CN214278036U - Detection apparatus for nitrogen oxide in high-purity gas - Google Patents
Detection apparatus for nitrogen oxide in high-purity gas Download PDFInfo
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- CN214278036U CN214278036U CN202120246963.5U CN202120246963U CN214278036U CN 214278036 U CN214278036 U CN 214278036U CN 202120246963 U CN202120246963 U CN 202120246963U CN 214278036 U CN214278036 U CN 214278036U
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Abstract
A detection device for nitrogen oxides in high-purity gas comprises a light converter, a nitrogen oxide detector, a nitrogen-containing gas detector and a nitrogen-containing gas detector, wherein the light converter is used for converting the nitrogen oxides into peroxyacetyl nitrate; the acetone gas unit is filled with acetone gas and is connected with an inlet of the optical converter through a first electromagnetic valve; the high-purity gas unit to be detected is filled with the high-purity gas to be detected and is connected with an inlet of the optical converter through a first electromagnetic valve; the separation detection unit is connected with the outlet of the optical converter through a second electromagnetic valve; and the air pump unit is connected with the outlet of the optical converter through a second electromagnetic valve. The utility model can realize the high-sensitivity detection of the nitrogen oxide in the high-purity gas; the system has stable operation, convenient operation and sensitive detection, and the price of the equipment constructed by the method is relatively low.
Description
Technical Field
The utility model relates to a chemical analysis technical field especially relates to a detection apparatus for nitrogen oxide in high-purity gas.
Background
Nitrogen Oxides (NO)X) The active nitrogen-containing compound is the most important active nitrogen-containing compound in the atmosphere, and not only directly influences the circulation of free radicals in the atmosphere through a complex photochemical reaction under solar radiation, but also can accelerate the generation of primary pollutants to secondary ozone and particulate matters, thereby having important influence on the regional atmospheric environment. The monitoring of nitrogen oxides has become one of the important indicators for atmospheric environmental monitoring. All nitrogen oxide monitors of the existing ambient air quality monitoring station need to be regularly calibrated through standard gas, and then relatively accurate concentration can be obtained. The standard gas usually needs to use high-purity gas (such as high-purity steel cylinder gas or zero-order air) as a dilution gas to dilute the high-concentration nitrogen oxide standard gas to obtain trace level standard gas, or as zero gas. The content of nitrogen oxides in the high-purity gas directly influences the concentration level of the nitrogen oxides in the diluted trace standard gas, directly influences the accuracy of the measured nitrogen oxides, particularly influences the monitoring of the low nitrogen oxides with the strongest photochemical activity, can influence the deviation of diagnosis of regional atmospheric pollution causes, and even obtains wrong conclusions. At present, the detection of the nitrogen oxides in the high-purity gas is realized by adopting technologies such as an atmospheric pressure ion mass spectrometer (API-MS), a chemiluminescence method nitrogen oxide analyzer and the like. The atmospheric pressure ion chromatograph is expensive and difficult to popularize, and the chemiluminescence method has high detection limit and cannot meet the detection of ultra-trace nitrogen oxides in high-purity gas. Therefore, it is highly desirable to develop a method and a device for analyzing high-purity gaseous nitrogen oxides with low cost, low operation and maintenance cost and high sensitivity.
SUMMERY OF THE UTILITY MODEL
In view of the above, one of the main objectives of the present invention is to provide a device for detecting nitrogen oxides in high purity gas, so as to at least partially solve at least one of the above technical problems.
In order to achieve the above object, the utility model provides a detection apparatus for nitrogen oxide in high-purity gas, include:
a light converter to convert the nitrogen oxides to peroxyacetyl nitrate;
the acetone gas unit is filled with acetone gas and is connected with an inlet of the optical converter through a first electromagnetic valve;
the high-purity gas unit to be detected is filled with the high-purity gas to be detected and is connected with an inlet of the optical converter through a first electromagnetic valve;
the separation detection unit is connected with the outlet of the optical converter through a second electromagnetic valve; and
and the air pump unit is connected with the outlet of the optical converter through a second electromagnetic valve.
