CN217112203U - Sample introduction and analysis system for trace multi-component volatile organic compound - Google Patents
Sample introduction and analysis system for trace multi-component volatile organic compound Download PDFInfo
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- CN217112203U CN217112203U CN202220856069.4U CN202220856069U CN217112203U CN 217112203 U CN217112203 U CN 217112203U CN 202220856069 U CN202220856069 U CN 202220856069U CN 217112203 U CN217112203 U CN 217112203U
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Abstract
The utility model discloses a trace multicomponent volatility organic matter advances appearance and analytic system belongs to analytical chemistry technical field. The system comprises a pre-concentration system and an analysis system, wherein the pre-concentration system comprises a sample gas sampling unit and a gas pre-concentration unit, the analysis system comprises a ten-way valve and two quantitative rings connected with the ten-way valve, and the quantitative rings are connected with a passage to form a first analysis passage and a second analysis passage which are independent. The utility model adopts a system composed of a multi-mode sample inlet or a temperature programming sample inlet to pre-concentrate trace multi-component volatile organic compounds, replaces a pre-concentration instrument in the prior art, obviously reduces the cost, saves the space and has short path; the utility model discloses can select the chromatographic column who is applicable to light component and heavy ends separation alone, realize the quantitative and qualitative analysis of trace multicomponent volatile organic compounds.
Description
Technical Field
The utility model belongs to the technical field of analytical chemistry, concretely relates to appearance and analytic system are advanced to trace multicomponent volatile organic compounds.
Background
Trace means chemically a very small amount, meaning a material present in the composition of matter in an amount of less than one part per million, and trace gases are atmospheric gases having a concentration of less than 10 parts per million -6 The seed of (1). Means that only one molecule to be investigated, such as CO or N in the atmosphere, is present in a total of 1,000,000 molecules 2 O、SO 2 、O 3 、NO、NO 2 、CH 4 、NH 3 、H 2 S, halides, volatile organic compounds, etc. are all trace gases.
The existing monitoring objects of Volatile Organic Compounds (VOCs) in the ambient air comprise alkanes, alkenes, aromatic hydrocarbons, oxygen-containing volatile organic compounds, halogenated hydrocarbons and the like, the content of the volatile organic compounds is mostly trace level, the existing detection instrument such as a gas chromatograph cannot meet the detection requirement of the trace level, the existing method is to adopt a pre-concentrator to carry out pre-concentration treatment before analysis and detection, but the pre-concentrator on the market is expensive and large in volume, and the gas path needs to be subjected to heat preservation treatment after pre-concentration.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a trace multicomponent volatility organic matter advances appearance and analytic system, the low multicomponent gaseous problem of high price, bulky of preconcentration appearance of adopting when concentrating of VOCs who has solved current content.
In order to solve the technical problem, the purpose of the utility model is realized through the following technical scheme: a sample introduction and analysis system for trace multi-component volatile organic compounds comprises a pre-concentration system and an analysis system, wherein the pre-concentration system comprises a sample gas sample introduction unit and a gas pre-concentration unit, and the sample gas sample introduction unit, the gas pre-concentration unit and the analysis system are respectively connected with a six-way valve A;
the sample gas sampling unit comprises a sample gas sampling channel and an emptying channel, wherein the sample gas sampling channel and the emptying channel are connected with a four-way valve together, and the four-way valve is connected with the six-way valve A in series;
the gas preconcentration unit comprises a multi-mode sample inlet or a temperature programmed sample inlet, a carrier gas inflow channel and a sample gas outflow channel, and the inlet and outlet ends of the multi-mode sample inlet or the temperature programmed sample inlet, the carrier gas inflow channel and the sample gas outflow channel are respectively connected with the six-way valve A;
the analysis system comprises a ten-way valve and two quantitative rings connected with the ten-way valve, wherein each quantitative ring is connected with a passage to form a first analysis passage and a second analysis passage which are independent, and the first analysis passage is formed by sequentially connecting a six-way valve B, a pre-separation column, a six-way valve B, a first separation column, a six-way valve B and a first detector in series;
the second analytical path includes, in order, a second separation column and a second detector.
