CN104716001A - Liquid continuous sampling device for heating and gasification - Google Patents
Liquid continuous sampling device for heating and gasification Download PDFInfo
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- CN104716001A CN104716001A CN201310684182.4A CN201310684182A CN104716001A CN 104716001 A CN104716001 A CN 104716001A CN 201310684182 A CN201310684182 A CN 201310684182A CN 104716001 A CN104716001 A CN 104716001A
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- gasification
- liquid
- vaporizer
- heating
- sample introduction
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0431—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a liquid continuous sampling device for heating and gasification. The liquid continuous sampling device for the heating and the gasification mainly applies to the gasification of volatile liquid. An adopted gasification device comprises a liquid sampling needle, a gasification chamber, a pipeline, sweeping gas, a gasification channel, a sweeping channel and a nut. The liquid is injected into the gasification chamber at a certain flow rate through the liquid sampling needle to conduct gasification, part of the gas after being gasified reaches to a gas analyzer through the pipeline, and part of the gas is brought out of the gasification chamber by the sweeping gas. The gasification quantity of the liquid in the gasification can be controlled by changing the flow rate of the liquid sampling needle. The liquid continuous sampling device for the heating and the gasification has the advantages that the repeatability is good, the memory effect is small, the size is small, and the structure is simple when the gasification is conducted on the gas.
Description
Technical field
The present invention is mainly used in the gasification sample introduction of difficult volatile liquid.Be exactly utilize this device to enter gas analyzer continuously by after difficult volatile liquid sample heating and gasifying specifically.Thus realize fluid sample continuous gasification sample introduction.
Background technology
Mass spectrum is a kind of spectrum method arranged side by side with spectrum, typically refers to and is widely used in every subjects field by ionizing, being separated, detect a kind of know-how that ion carrys out authenticating compound.Mass spectrum can provide abundant compound composition and molecular structure information.In numerous analysis test methods, mass spectrometry method is considered to a kind of method simultaneously possessing high specific and high sensitivity and universality.Mass spectrometric operation needs to run under vacuo, and this causes the bulky of instrument, and power consumption is high, expensive.For the mass spectrum of Liquid sample introduction, because volume after liquid gasification adds about 1000 times, this requires higher to mass spectrographic vacuum equipment, and vacuum equipment is bulky.
Along with the development of society is more and more urgent to portable mass spectrum demand, VUV characteristic of a navigation light spectrum is the mass spectrometer that new development is in recent years got up, and its feature is that the fragment peak of parent ion is few, and namely detecting blend sample is can without sample pre-treatments.But in order to reduce mass spectrographic volume, VUV characteristic of a navigation light spectrum is that structure is simple by capillary direct injected test sample, and especially the detection of commute volatile liquid is very suitable.If when detecting fluid sample, owing to transferring a large amount of gas when liquid gasifies in a vacuum to, thus the vacuum that broken obversion spectrum is inner.Detection for the difficult volatile samples of liquid needs to open up new method.
Detection for effumability sample is detected in Sample introduction to mass spectrum by capillary.But it is more difficult during the detection of this method to difficult volatile liquid.Such as to the detection of wine sample, if only undertaken detecting by the mode of headspace sampling, some volatile materials can only be detected, but few for those content, that boiling point is high, difficulty is volatilized material is then difficult to be detected, and this limits the scope of instrument detection material to a certain extent.
This device overcomes above-mentioned shortcoming to a certain extent, it can be used as sample pretreatment device and is connected with analytical instrument, also the material of volatilization difficult in fluid sample can be detected, be more conducive to the analysis that sample is follow-up while volatile substances being detected.
Summary of the invention
The object of this invention is to provide a kind of liquid continuous sample introduction device of heating and gasifying.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of liquid continuous sample introduction device of heating and gasifying comprises Liquid sample introduction pin, vaporizer, pipeline, sweep gas, gasification tunnel, purge passage, nut.
Described vaporizer is made up of gasification tunnel and purge passage.Purge passage is oblique through bottom gasification tunnel.Gasification tunnel top is step-like, and step is provided with sealing gasket, sample introduction needle syringe needle and vaporizer is sealed by nut crush seal pad.
