CN115932133A - Mobility spectrometry detection device and method with multiple sample injection modes - Google Patents
Mobility spectrometry detection device and method with multiple sample injection modes Download PDFInfo
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- CN115932133A CN115932133A CN202211495699.4A CN202211495699A CN115932133A CN 115932133 A CN115932133 A CN 115932133A CN 202211495699 A CN202211495699 A CN 202211495699A CN 115932133 A CN115932133 A CN 115932133A
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Abstract
The invention provides a mobility spectrometry detection device and a method with multiple sample injection modes, wherein the mobility spectrometry detection device comprises a multi-way valve, a quantitative ring, an enrichment tube, a chromatographic column and a mobility spectrometry analysis unit; the first switching module is used for enabling the port of the multi-way valve to be selectively communicated with the second switching module or the carrier gas, and the second switching module is used for enabling the flow control module to be selectively communicated with the first switching module or the sample injection pipe; the sample inlet pipe is communicated with a mobility spectrum analysis unit with two parallel migration pipes through a valve; two ends of the first damping column and the pre-column are respectively connected with a port of the multi-way valve, and when the multi-way valve is switched, carrier gas sequentially flows through the quantitative ring, the first damping column and the third switching module; the third switching module is used for enabling the sample gas discharged from the first damping column to be selectively communicated with the chromatographic column or directly communicated with the mobility spectrometry analysis unit; the first pump is respectively communicated with the outlets of the two transfer pipes, and the second pump is arranged at the downstream of the flow control module. The invention has the advantages of high sensitivity and the like.
Description
Technical Field
The invention relates to ion mobility spectrometry, in particular to a mobility spectrometry detection device and method with multiple sample injection modes.
Background
The gas chromatography utilizes the difference of the distribution coefficients of different substances in a stationary phase and a mobile phase to lead different compounds to flow out of a chromatographic column for different time, thereby achieving the purpose of separation. Analysis of substances is usually accomplished in conjunction with various types of detectors.
An Ion Mobility Spectrometry (IMS) technique is a method of separation and analysis using the difference in ion mobility of different compounds, and has a low detection limit, and is suitable for analysis of trace substances, but the difference in ion mobility of different compounds is small, and a commercial IMS instrument has a limited general resolution due to limitations of conditions such as volume, and is difficult to realize qualitative and quantitative analysis of a complex sample.
In order to detect complex samples, a gas chromatography-ion mobility spectrometry (GC-IMS) method is currently used, and has some disadvantages, such as:
the GC-IMS generally only has one sample injection mode, the switching of a plurality of sample injection analysis modes cannot be realized, and the IMS positive mode and the IMS negative mode cannot be used simultaneously.
For an IMS analysis unit, membrane sample injection is common, and the principle is as follows: the sample molecules are dissolved on the outer side surface of the membrane, and can be driven to diffuse to the other side surface of the membrane due to the distribution difference of concentration gradients on two sides of the membrane, and then the sample molecules are desorbed from the surface in an air flow purging elution mode and enter the IMS for detection.
The selectivity of the IMS is improved by utilizing the difference of the permeability of different samples penetrating through the membrane. For example, in patent CN202010647793.1, a multi-chamber device is used for membrane sample injection, and a sample gas selectively permeates a membrane and enters a detection chamber from a sample gas chamber, so that the sample injection efficiency and selectivity are improved by controlling the pressure at the rear end of the membrane.
The membrane sample injection mode has the defects that only a small part of target compounds in a sample can permeate through the membrane and be detected by the IMS, so that the detection sensitivity is reduced to a certain extent; when the concentration of the sample is changed, the response time of the signal intensity change is relatively long, and when the concentration of the sample is large, the memory effect on the membrane is serious. The traditional PDMS film is used for H when the humidity in a sample is higher 2 O has a good filtering effect but cannot effectively separate the sample of interest from the gas mixture.
And 2, the switching of the sample injection modes of the IMS and the GC-IMS can cause the conditions that the internal pressure of the IMS is unstable and the double-tube IMS is unequal, and if the two IMS pressures are different, the flow from sample injection to the double-tube IMS is different, so that the stability and the accuracy of the measurement result are influenced.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a mobility spectrometry detection device with multiple sample injection modes.