Based on above-mentioned technical scheme can know, the utility model discloses a detection device of nitrogen oxide in high-purity gas has one of following advantage or partly at least for prior art:
1. the utility model provides a nitrogen oxide detection device and method in high-purity gas adopts the chemical conversion method, can realize that nitrogen oxide in acetone gas and high-purity gas turns into peroxyacetyl nitrate; separating the peroxyacetyl nitrate by adopting a gas chromatography separation method, and detecting by using a high-sensitivity electron capture detector or a helium ionization detector; the high-sensitivity detection of the nitrogen oxide in the high-purity gas can be realized; the system is stable in operation, convenient to operate and sensitive in detection, and the price of the equipment constructed by the method is relatively low;
2. the utility model provides a current method and device measurement deviation big and the problem that the operation and maintenance cost is high.
Drawings
The accompanying drawings, which are described herein, serve to provide a further understanding of the invention and constitute a part of this specification, and the exemplary embodiments and descriptions thereof are provided for explaining the invention without unduly limiting it. In the drawings:
FIG. 1 is a flow chart of a method for detecting nitrogen oxides in a high purity gas according to an embodiment of the present invention;
fig. 2 is the schematic structural diagram of the device for detecting nitrogen oxides in high-purity gas in the embodiment of the present invention.
Description of reference numerals:
101-acetone gas bottle; 102-high-purity gas bottle to be detected; 103-a first mass flow controller;
104-a second mass flow controller; 201-polytetrafluoroethylene airbag; 202-ultraviolet lamp;
203-a first solenoid valve; 204-a second solenoid valve; 205-a first air pump; 300-separation detection unit.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples to assist those skilled in the art in fully understanding the objects, features and effects of the present invention. Exemplary embodiments of the present invention are illustrated in the accompanying drawings, but it should be understood that the present invention can be embodied in other various forms and should not be limited to the embodiments set forth herein. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention. In addition, the embodiments and technical features of the embodiments provided below of the present invention may be combined with each other in any manner.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Furthermore, the terms "comprises," "comprising," "includes," "including," "has," "having," and the like, when used herein, specify the presence of stated features, steps, operations, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, or components. The terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. Unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are intended to be inclusive and mean, for example, that they may be fixedly connected, detachably connected, or integrally connected; 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 meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art. All terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art unless otherwise defined. It is noted that the terms used herein should be interpreted as having a meaning that is consistent with the context of this specification and should not be interpreted in an idealized or overly formal sense.
The utility model provides a detection method and a device for nitrogen oxides in high-purity gas, which solve the problems of high price cost and poor detection capability of the existing method and device.
The utility model discloses a detection method of nitrogen oxide in high-purity gas, include:
introducing acetone gas into a light converter, converting nitrogen oxides in the acetone gas into peroxyacetyl nitrate, and measuring the concentration of the peroxyacetyl nitrate as a first concentration;
introducing high-purity gas to be detected into a light converter filled with acetone gas, converting nitrogen oxide in the light converter into peroxyacetyl nitrate, and measuring the concentration of the peroxyacetyl nitrate as a second concentration;
and obtaining the concentration of the nitrogen oxide in the high-purity gas to be detected according to the first concentration and the second concentration.
In some embodiments of the present invention, the method of measuring the first concentration comprises: the volume is V1Quantitatively introducing the acetone gas into the light converter through a mass flow controller, and converting nitrogen oxides in the acetone gas into peroxyacetyl nitrate under the condition of ultraviolet illumination to obtain background gas; then the acquisition volume is VSBackground gas of (2), detection backgroundThe concentration of the peroxyacetyl nitrate in the gas is the first concentration.
In some embodiments of the present invention, the method of measuring the second concentration comprises: the volume is V2The high-purity gas to be detected is quantitatively introduced through a mass flow controller, and the volume of the gas is collected to be VSIn the light converter of the residual acetone gas and the residual background gas after the background gas, under the condition of ultraviolet illumination, the nitrogen oxide in the high-purity gas is converted into peroxyacetyl nitrate to obtain converted gas; then the acquisition volume is VSDetecting the concentration of the peroxyacetyl nitrate to obtain a second concentration.
