CN112285216A - Fumigant detector and detection method - Google Patents
Fumigant detector and detection method Download PDFInfo
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- CN112285216A CN112285216A CN201910670704.2A CN201910670704A CN112285216A CN 112285216 A CN112285216 A CN 112285216A CN 201910670704 A CN201910670704 A CN 201910670704A CN 112285216 A CN112285216 A CN 112285216A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
Discloses a fumigant detector and a detection method, comprising the following steps: a sampling unit adapted to collect the fumigant sample gas; the inlet of the bundled capillary chromatographic column is communicated with the sampling unit and is suitable for separating the fumigant sample gas collected by the sampling unit so as to sequentially output each component contained in the fumigant sample gas in a single component form; and the air inlet of the ion mobility spectrometer is communicated with the outlet of the bundled capillary chromatographic column, so that the fumigant sample gas separated by the bundled capillary chromatographic column sequentially enters the ion mobility spectrometer in the form of a single component, and each component of the fumigant sample gas is sequentially detected by the ion mobility spectrometer. The fumigant detector and the detection method can detect the mixed gas of the fumigant in a complex environment.
Description
Technical Field
The disclosure relates to the technical field of detection, in particular to a fumigant detector and a detection method.
Background
Along with the rapid development of foreign trade, the number of containers entering and leaving China increases year by year. The customs quarantine work is necessary for ensuring the food sanitation and safety and resisting the invasion of foreign species. Chemical fumigation is widely applied to customs quarantine links due to the characteristics of broad spectrum, easy realization and high efficiency. At present, the fumigants commonly used by customs comprise methyl bromide, sulfuryl fluoride, phosphine, ethylene oxide and the like, and due to the strong toxicity and the strong permeability of the fumigants, the fumigants can effectively kill insects, mites, nematodes, mollusks, cell spores, viruses, fungi and the like in a container, thereby eliminating the hidden danger of foreign invasive species of customs. Because the corrosivity and the adsorptivity of the fumigation gas are stronger, and part of the fumigation gas has the burning and explosion characteristics (phosphine and ethylene oxide), if the fumigation gas is not properly treated, the fumigation agent residue in the container can cause harm to workers. At present, instruments for detecting toxic gas remained in container fumigation mainly comprise a portable Raman spectrum gas analyzer, a portable infrared spectrum gas analyzer, an electrochemical sensor, a gas chromatograph and the like.
However, the conventional fumigant detector and detection method cannot detect the mixed fumigant gas, and have low detection sensitivity and long response time.
Disclosure of Invention
An object of the present disclosure is to solve at least one aspect of the above problems and disadvantages in the related art.
According to an embodiment of the present disclosure, there is provided a fumigant detector including:
a sampling unit adapted to collect the fumigant sample gas;
the inlet of the bundled capillary chromatographic column is communicated with the sampling unit and is suitable for separating the fumigant sample gas collected by the sampling unit so as to sequentially output each component contained in the fumigant sample gas in a single component form; and
and the air inlet of the ion mobility spectrometer is communicated with the outlet of the bundled capillary chromatographic column, so that the fumigant sample gas separated by the bundled capillary chromatographic column sequentially enters the ion mobility spectrometer in the form of a single component, and each component of the fumigant sample gas is sequentially detected by the ion mobility spectrometer.
According to the fumigant detector of the embodiments of the present disclosure, detecting the components of the fumigant sample gas includes detecting the kinds and concentrations of the components of the fumigant sample gas.
According to the fumigant detector of the embodiment of this disclosure, the sampling unit includes:
a sampling device;
one end of the sampling pipeline is communicated with a sampling device, and the other end of the sampling pipeline is communicated with an inlet of the bundled capillary chromatographic column; and
the sampling pump is arranged on the sampling pipeline and used for driving the fumigant sample gas to flow.
According to the fumigant detector of the embodiment of this disclosure, the ion mobility spectrometer includes:
an ionization region and an ionization source located within the ionization region for ionizing fumigant molecules of a fumigant sample gas into charged ions;
a migration area and a positive migration pipe and a negative migration pipe which are positioned in the migration area;
an ion gate is arranged between the migration zone and the ionization zone and is periodically opened, so that charged ions generated after components of the fumigant sample gas are ionized enter the migration zone of the migration pipe at the same time; and
a detector located at an end of the migration zone distal from the ionization zone.
The fumigant detector according to the embodiment of the present disclosure further includes a signal amplification module, the signal amplification module is connected with the detector to amplify the signal of the ion mobility spectrometer
The fumigant detector according to the embodiment of the present disclosure further includes a display unit, and the display unit is connected to the signal amplification module and is adapted to an ion mobility spectrometer that sequentially displays each component of the fumigant sample gas.
