CN107174837A - A kind of deactivation method of capillary column - Google Patents
A kind of deactivation method of capillary column Download PDFInfo
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- CN107174837A CN107174837A CN201610133712.XA CN201610133712A CN107174837A CN 107174837 A CN107174837 A CN 107174837A CN 201610133712 A CN201610133712 A CN 201610133712A CN 107174837 A CN107174837 A CN 107174837A
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- deactivation
- capillary column
- gas chromatograph
- heat cracker
- deactivated
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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
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- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides a kind of capillary column deactivation method, and the capillary column not deactivated is deactivated by heat cracker gas chromatograph.This method utilizes heat cracker Pintsch process principle, deactivation reagent cracks the active small molecular for being fractured into gas phase state at high temperature, inert carrier gas imports the active small molecular for deactivating reagent in capillary column, is reacted with capillary column inner surface active site, completes deactivation.This method is compared to conventional method, and flow is simple, easy to operate, and treatment effeciency is high.
Description
Technical field
The present invention relates to the preparation method of capillary column, and in particular to a kind of deactivation method of capillary column.
Background technology
In gas-chromatography, the features such as capillary column is due to high inertia, efficient and stabilization is most widely used at present.Hair
The preparation process of capillary column includes：1) roughening of inwall；2) deactivate；3) it is coated.The silica material of capillary column is in itself
Containing hydroxyl activity point, capillary column inner wall coarse process can also increase inwall activity.Prepare post effect high, active
Good and retention repetition the capillary column of low, heat endurance to capillary column, it is necessary to carry out deactivation processing.
Polysiloxanes high temperature deactivation techniques are generally used in production and processing, capillary column inwall is deactivated.First use polysiloxanes
The static coated capillary column of stationary phase, then under nitrogen protection, carries out high temperature deactivation at 400~450 DEG C.Static coated hair
The operating performance of buttress shaft is complicated, time and effort consuming；375 DEG C of elastic quartz capillary column coating highest heatproof, high temperature deactivation needs nitrogen
Atmosphere protection, condition is harsh.It can be seen that, traditional polysiloxanes high temperature deactivation techniques complex operation, condition is harsh.
The content of the invention
The shortcoming of prior art, a kind of deactivation method of capillary column of present invention offer, are not deactivated in view of the above
Capillary column is deactivated by heat cracker-gas chromatograph.This method utilizes heat cracker Pintsch process principle, and deactivation reagent exists
Cracking is fractured into the active small molecular of gas phase state under high temperature, and the active small molecular for deactivating reagent is imported capillary by inert carrier gas
In post, reacted with capillary column inner surface active site, complete deactivation.This method is compared to conventional method, and flow is simple, behaviour
Facilitate, treatment effeciency is high.
In order to solve the above technical problems, the present invention is achieved by the following technical solutions：
A kind of deactivation method of capillary column, the capillary column not deactivated is deactivated by heat cracker-gas chromatograph.
Heat cracker-gas chromatograph is that heat cracker is connected by interface with gas chromatograph injection port.
The heat cracker cleavable sample state is liquid, solid-state or soluble solids.
The heat cracker is that cleavable sample size is 0.1mg-50mg.
Heat cracker highest interface temperature >=350 DEG C.
The heat cracker thermal cracking temperature scope is room temperature to 1400 DEG C.
The gas chromatograph uses N2, He is carrier gas.
The gas chromatograph injection port is shunting/Splitless injecting samples mouthful.
The gas chromatograph injection port maximum operation (service) temperature is 400 DEG C.
The gas chromatograph injection port pressure setting range 0-150PSI.
The gas chromatograph column flow setting range：0-200ml/min is (with N2During for carrier gas)
0-1250ml/min (during using He as carrier gas).
The gas chromatograph column temperature setting range is 0~450 DEG C.