The purpose of the invention is realized by the following technical scheme:
the device comprises a mobility spectrometry detection device with multiple sample injection modes, a sample injection unit and a sample injection unit, wherein the mobility spectrometry detection device with multiple sample injection modes comprises a multi-way valve, a quantitative ring, an enrichment pipe, a chromatographic column and a mobility spectrometry analysis unit, and an outlet of the chromatographic column is communicated with the mobility spectrometry analysis unit; the mobility spectrometry detection device with multiple sample injection modes further comprises:
the multi-way valve comprises a first switching module and a second switching module, wherein the first switching module is used for enabling a multi-way valve port to be selectively communicated with the second switching module or carrier gas, and the second switching module is used for enabling a flow control module to be selectively communicated with the first switching module or a sample inlet pipe;
the sample inlet pipe is communicated with the mobility spectrum analysis unit through a valve, the mobility spectrum analysis unit comprises two parallel migration pipes, and the two migration pipes work according to a positive mode and a negative mode;
the two ends of the first damping column and the two ends of the pre-column are respectively connected with the ports of the multi-way valves, and when the multi-way valves are switched, carrier gas sequentially flows through the quantitative ring, the first damping column and the third switching module;
the third switching module is used for enabling the sample gas discharged from the pre-column or the first damping column to be selectively communicated with the chromatographic column or directly communicated with the mobility spectrometry unit;
the first pump is communicated with the outlets of the two transfer pipes respectively, and the second pump is arranged at the downstream of the flow control module.
The invention also aims to provide a mobility spectrometry detection method with a plurality of sample injection modes, and the invention aims to be realized by the following technical scheme:
according to the detection method of the mobility spectrometry detection device with multiple sample injection modes, the detection method comprises the following steps:
a mobility spectrometry negative pressure sample injection mode, specifically, sample gas sequentially passes through the valve, the two migration pipes and the first pump;
a mobility spectrometry quantitative loop sampling mode, a chromatography-mobility spectrometry quantitative loop sampling mode and a chromatography-mobility spectrometry enrichment tube sampling mode which respectively comprise a pre-pumping state, a sampling state and a back-flushing state; the pre-pumping state is that a sample sequentially passes through a sampling pipe, a second switching module, a flow control module and a second pump; the sampling state is that a multi-way valve is used for switching, and sample gas sequentially passes through a sampling pipe, a quantitative ring, an enrichment pipe, a first switching module, a second switching module, a flow control module and a second pump; the back flushing state is that the multi-way valve is used for switching, and carrier gas sequentially passes through the first switching module, the enrichment pipe, the quantitative ring, the sampling pipe, the second switching module and the second pump.
Compared with the prior art, the invention has the beneficial effects that:
1. has a plurality of sample introduction modes;
various sample introduction modes are realized, including an IMS direct sample introduction mode, an IMS quantitative loop sample introduction mode, a GC-IMS quantitative loop sample introduction mode and a GC-IMS enrichment tube sample introduction mode;
2. the double migration tubes are respectively monitored simultaneously by using a positive mode and a negative mode, all factors which can be detected by the IMS can be detected simultaneously, and the time-consuming switching of the positive mode and the negative mode is not needed;
3. the split flow control of the sample injection flow of the double-tube IMS can be realized, the modes of differential pressure temperature measurement and float gas control for controlling the internal pressure of the IMS ensure that the sample injection flow split to the two IMS is equal, and the detection accuracy is improved.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic structural diagram of a mobility spectrometry detection apparatus having multiple sample injection modes according to an embodiment of the present invention.
Detailed Description
Fig. 1 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of explaining the technical solution of the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
the mobility spectrometry detection device with multiple sample injection modes of the embodiment of the invention comprises:
the device comprises a multi-way valve, a quantitative ring, an enrichment pipe, a chromatographic column and a mobility spectrometry unit, wherein an outlet of the chromatographic column is communicated with the mobility spectrometry unit, and the structures and the connection modes of the devices are the prior art in the field;
the device comprises a first switching module and a second switching module, wherein the first switching module is used for enabling a multi-way valve port to be selectively communicated with the second switching module or carrier gas, and the second switching module is used for enabling a flow control module to be selectively communicated with the first switching module or a sample inlet pipe;
the sample inlet pipe is communicated with the mobility spectrum analysis unit through a valve, the mobility spectrum analysis unit comprises two parallel migration pipes, and the two migration pipes work according to a positive mode and a negative mode so as to work in the positive mode and the negative mode simultaneously;
the two ends of the first damping column are respectively connected with the ports of the multi-way valves, and when the multi-way valves are switched, carrier gas sequentially flows through the quantitative ring, the first damping column and the third switching module;
the third switching module is used for enabling the sample gas discharged from the first damping column to be selectively communicated with the chromatographic column or directly communicated with the mobility spectrometry analysis unit;
the first pump is respectively communicated with the outlets of the two transfer pipes, and the second pump is arranged at the downstream of the flow control module.