According to the fumigant detector of an embodiment of the present disclosure, the ionization source is one of a radioactive source, a power source discharge source and a photo ionization source.
According to the fumigant detector of the embodiment of the present disclosure, the fumigant sample gas is a fumigant sample mixed gas.
According to the fumigant detector of the embodiment of the present disclosure, the fumigant sample mixed gas includes at least two of methyl bromide, sulfuryl fluoride, phosphine, and ethylene oxide.
According to another aspect of the present disclosure, there is also provided a fumigant detection method, including the steps of:
collecting fumigant sample gas through a sampling unit;
separating the collected fumigant sample gas by a bundled capillary chromatographic column;
the fumigant sample gas separated by the bundled capillary chromatographic column sequentially enters an ion mobility spectrometer in a single component form; and
and sequentially detecting each component of the fumigant sample gas by an ion mobility spectrometer.
According to the fumigant detection method of the embodiment of the present disclosure, in step S4, detecting the components of the fumigant sample gas includes detecting the kinds and concentrations of the components of the fumigant sample gas.
According to the fumigant detector disclosed by the embodiment of the disclosure, a fumigant sample gas is separated through a bundled capillary chromatographic column, so that the fumigant sample gas sequentially enters an ion mobility spectrometer in the form of a single component, and then each component of the fumigant sample gas is sequentially detected by the ion mobility spectrometer. The fumigant can be used for detecting mixed gas of the fumigant in a complex environment and can also be used for detecting pure fumigant.
Drawings
Fig. 1 is a schematic structural diagram of a fumigant detector according to the present disclosure.
Fig. 2 is a flow chart of a fumigant detection method according to the present disclosure.
Detailed Description
While the present invention will be fully described with reference to the accompanying drawings, which contain preferred embodiments of the invention, it is to be understood that, prior to the description herein, one of ordinary skill in the art can modify the invention described herein while obtaining the technical effects of the invention. Therefore, it should be understood that the foregoing description is a broad disclosure of those skilled in the art, and is not intended to limit the exemplary embodiments of the invention described herein.
Furthermore, in the following detailed description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the embodiments of the disclosure. It may be evident, however, that one or more embodiments may be practiced without these specific details. In other instances, well-known structures and devices are shown in schematic form in order to simplify the drawing.
According to a general inventive concept of the present disclosure, there is provided a fumigant detector including: a sampling unit adapted to collect the fumigant sample gas; the inlet of the bundled capillary chromatographic column is communicated with the sampling unit and is suitable for separating the fumigant sample gas collected by the sampling unit; and the air inlet of the ion mobility spectrometer is communicated with the outlet of the bundled capillary chromatographic column, so that the fumigant sample gas separated by the bundled capillary chromatographic column sequentially enters the ion mobility spectrometer in the form of single component, and each component of the fumigant sample gas is sequentially detected by the ion mobility spectrometer.
According to another general inventive concept of the present disclosure, there is also provided a fumigant detection method, including the steps of: collecting fumigant sample gas through a sampling unit;
separating the collected fumigant sample gas by a bundled capillary chromatographic column;
the fumigant sample gas separated by the bundled capillary chromatographic column sequentially enters an ion mobility spectrometer in a single component form; and
and sequentially detecting each component of the fumigant sample gas by an ion mobility spectrometer.
Fig. 1 is a schematic diagram of a fumigant detector according to the present disclosure.
In one exemplary embodiment, as shown in fig. 1, the fumigant detector comprises a sampling unit, a bundled capillary chromatography column 4 and an ion mobility spectrometer. Wherein, the sampling unit is suitable for gathering fumigant sample gas. The inlet of the cluster capillary chromatographic column 4 is communicated with the sampling unit and is suitable for separating the fumigant sample gas collected by the sampling unit. The gas inlet of the ion mobility spectrometer is communicated with the outlet of the bundled capillary chromatographic column 4, so that fumigant sample gas separated by the bundled capillary chromatographic column 4 sequentially enters the ion mobility spectrometer in the form of single component, and then each component of the fumigant sample gas is detected by the ion mobility spectrometer. Because the bundled capillary chromatographic column 4 has a sample separation function, the collected fumigant sample gas can be separated through the bundled capillary chromatographic column 4, so that the fumigant sample gas can sequentially enter the ion mobility spectrometer in the form of a single component, and then each component of the fumigant is sequentially detected through the ion mobility spectrometer.
