CN211179670U - VOC on-line extraction enrichment analysis system - Google Patents
VOC on-line extraction enrichment analysis system Download PDFInfo
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- CN211179670U CN211179670U CN201922158291.8U CN201922158291U CN211179670U CN 211179670 U CN211179670 U CN 211179670U CN 201922158291 U CN201922158291 U CN 201922158291U CN 211179670 U CN211179670 U CN 211179670U
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Abstract
The utility model discloses a VOC on-line extraction enrichment analysis system, which comprises a sample chamber, a heat preservation box, an enrichment column box, a flowmeter, a vacuum pump and a sample disposal chamber which are connected in sequence through connecting pipelines, wherein the enrichment column box is connected with an analysis column box, a detector and a controller; the enrichment column box comprises a first enrichment column box, a second enrichment column box and a third enrichment column box which are sequentially connected, the analysis column box comprises a first analysis column box, a second analysis column box and a third analysis column box which are sequentially connected, the first analysis column box is connected with the third enrichment column box, and the heat preservation box is respectively connected with the first electronic pressure meter and the sample processor through connecting pipelines. The extraction enrichment column of the utility model has simple and convenient installation and connection, strong universality and suitability for all VOC sample analysis which can be analyzed by gas chromatography; the whole enrichment system can be independent of a chromatographic analysis system, is provided with an electronic control system, can be used for automatically collecting outdoor gas samples, and can also be used for on-line extraction, enrichment and analysis of on-site VOC.
Description
Technical Field
The utility model relates to an environmental monitoring field especially relates to a VOC on-line extraction enrichment analytic system.
Background
In the fields of petrochemical and environmental monitoring, the solid phase extraction-thermal desorption-analysis technology is the most common measurement and analysis technology, has wide application, and can be used for off-line sampling analysis and on-line sampling analysis. The solid phase extraction is a key step of sample collection and enrichment, and a proper enrichment material needs to be searched and a proper enrichment tube needs to be manufactured so as to ensure that all target components in the sample gas are adsorbed and are not interfered by the background of the sample gas; although the dehydration treatment and heavy component back flushing technology can solve most of the background interference problems, when the mass spectrum detector is adopted in the method HJ 1010-2018, the signal attenuation of the mass spectrometer is still too fast, and the maintenance frequency needs to be increased to ensure the reliability and stability of continuous operation data; in addition, the thermal desorption/thermal desorption conditions require a large amount of recovery experimental data to verify the reliability of the method, time and labor are wasted, and target components are easily interfered by the background of the sample and the cleanliness of the pipeline, so that the linear range is narrow, and the stability and the repeatability are poor.
CN203870078U discloses a gas chromatography separation system, couples adsorption desorption device, sampling pump and miniature chromatogram through six-way valve, has realized the online instant determination of gas sample, and response speed is fast, and the device can independently operate, and portable is favorable to handling and handling the incident. However, in the separation system, the adsorption and desorption device is still the key for enriching the target components, the sample directly enters the adsorption and desorption device, the interference of the sample background cannot be eliminated, the selection and condition optimization of the adsorption material are complex, and the requirement on the temperature of the cold trap is high.
Solid phase extraction filling materials, especially some high polymer materials such as carbon fiber and nano materials, although good in adsorption performance to specific components, are expensive and have harsh adsorption and desorption conditions, due to expansion with heat and contraction with cold in the repeated heating process, the spacing between adsorption particles in the adsorption tube is not reproduced, so that the repeatability and reproducibility of the measurement result are not high, and the reliability of the measurement result is affected. Therefore, improvements in the prior art are needed.
SUMMERY OF THE UTILITY MODEL
In view of the above disadvantages of the prior art, a VOC online extraction enrichment analysis system is now provided, which solves the problems of the prior art, such as complexity, sample extraction enrichment susceptible to sample background interference, harsh analytical (thermal analytical) conditions, narrow linear range, and poor stability and repeatability.
