CN212301414U - Device for measuring ketone compounds in gas - Google Patents
Device for measuring ketone compounds in gas Download PDFInfo
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- CN212301414U CN212301414U CN202021190055.0U CN202021190055U CN212301414U CN 212301414 U CN212301414 U CN 212301414U CN 202021190055 U CN202021190055 U CN 202021190055U CN 212301414 U CN212301414 U CN 212301414U
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Abstract
The utility model discloses a device and a method for measuring ketone compounds in gas, wherein the device comprises an ionization channel, a gas channel and a mass spectrometer; the ionization channel comprises a discharge needle, a first carrier gas channel, a first pipeline, a high-pressure source, a first capillary, a sample placing device and a first flowmeter; the gas channel includes a gas source, a second carrier gas channel, a second flow meter, a second line, and a second capillary. The utility model utilizes the interaction of water free radical cation and ketone compound to form a base peak (M + H)2O]+·The method of the compound can improve the detection sensitivity of the ketone compound and reduce the corresponding detection limit so as to realize the rapid qualitative and quantitative analysis of the ketone substance in the gas, and can solve the problems in the prior art thatThe gas analysis process needs pretreatment, organic solvent, can not realize on-line detection, and the device is complex.
Description
Technical Field
The utility model relates to a gaseous detection technology field especially relates to a device of ketone compound in survey gas.
Background
Ketone compounds are ubiquitous in nature and have wide applications in a variety of fields. For example, acetone is the major ketone contained in human exhaled breath, and is often a marker of ketosis. The liver can produce a large number of ketone bodies, including acetoacetate, β -hydroxybutyrate and acetone, by oxidation and breakdown of fatty acids. Wherein acetone is produced in less quantity than the other two ketone bodies and is exhaled by breathing due to its higher vapor pressure. In addition, in cachexia, the content of ketone bodies, especially acetone, is increased by the metabolism of proteins, which occurs mainly in the late stages of the disease. In addition, acetone, butanone and pentanone are the marker components in the exhalation of lung cancer patients, and gradually increase with the severity of the disease. Therefore, the detection and analysis of ketone compounds in the exhaled breath can provide key information for early detection of diseases.
To date, the analysis of ketone compounds in exhaled breath has been relatively popular and numerous methods have been developed. For example, solid phase microextraction is combined with gas chromatography-mass spectrometry (SPME-GC-MS), which is a gold standard for off-line exhaled gas analysis. SPME-GC-MS, however, requires sample collection and pretreatment and cannot be performed in situ, which is relatively complex and time consuming. It is therefore important that the detection of acetone in exhaled breath can be performed directly without or with minimal sample pre-treatment. The current popular methods include ion flow mass spectrometry (SIFT-MS), proton transfer reaction mass spectrometry (PTR-MS), electrospray extraction ionization mass spectrometry (EESI-MS), and can analyze exhaled breath on line. However, these methods have the disadvantages of requiring the use of organic solvents, easily causing environmental pollution, complicated flow procedures, etc. For example, SIFT-MS requires a special microwave ionization source, while a quadrupole rod mass analyzer is coupled; PTR-MS requires the use of specialized ionization source devices such as hollow cathodes. These undoubtedly increase the cost of the detection analysis, and the general universality is not strong. Therefore, there is a need to develop a simpler and more versatile method and device for detecting ketone compounds in breath.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a device and method of ketone compound in survey gas to solve prior art, in carrying out the analytic process to gas, need the preliminary treatment, need organic solvent, can not realize on-line measuring scheduling problem.
The utility model provides a device for measuring ketone compounds in gas, which is characterized by comprising an ionization channel, a gas channel and a mass spectrometer;
the ionization channel comprises a discharge needle, a first carrier gas channel, a first pipeline, a high-pressure source, a first capillary tube, a sample placing device and a first flowmeter;
the first carrier gas channel is inserted into the lofting device and used for providing inert gas for the lofting device;
one end of the first pipeline is inserted into the lofting device, the other end of the first pipeline is connected with the first capillary through a first two-way valve, the discharge needle is arranged in the first capillary, and the high-voltage source is used for providing high voltage for the discharge needle;
the gas channel comprises a gas source, a second carrier gas channel, a second flowmeter, a second pipeline and a second capillary tube;
the gas source is connected with the second carrier gas channel, the second carrier gas channel is connected with the second flow meter, the second flow meter is connected with the second pipeline, and the second pipeline is connected with the second capillary;
the first and second capillaries are both located at a front end of the mass spectrometer inlet.
