KR20010112868A - 3-dimensional analytical apparatus for crystallized polymer - Google Patents

Abstract

Sulfonamide derivatives represented by general formula (1) or pharmaceutically acceptable salts thereof, which have little toxicity and a potent effect of inhibiting tubulin polymerization wherein R1preferably represents lower alkoxy; R 2, R3, R4, R 5and R6may be the same or different and each independently represents hydrogen, halogeno, nitro, lower alkyl, optionally substituted amino or alkylamino; A represents: (1) a 5- membered heterocyclic group having at least one nitrogen atom which may be substituted and contain as the heteroatom an atom selected from among nitrogen, oxygen and sulfur, provided that triazole is excluded therefrom; (2) an optionally substituted alicyclic hydrocarbon group; or (3) an alicyclic hydrocarbon group containing at least one nitrogen atom in the cycle and capable of further containing nitrogen, oxygen or sulfur as the heteroatom. Drugs containing these compounds as the active ingredient correct abnormalities in the immune system and, therefore, are useful as preventives or remedies for rheumatism such as inflammatory rheumatism or as anticancer agents.

Description

3-dimensional analytical apparatus for crystallized polymer

The present invention relates to an analytical device that enables three-dimensional analysis through projection of branches, three-dimensional crystal structure, etc. according to the molecular weight of the crystalline polymer, in particular the crystal structure and molecular weight of the polyolefin through cross-analysis and separation, etc. The present invention relates to a device capable of simultaneously analyzing information on stereocrystalline molecular structure and molecular weight.

For the analysis of the molecular weight of the existing crystalline polymers, the gel permeation chromatography, the melt viscosity, the light scattering device, etc., which are measured by passing through the stationary columns having different sizes after dissolving the polymer, are mainly used. However, the recent trend of R & D of crystalline polymers has been focused on new product development through in-depth research into polymerization catalyst research and polymerization process research.

For this purpose, there is an urgent need for a test and analysis apparatus capable of analyzing changes in branch concentration, crystallinity, and stereoregularity according to molecular weight distribution at one time.

In order to solve this problem and to analyze the crystalline distribution of the polymer for the three-dimensional cross analysis of the crystalline polymer, a method of using an analytical device has been attempted. As the reliability of analysis in Esso was significantly lowered, a more accurate analysis device was needed.

In order to compensate for this problem, a more reliable analytical device was proposed by Mitsubishi Chemical under the trade name of a cross classification device. With this analysis device, a three-dimensional cross classification analysis, which was difficult with the existing device, was possible, but the stability of the device was improved. There are many difficulties in the operation of the equipment in the field due to the problem that frequent failures occur frequently during the work due to lack, and it is expensive equipment, which has a disadvantage of costly in the introduction and operation.

In addition, this device does not have a separation and recovery device depending on the elution temperature of the sample when performing down analysis by separating the necessary parts for precise analysis of the sample. There is an urgent need for an improved new three-dimensional exchange analysis device.

The technical problem to be achieved by the present invention has been invented to improve the above-mentioned problems, using the newly invented separation device to separate and fractionate an appropriate amount of sample required for detailed molecular structure analysis through down analysis and crystallization of the sample. It is an object of the present invention to provide a measuring device that enables three-dimensional exchange analysis of distribution and molecular weight.

1 is a schematic configuration diagram of an apparatus of the present invention.

2 is a schematic configuration diagram of a sample separation recovery apparatus.

※ Explanation of Drawings

1: line temperature controller, 2: window temperature controller, 3: line temperature controller,

4: temperature monitor, 5: program temperature controller, 6: infrared source,

7: infrared detector, 8: heater, 9: heater,

10: crystal distribution processing system, 11: column cartridge,

12: window, 13: line temperature controller, 14: heater,

15: damper, 16: pump, 17: moisture, air removal device,

18: solvent storage tank, 19: molecular weight measuring instrument,

20: computer (three-dimensional analysis device),

21: 16-stage separation cartridge device, 22: solvent recovery tank,

23: molecular weight detector, 24: data transmission cable, 25: data transmission cable,

26: temperature control chamber, 27: preparative cartridge

28: stepper motor, 29: solvent recovery tank, 30: sample injector,

31: Solvent Transfer Line & Line Temperature Controller

An object of the present invention is a crystalline polymer analysis device sequentially composed of a crystallization distribution measuring device unit, a molecular weight measuring device unit and a separation unit for separating and separating a crystalline polymer sample at a constant concentration in order to proceed with the analysis of the sample sequentially, Crystallization, distribution, and branching of crystalline polymers, characterized in that the computer is equipped with a three-dimensional analysis program for real-time processing of the respective measurements of the crystallization distribution, molecular weight and branch measured from the device And it provides a three-dimensional analysis device of the crystalline polymer capable of simultaneously analyzing the distribution, molecular weight and distribution through the exchange analysis.

At this time, the crystallization distribution measuring unit unit a damper 15, pump 16, air and moisture removal device 17, the solvent tank 18 and the crystalline polymer sample which can transfer the sample under a constant pressure depending on the temperature Transfer line and line temperature controller (1, 3, 5), window temperature controller (2), temperature sensor (4), heater (8, 9, 14), infrared source (6) It is characterized by consisting of an infrared detector 7 and a window 12 and the like.

In addition, the molecular weight measuring device portion is composed of a molecular weight measuring device (19) and molecular weight detector (23), the separator device portion can be separated from the automatic sample injector 30 and stepper motor 28, 16 samples in one test. Preparative cartridge 27, the temperature control chamber 26 and the solvent transfer line and line temperature controller 31 and the solvent recovery tank 29 for recovering the remaining sample and solvent after separation and separation It is done.

