CN112014513A - Flame-out judgment device of hydrogen flame ionization detector - Google Patents

Flame-out judgment device of hydrogen flame ionization detector Download PDF

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Publication number
CN112014513A
CN112014513A CN201910462195.4A CN201910462195A CN112014513A CN 112014513 A CN112014513 A CN 112014513A CN 201910462195 A CN201910462195 A CN 201910462195A CN 112014513 A CN112014513 A CN 112014513A
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China
Prior art keywords
flame ionization
hydrogen
ionization detector
detector
ultraviolet
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CN201910462195.4A
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Chinese (zh)
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臧宗超
刘思坦
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Shanghai Dst Intelligent Technology Co ltd
Shanghai Dst Technoloyg Co ltd
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Shanghai Dst Intelligent Technology Co ltd
Shanghai Dst Technoloyg Co ltd
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Priority to CN201910462195.4A priority Critical patent/CN112014513A/en
Publication of CN112014513A publication Critical patent/CN112014513A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/64Electrical detectors
    • G01N30/68Flame ionisation detectors
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01DMEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
    • G01D5/00Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable
    • G01D5/26Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention relates to a flame-out judgment device of a hydrogen flame ionization detector, which comprises: the hydrogen flame ionization detector includes a hydrogen flame ionization detector, and an ultraviolet detector disposed in an exhaust passage of the hydrogen flame ionization detector and capable of detecting ultraviolet rays generated by combustion of hydrogen gas. The invention can quickly determine whether the FID flame is extinguished.