In some embodiments of the present invention, the concentration of nitrogen oxide in the high-purity gas to be examined is:
in some embodiments of the present invention, the method for measuring the first concentration uses a gas chromatography separation method to separate peroxyacetyl nitrate in the background gas, and uses an electron capture detection method or a helium ionization detection method to detect the concentration of the separated peroxyacetyl nitrate.
In some embodiments of the present invention, the method for measuring the second concentration uses a gas chromatography separation method to separate the peroxyacetyl nitrate in the converted gas, and uses an electron capture or helium ionization detection method to detect the concentration of the separated peroxyacetyl nitrate.
The utility model also discloses a detection apparatus of nitrogen oxide in high-purity gas for carry out as above detection method, include:
a light converter to convert the nitrogen oxides to peroxyacetyl nitrate;
the acetone gas unit is filled with acetone gas and is connected with an inlet of the optical converter through a first electromagnetic valve;
the high-purity gas unit to be detected is filled with the high-purity gas to be detected and is connected with an inlet of the optical converter through a first electromagnetic valve;
the separation detection unit is connected with the outlet of the optical converter through a second electromagnetic valve; and
and the air pump unit is connected with the outlet of the optical converter through a second electromagnetic valve.
In some embodiments of the invention, the light converter comprises an ultraviolet light source and a polytetrafluoroethylene gas pocket;
the ultraviolet light sources are arranged on two sides of the polytetrafluoroethylene air bag.
In some embodiments of the present invention, the acetone gas unit includes an acetone gas cylinder and a first mass flow controller, and the first mass flow controller controls the flow rate of the acetone gas.
The utility model discloses an in some embodiments, examine high-purity gas unit including examining high-purity gas cylinder and second mass flow controller, the high-purity gas's is examined in second mass flow controller control flow.
In an exemplary embodiment, the present invention provides a method for detecting nitrogen oxides in high purity gas, comprising the following steps:
introducing acetone gas into a light converter, and converting ultra-trace nitrogen oxides in the acetone gas into peroxyacetyl nitrate under the condition of ultraviolet illumination to obtain background gas;
introducing high-purity gas to be detected into a light converter filled with acetone gas, and converting ultra-trace nitrogen oxides in the high-purity gas to be detected into peroxyacetyl nitrate under the condition of ultraviolet illumination to obtain converted gas;
respectively separating and detecting the peroxyacetyl nitrate in the background gas and the conversion gas to respectively obtain a first concentration and a second concentration of the peroxyacetyl nitrate;
according to the first concentration and the second concentration of the peroxyacetyl nitrate, calculating the concentration of the nitrogen oxide in the high-purity gas to be detected as follows: the second concentration of peroxyacetyl nitrate minus the residual background gas peroxyacetyl nitrate concentration therein.
Preferably, the step of obtaining a background gas and converting a gas further comprises: the volume is V1Quantitatively introducing the acetone gas into the light converter through a mass flow controller, and converting the ultra-trace nitrogen oxide in the acetone gas into peroxyacetyl nitrate under the ultraviolet illumination condition to obtain the background gas; then quantitatively collecting volume V by using gas chromatographSDetecting the concentration of the peroxyacetyl nitrate, i.e. the first concentration C of the peroxyacetyl nitrate1。
The volume is V2The high-purity gas to be detected is quantitatively introduced into the gas containing the collected background gas V through a mass flow controllerSIn a light converter of the residual acetone gas and the background gas, converting trace nitrogen oxides in the high-purity gas into peroxyacetyl nitrate under the condition of ultraviolet illumination to obtain converted gas; then quantitatively collecting volume V by using gas chromatographSDetecting the concentration of the peroxyacetyl nitrate, i.e. the second concentration C of peroxyacetyl nitrate2。
The step of calculating the concentration of nitrogen oxides in the high-purity gas to be detected further comprises: according to the first concentration and the second concentration of the peroxyacetyl nitrate, the acetone gas introduction volume, the gas chromatography sampling volume and the high-purity gas introduction volume to be detected, calculating the concentration of nitrogen oxides in the high-purity gas to be detected as follows:
wherein C is the concentration in the high-purity gas to be detected, C1And C2Respectively a first concentration and a second concentration of said peroxyacetyl nitrate, V1、V2And VSThe volume of the acetone gas, the volume of the high-purity gas and the sampling volume of the gas chromatograph are respectively.