It is preferred that, comprise the following steps：
(1) deactivation reagent is positioned in heat cracker, the capillary column not deactivated is connected to the sample introduction of gas chromatograph
Mouthful；
(2) parameter of heat cracker-gas chromatograph is set, is deactivated.
It is furthermore preferred that one kind in polysiloxanes, polyethylene glycol, silylating reagent and containing hydrogen silicone oil of deactivation reagent or
It is a variety of, such as dimethyl polysiloxane.
It is furthermore preferred that the consumption of deactivation reagent is 0.1~50mg, such as 4mg.
It is preferred that, deactivation time is 1~48h, such as 12h.
It is preferred that, the parameter for setting heat cracker is as follows：
(1) heat cracker interface temperature is 300~500 DEG C, such as 300 DEG C；
(2) heat cracker thermal cracking temperature is 500~1400 DEG C, such as 550 DEG C.
It is preferred that, the parameter for setting gas chromatograph is as follows：
(1) gas chromatograph injection port temperature is 200~400 DEG C, such as 300 DEG C；
(2) gas chromatograph injection port pressure is 0~150PSI, such as 35PSI；
(3) gas chromatograph column oven temperature is 200~400 DEG C, such as 300 DEG C.
It is preferred that, it is further comprising the steps of：Capillary column after deactivation cleaned through organic solvent after with gas chromatograph
Injection port is connected, and removes organic solvent.The organic solvent includes the organic solvents such as acetone, dichloromethane.
It is furthermore preferred that the consumption of organic solvent is 1~50ml, such as 5ml.
It is furthermore preferred that when removing organic solvent, the column temperature of gas chromatograph is 50~400 DEG C, such as 200 DEG C, removes the time
For 5~60min, such as 30min.
It is preferred that, the capillary column length not deactivated is 1~300m, and such as 45m, internal diameter is 0.05~0.53mm, such as
0.53mm。
Beneficial effects of the present invention：A kind of deactivation method of capillary column of the present invention, utilizes heat cracker-gas-chromatography
Instrument carries out deactivation processing to the capillary column not deactivated.This method utilizes heat cracker Pintsch process principle, and deactivation reagent is in height
The lower cracking of temperature is fractured into the active small molecular of gas phase state, and the active small molecular for deactivating reagent is imported capillary column by inert carrier gas
In, reacted with capillary column inner surface active site, complete deactivation.This method is compared to conventional method, and flow is simple, operation
Convenient, treatment effeciency is high.
Brief description of the drawings
Fig. 1 be using embodiment 1 obtain deactivation capillary column as pre-column (10m × 0.53mm), with DB-5 chromatographic columns (30m
× 0.25mmid 0.25um) be connected aroma substance gas chromatogram in analysis tobacco leaf；Abscissa is the time, and unit is minute；It is vertical
Coordinate is signal intensity；
Fig. 2 be using buy commercial brand deactivate capillary column as pre-column (10m × 0.53mm), with DB-5 chromatographic columns (30m ×
0.25mmid 0.25um) be connected aroma substance gas chromatogram in analysis tobacco leaf；Abscissa is the time, and unit is minute；It is vertical to sit
It is designated as signal intensity.
Embodiment
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
Embodiment 1
(1) take 4mg dimethyl polysiloxanes SE30 to be placed in heat cracker, take length be 45m internal diameters be 0.53mm not
Deactivation capillary column is connected to the injection port of gas chromatograph；
(2) gas chromatograph uses N2For carrier gas, injector temperature is set to 300 DEG C, and inlet pressure is set to 35PSI, post
Temperature is set as 300 DEG C；Heat cracker interface temperature is 300 DEG C, and thermal cracking temperature is 550 DEG C；Deactivate 12h；
(3) after deactivation terminates, heat cracker-gas chromatograph is down to room temperature, and the capillary column after deactivation is through 5ml acetone
It is connected after cleaning with the injection port of gas chromatograph, removes organic solvent, column temperature rises to 200 DEG C, and the removal time is 30min.