In order to achieve the above and other related objects, the present invention provides an online extraction, enrichment and analysis system for VOC, comprising a sample chamber, a heat preservation box, an enrichment column box, a flowmeter, a vacuum pump, and a sample disposal chamber, which are connected in sequence by connecting pipelines, wherein the enrichment column box is connected to an analysis column box, a detector and a controller; the sample chamber, the heat preservation box, the enrichment column box, the analysis column box, the flow meter, the vacuum pump and the sample disposal chamber are all controlled by a controller, the enrichment column box comprises a first enrichment column box, a second enrichment column box and a third enrichment column box which are sequentially connected, the analysis column box comprises a first analysis column box, a second analysis column box and a third analysis column box which are sequentially connected, the first analysis column box is connected with the third enrichment column box, and the heat preservation box is respectively connected with the first electronic pressure meter and the sample disposal device through connecting pipelines; the three enrichment column boxes and the three analysis column boxes are independently controlled in temperature respectively, and after entering from the sample chamber, a gas sample is enriched and analyzed through the enrichment column boxes and the analysis column boxes and displayed on a display screen of the controller.
The VOC on-line extraction, enrichment and analysis system is characterized in that a third rotary valve is arranged in the heat preservation box and connected to a first electronic pressure gauge and a sample processor through connecting pipelines.
Foretell VOC on-line extraction enrichment analytic system, be equipped with first enrichment post in the first enrichment post box, be equipped with second enrichment post and two logical in the second enrichment post box, be equipped with third enrichment post and first ooff valve in the third enrichment post box, a plurality of enrichment posts, two logical and ooff valve pass through the connecting line and connect.
Foretell online extraction enrichment analytic system of VOC, be equipped with first analytical column and second rotary valve in the first analytical column box, be equipped with second analytical column and two-way in the second analytical column box, be equipped with the third analytical column in the third analytical column box, a plurality of analytical columns, two-way and rotary valve pass through connecting line and connect, just first rotary valve in the third enrichment column box is connected with the first analytical column in the first analytical column box.
In the online VOC extraction, enrichment and analysis system, the second rotary valve in the first analysis column box is connected with the second electronic pressure gauge through the connecting pipeline.
According to the VOC online extraction, enrichment and analysis system, the two-way is arranged in the second enrichment column box, and the second enrichment column is arranged between the two-way.
The utility model discloses owing to use above technical scheme, make its beneficial effect who has be:
1. the installation and connection of the extraction enrichment column are very simple and convenient, the universality is very strong, and the method is suitable for all VOC sample analysis which can be analyzed by gas chromatography;
2. the whole enrichment system can be independent of a chromatographic analysis system and is provided with an electronic control system;
3. the device can be used for automatically collecting outdoor gas samples and can also be used for on-site VOC (volatile organic compounds) on-line extraction, enrichment and analysis.
Drawings
FIG. 1 is a connection structure diagram of the on-line VOC extraction, enrichment and analysis system of the present invention;
FIG. 2 is a map of a first detector of the VOC on-line extraction, enrichment and analysis system of the present invention during analysis;
fig. 3 is a spectrum of the second detector of the online VOC extraction enrichment analysis system during analysis.
The reference numerals in the specification are as follows:
the device comprises a sample chamber 1, an insulation box 2, an enrichment column box 3, a flow meter 4, a vacuum pump 5, a sample handler 6, an analysis column box 7, a detector 8, a controller 9, a two-way valve 10, a first electronic pressure meter 20, a second electronic pressure meter 30, a third rotary valve 21, a first enrichment column box 31, a second enrichment column box 32, a third enrichment column box 33, a first analysis column box 71, a second analysis column box 72, a third analysis column box 73, a first enrichment column 311, a second enrichment column 321, a third enrichment column 331, a first rotary valve 332, a first analysis column 711, a second rotary valve 712, a second analysis column 721 and a third analysis column 731.
Detailed Description
The following description is provided for illustrative purposes, and other advantages and features of the present invention will become apparent to those skilled in the art from the following detailed description.
