CN212301457U - VOCs and IVOCs are online collection and detection device simultaneously - Google Patents

VOCs and IVOCs are online collection and detection device simultaneously Download PDF

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CN212301457U
CN212301457U CN202020926809.8U CN202020926809U CN212301457U CN 212301457 U CN212301457 U CN 212301457U CN 202020926809 U CN202020926809 U CN 202020926809U CN 212301457 U CN212301457 U CN 212301457U
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ivocs
vocs
sampling
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李英杰
黄成�
景盛翱
王红丽
楼晟荣
高雅琴
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Shanghai Academy of Environmental Sciences
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Shanghai Academy of Environmental Sciences
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Abstract

The utility model belongs to the technical field of environmental monitoring, concretely relates to volatile organic compound and medium volatile organic compound collect detection device on line simultaneously. The device for simultaneously collecting and detecting VOCs and IVOCs on line comprises a temperature control sampling channel, a TD system and a GC/MS analysis system, wherein the TD system comprises at least one group of sampling tube groups, and the sampling tube groups respectively comprise sampling tubes filled with VOCs and IVOCs adsorbents; the GC/MS analysis system comprises a sample transmission pipeline, a sample inlet and an IVOCs gas chromatographic column, wherein the outlet end of the IVOCs gas chromatographic column is respectively connected with the inlet end of the VOCs chromatographic column and the inlet end of the deactivated quartz capillary column through a Dean-Switch switching system, and the outlet end of the VOCs chromatographic column and the outlet end of the deactivated quartz capillary column are connected with the mass spectrum detector through a three-way valve. The utility model discloses a VOCs and IVOCs are online collection and detection device simultaneously, have realized a sampling, online collection simultaneously and the purpose of analysis VOCs and IVOCs.