Preferably, the step of separating and detecting the peroxyacetyl nitrate in the background gas and the converted gas respectively to obtain a first concentration and a second concentration of the peroxyacetyl nitrate respectively further comprises: respectively separating the peroxyacetyl nitrate in the background gas and the converted gas by adopting a gas chromatography separation method;
and respectively detecting the peroxyacetyl nitrate in the separated background gas and converted gas by adopting an electron capture or helium ionization detection method to respectively obtain a first concentration and a second concentration of the peroxyacetyl nitrate.
Further, the acetone gas is gas obtained by dispersing gaseous acetone in high-purity synthetic air, and can be obtained by blowing liquid acetone by high-pressure steel cylinder gas or high-purity air.
Further, the light converter comprises a flexible teflon air bag and an ultraviolet light source.
The embodiment of the utility model provides a nitrogen oxide detection device in high-purity gas is still pointed out, be used for the method, contain: the device comprises a gas unit, a conversion unit and a separation detection unit.
The gas unit is used for providing the acetone gas and the high-purity gas, and quantitatively outputting the gas to the conversion unit;
the conversion unit is used for converting nitrogen oxides in the high-purity gas to be detected into peroxyacetyl nitrate and outputting the background gas and converted gas;
the separation detection unit is used for collecting the background gas and the converted gas, and separating and detecting the peroxyacetyl nitrate in the background gas and the converted gas.
Further, the gas unit includes: the device comprises high-purity gas to be detected, acetone gas, a first mass flow controller and a second mass flow controller; the conversion unit comprises a flexible polytetrafluoroethylene air bag, an ultraviolet light source, a first electromagnetic valve, a second electromagnetic valve and a first air pump, and the first air pump is used for exhausting air of the polytetrafluoroethylene air bag; the separation detection unit comprises a gas chromatography sampling system, a separation system and an electronic capture detection system.
Further, the apparatus further comprises: a control unit; the control unit is used for controlling the high-purity gas flow of the high-purity gas conversion unit and the high-purity gas collection unit and controlling the separation and detection process of the peroxyacetyl nitrate in the separation and detection unit. The device is used for controlling the flow, the illumination and the gas circuit on-off of the gas unit and the conversion unit, and electrically controlling the separation of the peroxyacetyl nitrate and the start and stop of the detection process of the first separation detection unit and the second separation detection unit.
The technical solution of the present invention is further explained by the following specific embodiments with reference to the attached drawings. It should be noted that the following specific examples are only illustrative, and the scope of the present invention is not limited thereto.
FIG. 1 is a flow chart of a method for detecting nitrogen oxides in high purity gas, which is used for detecting nitrogen oxides in high purity gas. As shown in fig. 1, the method for detecting nitrogen oxides in high-purity gas according to the embodiment of the present invention specifically includes the following steps:
step 1, introducing acetone gas into a light converter to convert nitrogen oxides in the acetone gas into peroxyacetyl nitrate to obtain background gas.
And 2, separating and detecting the peroxyacetyl nitrate in the converted gas to obtain a first concentration of the peroxyacetyl nitrate.
And 3, introducing the high-purity gas to be detected into a light converter containing acetone gas and background gas, and converting nitrogen oxides in the high-purity gas to be detected into peroxyacetyl nitrate to obtain converted gas.
And 4, separating and detecting the peroxyacetyl nitrate in the converted gas to respectively obtain a second concentration of the peroxyacetyl nitrate.
