Method and apparatus for concentrating solution

Gas separation: processes – Chromatography – With heating or cooling

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95245, 96101, B01D 1508

Patent

active

061529893

DESCRIPTION:

BRIEF SUMMARY
TECHNICAL FIELD

The present invention relates to a method and a device for removing a solvent from a solution or concentrating a solution for processing a dilute solution of which solute is difficult to be directly detected and qualitatively analyzed by conventional analytical instruments. Especially, the present invention relates to the separation or concentration of the solution where the solute and the solvent have close boiling points or have different polarities with low or nearly the same boiling points. The present device is also used to combine a chromatograph such as high pressure liquid chromatograph (HPLC), a gel permeation chromatograph (GPC) or a super critical fluid chromatograph (SFC) with an instrument for structural elucidation or identification such as infrared spectrometer (IR), or nuclear magnetic resonance spectrometer (NMR).


BACKGROUND ART

As the regulations on automobile exhaust emissions have been strict, higher level analyses or evaluations of fuels are required more than they used to be. For example, microanalysis dealing with trace amounts of compounds such as polynuclear aromatics are required for light oil.
On the other hand, extremely small amount of samples or the samples including low concentration compounds have been routinely analyzed in the field of environmental science. The demand for the analysis with high sensitivity or high selectively also have increased in the other analytical field.
When analyzing these samples, their concentration is important. And, the analytical results depend on the quality of the procedure for concentration. In general, the method of vaporizing the solvent at room temperature or a heated temperature under an atmospheric pressure or a reduced pressure has been used for concentration of the solution samples. For example, an evaporator has been used as a typical concentration method. In addition, the mini-column packed with the packing material for liquid chromatography and so on has recently been used to extract the solute.
In the treatment of low concentration samples, the following problem is likely to arise: the concentration under an atmospheric or reduced pressure loses the solutes where boiling points are close to that of the solvent, and the concentration using the mini-column will dilute the solute to be obtained with a large amount of solvent or makes the solute go away in vapor at recovery.
By the way, automation of the analytical procedures has been promoted and the apparatuses for them have been developed.
The analysis of complex mixture sample is generally classified into pre-treatment, separation, identification and quantitation. The automation of these procedures serves to not only speed-up and labor-saving of the procedures but also improvement of accuracy, sensitivity and reproducibility of analytical results.
Among the above procedures, the method for pre-treatment is varied, depending on the sample conditions or the purposes of analysis. Accordingly, the effect of the automation is little except the case where the similar samples are treated repeatedly. On the other hand, the automation of the procedures in separation, identification and quantitation will be widely used. A typical example of the above automation is GC/MS (gas chromatography/mass spectrometer) in which a gas chromatograph is combined with a mass spectrometer. MS, which is effective in identification and structural analysis of very small amount of organic compounds, has been widely used in the analytical field, since it was combined with GC in 1964. Nowadays, the GC/MS is popularly used as a most powerful analytical systems. However, GC/MS can analyze only the samples which evaporate in GC column (where the temperature is lower than 350.degree. C. and the pressure is lower than 150 kPa). In other words, GC/MS is not applicable to the samples with high boiling point which cannot be separated by this column. As a method for solving the problem, the following method and the like, is employed in which the high boiling point substances are thermally cracked and

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