As shown in fig. 1, in one exemplary embodiment, detecting the constituents of the fumigant sample gas includes detecting the species and concentration of the constituents of the fumigant sample gas. For example, the species of each component can be qualitatively detected by comparing the time of arrival of the fumigant of each component at the detector of the ion mobility spectrometer with the values in the standard substance library, and the concentration of each component can be estimated by measuring the area of the peak of each component, so that the qualitative and quantitative detection of the fumigant sample gas containing multiple fumigants can be realized.
As shown in fig. 1, in an exemplary embodiment, the sampling unit includes a sampling device (e.g., sampling head) 1 and a sampling line 3, one end of the sampling line 3 is communicated with the sampling device 1, and the other end of the sampling line 3 is communicated with an inlet of a bundled capillary chromatography column 4. The sampling unit further comprises a sampling pump 2, the sampling pump 2 being arranged on the sampling pipe 3 for driving the flow of fumigant sample gas.
In one exemplary embodiment, as shown in fig. 1, an ion mobility spectrometer comprises an ionization region and an ionization source 5 located within the ionization region, the ionization source 5 for ionizing fumigant molecules entering the ion mobility spectrometer into charged ions; the ionization source 5 may be a radioactive source or a non-radioactive ionization source, such as a power source discharge source, a photoionization source, or the like. The ion mobility spectrometer also comprises a migration region, and a positive migration tube 7 and a negative migration tube 10 which are positioned in the migration region, wherein the positive migration tube 7 and the negative migration tube 10 provide a uniform electric field, so that positive ions and negative ions move in the electric field, and thus, each component of the fumigant can be qualitatively identified according to the difference of the movement speeds of the ions. Ion gates 6, 8 are provided between the migration zone and the ionization zone, the ion gates 6, 8 being periodically opened so that charged ions generated after ionization enter the migration zone of the migration tubes 7, 10 at the same time. The ion mobility spectrometer also includes detectors (e.g., faraday disks) 9, 11, the detectors 9, 11 being located at an end of the mobility region remote from the ionization region. When the ion gates 6, 8 are periodically opened, the charged ions generated after the components of the fumigant are ionized by the ionization source 5 are injected into the migration region and move towards the detectors 9, 11 under the action of the uniform electric field provided by the positive and negative migration tubes 7, 10. The migration velocity of the charged ions depends on parameters such as mass number, charge number and spatial structure, and therefore the arrival times of different product ions at the detectors 9, 11 are different. The signal of the detected substance can be obtained by collecting the weak current generated by the impact of the product ions with the detectors 9 and 11, and different kinds of fumigant samples can be qualitatively detected by measuring the time of arrival of the samples at the detectors 9 and 11 and comparing the measured time with the value in the standard substance library.
In an exemplary embodiment, as shown in fig. 1, the fumigant detector further comprises a signal amplification module 12, the signal amplification module 12 being connected to the detectors 9, 11. This allows the signal from the ion mobility spectrometer to be amplified by the signal amplification module 12.
In one exemplary embodiment, as shown in fig. 1, the ion mobility spectrometer is a dual mode ion mobility spectrometer, with the end of the bundled capillary chromatography column 4 connected directly to the dual mode ion mobility spectrometer.
In an exemplary embodiment, as shown in fig. 1, the fumigant detector further comprises a display unit connected to the signal amplification module 12 and adapted to display ion mobility spectrometer signals 13 of the components of the detected fumigant sample gas.
As shown in fig. 1, in an exemplary embodiment, the fumigant detector can simultaneously detect a currently common fumigant sample gas, which typically includes methyl bromide, sulfuryl fluoride, phosphine, ethylene oxide, and the like. The characteristic peaks of methyl bromide and sulfuryl fluoride are in the negative mode of an ion mobility spectrometer, and the characteristic peaks of phosphine and ethylene oxide are in the positive mode of ion mobility. However, it should be noted that in some other embodiments of the present disclosure, the fumigant detector may detect a pure fumigant comprising only a single component.
Fig. 2 is a flow chart of a fumigant detection method according to the present disclosure.
As shown in fig. 2, in an exemplary embodiment, the fumigant detection method includes the steps of:
s1: collecting fumigant sample gas through a sampling unit;
s2: separating the collected fumigant sample gas by a bundled capillary chromatographic column 4;
s3: the fumigant samples separated by the bundled capillary chromatographic column 4 sequentially enter an ion mobility spectrometer in the form of single components; and
s4: the ion mobility spectrometer detects each component of the fumigant sample gas in turn.
In some embodiments, in step S4, detecting the components of the fumigant sample gas includes detecting the species and concentration of the components of the fumigant sample gas. For example, the species of each component can be qualitatively detected by comparing the time of arrival of the fumigant of each component at the detector of the ion mobility spectrometer with the values in the standard substance library, and the concentration of each component can be estimated by measuring the area of the peak of each component, so that the qualitative and quantitative detection of the fumigant sample gas containing multiple fumigants can be realized.