Description

Flame-out judgment device of hydrogen flame ionization detector
Technical Field
The invention relates to a flameout judgment device of a hydrogen flame ionization detector.
Background
At present, the requirements of emission control regulations are becoming more strict, and with the coming of national regulations, online chromatography real-time monitoring equipment (GC-FID) is being widely applied as equipment of national standard detection methods. A FID (flame ionization detector), which is one of the core components of the device, does not have a good scheme for detecting whether the flame is extinguished at present, and whether the flame of the FID is extinguished is a crucial part of the whole system, which not only relates to whether the monitoring data is reliable and stable, but also concerns the safety of the system device. Since the on-line monitoring device needs to be operated continuously for 24 hours, a stable, reliable, real-time and fast method for detecting the flame condition is needed.
Disclosure of Invention
The invention aims to provide a flameout detection method which is high in timeliness and accuracy, can be used for directly detecting and eliminates interference of other factors.
According to an aspect of the present invention, there is provided an FID misfire determination apparatus including:
the hydrogen flame ionization detector is provided in an exhaust passage of the hydrogen flame ionization detector, and the ultraviolet detector is capable of detecting ultraviolet rays formed by combustion of hydrogen gas.
The invention can rapidly determine whether the FID flame is extinguished by directly detecting the ultraviolet ray formed by hydrogen combustion.
Further, the ultraviolet detector may be disposed at a side of the exhaust passage of the hydrogen flame ionization detector, and the judging device may further include a reflecting mirror disposed on the exhaust passage for reflecting ultraviolet rays formed by the combustion of the hydrogen gas into the ultraviolet detector. This configuration can reduce the overall height of the device and effectively reduce heat accumulation at the receiver of the ultraviolet detector. The reflector may be made of aluminum, and the aluminum may reflect ultraviolet rays by more than 90%.
Further, the receiver of the ultraviolet detector is disposed coaxially with and facing the exhaust passage of the hydrogen flame ionization detector. The arrangement is simple and direct, and the ultraviolet loss is less.
Further, a through hole is provided in the side surface of the combustion chamber of the hydrogen flame ionization detector, and the ultraviolet detector is provided in the through hole in the side surface of the combustion chamber of the hydrogen flame ionization detector, and captures ultraviolet rays generated by the combustion of hydrogen gas through the through hole. This configuration also allows for a reduction in the overall height of the device and more direct detection.
Further, a window lens is arranged between the receiver of the ultraviolet detector and the hydrogen flame ionization detector chamber to seal the chamber and insulate heat.
Furthermore, when the side face of the combustion chamber of the hydrogen flame ionization detector is provided with a through hole and the ultraviolet detector is arranged at the through hole on the side face of the combustion chamber of the hydrogen flame ionization detector, two layers of window lenses are arranged to better seal the cavity and isolate heat.
Further, the hydrogen flame ionization detector body includes: the sample injector is used for introducing a gas sample to be detected; a plurality of gas inlets and outlets for introducing hydrogen gas and air, respectively, and for discharging combustion exhaust gas; the combustion chamber is used for accommodating combustion of a gas sample to be tested, hydrogen and air; a polarizing pole for forming an electric field; and a collector for collecting the ion flow.
Compared with the prior art, the invention directly and rapidly detects whether the flame is extinguished through the optical sensor, and can improve the reliability of the FID device.
Drawings
Fig. 1 is a schematic configuration diagram of an FID misfire determination apparatus according to an embodiment of the present invention.
Fig. 2 is a schematic structural view of an FID misfire determination apparatus according to another embodiment of the present invention.
Fig. 3 is a schematic structural view of an FID misfire determination apparatus according to yet another embodiment of the present invention.
Detailed Description
The invention is further illustrated with reference to the following specific embodiments and the accompanying drawings. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be construed as limiting the invention. In addition, for convenience of description, only a part of structures or processes related to the present invention, not all of them, is illustrated in the drawings.
It should be noted that in this specification, like reference numerals and letters refer to like items in the following drawings, and thus, once an item is defined in one drawing, it need not be further defined and explained in subsequent drawings.
In the description of the present embodiment, it should be noted that the terms "upper", "lower", "inner", "bottom", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or orientations or positional relationships that are conventionally placed when the products of the present invention are used, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements indicated must have specific orientations, be configured in specific orientations, and operate, and thus, should not be construed as limiting the present invention.
In the description of the present embodiment, it should be further noted that, unless explicitly stated or limited otherwise, the terms "disposed," "connected," and "connected" are to be interpreted broadly, e.g., as a fixed connection, a detachable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present embodiment can be understood in specific cases by those of ordinary skill in the art.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Currently, methods for detecting the flame status of FID (flame ionization detector) can be basically divided into three types. The first is to observe by naked eyes manually, because the hydrogen burns to form water vapor, whether the exhaust gas can be fogged on the bright metal surface can be observed to judge whether the ignition is successful. The second method can judge whether the signal variation of the FID exceeds the threshold (for example, 0.5mv) through the FID signal value detection method, and if the signal variation exceeds the threshold, the FID ignition success can be judged. And thirdly, the temperature can be sensed by a temperature judgment method through a thermocouple, and when the sensed temperature is lower than a threshold (for example, 100 ℃), the flameout of the instrument is judged, so that whether the flameout of the instrument exists or not is quickly identified through the thermocouple.
In the signal value detection method, when the FID is ignited, the ignition is considered to be successful if the change of the signal value is about 0.5mv, then the signal value slowly drops to about 0.1mv, and the flameout is considered to be caused if the signal value is 0. However, in the actual operation process, if there is impurity contamination or improper maintenance, which causes a trace amount of foreign matter to contaminate the collector, the signal will be high and the data output still cannot return to 0 after flameout. If a similar situation or an FID fault occurs, the method cannot truly reflect the real state of the flame, if a signal is still available after flameout, the device cannot automatically shut off the gas source, and hydrogen can be continuously released and accumulated in the instrument to form the risk of potential accidents.