And 5, calculating the concentration of the nitrogen oxide in the high-purity gas to be detected as follows according to the first concentration and the second concentration of the peroxyacetyl nitrate: and subtracting the residual background gas peroxyacetyl nitrate concentration from the second concentration of peroxyacetyl nitrate to obtain the content of peroxyacetyl nitrate converted from the nitrogen oxide of the high-purity gas to be detected in the converted gas, and further obtaining the concentration of the nitrogen oxide in the high-purity gas to be detected in the converted gas, namely the concentration of the nitrogen oxide of the high-purity gas to be detected.
The embodiment of the utility model provides a nitrogen oxide detection method in high-purity gas adopts the chemical conversion method to combine the high selectivity of gas chromatography to detect, can the accurate nitrogen oxide concentration who surveys in the high-purity gas, detectivity is high and the testing result is accurate.
As shown in fig. 2, the apparatus for detecting nitrogen oxides in high purity gas used in the present embodiment specifically includes a gas unit, a conversion unit, a separation detection unit 300, and a control unit. The method for detecting nitrogen oxides in high-purity gas in the embodiment specifically comprises the following steps:
the first step is as follows: preparation of each unit. The gas unit, the conversion unit and the separation detection unit all control the unit to complete connection communication and self-detection and start a programmed work flow.
The second step is that: and (4) cleaning the conversion unit. First, the first electromagnetic valve 203 is opened; then starting a first mass flow controller 103, and quantitatively introducing the acetone gas 101 into a polytetrafluoroethylene air bag 201; subsequently closing the first mass flow controller 103 and the first solenoid valve 203; then opening a second electromagnetic valve 204 and a first air pump 205 to empty the acetone gas in the polytetrafluoroethylene air bag; closing the second electromagnetic valve 204 and the first air pump 205 to complete a cleaning process; the above cleaning process is circulated for more than 3 times.
The third step: a background gas. Turning on the ultraviolet lamp 202; opening the first solenoid valve 203; the first mass flow controller 103 is then turned on to quantify the amount of acetone gas 101 (i.e., the collection volume is V)1) Introducing into a polytetrafluoroethylene air bag 201; subsequently closing the first mass flow controller 103 and the first solenoid valve 203; when the nitrogen oxide in the acetone gas is converted into peroxyacetyl nitrate (the reaction lasts for more than 5 minutes), obtaining background gas;
and fourthly, detecting the peroxyacetyl nitrate in the background gas. The separation detection unit quantitatively collects (namely the collection volume is V)S) The background gas is obtained by separating and detecting the background gasThe concentration of peroxyacetyl nitrate in the body, i.e. the first concentration C of peroxyacetyl nitrate1。
The fifth step: the gas is converted. Opening the first solenoid valve 203; second mass flow controller 104 is opened and high purity gas to be detected 102 is quantified (i.e., volume collected as V)2) Introducing into a polytetrafluoroethylene air bag 201, wherein the polytetrafluoroethylene air bag 201 comprises a fourth step of acquiring the volume VSAll gases remaining after the background gas; subsequently closing the second mass flow controller 104 and the first solenoid valve 203; and (3) obtaining converted gas after the nitrogen oxide in the high-purity gas to be detected is converted into the peroxyacetyl nitrate (the reaction lasts for more than 5 minutes).
And a sixth step: and detecting the peroxyacetyl nitrate in the converted gas. The separation detection unit quantitatively collects (namely the collection volume is V)S) The converted gas is separated and detected to obtain the concentration of the peroxyacetyl nitrate in the converted gas, namely the second concentration C of the peroxyacetyl nitrate2。
The seventh step: the conversion gas is evacuated. Opening a second electromagnetic valve 204 and a first air pump 205 to evacuate the transfer gas in the polytetrafluoroethylene air bag; the second electromagnetic valve 204 and the first air pump 205 are closed, and the whole detection process is completed.