According to the fumigant detector disclosed by the embodiment of the disclosure, a fumigant sample gas is separated through a bundled capillary chromatographic column, so that the fumigant sample gas sequentially enters an ion mobility spectrometer in the form of a single component, and then each component of the fumigant sample gas is sequentially detected by the ion mobility spectrometer. The fumigant detector can detect mixed fumigant gas in a complex environment, such as currently common fumigants including methyl bromide, sulfuryl fluoride, phosphine, ethylene oxide and the like, and has detection sensitivity up to ppb level and response time less than 10 s. The fumigant can also be used for detecting pure fumigant.
It will be appreciated by those skilled in the art that the embodiments described above are exemplary and can be modified by those skilled in the art, and that the structures described in the various embodiments can be freely combined without conflict in structure or principle.
Having described preferred embodiments of the present invention in detail, it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the scope and spirit of the appended claims, and the invention is not to be limited to the exemplary embodiments set forth herein.
Claims (11)
1. A fumigant detector comprising:
a sampling unit adapted to collect the fumigant sample gas;
the inlet of the bundled capillary chromatographic column is communicated with the sampling unit and is suitable for separating the fumigant sample gas collected by the sampling unit so as to sequentially output each component contained in the fumigant sample gas in a single component form; and
and the air inlet of the ion mobility spectrometer is communicated with the outlet of the bundled capillary chromatographic column, so that the fumigant sample gas separated by the bundled capillary chromatographic column sequentially enters the ion mobility spectrometer in the form of a single component, and each component of the fumigant sample gas is sequentially detected by the ion mobility spectrometer.
2. The fumigant monitor of claim 1, wherein detecting components of the fumigant sample gas comprises detecting the type and concentration of components of the fumigant sample gas.
3. The fumigant monitor of claim 1, wherein the sampling unit comprises:
a sampling device;
one end of the sampling pipeline is communicated with a sampling device, and the other end of the sampling pipeline is communicated with an inlet of the bundled capillary chromatographic column; and
the sampling pump is arranged on the sampling pipeline and used for driving the fumigant sample gas to flow.
4. The fumigant detector of claim 1, wherein the ion mobility spectrometer comprises:
an ionization region and an ionization source located within the ionization region for ionizing fumigant molecules of a fumigant sample gas into charged ions;
a migration area and a positive migration pipe and a negative migration pipe which are positioned in the migration area;
an ion gate is arranged between the migration zone and the ionization zone and is periodically opened, so that charged ions generated after components of the fumigant sample gas are ionized enter the migration zone of the migration pipe at the same time; and
a detector located at an end of the migration zone distal from the ionization zone.
5. The fumigant detector of claim 4, further comprising a signal amplification module connected to the detector to amplify an ion mobility spectrometer signal.
6. The fumigant detector of claim 5, further comprising a display unit connected to the signal amplification module and adapted to display in sequence the ion mobility spectrometer signals of the components of the fumigant sample gas.
7. The fumigant detector of claim 4, wherein the ionization source is one of a radioactive source, a power discharge source and a photo ionization source.
8. A fumigant monitor according to any one of claims 1 to 7 wherein the fumigant sample gas is a fumigant sample mixed gas.
9. The fumigant monitor of claim 8, wherein the fumigant sample gas mixture comprises at least two of methyl bromide, sulfuryl fluoride, phosphine, and ethylene oxide.
10. A fumigant detection method comprises the following steps:
s1: collecting fumigant sample gas through a sampling unit;
s2: separating the collected fumigant sample gas by a bundled capillary chromatographic column;
s3: the fumigant sample gas separated by the bundled capillary chromatographic column sequentially enters an ion mobility spectrometer in a single component form; and
s4: and sequentially detecting each component of the fumigant sample gas by an ion mobility spectrometer.
11. The method of claim 10 wherein, in step S4, detecting the components of the fumigant sample gas includes detecting the species and concentration of the components of the fumigant sample gas.
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| CN109521081A (en) * | 2018-12-29 | 2019-03-26 | 同方威视技术股份有限公司 | Multifunction ion mobility spectrometer device |
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| US20040079651A1 (en) * | 2001-02-28 | 2004-04-29 | Reiner Kober | Method and device for detecting fumigants in air samples |
| CN102455318A (en) * | 2010-10-29 | 2012-05-16 | 中国科学院大连化学物理研究所 | Continuous monitor for detecting aerosol sample |
| CN104515824A (en) * | 2014-12-31 | 2015-04-15 | 同方威视技术股份有限公司 | Gas-phase substance analysis device and gas-phase introduction device |
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Application publication date: 20210129 |