In order to ensure the stable flow of the gas path and avoid the high boiling point component in the sample gas from entering the chromatographic column, further, the mobility spectrometry detection device with multiple sample injection modes further comprises:
one end of the second damping column is connected with the port of the multi-way valve, and the other end of the second damping column is communicated with carrier gas;
and the two ends of the pre-column are connected with the ports of the multi-way valves, and when the multi-way valves are switched, the carrier gas sequentially flows through the enrichment pipe, the pre-column and the third switching module.
In order to improve the working reliability, the multi-way valve is a fourteen-way valve, the first port is communicated with the sample injection pipe, the second port and the fifth port are communicated with two ends of the quantitative ring, the third port and the twelfth port are communicated with the carrier gas, the fourth port is communicated with the first damping column, the sixth port and the thirteenth port are communicated with two ends of the enrichment pipe, the seventh port and the eleventh port are communicated with two ends of the pre-column, the eighth port is communicated with the emptying pipe, the ninth port is communicated with the second damping column, the tenth port is communicated with an inlet of the third switching module, and the fourteenth port is communicated with the first switching module.
In order to realize the switching between the negative pressure mode and the positive pressure sample injection mode of the mobility spectrometry, further, the mobility spectrometry detection device with multiple sample injection modes further comprises:
and the fourth switching module is used for enabling the outlets of the two transfer pipes to be selectively communicated with the inlet or the emptying port of the first pump.
In order to realize the selection of the zero gas and the carrier gas, further, the mobility spectrometry detection device with multiple sample injection modes further comprises:
the device comprises a fifth switching module and a sixth switching module, wherein the fifth switching module is used for enabling zero gas or carrier gas to be selectively used as tail blowing gas, and the sixth switching module is used for enabling the zero gas or carrier gas to be selectively used as floating gas.
In order to monitor the pressure in the two migration tubes in real time, further, the mobility spectrometry detection device with multiple sample injection modes further comprises:
the pressure sensor obtains the pressure in one transfer pipe, and the differential pressure sensor obtains the difference between the pressures in the two transfer pipes.
Fig. 1 schematically shows a flow chart of a mobility spectrometry detection method with multiple sample injection modes according to an embodiment of the present invention, and as shown in fig. 1, the detection method includes:
a mobility spectrometry negative pressure sample injection mode, specifically, sample gas sequentially passes through the valve, the two migration pipes and the first pump;
a mobility spectrometry quantitative loop (positive pressure) sample injection mode, a chromatography-mobility spectrometry quantitative loop (positive pressure) sample injection mode and a chromatography-mobility spectrometry enrichment tube (positive pressure) sample injection mode which respectively comprise a pre-pumping state, a sampling state, a sample injection state and a back-flushing state; the pre-pumping state is that a sample sequentially passes through a sampling pipe, a second switching module, a flow control module and a second pump; the sampling state is that a multi-way valve is used for switching, and sample gas sequentially passes through a sampling pipe, a quantitative ring, an enrichment pipe, a first switching module, a second switching module, a flow control module and a second pump; the back flushing state is that the multi-way valve is used for switching, and the carrier gas sequentially passes through the first switching module, the enrichment pipe, the quantitative ring, the sampling pipe, the second switching module and the second pump;
in a mobility spectrum quantitative loop sample injection mode, the sample injection state is that a multi-way valve is used for switching, and carrier gas directly enters the two migration tubes after sequentially passing through the quantitative loop, the first damping column and the third switching module;
in a chromatogram-mobility spectrometry quantitative loop sample injection mode, a sample injection state is that carrier gas enters two migration tubes after sequentially passing through a quantitative loop, a first damping column, a third switching module and a chromatographic column;
in a sample introduction mode of the chromatographic-mobility spectrometry enrichment tube, carrier gas sequentially passes through the enrichment tube, the pre-column, the third switching module and the chromatographic column and then enters the two migration tubes.
In order to ensure the pressure in the two transfer pipes are consistent, further, the pressure difference between the two transfer pipes is obtained by using a differential pressure sensor, and the pressure of the floating gas entering the two transfer pipes is adjusted to ensure that the pressure in the two transfer pipes is equal.
Example 2:
the invention also discloses an application example of the mobility spectrometry detection device and method with multiple sample injection modes according to the embodiment 1 of the invention.