Further, an MFC is arranged on the evacuation channel.
Further, an MFC is provided on the sample gas outflow channel.
Further, a pressure reducing valve and a stop valve are arranged on the sample gas sampling channel.
Further, the first detector is a FID detector and the second detector is a mass spectrometer or FID detector.
Compared with the prior art, the utility model has the advantages of it is following and beneficial effect: the utility model discloses a trace multicomponent volatile organic compounds advances appearance and analytic system, trace multicomponent volatile organic compounds pass through the multi-mode introduction port of gas preconcentration unit or in the bushing pipe of procedure heating introduction port, cool off earlier and adsorb trace volatile organic compounds, and procedure heating brings the volatile organic compounds that adsorb in the bushing pipe into analytic system under the effect of carrier gas and detects again; the utility model discloses a system that multi-mode introduction port or temperature programming introduction port are constituteed carries out preconcentration to trace multicomponent volatile organic compounds, has replaced the preconcentration appearance among the prior art, is showing the cost is reduced, and this system practices thrift space, route weak point, need not carry out heat preservation to multicomponent volatile organic compounds after the preconcentration and handle. The utility model is suitable for a detection and analysis of trace multicomponent volatile organic compounds, the component of the required analysis of multicomponent gas divide into two sets of analyses according to carbonaceous quantity, and the analysis of light and heavy component is noiseless mutually, when light component analysis, utilizes the blowback technique to concentrate the heavy component and take precedence out the peak, has avoided the heavy component to stop at light component separation post, has improved analysis efficiency.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Fig. 2 is the gas sample introduction route schematic diagram of the pre-concentration system of the present invention.
Fig. 3 is the gas sampling path schematic diagram of the pre-concentration system of the present invention.
Fig. 4 is a schematic diagram of a blowback route of the analysis system of the present invention.
Wherein, 1-sample gas sample injection unit; 2-a gas pre-concentration unit; 3-a four-way valve; 4-six way valve a; 5-sample gas sample introduction channel; 6-evacuation of the channel; 7-carrier gas inflow channel; 8-sample gas outflow channel; 9-a pressure reducing valve; 10-a stop valve; 11-ten way valve; 12-a quantification ring; 13-six way valve B; 14-a pre-separation column; 15-a first separation column; 16-a first detector; 17-a second separation column; 18-second detector.
Detailed Description
The present invention is further described with reference to the following drawings and embodiments, and the protection scope of the present invention is not limited to the following:
as shown in fig. 1, a sample introduction and analysis system for trace multi-component volatile organic compounds includes a pre-concentration system and an analysis system, wherein the pre-concentration system includes a sample gas sample introduction unit 1 and a gas pre-concentration unit 2, and the sample gas sample introduction unit 1, the gas pre-concentration unit 2 and the analysis system are respectively connected to a six-way valve A4;
the sample gas sampling unit 1 comprises a sample gas sampling channel 5 and an emptying channel 6, wherein the sample gas sampling channel 5 and the emptying channel 6 are connected with a four-way valve 3 together, and the four-way valve 3 is connected with a six-way valve A4 in series; as a preferred scheme, a mass flow controller (MFC for short) is arranged on the evacuation channel 6, a pressure reducing valve 9 and a stop valve 10 are arranged on the sample gas sampling channel 5, and the gas sampling unit 1 is used for reducing the pressure of the sample gas and controlling the evacuation flow;
the gas preconcentration unit 2 comprises a multi-mode sample inlet (MMI) or a programmed temperature sample inlet (PTV), a carrier gas inflow channel 7 and a sample gas outflow channel 8, wherein the inlet and outlet ends of the MMI or the PTV are respectively connected with a six-way valve A4; the carrier gas inflow channel 7 and the sample gas outflow channel 8 are respectively connected with the six-way valve A4, and the sample gas outflow channel 8 is provided with an MFC for adjusting and controlling the flow of the sample gas through the MMI or the PTV. The gas pre-concentration unit 2 is made by adding an adsorbent material in the liner of the MMI or PTV, specifically selected for the trace amount of volatile organic gas components that need to be pre-concentrated, and the material is prior art and is not cumbersome here. Firstly, cooling gas through a cold trap to ensure that the trace target component volatile organic compounds are adsorbed on the adsorbing material, and then opening a program to heat up so as to bring the trace target component volatile organic compounds adsorbed in the liner tube into an analysis system under the action of carrier gas.