The structure, ratio, size and the like shown in the drawings attached to the present specification are only used for matching with the content disclosed in the specification, so as to be known and read by people familiar with the technology, and are not used for limiting the limit conditions which can be implemented by the present invention, so that the present invention does not have the substantial significance in the technology, and any structure modification, ratio relationship change or size adjustment should still fall within the scope which can be covered by the technical content disclosed by the present invention without affecting the efficacy which can be produced by the present invention and the purpose which can be achieved by the present invention. Meanwhile, the terms such as "upper", "lower", "left", "right", "middle" and "one" used in the present specification are for convenience of description, and are not intended to limit the scope of the present invention, and changes or adjustments of the relative relationship thereof may be made without substantial technical changes, and the present invention is also regarded as the scope of the present invention.
The first embodiment of the utility model provides a VOC on-line extraction enrichment analysis system, as shown in figure 1, comprising a sample chamber 1, a heat preservation box 2, an enrichment column box 3, a flowmeter 4, a vacuum pump 5 and a sample handler 6 which are connected in sequence through connecting pipelines, wherein the enrichment column box 3 is connected with an analysis column box 7, a detector 8 and a controller 9; the enrichment column box 3 comprises a first enrichment column box 31, a second enrichment column box 32 and a third enrichment column box 33 which are sequentially connected, a first enrichment column 311 is arranged in the first enrichment column box 31, a second enrichment column 321 and a two-way valve 10 are arranged in the second enrichment column box 32, a third enrichment column 331 and a first rotary valve 332 are arranged in the third enrichment column box 33, and the enrichment columns, the two-way valve 10 and the rotary valve are connected through connecting pipelines; the analytical column box 7 comprises a first analytical column box 71, a second analytical column box 72 and a third analytical column box 73 which are sequentially connected, a first analytical column 711 and a second rotary valve 712 are arranged in the first analytical column box 71, a second analytical column 721 and a two-way valve 10 are arranged in the second analytical column box 72, a third analytical column 731 is arranged in the third analytical column box 73, the plurality of analytical columns, the two-way valve 10 and the rotary valve are connected through connecting pipelines, and a first rotary valve 332 in the third enrichment column box 33 is connected with the first analytical column 711 in the first analytical column box 71; and the third stopcock 21 in the thermal insulation box 2 is connected to the first electronic pressure gauge 20 and the sample handler 6 through connection lines, respectively, and the second stopcock 712 is connected to the second electronic pressure gauge 30 through connection lines.
In addition, two-way ports 10 are provided in the second enrichment column cassette 32, and the second enrichment column 321 is provided between the two-way ports 10.
In specific use, after the heat preservation box 2, the enrichment column box 3 and the analysis column box 7 are installed, two ports of the third rotary valve 21 are connected with an inlet end of the first enrichment column 311, an outlet end of the first enrichment column 311 is connected with an inlet of the second enrichment column 321 through one of the two-way valves 10, an outlet end of the second enrichment column 321 is connected with an inlet of the third enrichment column 331 through the other two-way valve 10, an outlet end of the third enrichment column 331 is connected with the first rotary valve 332, one end of the first rotary valve 332 is directly connected with an inlet of the first analysis column 711, an outlet of the first analysis column 711 is connected with the second rotary valve 712, one end of the second rotary valve 712 is directly connected with an inlet end of the second analysis column 721, an outlet end of the second analysis column 721 is connected with an inlet end of the third analysis column 731 through the two-way valves 10, an outlet end of the third analysis column 731 is directly connected with the detector 8, and the other end of the second rotary valve 712 is connected with the second electronic 30, the other end of the first stopcock 332 is connected to the inlet end of the flow meter 4 through a connecting line, the outlet end of the flow meter 4 is connected to the inlet end of the vacuum pump 5, the outlet end of the vacuum pump 5 is connected to one inlet of the sample handler 6, the third port of the third stopcock 21 is connected to the first electronic pressure gauge 20 through a connecting line, and the fourth port is connected to the second inlet of the sample handler 6.