Deactivation capillary column that embodiment 1 is obtained and Agilent company's 0.53mm internal diameter deactivation fused quartz tubes are gone
Capillary column living is connected point respectively as pre-column (10m × 0.53mm) with DB-5 chromatographic columns (30m × 0.25mmid 0.25um)
Aroma substance in tobacco leaf is analysed, the gas chromatogram of acquisition is shown in Fig. 1 and Fig. 2.34min tailing peaks are nicotine in Fig. 1 and Fig. 2, are
DB-5 capillary column problems, it is unrelated with pre-column.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of deactivation method of capillary column, it is characterised in that the capillary column not deactivated passes through heat cracker-gas-chromatography
Instrument is deactivated.
2. deactivation method according to claim 1, it is characterised in that comprise the following steps：
(1) deactivation reagent is positioned in heat cracker, the capillary column not deactivated is connected to the injection port of gas chromatograph；
(2) parameter of heat cracker-gas chromatograph is set, is deactivated.
3. deactivation method according to claim 2, it is characterised in that deactivation reagent is selected from polysiloxanes, polyethylene glycol, silicon
One or more in Alkylators and containing hydrogen silicone oil.
4. deactivation method according to claim 2, it is characterised in that the consumption of deactivation reagent is 0.1~50mg.
5. deactivation method according to claim 1 or 2, it is characterised in that deactivation time is 1~48h.
6. deactivation method according to claim 1 or 2, it is characterised in that the parameter of setting heat cracker is as follows：
(1) heat cracker interface temperature is 300~500 DEG C；
(2) heat cracker thermal cracking temperature is 500~1400 DEG C.
7. deactivation method according to claim 1 or 2, it is characterised in that the parameter of setting gas chromatograph is as follows：
(1) gas chromatograph injection port temperature is 200~400 DEG C；
(2) gas chromatograph injection port pressure is 0~150PSI；
(3) gas chromatograph column temperature is 200~400 DEG C.
8. deactivation method according to claim 2, it is characterised in that further comprising the steps of：Capillary column after deactivation
It is connected after being cleaned through organic solvent with the injection port of gas chromatograph, removes organic solvent.
9. deactivation method according to claim 8, it is characterised in that the consumption of organic solvent is 1~50ml.
10. deactivation method according to claim 8, it is characterised in that when removing organic solvent, the column temperature of gas chromatograph
For 50~400 DEG C, the removal time is 5~60min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610133712.XA CN107174837B (en) | 2016-03-09 | 2016-03-09 | Deactivation method of capillary column |
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|---|---|---|---|
| CN201610133712.XA CN107174837B (en) | 2016-03-09 | 2016-03-09 | Deactivation method of capillary column |
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| CN107174837A true CN107174837A (en) | 2017-09-19 |
| CN107174837B CN107174837B (en) | 2019-12-31 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010041151A1 (en) * | 2000-03-03 | 2001-11-15 | Ufz-Umweltforschungszentrum Leipiz-Halle Gmbh | Device for pyrolysis gas chromatography, a method for analysing polymers using said device, and a pyrolyzator |
| 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 |
-
2016
- 2016-03-09 CN CN201610133712.XA patent/CN107174837B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010041151A1 (en) * | 2000-03-03 | 2001-11-15 | Ufz-Umweltforschungszentrum Leipiz-Halle Gmbh | Device for pyrolysis gas chromatography, a method for analysing polymers using said device, and a pyrolyzator |
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| 刘文 周学之: "《理化物证检验学》", 30 June 2003, 中国人民公安大学出版社 * |
| 史景江 等: "《色谱分析法》", 31 May 1995, 重庆大学出版社 * |
| 贾春晓 主编: "《仪器分析》", 31 August 2009, 河南科学技术出版社 * |
| 马红梅 刘宏伟: "《实用药物研发仪器分析》", 30 September 2014, 华东理工大学出版社 * |
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