CN109030615A - Thermal desorption device and mass spectrometric analysis method - Google Patents
Thermal desorption device and mass spectrometric analysis method Download PDFInfo
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- CN109030615A CN109030615A CN201811304057.5A CN201811304057A CN109030615A CN 109030615 A CN109030615 A CN 109030615A CN 201811304057 A CN201811304057 A CN 201811304057A CN 109030615 A CN109030615 A CN 109030615A
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- container
- groove
- thermal desorption
- desorption device
- cone mouth
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- 238000004949 mass spectrometry Methods 0.000 title claims abstract description 32
- 238000003795 desorption Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 10
- 230000001154 acute effect Effects 0.000 claims abstract description 4
- 238000001819 mass spectrum Methods 0.000 claims description 23
- 239000012774 insulation material Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 description 6
- 238000001601 dielectric barrier discharge ionisation Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001992 dielectric barrier discharge ionisation mass spectrometry Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000002301 combined effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000688 desorption electrospray ionisation Methods 0.000 description 1
- 238000000375 direct analysis in real time Methods 0.000 description 1
- 238000012063 dual-affinity re-targeting Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Abstract
The present invention provides a kind of thermal desorption device and mass spectrometric analysis method, the thermal desorption device includes: ontology, and the ontology has groove, and the angle between the bottom surface and horizontal plane of the groove is acute angle；Temperature control module, the temperature control module are used to adjust the temperature of the ontology；The first container, the ontology is arranged in the first container, and the groove is exposed outside the first container；The first container has the first through hole that the cable suitable for the temperature control module passes through；Heat-barrier material, the heat-barrier material filling is in the container.The present invention has many advantages, such as that detectability is strong, detection is efficient.
Description
Technical field
The present invention relates to mass spectral analyses, in particular to thermal desorption device, mass spectrometry system and its working method.
Background technique
It is in situ to ionize (ambient ionization) ion source with the release of the DART and DESI ion source of commercialization
New hot spot as industry development.Ionization ion source in situ does not need or only needs seldom sample treatment, so that it may quickly
Direct qualitative and quantitative analysis is carried out to complex sample, this is the maximum feature of such ion source, and high-throughput at present
The new direction of analytical technique of mass spectrum development.
DBDI-100 be it is a without the pre-treatment of sample complexity, polarity, low pole can be made under atmospheric pressure open environment very
The mass ion source ionized to nonpolar sample molecule.It can be combined, realize with the liquid matter mass spectrograph of a variety of mainstream mass spectrums producer
The samples direct injection analysis such as gas, liquid and solid.Suitable for food safety, drug safety, drugs inspection, environmental monitoring etc.
In situ, real-time, the quick detection in field.
In actual analysis detection application, the sample (such as sulfa antibiotics) for high, difficult volatilization that there are a kind of boiling points.By
Heating module is carried in DBDI and is only capable of being heated to 200 DEG C, and plasma actual temperature will may also be far below the numerical value, therefore DBDI
It is ineffective for such sample detection.
Summary of the invention
To solve the deficiency in above-mentioned prior art, the present invention provides a kind of pyrolysis suitable for mass spectral analysis
Device is inhaled, the sample of Mass Spectrometer Method larger class is facilitated.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of thermal desorption device, the thermal desorption device include:
Ontology, the ontology have groove, and the angle between the bottom surface and horizontal plane of the groove is acute angle；
Temperature control module, the temperature control module are used to adjust the temperature of the ontology；
The first container, the ontology is arranged in the first container, and the groove is exposed outside the first container；
The first container has the first through hole that the cable suitable for the temperature control module passes through；
Heat-barrier material, the heat-barrier material filling is in the container.
The object of the invention is also to provide the mass spectrometry system based on above-mentioned thermal desorption device, which is
It is achieved by the following technical programs:
Mass spectrometry system, the mass spectrometry system include ion source, mass spectrum cone mouth；The mass spectrometry system is into one
Step includes:
Above-mentioned thermal desorption device is arranged between the ion source and mass spectrum cone mouth, and is in ion source cone mouth and mass spectrum
The lower section of line between cone mouth.