The sample chamber 1 can be connected with an air bag, a Suma tank and the like, and can also be directly connected with the atmosphere for sampling; the first enrichment column 311, the second enrichment column 321 and the third enrichment column 331 are respectively installed in a first enrichment column box 31, a second enrichment column box 32 and a third enrichment column box 33 which can independently control the temperature; the three enrichment columns can be any commercial chromatographic column or self-made chromatographic column, the first enrichment column 311 is a nonpolar column, the second enrichment column 321 is a medium-polarity column, the third enrichment column 331 is a strong-polarity column, the temperature of the first enrichment column box 31, the temperature of the second enrichment column box 32 and the temperature of the third enrichment column box 33 are controlled independently, and the temperature control ranges are all-50 ℃ to 350 ℃; the first analytical column 711, the second analytical column 721 and the third analytical column 731 are respectively arranged in a first analytical column box 71, a second analytical column box 72 and a third analytical column box 73 which can independently control the temperature, the first analytical column 711, the second analytical column 721 and the third analytical column 731 can be any commercial chromatographic column or a self-made chromatographic column, the first analytical column 711 is a non-polar column, the second analytical column 721 is a medium-polar column, the third analytical column 731 is a strong-polar column, the first analytical column box 71, the second analytical column box 72 and the third analytical column box 73 are independently controlled the temperature, and the temperature control ranges from 30 ℃ to 350 ℃; the connecting pipelines are all inert pipes with the inner diameter of 0.5-3 mm, and can resist high temperature and high pressure, the high pressure range is 0-600 Psi, and the high temperature range is-50 ℃ to 350 ℃; the two through-holes 10 in the second enrichment column box 32 are zero dead volume, inert and capable of resisting high temperature and high pressure, the high pressure resistant range is 0-600 Psi, and the high temperature resistant range is-50-350 ℃; the first rotary valve 332, the second rotary valve 712 and the third rotary valve 21 are automatic control valves which have zero dead volume, are inert and can resist high temperature and high pressure, the high pressure resistance ranges are all 0-600 Psi, and the high temperature resistance ranges are all-50-350 ℃; the detector 8 may be any detector 8 useful for chromatographic analysis, including a hydrogen ion flame detector, a thermal conductivity detector, a sulfur chemiluminescence detector, a nitrogen chemiluminescence detector, a flame photometric detector, a helium ionization detector, or the like, or may be an infrared, laser, or the like detector or a combination of two or more thereof; the controller 9 is provided with a microcomputer and an electronic display screen, can automatically control the sample chamber 1, can independently and automatically control the temperature of the heat preservation box 2, the three enrichment column boxes and the three analysis column boxes, can automatically control the selective communication positions of the three rotary valves, can automatically control the flow meter 4, the first electronic pressure gauge 20 and the second electronic pressure gauge 30, can automatically control the working states of the vacuum pump 5 and the sample processor 6, and can realize all control programs through the chromatographic workstation and transmit signals to the chromatographic workstation.
When the system is used for carrying out online extraction enrichment analysis on atmosphere, chemical tail gas or process gas and the like, the gas flow of a normal-pressure gas sample can be adjusted through the vacuum pump 5 and the flow meter 4 so as to obtain the optimal enrichment effect; for a pressurized gas sample, the sample can directly pass through the chromatographic enrichment column, and the flow rate of the gas passing through the chromatographic enrichment column is controlled by the post-column flow meter 4 so as to obtain the optimal enrichment effect. For different sample gas analysis, the enrichment column can be any one of three column types or any combination of two of the three column types, and the target components are ensured to be completely enriched; the analytical column can be any one of three column types or any combination of two of the three column types, and the detector 8 selects according to the characteristics of the target components to ensure that the target components can be accurately analyzed; each sample analysis program has a back flushing function and a pipeline purging function of the enrichment column and the analysis column, so that the sample background (water and air) is not influenced on the detection result, and no heavy component residue influence is generated in the next analysis. When the standard sample and the actual sample are measured, the detection of each component is less than 0.1nmol/mol, the accuracy is less than +/-10 percent, and the precision is less than 10 percent. The consistency of the analysis result of the target component and the actual content is very good.