Described vaporizer being provided with calandria heat for vaporizer, being provided with attemperating unit, for controlling the temperature of vaporizer above vaporizer simultaneously.
Liquid in described sample introduction needle is injected directly in vaporizer by pump and gasifies.Described purge passage is incline structure, and the gas bottom gasification tunnel is more easily gone out by purging.
Described sweep gas have passed through preheating before entering vaporizer, makes sweep gas reach the temperature of vaporizer.
Described gasification tunnel is provided with the hole be connected with the locular wall that gasifies, is provided with pipeline inside hole, the gas in vaporizer is directly connected with extraneous gas analyzer by pipeline.
The course of work of this device:
During sample introduction, syringe pump is arranged on a suitable sample introduction speed, heated to vaporizer 2 by attemperating unit, fluid sample gasifies rapidly under high temperature action, a gas part after gasification 3 enters gas analyzer by the road, and another part is by blowing out vaporizer 2 after sweep gas 4 carrier band.When terminating sample introduction, temperature control and syringe pump are closed.
Beneficial effect of the present invention is: this purging gas circuit, with certain gradient, not only blows away rapidly the sample gas in vaporizer, avoids liquid remaining in bottom simultaneously; This device is the device of a continuous sample introduction, and structure is simple, volume is little, reproducible.
Accompanying drawing explanation
Fig. 1 is the liquid continuous sample introduction device schematic diagram of heating and gasifying;
Wherein, 1-Liquid sample introduction pin; 2-vaporizer; 3-pipeline; 4-sweep gas; 5-gasification tunnel; 6-purge passage; 7-nut.
Embodiment
First, utilize attemperating unit that heating-up temperature is set for XX, after treating temperature stabilization, the wine sample of XXml is loaded in Liquid sample introduction pin 1, Liquid sample introduction pin 1 is placed on syringe pump, setting injection speed is XXXX, liquid wine sample is driven into the gasification tunnel 5 of vaporizer 2, because the temperature of heating is higher, in Liquid sample introduction pin, the wine sample of 1 is vaporized rapidly at injection gasification tunnel 5, the wine sample of gasification is entered in mass spectrum by the pipeline 3 of vaporizer sidewall and detects, purge passage 6 bottom gasification tunnel 5 passes into purge gas 4(dry air), main effect is the wine sample gas blown away rapidly in vaporizer 2, avoid wine sample remaining in bottom simultaneously.
Embodiment
Adopt the liquid continuous sample introduction device of capillary headspace sampling and heating and gasifying to detect wine sample respectively, under contrasting two kinds of modes, detect the difference of spectrogram.During headspace sampling, ionized region air pressure is about 18Pa, accumulated samples number of times is 1,000,000 times, the wine sample mass spectrogram recorded, during employing heating and gasifying device, ionized region air pressure is about 20Pa, vaporizer heating-up temperature is 180 degree, accumulated samples number of times is 1,000,000 times, the wine sample mass spectrogram recorded, contrast two mass spectrograms and can find out that the peak that the number at the peak adopting heating and gasifying device to record between mass number 150 to 200 is wanted obviously to record than headspace sampling is many, and between mass number 200 to 225, detect new peak, adopt heating and gasifying device to detect wine sample as can be seen here and obviously will be better than headspace sampling.
Claims (6)
1. a liquid continuous sample introduction device for heating and gasifying, is characterized in that: comprise Liquid sample introduction pin (1), vaporizer (2), pipeline (3), sweep gas (4), gasification tunnel (5), purge passage (6), nut (7);
Described vaporizer (2) is made up of gasification tunnel (5) and purge passage (6); Purge passage (6) is oblique through gasification tunnel (5) bottom; Gasification tunnel (5) top is step-like, and step is provided with sealing gasket, Liquid sample introduction pin (1) syringe needle and vaporizer (2) is sealed by nut (7) crush seal pad.
2. the liquid continuous sample introduction device of heating and gasifying according to claim 1, is characterized in that:
Vaporizer (2) is provided with calandria for vaporizer (2) heating, vaporizer (2) is provided with attemperating unit, for controlling the temperature of vaporizer above simultaneously.