The utility model discloses another aspect provides a method of ketone compound in survey gas, uses above-mentioned device, and this method includes:
closing the gas channel, and introducing wet water vapor into the ionization channel to the needle point of the discharge needle; simultaneously applying high voltage of 1.5-2.5 kV to the discharge needle to prepare the high-abundance water radical cation cluster (H)2O)2 +·Ion m/z 36; under the condition that the gas channel is closed, a ketone compound aqueous solution sample with a certain concentration is added into a sample placing device of the ionization channel, and under the drive of carrier gas flow, ketone and water vapor flow into the first capillary and form rich (H) when reaching the vicinity of the discharge needle2O)2 +·At the same time, the surrounding ketone vapor rapidly interacts with the forming water radical cation (H)2O)2 +·Interacting in three-dimensional space to generate base peak ions (M + H) with mass number increased by 18Da2O]+·A complex; using deuterium isotopes and18o label is used for replacing solvent water in ketone compound solution with D2O and H2 18And O, other conditions are kept unchanged, and ions with mass number increased by 18Da can be determined to be H through corresponding analysis of primary mass spectrum data and secondary mass spectrum data2O+·A complex formed by interaction with a ketone compound;
closing the gas channel, and sequentially adding aqueous solutions of the ketone compounds with different concentrations into a sample placing device of the ionization channel to obtain a better linear relation between the aqueous solutions of the ketone compounds with different concentrations and a water-adding free radical cation signal m/z 76;
and changing the sample in the ionization channel into pure water, opening the gas channel, detecting the gas component in the gas source, and measuring the concentration of the ketone compound in the gas source.
According to the utility model provides a record device and method of ketone compound in gas has following beneficial effect:
by adopting the device and the method for measuring the ketone compounds in the gas, when the humidity of the air is low, the carrier gas can be used for introducing the water vapor; when the air humidity is higher, the water vapor in the air can be directly ionized without introducing carrier gas, and the use is convenient. The ionization water vapor generates a large amount of water radical cation clusters by regulating the electric field intensity, the formed water radical cation clusters interact with ketone compounds in exhaled air to generate high-abundance adducted water radical cation product peaks, the whole device is simple, the refitting cost is low, online in-situ analysis can be realized, any sample pretreatment is not needed, the whole analysis process is less than 1 minute, the analysis can be carried out at normal temperature and normal pressure, water is used as a carrier, the device is green and pollution-free, the reaction time of the water radical cation clusters and the ketone compounds is short, high-throughput analysis can be realized, and the device has important significance for the rapid detection and analysis of the ketone compounds in a gas source. When the gas source is provided with the expiration device, the online expiration detection of the human body can be realized, and a quick, simple and convenient method and a device with low cost are provided for the early discovery of human diseases.
In addition, according to the utility model provides an apparatus for measuring ketone compound in gas, can also have following additional technical characterstic:
further, the discharge needle adopts a conical discharge needle made of stainless steel.
Further, the ionization channel further comprises a first flow meter, and the first flow meter is arranged on the first carrier gas channel.
Further, the gas source comprises an exhalation device for direct exhalation by the human body.
Further, the gas source comprises a gas collection bag for collecting gas for detection.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a schematic structural diagram of an apparatus for measuring ketone compounds in a gas according to an embodiment of the present invention;
FIG. 2 is a mass spectrum (gas channel closed) of free radical cation of water prepared by regulating the energy-to-charge transfer law in example 1;
FIG. 3 is a first and second mass spectrum of the water radical cation formed in the ionization channel interacting with acetone to form an adducted water radical cation product (m/z 76), along with corresponding isotopic labeling;
FIG. 4 is a total ion flow diagram and a selected ion flow diagram of the interaction of water radical cations with acetone;
FIG. 5 is a schematic diagram of the interaction of water radical cations with acetone to form water radical cation addition products and the reaction mechanism of the corresponding products after fragmentation by tandem mass spectrometry;
FIG. 6 is a total ion flow graph and a first order mass spectrum of water radical cations formed in an ionization channel reacting with acetone in the gas of a gas channel to form an adduct product (m/z 76);
FIG. 7 is a diagram of the structure of different types of ketones.
FIG. 8 is a mass spectrum of the action of different types of ketones with water radical cations.