Hereinafter, the present invention will be described in more detail.

The present invention relates to an analysis device designed and manufactured to enable simultaneous analysis of information on molecular weight, crystallinity, branching, etc. in three dimensions through cross-sectional analysis of crystalline polymers.

The present invention is a device (1-18) for measuring the crystalline powder, the device (19, 23) capable of measuring the molecular weight and distribution, and the connection device 25 and the crystallization to receive information on the molecular weight online Connection device 24 for receiving distribution information, separation device 21 that can be separated from crystallization distribution device in 1 ~ 16 steps according to elution temperature, 3D cross analysis of molecular weight, branch, crystallization distribution is possible It includes a central processing unit 20 capable of real-time processing, and a solvent recovery storage tank 22 having a discharge recovery pipe for recovering the eluate, and the sample eluted from the crystallization distribution measuring instrument according to the elution temperature. It features automatic program control that allows separation, and concentration control of samples for direct use in molecular weight measurements.

In particular, the separation device 21 is composed of 16 stainless containers to accurately separate the sample, the heating chamber 26 is capable of raising the temperature up to 160 ℃ and maintaining a constant temperature, and to automatically collect a certain amount of sample It is characterized by consisting of a program and a cable for transmitting the infrared absorption value obtained through this to a computer.

The configuration of the three-dimensional exchange analysis device according to the present invention for achieving the above object will be described.

1 and 2 are respectively a schematic view showing a device for measuring a three-dimensional exchange analysis of the crystalline polymer according to the present invention and a perspective view separately showing only the main parts thereof.

As described in the accompanying drawings, the measuring device of the present invention includes a damper 15, a pump 16, an air and water removing device 17, a solvent tank 18, and a crystalline polymer capable of transferring a sample under a constant pressure. Transfer line and line temperature controller (1, 3, 5), window temperature controller (2), temperature sensor (4), heater (8, 9, 14), infrared ray Sample (6), infrared detector (7) and window (12), sample separation and collection device (21) and solvent recovery device (22) capable of separating and separating samples necessary for molecular weight measurement at a constant concentration Network cables (24, 25) for transferring elution information and molecular weight information to the main computer, and a data processing system analysis device (20) for statistically processing all analysis information in three dimensions using a computer.

Figure 2 is a schematic enlarged view for separating and separating the eluted crystalline polymer sample to an appropriate concentration. More specifically, the sample separation recovery apparatus 21 includes a heating chamber 26, a preparative cartridge 27, a stepper motor 28, a solvent recovery tank 29, an automatic sample injector 31, and a line temperature, which can be controlled in temperature. Regulator 30. The separation concentration of the sample is designed to adjust the concentration while looking at the infrared absorbance monitored by the infrared detector. The characteristics of this device allow the operator to adjust the sample concentration as desired and separate the sample into up to 16 sections. If only the crystallization distribution analysis is desired, the crystallization distribution can be directly performed without setting the analysis conditions after setting this analysis condition. Parallel experiments are made so that only experiments are possible.

The molecular structure of the sample analyzed through the three-dimensional statistical process can grasp all the detailed information on the molecular weight of the crystalline polymer, and since the very large polymer region is separated and photographed in the low molecular weight region, the molecular weight and distribution of each region are detailed. The information on the side branch structure according to the molecular weight can be easily analyzed by analyzing the correction curve obtained in the existing crystallographic distribution experiment, and analyzing the characteristics of the side branch structure, distribution, stereoregularity, and crystallization distribution.

The effect of the present invention is to analyze the information on the molecular weight, crystallinity, branching, etc. through the three-dimensional cross-sectional analysis of the crystalline polymer, the crystal composition, stereoregularity, branch structure distribution, etc. It has the advantage of obtaining very good analysis information through 3D simultaneous analysis of.

Claims (4)

In the crystalline polymer analysis device sequentially composed of a crystallization distribution measuring device unit, a molecular weight measuring device unit and a separation unit for separating and separating a crystalline polymer sample at a constant concentration in order to proceed with the analysis of the sample sequentially, Crystallization and distribution, branching and distribution, molecular weight and molecular weight of a crystalline polymer, characterized in that it is composed of a computer equipped with a three-dimensional analysis program for real-time processing of individual measurements of crystallization distribution, molecular weight and branching by cable. Three-dimensional analysis device of crystalline polymers that can simultaneously analyze the structure through exchange analysis According to claim 1, wherein the crystallization distribution measuring unit portion damper 15, pump 16, air and moisture removal device 17, the solvent tank 18 and the crystalline polymer sample capable of transferring the sample under a constant pressure Line and line temperature controllers (1, 3, 5), window temperature controllers (2), temperature sensors (4), heaters (8, 9, 14), infrared sources (6), the three-dimensional analysis device of the crystalline polymer, characterized in that composed of an infrared detector (7), a window (12) According to claim 1, wherein the molecular weight measuring unit is a three-dimensional analysis device of the crystalline polymer, characterized in that consisting of the molecular weight measuring device 19 and the molecular weight detector (23) According to claim 1, wherein the separator unit automatic sample injector 30 and stepper motor 28, preparative cartridge 27 for separating the 16 samples in a single experiment, temperature control chamber 26 and the solvent Three-dimensional analysis device of the crystalline polymer, characterized in that consisting of the transfer line and the line temperature controller 31 and the solvent recovery tank 29 for recovering the sample and solvent remaining after separation and separation