In the application example, the multi-way valve is a fourteen-way valve, a first port is communicated with the sample inlet pipe, a second port and a fifth port are communicated with two ends of the quantitative ring, a third port is communicated with first carrier gas, a twelfth port is communicated with second carrier gas, a fourth port is sequentially communicated with inlets of a first damping column and a third switching module, a sixth port and a thirteenth port are communicated with two ends of the enrichment pipe, a seventh port and an eleventh port are communicated with two ends of a pre-column, an eighth port is communicated with an emptying pipe, a ninth port is communicated with one end of a second damping column, the other end of the second damping column is communicated with second carrier gas, a tenth port is communicated with an inlet of the third switching module, and a fourteenth port is communicated with the first switching module;
the first carrier gas and the second carrier gas are respectively sent to the multi-way valve through the pressure control module by using nitrogen
The sampling pipe is connected with a second switching module, and a flow control module and a second pump are sequentially arranged at the downstream of the second switching module; one outlet of the third switching module is sequentially connected with the chromatographic column and the mobility spectrometry unit, and the other outlet of the third switching module is directly connected with the mobility spectrometry unit; a flow path between the third switching module and the chromatographic column is sequentially connected with the pressure control module, the shunt module and the emptying pipe, an outlet of the first pump is communicated with the emptying pipe, an inlet of the fourth switching module is communicated with outlets of the two migration pipes, one outlet is connected with the first pump, and the other outlet is connected with the emptying pipe;
two inlets of a fifth switching module and a sixth switching module are respectively communicated with carrier gas and zero gas, an outlet of the fifth switching module is sequentially communicated with a pressure control module, a flow path (between a chromatographic column and a mobility spectrometry analysis unit), an outlet of the sixth switching module is connected with two flow paths, each flow path is provided with a pressure control module, and the flow paths are communicated with a floating gas inlet of a migration pipe;
the first switching module and the sixth switching module are all electromagnetic three-way valves, valves are electromagnetic valves, the flow control module uses EFC, and the pressure control module uses EPC.
As shown in fig. 1, the mobility spectrometry detection method with multiple sampling modes in the embodiment of the present invention, that is, the working method of the detection apparatus in the embodiment of the present invention, includes:
a mobility spectrometry negative pressure sample injection mode, specifically, sample gas sequentially passes through the valve, the two migration pipes and the first pump;
a mobility spectrometry quantitative loop (positive pressure) sample injection mode, a chromatography-mobility spectrometry quantitative loop (positive pressure) sample injection mode and a chromatography-mobility spectrometry enrichment tube (positive pressure) sample injection mode which respectively comprise a pre-pumping state, a sampling state, a sample injection state and a back-flushing state; the pre-pumping state is that a sample sequentially passes through a sampling pipe, a second switching module, a flow control module and a second pump; the sampling state is that a multi-way valve is used for switching, and sample gas sequentially passes through a sampling pipe, a quantitative ring, an enrichment pipe, a first switching module, a second switching module, a flow control module and a second pump; the back flushing state is that a multi-way valve is used for switching, and carrier gas sequentially passes through a first switching module, an enrichment pipe, a quantitative ring, a sampling pipe, a second switching module and a second pump;
in a mobility spectrometry quantitative loop sample injection mode, the sample injection state is that a multi-way valve is used for switching, and carrier gas directly enters the two migration tubes after passing through the quantitative loop, the first damping column and the third switching module in sequence;
in a chromatogram-mobility spectrometry quantitative loop sample injection mode, a sample injection state is that carrier gas enters two migration tubes after sequentially passing through a quantitative loop, a first damping column, a third switching module and a chromatographic column;
in a sample introduction mode of the chromatographic-mobility spectrometry enrichment tube, carrier gas sequentially passes through the enrichment tube, the pre-column, the third switching module and the chromatographic column and then enters the two migration tubes;
in the three positive pressure sampling modes, the first pump is closed, and the fourth switching module is switched, so that the outlet (not passing through the first pump) of the migration pipe is communicated with the evacuation port;
in various sample introduction modes, a differential pressure sensor is utilized to obtain the pressure difference between the two migration pipes, and the pressure of the floating gas entering the two migration pipes is adjusted to ensure that the pressures in the two migration pipes are equal.