The object of the invention is also to provide the mass spectrometric analysis method based on above-mentioned mass spectrometry system, the goals of the invention
It has the technical scheme that
According to the mass spectrometric analysis method of above-mentioned mass spectrometry system, the mass spectrometric analysis method the following steps are included:
(A1) sample is added in groove by liquid-transfering gun；
(A2) ontology is heated, and reaches set temperature；Sample Fu Ji, not desorb in the groove；
(A3) ion source works, and sample is ionized, and enters analyzer by mass spectrum cone mouth, to know the letter of sample
Breath.
Compared with prior art, the device have the advantages that are as follows:
1. detectability is strong, sample classification that can be detected is more；
When with the ionization ion source combination (i.e. mass spectrometry system) in situ such as DBDI, improve DBDI-MS to be difficult to resolve suction, difficulty is waved
At least 10 times or more of detectability of hair, the difficult sample ionized；
2. easy to operate；
Outer cover is provided, fool-proof design is covered with, avoids operation error damage mass spectrum and ion source；
3. providing relative closure environment using outer cover, detection collimation is preferable；
4. by heater body, so that remaining hardly possible volatile samples volatilization in groove, so that the self-cleaning of equipment is realized,
Cleaning treatment without complexity after use, and noresidue, it is reusable；
5. after thermal desorption device and DBDI-MS combination (i.e. mass spectrometry system), in the shape of plasma flow, groove
And under the interaction of gradient, gravity, temperature, unstable Leiden Forrester effect is formed, there is significant concentration effect to sample
Fruit, detection are efficiently controllable.
Detailed description of the invention
Referring to attached drawing, the disclosure of the present invention will become more readily understood.Skilled addressee readily understands that: this
It is only used to illustrate the technical scheme of the present invention for a little attached drawings, and is not intended to limit the scope of protection of the present invention.
In figure:
Fig. 1 is the structure diagram of the mass spectrometry system of the embodiment of the present invention；
Fig. 2 is the structure diagram of the thermal desorption device of the embodiment of the present invention.
Specific embodiment
Fig. 1-2 and following description describe optional embodiments of the invention to instruct how those skilled in the art implement
It is of the invention with reproducing.In order to teach the technical scheme of the invention, it has simplified or omitted some conventional aspects.Those skilled in the art
It should be understood that the variation or replacement from these embodiments will within the scope of the invention.Those skilled in the art should understand that
The following features can be combined in various ways to form multiple variations of the present invention.As a result, the invention is not limited to it is following can
Embodiment is selected, and is only limited by the claims and their equivalents.
Embodiment 1:
Fig. 1 schematically illustrates the structure diagram of the mass spectrometry system of the embodiment of the present invention 1, as shown in Figure 1, described
Mass spectrometry system includes:
Ion source 1, such as DBDI；
Mass spectrometer 3 has mass spectrum cone mouth etc.；Distance between ion source cone mouth and mass spectrum cone mouth is 15-30mm, such as
15mm,20mm,30mm；
Thermal desorption device 2, the thermal desorption device are arranged between the ion source and mass spectrometer, and are in ion
The lower section of line between source cone mouth and mass spectrum cone mouth；
Fig. 2 schematically illustrates the structure diagram of the thermal desorption device of the embodiment of the present invention 1, as shown in Fig. 2, the heat
Desorption apparatus includes:
Ontology 26 selects the material of good heat conductivity, such as aluminium, and the ontology has groove 28, as hollow cylinder is recessed
The top of the ontology is arranged in slot, and the angle between the bottom surface and horizontal plane of the groove is acute angle；The bottom surface of the groove
The vertical range of center to the line is 5-10mm, and such as 5mm, 70mm, 10mm, the center of the bottom surface of the groove is in the company
The distance of vertical point to the ion source cone mouth on line is 3-10mm, such as 3mm, 7mm, 10mm, the center of the bottom surface of the groove
Distance to the vertical plane with the line is 0.5-2.5mm, such as 0.5mm, 1mm, 2.5mm；
Temperature control module, such as the combination of heating device and temperature measuring device, the temperature control module is used to adjust the temperature of the ontology
Degree；
The first container 22, the ontology is arranged in the first container, and the groove is exposed in the first container
Outside；The first container has the first through hole that the cable suitable for the temperature control module passes through；
Heat-barrier material, the heat-barrier material filling in the container, avoid heat from conducting between ontology and the first container.
In order to improve groove to the inspissation of sample, further, the angle is 1-10 degree, the depth of the groove
For 1-5mm, such as 1mm, 3mm, 5mm, the external diameter of a circle in the section perpendicular to central axis of the groove is 3-10mm, such as
3mm、7mm、10mm。
In order to connect and fix ontology, further, the thermal desorption device further comprises:
Connector, the connector are used to connect bottom and the first container of the ontology.
