface.

First, I put it in a quartz glass tube! Microbeads were heated and evacuated at 120°C for 1 hour at 0-'Torr.9. Here, while flowing helium gas into the tube, it was heated for 500°C at a temperature increase rate of 10°C/-.
~1000℃ is heated again at a temperature increase rate of 70℃/-, 1
After holding the temperature at 000°C for 1 hour, the system was further evacuated and dry hydrogen gas was introduced into the system.

After being held at ℃ for 2θ minutes, it was allowed to cool naturally.

3 Surface modification First, anhydrous aluminum chloride was added to nitromethane in a nitrogen gas atmosphere.

there! The bead sample was dispersed, and then a predetermined amount of octadecyl chloride was dropped into the system while helium gas was introduced into the system to carry out the reaction.9. The reaction time was d/hour, the reaction temperature was changed, and finally the beads were washed with acetone to obtain Makerbon microbeads with a stationary phase of otatadecyl radical chemically bonded to the surface.

Filling the column with O. Filling the column for high performance liquid talomadography with f.
This was carried out using the one-pack filling method.

First, mix the sample with acetonitrile to make a slurry), put it into a slurry storage tank, operate the pump, and flow acetonitrile into the column! The liquid was then pumped at 00 ATM for 1 hour to perform filling. The column used was made of stainless steel.

! A high-speed housing that exhibits O separation performance WJIK as a column packing material for high-performance liquid chromatography! To the thornfish device! Separation experiments were performed using Iterbead columns. The injected samples include Tano aromatic compounds, pen(III) forms, benzene-substituted forms, di-7-enyl-1, etc. Table 90 shows the percentages of these solute systems and their O measurement conditions.

[Brief explanation of the drawing]

No. 1 is an explanatory diagram showing the nine high-speed liquid extraction equipment used in the examples. slam ram, 4 magnification detector, tF17 my collector. Part 1~/*@Hiroki Thesis example ')Each component OII showing the results of separation by the high shielding body Talomado l Raffy - and I
11 is a graph showing the relationship with the output amount. Applicant Hiroshi Takahashi

Claims (1)

[Claims] ■ Column packing for liquid chromatography made by surface alkylating particles ll/~/apW10 optically anisotropic small spheres obtained by heating pitches in SSO~toocpc.