Detailed Description
In order to make the objects, features and advantages of the present invention more comprehensible, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Several embodiments of the invention are given in the accompanying drawings. The invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. As used herein, the terms "vertical," "horizontal," "left," "right," "up," "down," and the like are for illustrative purposes only and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, 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 according to specific situations by those skilled in the art. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, an apparatus for measuring ketone compounds in a gas according to an embodiment of the present invention includes an ionization channel, a gas channel, and a mass spectrometer 30;
the ionization channel comprises a discharge needle 11, a first pipeline 12, a first carrier gas channel 13, a high-pressure source 14, a first capillary 15 and a sample placing device 16.
The sample placing device 16 can be used for storing samples or pure water, etc., the first carrier gas channel 13 is inserted into the sample placing device 16, and the first carrier gas channel 13 is used for supplying inert gas, such as argon, to the sample placing device 16. The purpose of providing the inert gas in the ionization path is to bring water out while avoiding interference of other impurities when the needle tip of the discharge needle 11 ionizes the water.
One end of the first pipeline 12 is inserted into the sample discharge device 16, the other end of the first pipeline 12 is connected to the first capillary 15 through a first flow meter such as a two-way valve (not shown), the discharge needle 11 is disposed in the first capillary 15, and the high voltage source 14 is configured to apply a high voltage provided by the discharge needle 11, for example, a high voltage of 2kV to the discharge needle 11, so as to ionize water vapor and generate radical cation clusters through corona discharge ionization. Specifically, the discharge needle 11 is a conical discharge needle made of stainless steel.
Among other things, the lofting device 16 serves two functions: (1) the water storage device is used for storing water, providing water vapor and generating water radical cations through corona discharge; (2) the water vapor carries the ketone out to the position of a power supply discharge needle, water molecules are ionized to form water radical cations, and the water radical cations fully react with surrounding ketone compounds and react.
Wherein, the arrangement of the first capillary 15 has two functions: (1) the discharge needles 11 are wrapped to prevent the whole discharge needles 11 from being exposed outside; (2) a neutral water/sample gas flow is introduced to bring the water flow into full operative contact with the discharge needles 11.
The gas channel comprises a gas source 23, a second carrier gas channel 22, a second flow meter 25, a second pipeline 21 and a second capillary 24;
the gas source 23 is connected with the second carrier gas channel 22, the second carrier gas channel 22 is connected with the second flow meter 25, and the second flow meter 25 is used for controlling the size of the gas source;
one end of the second pipe 21 is connected to the second flowmeter 25, and the other end of the second pipe 21 is connected to the second capillary 24.
The gas source 23 may be a human body breath in situ, in which case the gas source includes an exhalation device, such as an oxygen mask, for exhalation purposes, the second flow meter 25 is used to control the flow of the exhaled gas to maintain a steady state, and the second carrier gas channel 22 is used to deliver a flow of gas to introduce the chemical components of the exhalation into the front end of the inlet of the mass spectrometer 30.
The gas source 23 may also be an ex vivo breath and collected using a gas collection bag, in which case the gas source comprises a gas collection bag.
The gas source 23 may also be another type of gas, such as ambient gas, etc., and is collected using a collection bag, in which case the gas source comprises a collection bag.
The exit end of the first capillary 15 is located at the front end of the entrance of the mass spectrometer 30, and is separated from the front end of the entrance of the mass spectrometer 30 by a distance a of 15mm, the exit end of the second capillary 24 is also located at the front end of the entrance of the mass spectrometer 30 by a distance a of 15mm, the exit end of the first capillary 15 is separated from the exit end of the second capillary 24 by a distance b of 5mm, an included angle α between the exit end of the first capillary 15 and the front end of the entrance of the mass spectrometer 30 is 150 °, an included angle α between the exit end of the second capillary 24 and the front end of the entrance of the mass spectrometer 30 is also 150 °, an included angle β between the exit end of the first capillary 15 and the exit end of the second capillary 24 is 60 °, the exit end of the first capillary 15, the exit end of the second capillary 24 and the front end of the entrance of the mass spectrometer 30 are all located in a closed device, this enables the water radical cation clusters formed in the ionization channel and the ketone compounds in the gas to join at the front of the inlet of the mass spectrometer 30 and act sufficiently to cause as little loss of sample as possible.
Preferably, the ionization channel further comprises a first flow meter 17, and the first flow meter 17 is arranged on the first carrier gas channel 13 and is used for controlling the flow of the gas in the ionization channel.