Description

VOCs and IVOCs are online collection and detection device simultaneously
Technical Field
The utility model belongs to the technical field of environmental monitoring, concretely relates to volatile organic compound and medium volatile organic compound collect detection device on line simultaneously.
Background
The organic compounds in the atmosphere can be classified into medium volatile organic compounds (IVOCs, with a saturation concentration range of 10) according to their saturation concentration (C;)3μg/m3＜C*＜106μg/m3) And volatile organic compounds (VOCs, saturated concentration range C > 10)6μg/m3). Since VOCs are considered to be O3And Secondary Organic Aerosol (SOA), and has been the focus of research by researchers and related management departments. Recent studies have shown that IVOCs are also atmospheric O3And important precursors of SOAs, and has attracted extensive interest to researchers. In addition, VOCs and IVOCs also pose significant health risks to humans.
The range of saturated concentrations of VOCs corresponds to C3～C12In the range of saturated concentration of IVOCs corresponding to C12～C22And (3) n-alkanes. At present, the detection technology for the organic matter components and concentration levels of the VOCs is relatively mature, and a monitoring technical guide or standard is established, such as the US EPA 5030C; technical Guide Note (TGN) M8 and M16, the monitoring Technical guide Note established by the European Union environmental protection agency; and the measurement of volatile organic compounds in the environmental air (HJ 759-. In addition, due to the characteristics that the boiling point of the VOCs is low, the VOCs are generally at 50-250 ℃, are easy to volatilize and the like, the VOCs are collected and analyzed on line based on thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS). However, IVOCs are relatively low in ambient concentration levels relative to VOCs and relatively viscous and prone to remain in the system. Therefore, analysis of IVOCs is mainly based on TD-GC/MS for off-line collection and analysis, with lower time resolution. At present, the number of the current day,the pollution level of the IVOCs is continuously tracked and observed by lacking an effective means, so that the exact response relation between different IVOCs monomers and the SOA cannot be accurately obtained, and the contribution of the IVOCs to the SOA generation is difficult to scientifically evaluate.
Chinese patent CN201910212822.9 discloses a near online detection device for moderate volatile organic compounds, which modifies the original TD-GC/MS system for online collection and analysis of VOCs and adds the online collection and analysis capability of IVOCs on the basis of the original device. In addition to the differences in saturation vapor pressure and viscosity, the concentrations of VOCs and IVOCs in ambient atmosphere differ by orders of magnitude, and thus, simultaneous on-line collection and real-time analysis on a single sample tube is difficult to achieve. Thus, the improved device can only be used for on-line collection and analysis of VOCs or IVOCs as a target alone. However, VOCs or IVOCs are considered to be both on O3And SOA generation have important contributions. Therefore, if the capability of analyzing organic matters of the original device can be widened, the simultaneous online collection and analysis of VOCs and IVOCs can be realized, valuable data information can be provided for the analysis and detection in the field of organic matters, and data support can be provided for the exposure evaluation of environmental pollution, human health risks and the like.
SUMMERY OF THE UTILITY MODEL
The utility model discloses be difficult to the technical problem of collecting simultaneously and analyzing VOCs and IVOCs to current on-line measuring device, aim at provides a VOCs and IVOCs are collected simultaneously on line and detection device.
The device for simultaneously collecting and detecting VOCs and IVOCs on line comprises a temperature-controlled sampling channel, a TD (thermal desorption) system connected with the temperature-controlled sampling channel and a GC/MS (gas chromatography/mass spectrometry) analysis system connected with the TD system, wherein the TD system comprises at least one group of sampling tube groups, each sampling tube group comprises a sampling tube filled with a VOCs adsorbent and a sampling tube filled with an IVOCs adsorbent, and the temperature-controlled sampling channel is respectively connected with two sampling tubes through a tee;
the GC/MS analysis system comprises a sample transmission pipeline connected with the TD system, a sample injection port and an IVOCs gas chromatographic column communicated with the sample injection port, wherein the outlet end of the IVOCs gas chromatographic column is respectively connected with the inlet end of the VOCs chromatographic column and the inlet end of the deactivated quartz capillary column through a Dean-Switch switching system, and the outlet end of the VOCs chromatographic column and the outlet end of the deactivated quartz capillary column are connected with a mass spectrum detector through a three-way valve.
When the utility model is used, a standard sample or ambient air enters the TD system through the temperature control sampling channel, a group of sampling tube groups in the TD system simultaneously carry out adsorption sampling on a target substance, the sampling tube groups after adsorbing the sampled target substance adopt inert gas to desorb the target substance, and the desorbed target substance is loaded into the GC/MS analysis system through a sample transmission pipeline connected with the GC/MS analysis system by the inert gas; in the GC/MS analysis system, a Dean-Switch switching system is adopted to firstly separate VOCs target substances from an IVOCs gas chromatographic column, Switch the VOCs target substances to the VOCs gas chromatographic column for secondary separation to obtain target substances VOCs, after a certain period of time, the IVOCs target substances separated from the IVOCs gas chromatographic column are switched to a deactivated quartz capillary column to obtain target substances IVOCs, and the VOCs target substances and the IVOCs target substances after secondary separation are converged by a three-way valve and then are simultaneously detected and analyzed by a mass spectrum detector.