Claims (10)
1. The device comprises a multi-way valve, a quantitative ring, an enrichment tube, a chromatographic column and a mobility spectrum analysis unit, wherein an outlet of the chromatographic column is communicated with the mobility spectrum analysis unit; the device is characterized in that the mobility spectrometry detection device with multiple sample injection modes further comprises:
the multi-way valve comprises a first switching module and a second switching module, wherein the first switching module is used for enabling a multi-way valve port to be selectively communicated with the second switching module or carrier gas, and the second switching module is used for enabling a flow control module to be selectively communicated with the first switching module or a sample inlet pipe;
the sample inlet pipe is communicated with the mobility spectrum analysis unit through a valve, the mobility spectrum analysis unit comprises two parallel migration pipes, and the two migration pipes work according to a positive mode and a negative mode;
the two ends of the first damping column and the two ends of the pre-column are respectively connected with the ports of the multi-way valves, and when the multi-way valves are switched, carrier gas sequentially flows through the quantitative ring, the first damping column and the third switching module;
the third switching module is used for enabling the sample gas discharged from the first damping column to be selectively communicated with the chromatographic column or directly communicated with the mobility spectrometry analysis unit;
the first pump is respectively communicated with the outlets of the two transfer pipes, and the second pump is arranged at the downstream of the flow control module.
2. The apparatus of claim 1, further comprising:
one end of the second damping column is connected with the port of the multi-way valve, and the other end of the second damping column is communicated with carrier gas;
and the two ends of the pre-column are connected with the ports of the multi-way valves, and when the multi-way valves are switched, the carrier gas sequentially flows through the enrichment pipe, the pre-column and the third switching module.
3. The apparatus of claim 2, further comprising:
one end of the emptying pipe is connected with the port of the multi-way valve;
shunt module and pressure control module, the evacuation pipe communicates in proper order shunt module, pressure control module and the flow path between third switching module and chromatographic column.
4. The apparatus according to claim 3, wherein the multi-way valve is a fourteen-way valve, the first port communicates with the sample injection tube, the second port and the fifth port communicate with two ends of the quantitative ring, the third port and the twelfth port communicate with the carrier gas, the fourth port communicates with the first damping column, the sixth port and the thirteenth port communicate with two ends of the enrichment tube, the seventh port and the eleventh port communicate with two ends of the pre-column, the eighth port communicates with the evacuation tube, the ninth port communicates with the second damping column, the tenth port communicates with an inlet of the third switching module, and the fourteenth port communicates with the first switching module.
5. The apparatus of claim 1, further comprising:
and the fourth switching module is used for enabling the outlets of the two transfer pipes to be selectively communicated with the inlet or the emptying port of the first pump.
6. The apparatus of claim 1, further comprising:
the device comprises a fifth switching module and a sixth switching module, wherein the fifth switching module is used for enabling zero gas or carrier gas to be selectively used as tail blowing gas, and the sixth switching module is used for enabling the zero gas or carrier gas to be selectively used as floating gas.
7. The apparatus of claim 1, further comprising:
the pressure sensor obtains the pressure in one transfer pipe, and the differential pressure sensor obtains the difference between the pressures in the two transfer pipes.
8. The method for detecting the mobility spectrometry detection device with multiple sample injection modes according to any one of claims 1 to 7, wherein the method for detecting comprises the following steps:
a mobility spectrometry negative pressure sample injection mode, specifically, sample gas sequentially passes through the valve, the two migration pipes and the first pump;
a mobility spectrometry quantitative loop sampling mode, a chromatography-mobility spectrometry quantitative loop sampling mode and a chromatography-mobility spectrometry enrichment tube sampling mode which respectively comprise a pre-pumping state, a sampling state and a back-flushing state; the pre-pumping state is that a sample sequentially passes through a sampling pipe, a second switching module, a flow control module and a second pump; the sampling state is that a multi-way valve is used for switching, and sample gas sequentially passes through a sampling pipe, a quantitative ring, an enrichment pipe, a first switching module, a second switching module, a flow control module and a second pump; the back flushing state is that the multi-way valve is used for switching, and the carrier gas sequentially passes through the first switching module, the enrichment pipe, the quantitative ring, the sampling pipe, the second switching module and the second pump.
9. The detection method according to claim 8, wherein in the mobility spectrometry quantitative loop sample injection mode, the sample injection state is that a multi-way valve is used for switching, and carrier gas directly enters the two migration tubes after sequentially passing through the quantitative loop, the first damping column and the third switching module;
in a chromatogram-mobility spectrometry quantitative loop sample injection mode, a sample injection state is that carrier gas enters two migration tubes after sequentially passing through a quantitative loop, a first damping column, a third switching module and a chromatographic column;
in the sample introduction mode of the chromatographic-mobility spectrometry enrichment tube, the sample introduction state is that carrier gas enters the two migration tubes after sequentially passing through the enrichment tube, the pre-column, the third switching module and the chromatographic column.
10. The detection method according to claim 8, wherein the pressure difference between the two transfer tubes is obtained by a pressure difference sensor, and the drift pressure entering the two transfer tubes is adjusted so that the pressures in the two transfer tubes are equal.
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