CN107174837B - Deactivation method of capillary column - Google Patents
Deactivation method of capillary column Download PDFInfo
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- CN107174837B CN107174837B CN201610133712.XA CN201610133712A CN107174837B CN 107174837 B CN107174837 B CN 107174837B CN 201610133712 A CN201610133712 A CN 201610133712A CN 107174837 B CN107174837 B CN 107174837B
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- capillary column
- gas chromatograph
- deactivation
- temperature
- thermal cracker
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
Abstract
The invention provides a method for deactivating a capillary column, wherein the undectivated capillary column is deactivated by a thermal cracker-gas chromatograph. The method utilizes the high-temperature cracking principle of a thermal cracker, the deactivation reagent is cracked and cracked into active small molecules in a gas phase state at high temperature, and the active small molecules of the deactivation reagent are introduced into the capillary column by inert carrier gas and react with active points on the inner surface of the capillary column to complete deactivation. Compared with the traditional method, the method has the advantages of simple process, convenient operation and high treatment efficiency.
Description
Technical Field
The invention relates to a preparation method of a capillary column, in particular to a deactivation method of the capillary column.
Background
In gas chromatography, capillary columns are currently most widely used due to their characteristics of high inertness, high efficiency, stability, etc. The preparation process of the capillary column comprises the following steps: 1) roughening the inner wall; 2) deactivating; 3) and (4) coating. The silica raw material of the capillary column contains hydroxyl active points, and the roughening processing process of the inner wall of the capillary column can also increase the activity of the inner wall. To prepare a capillary column with high column efficiency, low activity, good thermal stability and repeated retention values, the capillary column needs to be deactivated.
Polysiloxane high-temperature deactivation technology is commonly adopted in production and processing, and the inner wall of a capillary column is deactivated. The method comprises the steps of statically coating a capillary column with a polysiloxane stationary phase, and deactivating at a high temperature of 400-450 ℃ under the protection of nitrogen. The operation procedure of statically coating the capillary column is complex, time-consuming and labor-consuming; the elastic quartz capillary column coating can resist the temperature of 375 ℃ at most, and the high-temperature deactivation needs the protection of nitrogen atmosphere, and the conditions are harsh. As can be seen, the conventional high temperature deactivation of polysiloxanes is complicated to operate and is harsh.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention provides a method for deactivating a capillary column, the capillary column not being deactivated by means of a thermal cracker-gas chromatograph. The method utilizes the high-temperature cracking principle of a thermal cracker, the deactivation reagent is cracked and cracked into active small molecules in a gas phase state at high temperature, and the active small molecules of the deactivation reagent are introduced into the capillary column by inert carrier gas and react with active points on the inner surface of the capillary column to complete deactivation. Compared with the traditional method, the method has the advantages of simple process, convenient operation and high treatment efficiency.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a method for deactivating a capillary column, wherein the capillary column which is not deactivated is deactivated by means of a thermal cracker-gas chromatograph.
The thermal cracker-gas chromatograph is a thermal cracker and is connected with a sample inlet of the gas chromatograph through an interface.
The pyrolysis device can crack the sample in a liquid state, a solid state or a soluble solid state.
The amount of the cracking sample of the thermal cracker is 0.1mg-50 mg.
The maximum interface temperature of the thermal cracker is more than or equal to 350 ℃.
The thermal cracking temperature range of the thermal cracker is from room temperature to 1400 ℃.
The gas chromatograph uses N2And He is a carrier gas.
The sample inlet of the gas chromatograph is a split/non-split sample inlet.
The maximum service temperature of the sample inlet of the gas chromatograph is 400 ℃.
The pressure setting range of the sample inlet of the gas chromatograph is 0-150 PSI.
The gas chromatograph column flow setting range is as follows: 0-200ml/min (in N)2When carrying gas)
0-1250ml/min (when He is used as carrier gas).
The set range of the column temperature of the gas chromatograph is 0-450 ℃.
Preferably, the method comprises the following steps:
(1) placing the deactivating reagent in a thermal cracker, and connecting an undeactivated capillary column to a sample inlet of a gas chromatograph;
(2) and setting parameters of a thermal cracker-gas chromatograph, and deactivating.
More preferably, the deactivating agent is selected from one or more of polysiloxanes, polyethylene glycols, silanization agents and hydrogen containing silicone oils, such as dimethylpolysiloxanes.
More preferably, the deactivating agent is present in an amount of 0.1 to 50mg, such as 4 mg.
Preferably, the deactivation time is 1-48 h, such as 12 h.
Preferably, the thermal cracker parameters are set as follows:
(1) the interface temperature of the thermal cracker is 300-500 ℃, such as 300 ℃;
(2) the thermal cracking temperature of the thermal cracker is 500-1400 ℃, such as 550 ℃.
Preferably, the parameters of the gas chromatograph are set as follows:
(1) the temperature of a sample inlet of the gas chromatograph is 200-400 ℃, such as 300 ℃;
(2) the pressure of a sample inlet of the gas chromatograph is 0-150PSI, such as 35 PSI;
(3) the temperature of the gas chromatograph column oven is 200-400 ℃, such as 300 ℃.
