CN208847689U - It is a kind of to control the sample injector of carrier gas preheating and sample Thermal desorption by changing voltage - Google Patents

It is a kind of to control the sample injector of carrier gas preheating and sample Thermal desorption by changing voltage Download PDF

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Publication number
CN208847689U
CN208847689U CN201821412512.9U CN201821412512U CN208847689U CN 208847689 U CN208847689 U CN 208847689U CN 201821412512 U CN201821412512 U CN 201821412512U CN 208847689 U CN208847689 U CN 208847689U
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China
Prior art keywords
sample
carrier gas
thermal desorption
chamber
gas preheating
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Expired - Fee Related
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CN201821412512.9U
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Chinese (zh)
Inventor
王新
张远智
李海洋
李函蔚
王祯鑫
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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Priority to CN201821412512.9U priority Critical patent/CN208847689U/en
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Abstract

The sample injector of carrier gas preheating and sample Thermal desorption is controlled by changing voltage the utility model discloses a kind of, is made of carrier gas pulse control unit module, carrier gas preheating chamber module and sample Thermal desorption chamber modules.Carrier gas pulse control unit module is realized that carrier gas preheating and sample Thermal desorption are to realize by two for thermal modules by two three-way electromagnetic valves.Traditional integral type pyrolysis analysis sample injector is divided into carrier gas preheating and sample Thermal desorption two parts in structure;Heating module substitutes traditional heating rod by adjustable voltage transformation module and ceramic thermal resistance PTC fever tablet and directly heats mode.The present apparatus provides a kind of new-type Thermal desorption sample injector for ionic migration spectrum detection instrument, substantially increases sample introduction process to the utilization rate and sample Thermal desorption efficiency of heat.