Based on the device, the method for measuring the ketone compounds in the gas comprises the following steps:
introducing an inert gas into the sample placing device 16 through the first carrier gas channel 13 to form an inert gas with water vapor, and simultaneously introducing a sample in the gas into the front end of the inlet of the mass spectrometer 30 in the form of a gas by a gas source through the second carrier gas channel 22;
applying a high voltage of 1.5-2.5 kV to the needle point of the discharge needle 11 through the high voltage source 14 to enable water radical cations to be a base peak, and introducing wet water vapor to the needle point of the discharge needle 11 through the first pipeline 12 to ionize through corona discharge to generate water radical cation clusters;
the formed water radical cation cluster and ketone sample molecules in the gas source act in a three-dimensional space to generate a peak containing ketone addition water radical cations;
the formed free radical cation product containing ketone and water is detected by the mass spectrometer 30, and the mass spectrometer 30 analyzes the product to obtain a characteristic ion fragment with a determinable structure, so that the high-sensitivity analysis of the ketone component in the gas source is realized.
The present invention will be further explained below by way of examples.
Example 1
With the arrangement shown in fig. 1, the ionization channel is guided in the closed gas channelThe moist water vapor enters the needle point of the discharge needle, and the high pressure of 2kV is applied to the discharge needle at the same time, so that the high-abundance water free radical cation cluster (H) can be prepared2O)2 +·Ion m/z 36, as shown in FIG. 2. Wherein m/z54 is (H)2O)3 +·Ion, m/z 55 is (H)2O)3H+Ions.
Example 2
With the apparatus shown in FIG. 1, a sample of aqueous acetone (Mw 58) was added to the sample holder of the ionization channel at a concentration that was sufficient to react with the formed water radical cations (H) with the gas channel closed2O)2 +·The three-dimensional space interaction further generates a base peak ion m/z 76 with mass number increased by 18Da, and the preliminary inference is that H is added2O+·(shown in FIG. 3 a). Further by isotopic deuterium labelling and isotopic18O labelling experiment replacement of aqueous acetone with (D)2O and acetone) solution and (H)2 18O and acetone), and other conditions are kept unchanged, and ions with the mass number increased by 18Da can be determined to be H through corresponding primary mass spectrum data analysis2O+·The product of the interaction with acetone (shown in FIGS. 3b and 3 c), the product ion for 18Da increase, is derived from H2And O. Further through [ M + H2O]+·Second order mass spectrum of (FIG. 3D), [ M + D [ ]2O]+·Second order mass spectrum (shown in FIG. 3 e) and isotope18O labelling of [ M + H ] formed in the experiment2 18O]+·Comparative analysis of the secondary mass spectrum (shown in FIG. 3 f) revealed that [ M + H [ + ]2O]+·Mainly OH loss and H loss by collision2O forms protonated acetone m/z 59 and acetone radical cation m/z 58, respectively (FIG. 3 e); [ M + D ]2O]+·Mainly resulting in lost OD through collision, H/D exchange and lost D after OD is lost2O forms deuterated acetone m/z 60, protonated acetone m/z 59, and acetone radical cation m/z 58, respectively (shown in FIG. 3 f); [ M + H ]2 18O]+·Mainly lost H through collision2O, throw18OH and loss of H2 18O forms acetone respectively18O radical cation m/z 60, protonated acetone m/z 59, and acetone radical cation m/z 58 (shown in FIG. 3 f). Thus, it was determined that the ion with the mass number increased by 18Da was H2O+·The product of the interaction with acetone, i.e. the 18Da increase, comes from the H introduced by the apparatus2O。
Referring to FIG. 5, FIG. 5 shows the interaction of water radical cations with acetone to form [ M + H ]2O]+·(FIG. 5a) and [ M + H ] in tandem mass spectrometry2O]+·Further fragmentation occurs with loss of OH and H2The specific mechanism by which O forms protonated acetone m/z 59 and acetone radical cation m/z 58 (FIG. 5 b).
Referring to fig. 4, fig. 4 shows a total ion flow chart (TIC) and an optional ion flow chart (EIC) obtained by introducing a certain amount of water vapor into the ionization channel and then a certain amount of aqueous acetone under the condition that the gas channel is closed, and it can be found that m/z 36 rapidly decreases and m/z 76 rapidly increases after acetone is introduced. This indicates that m/z 36 is reacted away to form a new m/z 76.