The general VOC on-line extraction enrichment-analysis system has the following three working modes:
(one) enrichment state: when the sample chamber 1 is connected with the first enrichment column 311 through the third rotary valve 21, the first electronic pressure gauge 20 and the second electronic pressure gauge 30 are in a closed state, and the outlet of the third enrichment column 331 is connected with the sample processor 6 through the first rotary valve 332, the flow meter 4 and the vacuum pump 5, the system is in a target component enrichment state, all target components are collected by the three enrichment columns, and background gas in an analysis sample is collected by the sample processor 6 and then discharged;
(II) analyzing the state: when the first electronic pressure gauge 20 is connected with the first enrichment column 311 through the third rotary valve 21, the first electronic pressure gauge 20 is in an open state, the second electronic pressure gauge 30 is in a closed state, and the outlet of the third enrichment column 331 is connected with the first analysis column inlet through the first rotary valve 332, the device is in a target component analysis state, all target components are heated, analyzed from the three enrichment columns and blown to the second analysis column 721 and the third analysis column 731 through the first analysis column 711;
(III) analyzing a back flushing state: when the sample processor 6 is connected with the first enrichment column 311 through the third rotary valve 21, the first electronic pressure gauge 20 is in a closed state, the second electronic pressure gauge 30 is in an open state, and the outlet of the third enrichment column 331 is connected with the inlet of the first analysis column 711 through the first rotary valve 332, the device is in a target component analysis state, meanwhile, the three enrichment columns and the first analysis column 711 are in a back flushing state, and heavy components are blown out in a back flushing mode.
The following are experimental data performed on the present system:
example 1:
the prepared standard gas sample is taken as an analysis sample 1, and enrichment, analysis and back-flushing conditions are selected and optimized on the general-purpose VOC on-line extraction enrichment-analysis system, wherein the conditions comprise the types and the sizes of the enrichment columns and the analysis columns, the pressure of each pressure control point and the adjustment of valve switching time, the temperature of each temperature control point, the lift rate and the switching time, the flow control of each flow control point and the like. The system, enrichment first and separation detection second, optimized typical conditions as table 1.
TABLE 1
Under the optimized online extraction, enrichment and analysis conditions of the VOC, the prepared environmental gas standard sample 1 is used as a calibration sample, the prepared environmental gas standard sample 2 is used as an analyte, and the general system is evaluated, wherein the evaluation comprises the accuracy and the repeatability of a data analysis result and the stability of the system, and the analysis result is shown in a table 2.
As can be seen from Table 2, when the system is used for the online extraction enrichment analysis of the environmental standard gas, the relative standard deviation of the system after continuously running for 6 times is lower than 3.79 percent, and the analysis result is consistent with the actual composition of the sample.
TABLE 2 Standard gas test data
Example 2: qualitative and quantitative analysis of unknown impurity enrichment
In the same way as example 1, the actual atmospheric sample as the sample to be analyzed was subjected to enrichment and then separation detection by the system under the conditions of enrichment, analysis, back flushing and the like optimized in example 1 in the system shown above. The analytical results are shown in FIG. 2, FIG. 3, Table 3 and Table 4. Where fig. 2 is the profile of the first detector (FID) at the time of actual analysis, fig. 3 is the profile on the second detector (mass spectrometer MSD), and tables 3 and 4 are the two detector test results, respectively.
TABLE 3
TABLE 4
As can be seen from Table 2, when the system is used for carrying out online extraction enrichment analysis on the environmental standard gas, the relative standard deviation of 5 times of continuous operation is low, and the analysis result is quite reliable.
The utility model discloses a VOC on-line extraction enrichment analysis system, through adopting the ripe chromatographic column/pipe that can refrigerate fast and heat as sample extraction enrichment system, adopt behind the post flowmeter to adjust the sample and pass through the flow velocity of the chromatographic enrichment post, adopt the chromatographic enrichment post rapid heating technique, better solved this problem; the installation and connection of the extraction enrichment column are very simple and convenient, the universality is very strong, and the method is suitable for all VOC sample analysis which can be analyzed by gas chromatography; the method can be used for VOC on-line extraction enrichment analysis and can also be used for off-line determination; and the whole enrichment system can be independent of a chromatographic analysis system, is provided with an electronic control system, can be used for automatically collecting outdoor gas samples, and can also be used for on-line extraction, enrichment and analysis of on-site VOC.