In the third temperature judgment method, when the temperature sensed by the thermocouple is below 100 ℃, the instrument is judged to be flameout. Due to the heat accumulation of combustion and the heating of the FID detector body, the temperature cannot be lowered to 100 ℃ or below other set alarm values immediately after flameout, so that the flameout alarm has long time delay, and potential safety risks can be caused when the air source is not closed in time after flameout. In some cases, the hydrogen generator may be dry-burned to damage equipment if the hydrogen generator cannot be found and shut down in time due to flameout caused by hydrogen gas supply interruption caused by failure of the hydrogen generator or after pure water is consumed.
Based on the above problems, the present invention provides a solution for directly and rapidly detecting whether a flame is extinguished by an optical sensor. When hydrogen in the FID is combusted, the flame can release ultraviolet rays, and the method judges the flame state by detecting the ultraviolet rays with the wavelength of 185-260 nm. Since the ultraviolet ray having a wavelength of 300nm or less generated by the sun is substantially absorbed by the ambient atmosphere, the ultraviolet ray of 300nm or less band does not exist in a normal state, and thus the sensor is not interfered by the ultraviolet ray of the corresponding band.
(first embodiment)
Fig. 1 shows a configuration example of an FID misfire determination apparatus 100 as an embodiment of the present invention. As shown in fig. 1, the FID misfire determination apparatus 100 includes: FID body and ultraviolet detector 11. Wherein the FID ontology may include: exhaust port 1, ignition coil 3, collector 4, combustion chamber 5, polarizing electrode 6, injector 7, hydrogen inlet 8, and air inlet 9.
The sample injector 7 may be a capillary column or a packed column, and is used for introducing a trace amount of the gas sample to be measured. The hydrogen inlet 8 is used for introducing hydrogen; the air inlet 9 is for introducing air. The sample to be measured, hydrogen and air are introduced and collected in the combustion chamber 5, ignited by the ignition coil 3 and mixed and combusted, and exhaust gas generated after combustion passes through the exhaust passage and is finally discharged through the exhaust port 1. The polarizing pole 6 is used for forming an electric field; the collector 4 is used for collecting ion flow for subsequent circuit processing, for detecting sample concentration and the like.
The ultraviolet detector 11 is disposed on the exhaust passage of the FID and can capture ultraviolet rays of a specific frequency band, and a receiver of the ultraviolet detector 11 may be disposed coaxially with and facing the exhaust passage of the FID. With this structure, the ultraviolet rays formed by the combustion of hydrogen gas can be directly captured by the ultraviolet detector 11. When the ultraviolet detector 11 captures the ultraviolet rays, the ignition success can be judged; similarly, if the ultraviolet detector 11 cannot capture the ultraviolet rays, it indicates that the flame is extinguished. In this way, the state of the flame in the FID, i.e., whether the flame is extinguished, can be directly and quickly detected.
In some embodiments, a window lens 10 may be disposed between the receiver of the ultraviolet detector 11 and the FID to enclose the chamber and insulate heat. The window lens 10 may be made of quartz glass because quartz glass has high temperature resistance and transmits ultraviolet rays.
It should be noted that the structure of the FID shown in fig. 1 is merely for illustration, and the shape, the position relationship between the components, and other features shown in the structure are not intended to limit the present invention, and various FIDs that may appear in the prior art and the future may be used in the misfire determination method and structure of the present invention.
In addition, the scheme of the optical detection provided by the invention can be used together with the signal value detection method of the second detection method, and cross validation is carried out, so that the reliability of the judgment device is further improved.
(second embodiment)
Next, an FID misfire determination apparatus 200 according to a second embodiment will be described, as shown in fig. 2. The FID misfire determination device 200 according to the second embodiment has substantially the same function and structure as the FID misfire determination device 100 according to the first embodiment. Components having substantially the same functions and structures as in the first embodiment are denoted by the same reference numerals, and detailed description thereof will not be repeated. Only the differences between the second embodiment and the first embodiment will be described.
As shown in fig. 2, the FID misfire determination apparatus 200 also includes: FID body and ultraviolet detector 11. Unlike FID misfire determination apparatus 200 shown in fig. 1: the ultraviolet ray detector 11 is provided on the side of the exhaust passage of the FID, and a reflecting mirror is provided on the exhaust passage in the FID body for reflecting ultraviolet rays formed by the combustion of hydrogen gas into the ultraviolet ray detector. This configuration enables the overall height of the device 200 to be reduced and effectively reduces heat accumulation at the receiver of the ultraviolet detector 11.
In this embodiment, after the gas sample to be measured enters the combustion chamber 5 through the injector 7, it is mixed and burned in the combustion chamber 5 together with the hydrogen gas introduced through the hydrogen gas inlet 8 and the air introduced through the air inlet 9, and the ultraviolet rays formed by the combustion of the hydrogen gas are reflected by the reflecting mirror provided in the gas discharge path, pass through the window lens 10, and are captured by the ultraviolet ray detector 11. The reflector can be selected for use as the aluminium material because aluminium can reflect the ultraviolet ray more than 90%, in addition, considers that vapor may form the fog on the mirror surface and influence the reflection, and this reflector can heat with the FID body jointly or heat to higher temperature alone under the heat engine state.
(third embodiment)
Next, a FID misfire determination apparatus 300 according to a third embodiment will be described, as shown in fig. 3. The FID misfire determination device 300 according to the third embodiment has substantially the same function and structure as the FID misfire determination device 100 according to the first embodiment. Components having substantially the same functions and structures as in the first embodiment are denoted by the same reference numerals, and detailed description thereof will not be repeated. Only the differences between the third embodiment and the first embodiment will be described.
As shown in fig. 3, the FID misfire determination apparatus 300 also includes: FID body and ultraviolet detector 11. The difference from FID misfire determination apparatus 300 shown in fig. 1 is that: the side of the combustion chamber 5 is provided with a through hole 12, and an ultraviolet detector 11 is provided at the side of the combustion chamber of the FID and captures ultraviolet rays formed by the combustion of hydrogen gas through the through hole 12.
In this embodiment, after the gas sample to be measured enters the combustion chamber 5 through the sample injector 7, it is mixed and combusted in the combustion chamber 5 together with hydrogen gas introduced through the hydrogen gas inlet 8 and air introduced through the air inlet 9, and ultraviolet rays formed by the combustion of the hydrogen gas are directly captured by the ultraviolet ray detector 11 on the side of the combustion chamber 5. This arrangement is more direct in capturing uv light and in practical designs, two layers of window lenses 10 can be placed at the through holes to better seal the chamber and isolate heat.
While the embodiments of the present invention have been described in detail with reference to the accompanying drawings, the use of the technical solution of the present invention is not limited to the applications mentioned in the embodiments of the patent, and various structures and modifications can be easily implemented with reference to the technical solution of the present invention to achieve various advantageous effects mentioned herein. Variations that do not depart from the gist of the invention are intended to be within the scope of the invention as defined by the appended claims.