The analysis system comprises a ten-way valve 11 and two quantitative rings 12 connected with the ten-way valve 11, wherein each quantitative ring 12 is connected with a passage to form a first analysis passage and a second analysis passage which are independent, and the first analysis passage is formed by sequentially connecting a six-way valve B13, a pre-separation column 14, a six-way valve B13, a first separation column 15, a six-way valve B13 and a first detector 16 in series; the first detector 16 is a hydrogen flame ionization detector (FID detector for short). The analysis gas enters the first analysis passage under the action of the carrier gas, and the six-way valve B13 is adjusted to enable C in the analysis gas to be 2 -C X When the target component passes through an air path formed by the six-way valve 14, the first separation column 15 and the six-way valve B13, the six-way valve 14 is switched to perform blowback, and the target component enters the first detector 16 through a blowback route to be detected and analyzed.
The second analysis path comprises a second separation column 17 and a second detector 18 in sequence, and the second detector 18 is a mass spectrometry or FID detector. Separating at least the components with carbon number more than X by a second separation column 17.
The utility model discloses can detect the multicomponent volatile organic compounds of trace, for example 57 kinds of volatile organic compounds (PAMs) stipulated in the current key area ambient air volatile organic compounds monitoring scheme now with containing trace ethane, ethylene, propane, propylene, isobutane, normal butane, acetylene, benzene, toluene, ethylbenzene, styrene in the sample gas further illustrate for the example the utility model discloses a theory of operation.
As shown in fig. 1, the pressure reducing valve 9 and the stop valve 10 are opened, the sample gas to be detected is introduced into the sample gas sampling channel 5, the sample gas is evacuated through the evacuation channel 6 via a-b in the four-way valve 3, and the gas flow is controlled by the MFC arranged on the evacuation channel 6; after the gas flow is stable, the a-c of the four-way valve 3 is communicated; adsorbing material glass beads are added into a liner tube of the MMI, carrier gas is introduced into a carrier gas inflow channel 7 and is communicated with e-f of a six-way valve A4, sample gas flows to the six-way valve A4 and flows to the MMI through the e-f of the six-way valve A4, a cold trap button of the MMI is opened, volatile organic matters of trace target components in the sample gas are adsorbed on the glass beads, the adsorbed sample gas is discharged from an outflow channel 8 through j-k of the six-way valve A4, the flow rate and time of the sample gas passing through the MMI are controlled through an MFC arranged on the outflow channel 8, and the gas flows in the direction indicated by an arrow in figure 2.
When the multi-component volatile organic compound in the MMI reaches the detectable concentration, the stop valve 10 is closed, a-c in the four-way valve 3 is disconnected, i-j in the six-way valve 4 is communicated, the temperature of a programmed temperature rise sample inlet of the MMI is set, carrier gas in the carrier gas inflow channel 7 flows to the MMI through the i-j in the six-way valve 4, the volatile organic compound adsorbed in the liner tube is changed into gas at high temperature, the gas flows to the analysis system through the f-h channel in the six-way valve 4 under the action of the carrier gas, and the gas flows in the direction indicated by the arrow in figure 3.