The above embodiments are merely illustrative of the principles and effects of the present invention, and are not to be construed as limiting the invention. Modifications and variations can be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which may be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (6)
1. The utility model provides a VOC on-line extraction enrichment analytic system which characterized in that: the device comprises a sample chamber, a heat preservation box, an enrichment column box, a flowmeter, a vacuum pump and a sample treatment chamber which are sequentially connected through connecting pipelines, wherein the enrichment column box is connected with an analysis column box, a detector and a controller; the sample chamber, the heat preservation box, the enrichment column box, the analysis column box, the flow meter, the vacuum pump and the sample disposal chamber are all controlled by a controller, the enrichment column box comprises a first enrichment column box, a second enrichment column box and a third enrichment column box which are sequentially connected, the analysis column box comprises a first analysis column box, a second analysis column box and a third analysis column box which are sequentially connected, the first analysis column box is connected with the third enrichment column box, and the heat preservation box is respectively connected with the first electronic pressure meter and the sample disposal device through connecting pipelines; the three enrichment column boxes are internally provided with any commercialized chromatographic column or self-made chromatographic column, the three analysis column boxes are internally provided with any commercialized chromatographic column or self-made chromatographic column, the temperature of the three enrichment column boxes and the temperature of the three analysis column boxes are controlled independently respectively, and after a gas sample enters from the sample chamber, the gas sample is enriched and analyzed through the enrichment column boxes and the analysis column boxes and is displayed on a display screen of the controller.
2. An online VOC extraction, enrichment, and analysis system according to claim 1, wherein: and a third stopcock is arranged in the heat preservation box and is connected to the first electronic pressure gauge and the sample processor through a connecting pipeline.
3. An online VOC extraction, enrichment, and analysis system according to claim 1, wherein: the enrichment device is characterized in that a first enrichment column is arranged in the first enrichment column box, a second enrichment column and a two-way valve are arranged in the second enrichment column box, a third enrichment column and a first rotary valve are arranged in the third enrichment column box, and the enrichment columns, the two-way valve and the rotary valve are connected through a connecting pipeline.
4. An online VOC extraction, enrichment, and analysis system according to claim 3, wherein: be equipped with first analytical column and second stopcock in the first analytical column box, be equipped with second analytical column and two logical in the second analytical column box, be equipped with the third analytical column in the third analytical column box, a plurality of analytical columns, two logical and stopcock pass through connecting line and connect, just first stopcock in the third enrichment column box is connected with the first analytical column in the first analytical column box.
5. An online VOC extraction, enrichment and analysis system as claimed in claim 4, wherein: and a second stopcock in the first analytical column box is connected with a second electronic pressure gauge through a connecting pipeline.
6. An online VOC extraction, enrichment, and analysis system according to claim 3, wherein: two-way pipes are arranged in the second enrichment column box, and the second enrichment column is arranged between the two-way pipes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112881609A (en) * | 2021-01-19 | 2021-06-01 | 武汉微纳传感技术有限公司 | Miniature multichannel trace gas concentration analyzer |
| CN112924564A (en) * | 2019-12-05 | 2021-06-08 | 上海炫一电气有限公司 | VOC on-line extraction enrichment analysis system |
| CN114371245A (en) * | 2022-01-21 | 2022-04-19 | 北京雪迪龙科技股份有限公司 | Low-heat-capacity micro-chromatographic column box system, and atmospheric organic matter online measurement system and method |
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2019
- 2019-12-05 CN CN201922158291.8U patent/CN211179670U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112924564A (en) * | 2019-12-05 | 2021-06-08 | 上海炫一电气有限公司 | VOC on-line extraction enrichment analysis system |
| CN112881609A (en) * | 2021-01-19 | 2021-06-01 | 武汉微纳传感技术有限公司 | Miniature multichannel trace gas concentration analyzer |
| CN114371245A (en) * | 2022-01-21 | 2022-04-19 | 北京雪迪龙科技股份有限公司 | Low-heat-capacity micro-chromatographic column box system, and atmospheric organic matter online measurement system and method |
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