JPS6041018B2 - Ceramic body for chromatography - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention uses a solid as a stationary phase, and a sample mixture placed at one end of the phase is moved using a developer. It relates to chromatography for mutually separating pesticides and other various compounds.

Chromatography that has been commonly used in the past can be broadly classified into adsorption type and distribution type. Thin layer chromatography is a method that applies the principles of both adsorption and distribution to separate substances, and liquid phase chromatography is a method that uses distribution. Thin-phase chromatography mainly uses inorganic or organic adsorbents such as silica gel alumina and polyamide mixed with a binder, water, and other appropriate ingredients in a mixed solvent, and is used to process materials such as glass, synthetic resins, metals, etc. The unknown sample is applied to a thin layer on a plate-shaped support and dried under predetermined conditions, and an unknown sample is dripped onto the thin layer to scatter the solvent and the bottom (or top) of the plate-shaped support. ) is immersed in a solvent solution, and after a certain development time, the unknown sample is separated and analyzed by utilizing the repeated adsorption and separation of the sample as the solvent passes through the thin layer due to capillary action. This is what I am trying to do. Thin layer.

Matography requires additional expensive equipment such as an applicator to create thin layers, and requires considerable skill to create thin layers using such equipment. Moreover, it is difficult to obtain a thin layer of uniform thickness even with the thin layer made in this way, and unless the thickness is uniform, it is difficult to spread it uniformly, and even when it is spread, the reliability and reproducibility are poor. , the degree of activity differs even with the same material due to the difference in the degree of dryness of the adsorbent, it is difficult to continuously produce many thin layers, and the thin layers produced are coated on a glass substrate, etc. It had many drawbacks, such as being easily peeled off due to vibration when being carried. On the other hand, the partition type uses liquid chromatography, which separates and flows out substances with larger distribution coefficients first.

In other words, it is necessary to quickly and accurately inject a small amount of liquid into the carrier liquid in front of the column against the pressure (for example, 300 atmospheres), and a through-cap that is injected using a commonly used piston-type injection mechanism is required. The technique does not always have good reproducibility due to the high internal pressure of the carrier liquid. Furthermore, different materials must be used for the through-cap depending on the solution. Moreover, due to the incompressibility of the carrier liquid used when introducing the capillary of the injection device into the liquid, an impact pressure is generated, which continues from the column to the detector, and has a sensitive effect on the analysis process. In liquid phase chromatography, which is a partition type, the amount that can be developed at one time is small, and the separation performance is poor unless it is diluted, so it takes time to separate and collect the amount needed for analysis. There were such drawbacks. Furthermore, it is difficult to uniformly pack a fixed bed into a column, and commercially available products are very expensive. In addition, ■Ultraviolet analysis (U) is used when separating and sampling.
・V), it is necessary to detect by means such as refractive index analysis (R・1), and the entire inspection becomes large-scale. ■The equipment mentioned above must be thoroughly cleaned before and after use. As described above, conventional chromatography, either adsorption type or distribution type, has many drawbacks in terms of function and operation.

The present invention aims to eliminate the above-mentioned drawbacks, provide a ceramic body for chromatography that is excellent in uniformity and separation, and is inexpensive.

The ceramic body according to the present invention will be described in detail below.The main ingredient is Q-AI2Q (alumina) with a particle size of 30 μm or less and a narrow particle size distribution, and acrylic resin and polyvinyl butyral (PVB) as a binder. ) is kneaded with a solvent such as toluene or methanol, and then molded into a predetermined shape by, for example, a tape casting method using a doctor blade method, a pressing method, an extrusion method, or the like.

In this embodiment, a ceramic body cut into a rectangular shape of 5 arcs x 1 ratio E will be described. Raw material Q-AI203 (alumina)
The main ingredients are talc and limestone at 0 to 10% (preferably 4%).
) In addition, with the particle size distribution shown in Figure 1, ■,
A ceramic body was fabricated by preliminarily forming a molded body mainly composed of Q-alumina having a distribution of 5% by weight as shown in (2).

In this case, if the average particle size of the Q-alumina used is x, then 0. Soft ~ 1. Particle size distributions in the narrow range shown in the graph in Figure 1 ■■, which are spheres, are best; particles with particle size distributions shown in ■ and ■ in the same figure have poor chromatographic separation performance and large tailing. Or, if the average particle size exceeds 30 μm, it is difficult to form it into a sheet and it cannot be used. Therefore, ■ in the same figure
Q-alumina raw material powder with a particle size distribution of 8 pieces of skin plate-shaped
It was baked at 50°C, 125,000, and 139,000, and the relationship between each temporary phosphorus temperature and development rate was investigated.

The results using chloroform as a developing solution were as follows. Of the ceramic bodies calcined in this way, 850
The development time of the ceramic body temporarily held at 1250 qC was the fastest at 38 minutes, but the ceramic body temporarily held at 1250 qC was the best in terms of strength for chromatography.

Therefore, the results of an experiment using a ceramic body that was pre-dawned at 1250°C are shown below. [Example 1] Naphthalene, fluorene, biphenyl and a mixture thereof were developed with methanol:water=1:1 (V/V).

* Solvent development distance: 5.8 mm The sample to be separated in Example 1 is often used to examine the separation properties of liquid phase chromatography, and when iodine was used for color development, it was divided into three components as shown above. I was able to separate it.

[Example B]

The results of separating amino acids are shown in the figure, and n is used as a developing agent.
-Butanol:acetic acid:water:chloroform:54:18:
18:10 (V/V) was used, and nihydrin was used for color development.

As a result, as shown in the figure, in the chromatography using the ceramic body of the present invention, the spots after development of substances with relatively high Rf values (phenylalanine, alanine) do not cause any tailing phenomenon, are clustered small, and the peripheral areas are clear. there were.

As described above, since stable Q-M203 was used as the alumina for the ceramic body according to the present invention, it had almost no adsorption properties and could be separated very clearly due to the difference in the acid fraction coefficient.

The features of the ceramic body for chromatography according to the present invention are: ■ The activity of alumina is low.
Since Q-A et al. 03 is stable, it has almost no adsorption properties and can be used as is in systems where only conventional liquid phase chromatography has been used.

■ Can be easily separated in large quantities in a short period of time.

■ Because it is made by molding alumina that has uniform grains using a binder, it has a uniform thickness, excellent separability, and is reproducible.

■ It has great mechanical strength because it is calcined after forming.
No deformation occurs.

■ It can be easily attached and detached by cutting only the separated part and using a sharp solvent.

■ It is extremely inexpensive because it can be molded continuously.

The effects are extremely large.

[Brief Description of the Drawings] Figure 1 is a graph for explaining the particle size distribution of Q-alumina forming the ceramic body for chromatography according to the present invention, and Figure 2 is a graph for explaining the particle size distribution of Q-alumina forming the ceramic body for chromatography according to the present invention. This figure shows the separation of amino acids. Figure 1 Figure 2

Claims (1)

[Claims] 1. Calculating a molded body mainly composed of α-alumina with an average particle size of 30μ or less, and where the average particle size is x, the particle size in the range of 0.5x to 1.5x accounts for 50% by weight or more. Ceramic body for chromatography.