Description

It is a kind of to control the sample injector of carrier gas preheating and sample Thermal desorption by changing voltage
Technical field
The utility model relates to a kind of Thermal desorption sample injectors in ion mobility spectrometry, are a kind of detection multicomponents The improvement structure of the Thermal desorption sample injector of complex fluid sample.The present apparatus is in Ion transfer spectrum analysis blood complex sample matrix The blood concentration of drug provides guarantee.Sample introduction process is improved to the utilization rate and sample Thermal desorption efficiency of heat source.
Background technique
The principle of PTC fever tablet constant temperature warming is: when PTC fever tablet is powered, because room temperature resistance is smaller, and starting electricity It flows larger, PTC fever tablet can be made heating up quickly, cause resistance value itself to increase sharply into transition area, at this moment can pass through The electric current of PTC fever tablet is very small, and PTC fever tablet surface temperature is made to remain steady state value, substantially unrelated with environment temperature.
The PTC heat generating core used inside PTC heater has many specification kinds, determine PTC heater voltage, temperature, Difference on power.The constant temperature point of PTC heat generating core may be set within the scope of 50-300 DEG C, and normal temperature resistance is generally in 500-5000 Between Ω.Its shape is usually flat-shaped bar shaped, two lead-out wires, outsourcing insulating materials.It is former using the heated at constant temperature of PTC heat generating core Characteristic is managed, the sample injector in ion mobility spectrometry is applied in present invention design.
Sample injector is its performance quality for the essential element in multifunction ion migration spectrum fast detector, directly Determine the overall performance of sample introduction efficiency and ion mobility spectrometry, existing ion mobility spectrometry Thermal desorption sample injector have motor driven and Electromagnetic drive two ways, heating are all by heating rod temperature control heating, and heating temperature belongs to thermostatic control mode, when heating Between it is different according to heating rod power, use time range 10-30min at present.Heat slow, and the energy consumption for instrument It is relatively high.Traditional Thermal desorption sample injector does not have carrier gas warm-up block, and cold carrier gas, which enters sample injector, influences Thermal desorption process It is quite big.Existing granted patent 201220459129.5 at present, a kind of multifunctional assembled sample injector for ion mobility spectrometry; 201210563261.5 a kind of halogen lamp sample injector etc. for Thermal desorption sample introduction;Patent innovation point in the present invention with it is above-mentioned Granted patent is entirely different.
Utility model content
A kind of to control the sample injector of carrier gas preheating and sample Thermal desorption by changing voltage, sample injector main structure includes One closed container is equipped with a lateral partitions in the middle part of container, and lateral partitions will be separated into upper and lower two chambers inside container, under Side is carrier gas preheating chamber, and top is sample Thermal desorption chamber), through-hole is equipped in lateral partitions;In carrier gas preheating cavity Room lower part is equipped with carrier gas inlet, sample gas outlet is equipped in sample Thermal desorption chamber top, in the indoor cross of sample Thermal desorption chamber The sample introduction slide glass for placing sample is equipped with to partition;
It is respectively equipped in carrier gas preheating chamber and sample Thermal desorption chamber with adjustable voltage transformation module and ceramics Thermistor PTC fever tablet, ceramic thermal resistance PTC fever tablet are connected with adjustable DC power supply;Each chamber can be distinguished Independent temperature control is realized by changing voltage;
Solenoid valve opens and closes control carrier gas transfer.Carrier gas gas source is connected with solenoid valve carrier gas inlet end, solenoid valve Carrier gas outlet end is connected with Thermal desorption sample injector carrier gas preheating chamber;Heat is carried through partition and sample introduction slide glass after carrier gas preheating The sample gas of parsing, the outlet end outflow through sample Thermal desorption chamber enter in detector.
Carrier gas preheating chamber volume is greater than sample Thermal desorption cavity volume, carrier gas preheating chamber volume and sample Thermal desorption chamber The volumetric ratio of room is 2:1.Sample Thermal desorption chamber, which is equipped with to open, is put into mouth with closed sample.Through-hole in lateral partitions Circumference arrangement is presented, through-hole rate is greater than 50%, and is evenly distributed in circular platform type diaphragm internal.
Carrier gas preheating chamber module and sample Thermal desorption chamber modules are originally the cylindrical cavity of an one, carrier gas preheating The external screw thread of chamber upper port cylinder type and the internal screw thread of sample Thermal desorption chamber lower port cylinder type mutually screw togather, And there is high temperature resistant O circle to guarantee internal chamber sealing at the contact surface mutually screwed togather.There is a band internal screw thread in carrier gas preheating chamber side Through-hole, for connecting quick coupling;Sample Thermal desorption chamber-side has a band internal thread through hole, for connecting quick coupling;
Two grooves are respectively equipped in total body upper and lower surfaces, placing ceramic thermistor PTC generates heat in groove Piece provides heat source by the supply voltage for providing different for carrier gas preheating and Thermal desorption room.Not equality of temperature is realized by changing voltage Sample gradient Thermal desorption discharges under degree mode.Sample injector is under the conditions of fixed voltage, it can be achieved that constant temperature heating parses;In variable finger , it can be achieved that lasting temperature programming gradient pyrolysis is analysed under the conditions of constant voltage.
Sample introduction slide glass is filter paper or film, it can carrying sample, and hot-air can be made to penetrate.
Sample injector in the utility model can connect ion mobility spectrometry analyzer, corresponding not according to different voltage conditions Same pyrolysis eutectoid temperature establishes different carrier gas preheating and sample Thermal desorption program, can realize respectively to single or mixing sample It is layered Thermal desorption, realizes the separation analysis of multicomponent sample.
The advantages of the utility model, is as follows:
1. increasing carrier gas preheating chamber module compared with traditional Thermal desorption sample injector;Improve Thermal desorption efficiency.
2. being added to a solenoid valve between carrier gas gas source and Thermal desorption sample injector;Carrier gas pulse control unit module is slow The circulation of carrier gas preheating chamber modular gas has been solved, carrier gas preheating is conducive to;
3. ceramic thermal resistance PTC fever tablet is used to provide plane stable state heat source for Thermal desorption, sheet design makes heated cut Face is uniform, is conducive to the preheating of carrier gas moment involved in the utility model;
4. through mode sample analysis mode is purged instead of sample introduction slide surface, sample introduction slide glass inner sample is greatly accelerated Parsing, improve ionic migration spectrum detection sensitivity for analysis, shorten Thermal desorption time long problem.
Detailed description of the invention
Fig. 1 is a kind of Thermal desorption sample injector overall structure appearance diagram.
Fig. 2 is a kind of cross-section structure (longitudinal direction) schematic diagram of Thermal desorption sample injector.
Fig. 3 is a kind of intermediate membrane schematic diagram of Thermal desorption sample injector.
In figure: 1 is two three-way electromagnetic valves;2 be carrier gas preheating chamber module;3 be sample Thermal desorption chamber modules;4 be quick Connector I, carrier gas inlet;5 be quick coupling II, carrier gas exports;6 be carrier gas preheating chamber module PTC heating piece component groove;7 For sample Thermal desorption chamber modules PTC heating piece component groove;8 be two chambers intermediate bulkhead;9 be sample introduction slide glass.
Specific embodiment
It is combined using the Thermal desorption sample injector and ion mobility spectrometry analyzer of the utility model.When standby, solenoid valve is closed, No carrier gas transmits in sample injector.Preheated carrier gas when sample feeding, solenoid valve are opened, and have carrier gas circulation in preheating chamber.Carrier gas is pre- Heat is using adjustable voltage transformation module and ceramic thermal resistance PTC fever tablet.Voltage uses Switching Power Supply, in 0- Voltage value can be set by software within the scope of 12V, interval is 0.1V.Pass through control flow rate of carrier gas (100-500ml/min) and electricity The magnet valve opening time (5-30S) controls sample volume and sample Thermal desorption time.Carrier gas after preheating pass through partition board hole penetrate into Sample slide glass enters sample Thermal desorption chamber;When carrier gas passes through sample introduction slide glass, enter ion mobility spectrometry using quick coupling II Detector.
Embodiment 1
It is used in conjunction using the sample injector device in the present invention with ion mobility spectrometry analyzer, carrier gas preheating chamber sets voltage value 7.5V, carrier gas preheating temperature are 180 DEG C;Thermal desorption Chamber voltage value 6.0V, pyrolysis eutectoid temperature are 150 DEG C;Detection anesthesia Agent Propofol, detection sensitivity is in 0.2 μ g/mL;If no carrier gas preheats, detection sensitivity is in 0.5 μ g/mL;Sensitivity improves 2.5 Times.
Embodiment 2
Other conditions are constant, the effect of experimental study solenoid valve.Utilize the sample injector device and Ion transfer in the present invention Spectrum analysis instrument is used in conjunction, and carrier gas preheating chamber sets voltage value 7.5V, and carrier gas preheating temperature is 180 DEG C;Thermal desorption Chamber electricity Pressure value 6.0V, pyrolysis eutectoid temperature are 150 DEG C;
Two ways: it is normally opened that one is solenoid valves;It is closed after opening 10S one is solenoid valve, realizes moment sample introduction.Simultaneously 5ppm anesthetic Propofol sample is detected, Pulsed Sampling signal strength peak value enhances 1 times.