Example 3
The apparatus shown in FIG. 1 was used to evaluate the process performance of the apparatus. Meanwhile, by adopting the same method, the same experimental parameter conditions and the same mass spectrum experimental conditions as in example 2, the gas channel is closed first, acetone aqueous solutions with different concentrations (0.01 μ M, 0.1 μ M, 0.25 μ M, 0.5 μ M and 1 μ M) are sequentially added into the sample device of the ionization channel, so that a better linear relation between the different concentrations of the acetone aqueous solution and the water-added radical cation signal M/z 76 can be obtained (fig. 6b), and when the concentration of the acetone is 0.01 μ M, obvious M/z 76 ions can be still detected (fig. 6 a). Changing the sample in the ionization channel into water, opening the gas channel, detecting the gas component in the gas source, and observing that the signal of m/z 76 is obviously enhanced; FIG. 6c is an EIC chart of m/z 76 when examined, and it can be seen that m/z 76 is significantly increased and is stable; FIG. 6d shows the corresponding mass spectrum, which indicates that the concentration of acetone in the gas source is about 0.25. mu.M.
Example 4
The apparatus shown in fig. 1 was used to evaluate the universality of the method. The same experiment was performed on a series of ketones, the structures of which are shown in FIG. 7. By adopting the same method, the same experimental parameter conditions and the same mass spectrum experimental conditions as in example 2, the gas channel is closed first, and different types of ketone aqueous solutions are sequentially added into the sample placing device of the ionization channel, so that signals of the action of various types of ketone compounds and the water-added radical cations can be obtained (fig. 8), which shows that the ketone compound non-solution and the water radical cations form a high-abundance water-added radical cation peak.
In summary, with the above apparatus and method for measuring ketone compounds in gas, when the humidity of air is low, water vapor can be carried in by using carrier gas; when the air humidity is higher, the water vapor in the air can be directly ionized without introducing carrier gas, and the use is convenient. The ionization water vapor generates a large amount of water radical cation clusters by regulating the electric field intensity, the formed water radical cation clusters interact with ketone compounds in exhaled air to generate high-abundance adducted water radical cation product peaks, the whole device is simple, the refitting cost is low, online in-situ analysis can be realized, any sample pretreatment is not needed, the whole analysis process is less than 1 minute, the analysis can be carried out at normal temperature and normal pressure, water is used as a carrier, the device is green and pollution-free, the reaction time of the water radical cation clusters and the ketone compounds is short, high-throughput analysis can be realized, and the device has important significance for the rapid detection and analysis of the ketone compounds in a gas source. When the gas source is provided with the expiration device, the online expiration detection of the human body can be realized, and a quick, simple and convenient method and a device with low cost are provided for the early discovery of human diseases.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above-mentioned embodiments only represent some embodiments of the present invention, and the description thereof is specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (5)
1. The device for measuring the ketone compounds in the gas is characterized by comprising an ionization channel, a gas channel and a mass spectrometer;
the ionization channel comprises a discharge needle, a first carrier gas channel, a first pipeline, a high-pressure source, a first capillary tube, a sample placing device and a first flowmeter;
the first carrier gas channel is inserted into the lofting device and used for providing inert gas for the lofting device;
one end of the first pipeline is inserted into the lofting device, the other end of the first pipeline is connected with the first capillary through a first two-way valve, the discharge needle is arranged in the first capillary, and the high-voltage source is used for providing high voltage for the discharge needle;
the gas channel comprises a gas source, a second carrier gas channel, a second flowmeter, a second pipeline and a second capillary tube;
the gas source is connected with the second carrier gas channel, the second carrier gas channel is connected with the second flow meter, the second flow meter is connected with the second pipeline, and the second pipeline is connected with the second capillary;
the first capillary and the second capillary are both located at the mass spectrometer inlet front end.
2. The apparatus for detecting ketone compounds in gas according to claim 1, wherein the discharge needle is a conical discharge needle made of stainless steel.
3. The apparatus of claim 1, wherein the first flow meter is a two-way valve.
4. The apparatus of claim 1, wherein the gas source comprises an exhalation system.
5. The apparatus of claim 1, wherein the gas source comprises a gas collection bag.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111650272A (en) * | 2020-06-24 | 2020-09-11 | 东华理工大学 | Device and method for measuring ketone compounds in gas |
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| CN111650272A (en) * | 2020-06-24 | 2020-09-11 | 东华理工大学 | Device and method for measuring ketone compounds in gas |
| CN111650272B (en) * | 2020-06-24 | 2024-07-05 | 东华理工大学 | Device and method for measuring ketone compounds in gas |
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