3. the liquid continuous sample introduction device of heating and gasifying according to claim 1, is characterized in that: the liquid in Liquid sample introduction pin (1) is injected directly into gasification in vaporizer (2) by pump.
4. the liquid continuous sample introduction device of heating and gasifying according to claim 1, is characterized in that: purge passage (6) is incline structure, the gas bottom gasification tunnel is more easily gone out by purging.
5. the liquid continuous sample introduction device of heating and gasifying according to claim 1, is characterized in that: sweep gas (4) enters that vaporizer (2) is front have passed through preheating, makes sweep gas (4) reach the temperature of vaporizer.
6. the liquid continuous sample introduction device of heating and gasifying according to claim 1, it is characterized in that: gasification tunnel (5) is provided with the hole be connected with the locular wall that gasifies, be provided with pipeline (3) inside hole, the gas in vaporizer (2) is directly connected with extraneous gas analyzer by pipeline (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310684182.4A CN104716001B (en) | 2013-12-13 | 2013-12-13 | A kind of liquid continuous sample introduction device of heating and gasifying |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310684182.4A CN104716001B (en) | 2013-12-13 | 2013-12-13 | A kind of liquid continuous sample introduction device of heating and gasifying |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104716001A true CN104716001A (en) | 2015-06-17 |
| CN104716001B CN104716001B (en) | 2017-03-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201310684182.4A Expired - Fee Related CN104716001B (en) | 2013-12-13 | 2013-12-13 | A kind of liquid continuous sample introduction device of heating and gasifying |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105470095A (en) * | 2016-01-12 | 2016-04-06 | 黑龙江大学 | Thermal shock gasifying electrospray ionization source and mass spectrometry (MS) system |
| CN106645370A (en) * | 2015-11-03 | 2017-05-10 | 中国科学院大连化学物理研究所 | Online detector for sevoflurane in blood, and applications thereof |
| CN106645367A (en) * | 2015-11-03 | 2017-05-10 | 中国科学院大连化学物理研究所 | Online detector combining ultrasonic atomization and ion mobility spectrometry and application |
| CN107490554A (en) * | 2017-09-29 | 2017-12-19 | 贵州国台酒业有限公司 | A kind of liquor determination device |
| CN112946308A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Sampling device integrating gas, liquid and solid sampling functions |
| CN114994224A (en) * | 2022-07-06 | 2022-09-02 | 核工业理化工程研究院 | Liquid sample introduction device and method for gas isotope mass spectrometer |
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- 2013-12-13 CN CN201310684182.4A patent/CN104716001B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN2058492U (en) * | 1990-01-20 | 1990-06-20 | 陈新民 | Fixed-point gasifier for raising accuracy of gas phase chromatograph |
| JPH08138619A (en) * | 1994-11-08 | 1996-05-31 | Yokogawa Analytical Syst Kk | Sample introduction device for high frequency inductive coupling plasma mass spectrometer |
| JP2003036810A (en) * | 2001-07-23 | 2003-02-07 | Hitachi Ltd | Sample ionization equipment and mass analytical instrument |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645370A (en) * | 2015-11-03 | 2017-05-10 | 中国科学院大连化学物理研究所 | Online detector for sevoflurane in blood, and applications thereof |
| CN106645367A (en) * | 2015-11-03 | 2017-05-10 | 中国科学院大连化学物理研究所 | Online detector combining ultrasonic atomization and ion mobility spectrometry and application |
| CN105470095A (en) * | 2016-01-12 | 2016-04-06 | 黑龙江大学 | Thermal shock gasifying electrospray ionization source and mass spectrometry (MS) system |
| CN107490554A (en) * | 2017-09-29 | 2017-12-19 | 贵州国台酒业有限公司 | A kind of liquor determination device |
| CN112946308A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Sampling device integrating gas, liquid and solid sampling functions |
| CN114994224A (en) * | 2022-07-06 | 2022-09-02 | 核工业理化工程研究院 | Liquid sample introduction device and method for gas isotope mass spectrometer |
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| Publication number | Publication date |
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| CN104716001B (en) | 2017-03-08 |
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