After the quantitative rings 12 are filled with the gas to be analyzed, the ten-way valve 11 is adjusted to communicate the carrier passages corresponding to the quantitative rings 12, the carrier gas is introduced into the ten-way valve 11, the gas to be analyzed enters the first analysis passage under the action of the carrier gas, namely, the gas to be analyzed sequentially passes through the six-way valve B13, the pre-separation column 14, the six-way valve B13 and the first separation column 15, the six-way valve B13 is adjusted to enable target components of C2-C3 in the gas to pass through a gas passage formed by the six-way valve B13, the first separation column 15 and the six-way valve B13, the six-way valve 14 is switched to perform back blowing, the gas enters the first detector FID (benzene, toluene, ethylbenzene and styrene flow out as a peak first) through the back blowing route shown in fig. 4, and the components for quantitative analysis are ethane, ethylene, propane, propylene, isobutane, n-butane and acetylene.
Under the action of carrier gas, the analysis gas in the other quantitative ring 12 enters a second analysis passage, benzene, toluene, ethylbenzene and styrene are separated by a second separation column 17, the separated components enter a second detector mass spectrum 18 for quantitative analysis, and C2-C3 cannot be effectively separated and cannot be quantitatively analyzed on the mass spectrum through solvent delay.
The above, only be the embodiment of the preferred of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, which are designed to be replaced or changed equally, all covered within the protection scope of the present invention.
Claims (5)
1. The sample introduction and analysis system for trace multi-component volatile organic compounds is characterized by comprising a pre-concentration system and an analysis system, wherein the pre-concentration system comprises a sample gas sample introduction unit (1) and a gas pre-concentration unit (2), and the sample gas sample introduction unit (1), the gas pre-concentration unit (2) and the analysis system are respectively connected with a six-way valve A (4);
the sample gas sampling unit (1) comprises a sample gas sampling channel (5) and an emptying channel (6), wherein the sample gas sampling channel (5) and the emptying channel (6) are connected with a four-way valve (3) together, and the four-way valve (3) is connected with a six-way valve A (4) in series;
the gas preconcentration unit (2) comprises a multi-mode sample inlet or a temperature programming sample inlet, a carrier gas inflow channel (7) and a sample gas outflow channel (8), and the inlet and outlet ends of the multi-mode sample inlet or the temperature programming sample inlet, the carrier gas inflow channel (7) and the sample gas outflow channel (8) are respectively connected with the six-way valve A (4);
the analysis system comprises a ten-way valve (11) and two quantitative rings (12) connected with the ten-way valve (11), wherein each quantitative ring (12) is connected with a passage to form a first analysis passage and a second analysis passage which are independent, and the first analysis passage is formed by sequentially connecting a six-way valve B (13), a pre-separation column (14), a six-way valve B (13), a first separation column (15), the six-way valve B (13) and a first detector (16) in series; the second analysis path comprises, in turn, a second separation column (17) and a second detector (18).
2. A trace amount multi-component voc sampling and analysis system according to claim 1, wherein the evacuation channel (6) is provided with MFC.
3. A trace amount multi-component voc sampling and analysis system according to claim 1, wherein the sample gas outflow channel (8) is provided with MFC.
4. The system for sampling and analyzing trace amounts of multi-component volatile organic compounds according to claim 1, wherein a pressure reducing valve (9) and a stop valve (10) are disposed on the sample gas sampling channel (5).
5. The system for trace sampling and analysis of multi-component volatile organic compounds according to claim 1, wherein the first detector (16) is a FID detector and the second detector (18) is a mass spectrometer or FID detector.
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| CN202220856069.4U CN217112203U (en) | 2022-04-13 | 2022-04-13 | Sample introduction and analysis system for trace multi-component volatile organic compound |
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| CN202220856069.4U CN217112203U (en) | 2022-04-13 | 2022-04-13 | Sample introduction and analysis system for trace multi-component volatile organic compound |
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| CN202220856069.4U Active CN217112203U (en) | 2022-04-13 | 2022-04-13 | Sample introduction and analysis system for trace multi-component volatile organic compound |
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