Preferably, the method further comprises the following steps: and cleaning the deactivated capillary column with an organic solvent, and connecting the capillary column with a sample inlet of a gas chromatograph to remove the organic solvent. The organic solvent includes acetone, dichloromethane and other organic solvents.
More preferably, the amount of the organic solvent is 1 to 50ml, such as 5 ml.
More preferably, the column temperature of the gas chromatograph is 50-400 ℃, such as 200 ℃, and the removal time is 5-60 min, such as 30min, when the organic solvent is removed.
Preferably, the non-deactivated capillary column has a length of 1 to 300m, such as 45m, and an internal diameter of 0.05 to 0.53mm, such as 0.53 mm.
The invention has the beneficial effects that: the invention relates to a method for deactivating a capillary column, which is characterized in that a thermal cracker-gas chromatograph is used for deactivating the undeactivated capillary column. The method utilizes the high-temperature cracking principle of a thermal cracker, the deactivation reagent is cracked and cracked into active small molecules in a gas phase state at high temperature, and the active small molecules of the deactivation reagent are introduced into the capillary column by inert carrier gas and react with active points on the inner surface of the capillary column to complete deactivation. Compared with the traditional method, the method has the advantages of simple process, convenient operation and high treatment efficiency.
Drawings
FIG. 1 is a gas chromatogram of an aroma substance in tobacco leaves analyzed by connecting a deactivated capillary column obtained in example 1 as a pre-column (10 m.times.0.53 mm) with a DB-5 chromatographic column (30 m.times.0.25 mmid 0.25 um); the abscissa is time in minutes; the ordinate is the signal strength;
FIG. 2 is a gas chromatogram of the analysis of aroma in tobacco leaves using a commercial brand deactivation capillary column as a pre-column (10 m.times.0.53 mm) in conjunction with a DB-5 chromatographic column (30 m.times.0.25 mmid 0.25 um); the abscissa is time in minutes; the ordinate is the signal strength.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
(1) Placing 4mg of dimethylpolysiloxane SE30 in a thermal cracker, connecting an undeactivated capillary column with a length of 45m and an inner diameter of 0.53mm to a sample inlet of a gas chromatograph;
(2) gas chromatograph employing N2The temperature of a sample inlet is set to 300 ℃, the pressure of the sample inlet is set to 35PSI, and the temperature of a column is set to 300 ℃ as carrier gas; the interface temperature of the thermal cracker is 300 ℃, and the thermal cracking temperature is 550 ℃; deactivation is carried out for 12 h;
(3) after deactivation, the temperature of the thermal cracker-gas chromatograph is reduced to room temperature, the deactivated capillary column is cleaned by 5ml of acetone and then is connected with a sample inlet of the gas chromatograph, the organic solvent is removed, the temperature of the column is raised to 200 ℃, and the removal time is 30 min.
The deactivated capillary column obtained in example 1 and the deactivated capillary column of 0.53mm inner diameter deactivated fused silica tube from Agilent corporation were used as pre-columns (10 m.times.0.53 mm), respectively, and the aroma substances in the tobacco leaves were analyzed by connecting to a DB-5 chromatographic column (30 m.times.0.25 mmid.0.25 um), and the obtained gas chromatograms were shown in FIGS. 1 and 2. The 34min tail peak in fig. 1 and 2 is nicotine, which is a DB-5 capillary column problem, independent of the pre-column.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (6)
1. A method for deactivating a capillary column, wherein the capillary column that has not been deactivated is deactivated by means of a thermal cracker-gas chromatograph, comprising the steps of:
(1) placing the deactivating reagent in a thermal cracker, and connecting an undeactivated capillary column to a sample inlet of a gas chromatograph; the dosage of the deactivation reagent is 0.1-50 mg;
(2) setting parameters of a thermal cracker-gas chromatograph, deactivating, wherein the interface temperature of the thermal cracker is 300-500 ℃; the thermal cracking temperature of the thermal cracker is 500-1400 ℃; the temperature of a sample inlet of the gas chromatograph is 200-400 ℃; and cleaning the deactivated capillary column with an organic solvent, and connecting the capillary column with a sample inlet of a gas chromatograph to remove the organic solvent.
2. Deactivation method according to claim 1, characterized in that the deactivation agent is selected from one or more of polysiloxanes, polyethylene glycols, silanization agents and hydrogen containing silicone oils.
3. The deactivation method according to claim 1, wherein the deactivation time is 1 to 48 hours.
4. Deactivation method according to claim 1, characterized in that the parameters of the gas chromatograph are set as follows:
(1) the pressure of a sample inlet of the gas chromatograph is 0-150 PSI;
(2) the column temperature of the gas chromatograph is 200-400 ℃.
5. The deactivation method according to claim 1, wherein the organic solvent is used in an amount of 1 to 50 ml.
6. The deactivation method according to claim 1, wherein the removal of the organic solvent is performed at a column temperature of 50 to 400 ℃ for 5 to 60min in a gas chromatograph.
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| CN201610133712.XA CN107174837B (en) | 2016-03-09 | 2016-03-09 | Deactivation method of capillary column |
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| CN103893833A (en) * | 2014-04-04 | 2014-07-02 | 深圳市顺美医疗科技有限公司 | Intravascular catheter capable of improving surface lubrication and preparation method for same |
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