In order to carry the first container and improve heat-insulating capability, further, the thermal desorption device is further wrapped
It includes:
Second container 23, the second container have upper cover, cavity and the second through-hole；The cable pass through the cavity and
Second through-hole extends to outside second container, and the first container is connect with the upper cover；
The side wall of the first container 22 has protruding portion 29, and the protruding portion is fixed on the upper cover by connector
On.
Contacing by mistake in operation in order to prevent, further, the thermal desorption device further comprises:
The periphery of the first container 22, the bottom end of outer cover 21 and the top cap is arranged in outer cover 21, the outer cover 21
It connects；Opposite two side of the outer cover, which has, is suitable for through-hole or slot that the line passes through, and the top of the outer cover has
The through-hole of fixed liquid-transfering gun, the groove are in the downside of the through-hole of the fixed liquid-transfering gun.
In order to preferably heat-insulated, further, the upper cover has inner fovea part, and the part of the first container is arranged in institute
It states in inner fovea part；Filling with insulation material between the first container and upper cover.
The working method of the mass spectrometric analysis method of the embodiment of the present invention namely above-mentioned mass spectrometry system, the mass spectrum point
Analysis method the following steps are included:
(A1) sample is added in groove by liquid-transfering gun；
(A2) ontology is heated, and reaches set temperature；Sample Fu Ji, not desorb in the groove；
(A3) ion source works, and sample is ionized, and enters analyzer by mass spectrum cone mouth, to know the letter of sample
Breath.
Embodiment 2:
According to embodiments of the present invention 1 thermal desorption device and the application examples of method.
As shown in Figs. 1-2, in the mass spectrometry system of the application examples, ion source 1 uses DBDI；The setting of groove 28 is at this
The top of body, the groove 28 are in hollow cylindrical body, the plane perpendicular of the central axis of cylindrical body and the groove, bottom surface
Angle between horizontal plane is 5 degree；The diameter of cylindrical body is 6mm；The depth of groove is 4mm；The center of the bottom surface of the groove
Vertical range to line between the ion source cone mouth and mass spectrum cone mouth is 5-10mm, and the center of the bottom surface of the groove is described
The distance of vertical point to the ion source cone mouth on line is 3-10mm, and the center of the bottom surface of the groove is to the line
Vertical plane distance be 0.5-2.5mm；
Two opposite sides of the position of outer cover 21 have groove, suitable for blocking ion source cone mouth and mass spectrum cone mouth respectively,
To realize the positioning of ion source cone mouth and mass spectrum cone mouth；The top of outer cover 21 has through-hole, and liquid-transfering gun is adapted to pass through through-hole
And be fixed on through-hole, the groove 28 on ontology 26 is in the downside of the through-hole of fixed liquid-transfering gun, so that liquid-transfering gun is to groove
The distance at bottom is 3-10mm, such as 7mm；The outer cover 21 is fixed on the upper lid of second container by magnet, at position 25；Temperature
Control module includes ceramic heating flake and thermocouple, and thermocouple is inserted into ontology, and ceramic heating flake is fixed on the body.
The bottom of the first container 22 has the through-hole that the cable suitable for temperature control module passes through, and the bottom of the first container is logical
Cross the bottom of connector connection and fixed ontology；There is gap, filling with insulation material in gap between the first container and ontology；The
The side of one container has protruding portion 29, and protruding portion is fixed on the upper lid of second container by screw etc., so that first holds
The part of device is exposed, is partially in the downward inner fovea part of upper cover；It is stuffed heat insulated between the first container and the inner fovea part of upper cover
Material；The cable enters in the cavity of second container after the through-hole of the first container, passes through the side plate of second container later
Through-hole on 24 is fixed in the Aviation Connector 27 on the side plate, and the side plate is fixed on second by connectors such as screws
On the shell of container；
The working method of the mass spectrometric analysis method of the embodiment of the present invention namely above-mentioned mass spectrometry system, the mass spectrum point
Analysis method the following steps are included:
(A1) liquid-transfering gun extracts quantitative sample, and such as 6-10 microlitres, liquid-transfering gun is fixed on the through-hole at the top of outer cover, moves
Sample is added in groove by liquid rifle；
(A2) ontology is heated, and reaches set temperature；Sample Fu Ji, not desorb in the groove；
By the multiple parameters of above-mentioned groove, (center of the bottom surface of depth, diameter and tilt angle and groove is described
The distance of vertical point on line to the ion source cone mouth) restriction combined effect so that forming unstable Leiden good fortune Lay
This special efficacy is answered, and the concentrated effect of sample is improved；
(A3) ion source works, and sample is ionized, and enters analyzer by mass spectrum cone mouth, to know the letter of sample
Breath.