Claims (8)

1. A flame-out determination device for a hydrogen flame ionization detector, comprising:
a hydrogen flame ionization detector, and
and an ultraviolet detector provided in an exhaust passage of the hydrogen flame ionization detector and capable of detecting ultraviolet rays generated by combustion of hydrogen gas.
2. The flame ionization detector quenching judgment device according to claim 1,
the ultraviolet detector is arranged on the side surface of the exhaust channel of the hydrogen flame ionization detector,
the judgment device further comprises a reflecting mirror arranged on the exhaust channel and used for reflecting ultraviolet rays formed by the combustion of the hydrogen to the ultraviolet detector.
3. The flame ionization detector flameout determination device according to claim 2, wherein the reflector is made of aluminum.
4. The flame ionization detector flameout determination device according to claim 1, wherein the receiver of the ultraviolet detector is coaxial with and disposed directly opposite to the exhaust passage of the hydrogen flame ionization detector.
5. The flame-out determination device for a hydrogen flame ionization detector as defined in claim 1, wherein a through hole is provided in a side surface of the combustion chamber of the hydrogen flame ionization detector, and the ultraviolet detector is provided in the through hole in the side surface of the combustion chamber of the hydrogen flame ionization detector, and captures ultraviolet rays generated by combustion of the hydrogen gas through the through hole.
6. The flame ionization detector flameout determination device according to claim 1, wherein a window lens is provided between the receiver of the ultraviolet detector and the hydrogen flame ionization detector.
7. The flame-out determination device for a hydrogen flame ionization detector as defined in claim 6, wherein when the side surface of the combustion chamber of the hydrogen flame ionization detector is provided with a through hole and the ultraviolet detector is disposed at the through hole, two layers of the window lenses are disposed.
8. The hydrogen flame ionization detector flameout determination device according to any one of the preceding claims, wherein the hydrogen flame ionization detector body includes:
a sample injector for introducing a gas sample to be measured,
a plurality of gas inlets and outlets for introducing hydrogen gas, air, and discharging combustion exhaust gas, respectively,
a combustion chamber for accommodating combustion of the gas sample to be measured, hydrogen and air,
the polarizing pole is used for forming an electric field, so that positive and negative ions are separated and effectively collected,
the collector is used for collecting the formed corresponding ion current and finally forming a signal value.
CN201910462195.4A 2019-05-30 2019-05-30 Flame-out judgment device of hydrogen flame ionization detector Pending CN112014513A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1781014A (en) * 2003-11-05 2006-05-31 株式会社山武 Flame detection method and flame detection device
JP3129011U (en) * 2006-11-15 2007-02-01 株式会社島津製作所 Gas chromatograph
CN101975836A (en) * 2010-08-16 2011-02-16 聚光科技(杭州)股份有限公司 FID ignition method and device for chromatographic analysis
CN203147811U (en) * 2013-03-14 2013-08-21 华油天然气广安有限公司 Regenerative gas heating furnace flame detection device of LNG production device
JP2015190846A (en) * 2014-03-28 2015-11-02 アズビル株式会社 flame detection system
CN208206897U (en) * 2018-04-17 2018-12-07 武汉工控检验检测有限公司 A kind of gas chromatograph flame ionization ditector flame automated watch-keeping facility
CN210109053U (en) * 2019-05-30 2020-02-21 上海迪勤传感技术有限公司 Flame-out judgment device of hydrogen flame ionization detector

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1781014A (en) * 2003-11-05 2006-05-31 株式会社山武 Flame detection method and flame detection device
JP3129011U (en) * 2006-11-15 2007-02-01 株式会社島津製作所 Gas chromatograph
CN101975836A (en) * 2010-08-16 2011-02-16 聚光科技(杭州)股份有限公司 FID ignition method and device for chromatographic analysis
CN203147811U (en) * 2013-03-14 2013-08-21 华油天然气广安有限公司 Regenerative gas heating furnace flame detection device of LNG production device
JP2015190846A (en) * 2014-03-28 2015-11-02 アズビル株式会社 flame detection system
CN208206897U (en) * 2018-04-17 2018-12-07 武汉工控检验检测有限公司 A kind of gas chromatograph flame ionization ditector flame automated watch-keeping facility
CN210109053U (en) * 2019-05-30 2020-02-21 上海迪勤传感技术有限公司 Flame-out judgment device of hydrogen flame ionization detector

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