Eighth step: and calculating the content of the nitrogen oxide in the high-purity gas to be detected. According to the first concentration and the second concentration of the peroxyacetyl nitrate, the acetone gas introduction volume, the gas chromatography sampling volume and the high-purity gas introduction volume to be detected, calculating the concentration of nitrogen oxides in the high-purity gas to be detected as follows:
C＝((V1+V2-VS)×C2-(V1-VS)×C1)/V2
wherein C is the concentration of nitrogen oxide in the high-purity gas to be detected, C1And C2Respectively a first concentration and a second concentration of said peroxyacetyl nitrate, V1、V2And VSThe volume of the acetone gas, the volume of the high-purity gas and the sampling volume of the gas chromatograph are respectively.
The embodiment of the utility model provides a nitrogen oxide detection device in high-purity gas, the conversion unit that adopts the chemical conversion method is to the conversion of nitrogen oxide in acetone gas in the gas unit and the high-purity gas of examining to be examined to peroxyacetyl nitrate, can carry out effective conversion to the nitrogen oxide in acetone gas and the high-purity gas of examining to be examined; the separation detection unit is used for separating and detecting the peroxyacetyl nitrate by adopting a method of phase chromatography separation and electron capture or helium ionization detection, so that the high-sensitivity detection of the peroxyacetyl nitrate can be realized, and the accurate detection of the content of the nitrogen oxide in the high-purity gas to be detected can be further realized.
The embodiment of the utility model provides a nitrogen oxide detection device still contains the control unit in the high-purity gas, can realize the automated control to nitrogen oxide detection in the high-purity gas.
As an embodiment of the present invention, the control unit is configured to set, open and close the flow rates of the first mass flow controller 103 and the second mass flow controller 104 of the gas unit; the conversion unit ultraviolet lamp 202, the first electromagnetic valve 203, the second electromagnetic valve 204 and the first air pump 205 are connected to control the on and off of the conversion unit ultraviolet lamp 202, the first electromagnetic valve 203, the second electromagnetic valve 204 and the first air pump 205; and is also used for controlling the separation and detection processes of the peroxyacetyl nitrate by the gas chromatography of the separation detection unit 300.
It should be noted that, although the invention has been shown and described with reference to the specific exemplary embodiments thereof, it should be understood by those skilled in the art that the invention is not limited to the above-mentioned embodiments, and that various changes and modifications may be made without departing from the spirit and scope of the invention, and it is intended to cover such changes and modifications also if they fall within the scope of the claims and their equivalents.
In particular, various combinations and/or combinations of features recited in the various embodiments and/or claims of the present invention can be made without departing from the spirit and teachings of the invention, even if such combinations or combinations are not expressly recited in the present invention. All such combinations and/or associations are within the scope of the present invention. The scope of the invention should, therefore, be determined not with reference to the appended claims, but should instead be determined with reference to the following claims, along with the full scope of equivalents to which such claims are entitled.
Claims (4)
1. A device for detecting nitrogen oxides in high purity gases, comprising:
a light converter to convert the nitrogen oxides to peroxyacetyl nitrate;
the acetone gas unit is filled with acetone gas and is connected with an inlet of the optical converter through a first electromagnetic valve;
the high-purity gas unit to be detected is filled with the high-purity gas to be detected and is connected with an inlet of the optical converter through a first electromagnetic valve;
the separation detection unit is connected with the outlet of the optical converter through a second electromagnetic valve; and
and the air pump unit is connected with the outlet of the optical converter through a second electromagnetic valve.
2. The detection apparatus according to claim 1,
the light converter comprises an ultraviolet light source and a polytetrafluoroethylene air bag;
the ultraviolet light sources are arranged on two sides of the polytetrafluoroethylene air bag.
3. The detection apparatus according to claim 1,
the acetone gas unit comprises an acetone gas cylinder and a first mass flow controller, and the first mass flow controller controls the flow of acetone gas.
4. The detection apparatus according to claim 1,
the high-purity gas unit to be detected comprises a high-purity gas cylinder to be detected and a second mass flow controller, and the second mass flow controller controls the flow of the high-purity gas to be detected.
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| CN202120246963.5U CN214278036U (en) | 2021-01-28 | 2021-01-28 | Detection apparatus for nitrogen oxide in high-purity gas |
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