Claims (10)
1. a kind of thermal desorption device, it is characterised in that: the thermal desorption device includes:
Ontology, the ontology have groove, and the angle between the bottom surface and horizontal plane of the groove is acute angle；
Temperature control module, the temperature control module are used to adjust the temperature of the ontology；
The first container, the ontology is arranged in the first container, and the groove is exposed outside the first container；It is described
The first container has the first through hole that the cable suitable for the temperature control module passes through；
Heat-barrier material, the heat-barrier material filling is in the container.
2. thermal desorption device according to claim 1, it is characterised in that: the central axis of the groove and the groove
Plane perpendicular.
3. thermal desorption device according to claim 1, it is characterised in that: the angle is 1-10 degree, the depth of the groove
Degree is 1-5mm, and the external diameter of a circle in the section perpendicular to central axis of the groove is 3-10mm.
4. thermal desorption device according to claim 1, it is characterised in that: the thermal desorption device further comprises:
Second container, the second container have upper cover, cavity and the second through-hole；The cable passes through the cavity and second and leads to
Hole extends to outside second container, and the first container is connect with the upper cover；
The side wall of the first container has protruding portion, by connector that the protruding portion is fixed on the cover.
5. thermal desorption device according to claim 4, it is characterised in that: the upper cover has inner fovea part, and described first holds
The part of device is arranged in the inner fovea part；Filling with insulation material between the first container and upper cover.
6. the mass spectrometry system of -5 any thermal desorption devices, the mass spectrometry system include according to claim 1
Ion source, mass spectrum cone mouth；It is characterized by: the mass spectrometry system further comprises:
Any thermal desorption device of claim 1-5 is arranged between the ion source and mass spectrum cone mouth, and is in ion
The lower section of line between source cone mouth and mass spectrum cone mouth.
7. mass spectrometry system according to claim 6, it is characterised in that: the center of the bottom surface of the groove to the company
The vertical range of line is 5-10mm, vertical point of the center of the bottom surface of the groove on the line to the ion source cone mouth
Distance is 3-10mm, and the distance of center to the vertical plane with the line of the bottom surface of the groove is 0.5-2.5mm；It is described
Mass spectrum cone mouth is at a distance from ion source cone mouth in 15-30mm.
8. mass spectrometry system according to claim 6, it is characterised in that: the thermal desorption device further comprises:
The periphery of the first container is arranged in outer cover, the outer cover, and the bottom end of outer cover is connect with the upper cover；The outer cover
Two opposite sides, which have, is suitable for through-hole or slot that the line passes through, and the top of the outer cover has the logical of fixed liquid-transfering gun
Hole, the groove are in the downside of the through-hole of the fixed liquid-transfering gun.
9. mass spectrometry system according to claim 8, it is characterised in that: ion source cone mouth and/mass spectrum cone mouth are caught in institute
It states in the through-hole or slot of opposite two side of outer cover.
10. according to the mass spectrometric analysis method of any mass spectrometry system of claim 6-9, the mass spectrometric analysis method packet
Include following steps:
(A1) sample is added in groove by liquid-transfering gun；
(A2) ontology is heated, and reaches set temperature；Sample Fu Ji, not desorb in the groove；
(A3) ion source works, and sample is ionized, and enters analyzer by mass spectrum cone mouth, to know the information of sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811304057.5A CN109030615A (en) | 2018-11-03 | 2018-11-03 | Thermal desorption device and mass spectrometric analysis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811304057.5A CN109030615A (en) | 2018-11-03 | 2018-11-03 | Thermal desorption device and mass spectrometric analysis method |
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| Publication Number | Publication Date |
|---|---|
| CN109030615A true CN109030615A (en) | 2018-12-18 |
Family
ID=64614329
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811304057.5A Pending CN109030615A (en) | 2018-11-03 | 2018-11-03 | Thermal desorption device and mass spectrometric analysis method |
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