Claims (5)

1. a kind of control the sample injector of carrier gas preheating and sample Thermal desorption by changing voltage, it is characterised in that:
Sample injector main structure includes a closed container, a lateral partitions is equipped in the middle part of container, lateral partitions will be inside container Upper and lower two chambers are separated into, lower section is carrier gas preheating chamber, and top is sample Thermal desorption chamber, in lateral partitions Equipped with through-hole;It is equipped with carrier gas inlet in carrier gas preheating chamber lower part, is equipped with sample gas outlet in sample Thermal desorption chamber top, in The indoor lateral partitions of sample Thermal desorption chamber are equipped with the sample introduction slide glass for placing sample;
In being respectively equipped in carrier gas preheating chamber and sample Thermal desorption chamber with adjustable voltage transformation module and ceramic temperature-sensitive Resistance PTC fever tablet, ceramic thermal resistance PTC fever tablet are connected with adjustable DC power supply;Each chamber can pass through respectively Change voltage and realizes independent temperature control;
Carrier gas gas source is connected with solenoid valve carrier gas inlet end, solenoid valve carrier gas outlet end and Thermal desorption sample injector carrier gas preheating cavity Room is connected;The sample gas of Thermal desorption, going out through sample Thermal desorption chamber are carried after carrier gas preheating through partition and sample introduction slide glass The outflow of mouth end enters in detector, and solenoid valve opens and closes control carrier gas transfer.
2. sample injector described in accordance with the claim 1, it is characterised in that: carrier gas preheating chamber volume is greater than sample Thermal desorption chamber The volumetric ratio of volume, carrier gas preheating chamber volume and sample Thermal desorption chamber is 2:1.
3. sample injector described in accordance with the claim 1, it is characterised in that: sample Thermal desorption chamber be equipped with can open with it is closed Sample is put into mouth.
4. according to sample injector described in claim 1 or 3, it is characterised in that: carrier gas preheating chamber upper port cylinder type Have at the contact surface that the internal screw thread of external screw thread and sample Thermal desorption chamber lower port cylinder type is mutually screwed togather, and mutually screwed togather High temperature resistant O circle guarantees internal chamber sealing.
5. sample injector described in accordance with the claim 1, it is characterised in that: circumference arrangement, through-hole is presented in the through-hole in lateral partitions Rate is greater than 50%, and is evenly distributed in circular platform type diaphragm internal.
CN201821412512.9U 2018-08-30 2018-08-30 It is a kind of to control the sample injector of carrier gas preheating and sample Thermal desorption by changing voltage Expired - Fee Related CN208847689U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112903803A (en) * 2019-11-19 2021-06-04 中国科学院大连化学物理研究所 Device and method for improving detection sensitivity of etomidate blood concentration in operation

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112903803A (en) * 2019-11-19 2021-06-04 中国科学院大连化学物理研究所 Device and method for improving detection sensitivity of etomidate blood concentration in operation

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CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20190510

Termination date: 20210830