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Method for filling high-temperature liquid-phase chromatographic column of padding with fine particle size and dedicated device for method

A liquid chromatographic column and fine particle size technology, which is applied in the field of special equipment, can solve the problems of extremely high requirements for filling equipment and high filling pressure, and achieve the goals of reducing high-pressure sealing requirements, reducing filling pressure, and improving repeatability and stability. Effect

Inactive Publication Date: 2014-09-10
DALIAN ELITE ANALYTICAL INSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The filling pressure is too high, the requirements for the filling equipment are extremely high, and there are certain safety hazards. Therefore, there is a need for a chromatographic column filling method or device that can solve the above problems.

Method used

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  • Method for filling high-temperature liquid-phase chromatographic column of padding with fine particle size and dedicated device for method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Place an elastic quartz capillary chromatographic column 5 with an inner diameter of 100 μm, an outer diameter of 360 μm, and a length of 15 cm in the chromatographic column sleeve 4, and fix it at the bottom of the homogenate tank 3; weigh 50 mg of C18 reverse-phase chromatography silica gel filler with a diameter of 3 μm, and add Prepare a homogenate solution with a concentration of 5mg / mL in 10mL acetone, oscillate and mix, and disperse by ultrasonic for more than 10min; control the heating wire to work through the temperature control system, and heat the pressurized solvent (methanol), homogenate tank 3 and chromatographic column 5 to 50°C, pour 200 μL of the homogenate solution into the homogenate tank 3; seal the homogenate tank 3, connect the pressurized solvent tank 1, the homogenate tank 3 and the chromatographic column 4 through pipelines, and turn on the column packing pump 6, Fill for 30min under 100MPa pressure; unload the capillary chromatographic column, h...

Embodiment 2

[0021] Place an elastic quartz capillary chromatographic column 5 with an inner diameter of 100 μm, an outer diameter of 360 μm, and a length of 15 cm in the chromatographic column sleeve 4, and fix it at the bottom of the homogenate tank 3; weigh 50 mg of C18 reverse-phase chromatography silica gel filler with a diameter of 3 μm, and add Prepare a homogenate solution with a concentration of 5mg / mL in 10mL acetone, oscillate and mix, and disperse by ultrasonic for more than 10min; control the heating wire to work through the temperature control system, and heat the pressurized solvent (methanol), homogenate tank 3 and chromatographic column 5 to 70°C, pour 200 μL of the homogenate solution into the homogenate tank 3; seal the homogenate tank 3, connect the pressurized solvent tank 1, the homogenate tank 3 and the chromatographic column 4 through pipelines, and start the column packing pump 6, Fill for 30min under 100MPa pressure; unload the capillary chromatographic column, han...

Embodiment 3

[0024] Place an elastic quartz capillary chromatographic column 5 with an inner diameter of 100 μm, an outer diameter of 360 μm, and a length of 15 cm in the chromatographic column sleeve 4, and fix it at the bottom of the homogenate tank 3; weigh 50 mg of C18 reverse-phase chromatography silica gel filler with a diameter of 3 μm, and add Prepare a homogenate solution with a concentration of 5mg / mL in 10mL acetone, oscillate and mix, and disperse by ultrasonic for more than 10min; control the heating wire to work through the temperature control system, and heat the pressurized solvent (methanol), homogenate tank 3 and chromatographic column 5 to 90°C, pour 200 μL of the homogenate solution into the homogenate tank 3; seal the homogenate tank 3, connect the pressurized solvent tank 1, the homogenate tank 3 and the chromatographic column 4 through pipelines, and turn on the column packing pump 6, Fill for 30min under 100MPa pressure; unload the capillary chromatographic column, h...

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Abstract

The invention discloses a method for filling a high-temperature liquid-phase chromatographic column of padding with the fine particle size. The method is characterized by comprising the following steps: firstly stirring and mixing the padding with a homogenate solvent, performing ultrasonic dispersing treatment to obtain homogenate, then heating a pressurized solvent pipeline, a homogenate tank and the chromatographic column to enable the temperatures of the pressurized solvent pipeline, the homogenate tank and the chromatographic column to reach 50-90 DEG C, pouring the homogenate into the homogenate tank, connecting the pressurized solvent pipeline, a column filling pump, the homogenate tank and the chromatographic column through a pipeline, sealing the homogenate tank, pressurizing the homogenate tank to 50-200MPa after the temperature of the homogenate is uniform with that of the homogenate tank, and filling the column filling pump with the homogenate and a pressurized solvent. The filling method has relatively low requirements on the high pressure sealing property of filling equipment. Meanwhile, the invention further relates to a dedicated filling device necessary for the filling method.

Description

technical field [0001] The invention relates to a chromatographic column filling method and a special device required for the method. Background technique [0002] The packing of the chromatographic column directly affects its separation performance. Poorly packed chromatographic columns, or the column efficiency is not high, or after a short period of use, the column head will collapse due to the compression of the packed bed, and the chromatographic column efficiency will suddenly decrease. [0003] The filling of liquid chromatography column can adopt different methods according to the nature of the filler and the size of the column. In principle, dry packing can be used to pack large-size chromatographic columns with particles larger than 20 μm. The packing material is directly added to the column tube and compacted by vibration to obtain a uniform packed bed. For chromatographic columns with small inner diameters filled with small particles, high-pressure homogenate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/56
Inventor 孙元社唐涛于淑新张维冰李彤
Owner DALIAN ELITE ANALYTICAL INSTR
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