The TD system comprises two groups of sampling pipe groups, the temperature control sampling channel and the two groups of sampling pipe groups are respectively connected with two inlet ends of a four-way valve through an interface I end of a tee joint, and an outlet end of the four-way valve is connected with a sample inlet of the GC/MS analysis system through a sample transmission pipeline. After the design, the utility model discloses a when a set of sampling nest of tubes adsorbs the sampling to the target material simultaneously, adopt inert gas desorption target material to another group's sampling nest of tubes, two sets of sampling nest of tubes can sample and desorption simultaneously in turn.
The temperature controllable range of the temperature control sampling channel is 220-350 ℃.
The sampling pipe is a sampling pipe with controllable temperature, and the temperature of the sampling pipe is controllable within the range of-40-20 ℃.
The tee joint and the four-way valve adopt temperature-controllable electromagnetic valves, and the temperature controllable ranges of the tee joint and the four-way valve are both room temperature-350 ℃.
The sample transmission pipeline adopts a transmission pipeline with controllable temperature, and the temperature of the sample transmission pipeline is controllable within the range of room temperature to 300 ℃.
And a flow distribution pipeline is also arranged at the downstream of the outlet end of the four-way valve.
The sampling inlet end of each sampling pipe is connected with the interface II end of the tee joint, and the sampling outlet end of each sampling pipe is communicated with the outside or an inert gas pipeline through a flow rate control valve;
and the two flow rate control valves in the same group are connected with the same mass flow meter. The utility model discloses when two sampling pipes in the same group are sampling the target material and are adsorbing, adopt same mass flow meter to control two sampling pipes simultaneously and with the sampling of different sampling velocity of flow respectively. The sampling tube filled with the VOCs adsorbent can be controlled by a mass flow meter to realize simultaneous sampling at a low sampling flow rate of 0-100ml/min and at a high sampling flow rate of 100-500 ml/min.
The inert gas in the inert gas pipeline adopts high-purity helium gas with the purity of 99.999 percent.
The flow rate control valve is communicated with the outside or an inert gas pipeline through a gas flow switching valve. And the sampling pipe is switched to be communicated with the outside or an inert gas pipeline by a gas flow switching valve.
The utility model discloses an actively advance the effect and lie in: the utility model discloses a VOCs and IVOCs are online collection and detection device simultaneously, have realized a sampling, online collection simultaneously and the purpose of analysis VOCs and IVOCs.
Drawings
FIG. 1 is a schematic view of the overall structure of the device of the present invention;
FIG. 2 is a schematic view of a gas circuit for alternately sampling and desorbing two sets of sampling tube sets according to the present invention;
FIG. 3 is a schematic view of another gas circuit for alternately sampling and desorbing two sets of sampling tube sets according to the present invention;
fig. 4 is a schematic diagram of the Dean-Switch switching system according to the present invention;
fig. 5 is another schematic diagram of the Dean-Switch switching system of the present invention.
Detailed Description
In order to make the technical means, creation features, achievement purposes and functions of the present invention easy to understand, the present invention will be further explained with reference to the specific drawings.
Referring to fig. 1, the device for simultaneously collecting and detecting VOCs and IVOCs on line comprises a temperature-controlled sampling channel 1, a TD (thermal desorption) system 2 and a GC/MS (gas chromatography/mass spectrometry) analysis system 3, wherein the TD system 2 comprises at least one group of sampling tube groups, each group of sampling tube groups comprises a sampling tube 21 filled with VOCs adsorbent and a sampling tube 22 filled with IVOCs adsorbent, and the two sampling tubes are respectively connected with two parallel interfaces (II ends) of a tee 23. Preferably, the TD system 2 includes two sets of sampling tube sets, a sampling tube set a and a sampling tube set B. The interface (I end) of the tee 23 in each group of sampling tube sets and the temperature control sampling channel 1 are respectively connected with two inlet ends of a four-way valve 24. The temperature controllable range of the temperature control sampling channel 1 is 220-350 ℃. The sampling tube adopts a sampling tube with controllable temperature, and the temperature of the sampling tube can be controlled within the range of minus 40 to 20 ℃. The three-way 23 and the four-way valve 24 adopt temperature-controllable electromagnetic valves, and the temperature controllable ranges of the three-way 23 and the four-way valve 24 are both room temperature-350 ℃.
The sampling inlet end of each sampling pipe is connected with the II end of the tee 23, and the sampling outlet end of each sampling pipe is communicated with the outside or an inert gas pipeline through a flow rate control valve 25. Preferably, a gas flow switching valve can be arranged between the flow rate control valve 25 and the outside or inert gas pipeline, and the gas flow switching valve is used for switching to realize the communication between the sampling pipe and the outside or inert gas pipeline. Both flow rate control valves in the same group are connected to the same mass flow meter 26. As shown in fig. 1, there are two mass flowmeters 26, mass flowmeter 1 and mass flowmeter 2, respectively. The two mass flowmeters 26 each independently control a set of sampling tube sets.
The outlet end of the four-way valve 24 is connected with the sample inlet 31 of the GC/MS analysis system 3 through a sample transmission pipeline 4, the sample transmission pipeline 4 adopts a transmission pipeline with controllable temperature, and the temperature of the sample transmission pipeline 4 is controllable within the range of room temperature to 300 ℃. A shunt line 5 is also provided downstream of the outlet end of the four-way valve 24.
The GC/MS analysis system 3 comprises a sample transmission pipeline 4 connected with the TD system 2, a sample injection port 31, and an IVOCs gas chromatographic column 32(DB-5MS chromatographic column) communicated with the sample injection port 31, wherein the outlet end of the IVOCs gas chromatographic column 32 is respectively connected with the inlet end of a VOCs chromatographic column 34(DB624 chromatographic column) and the inlet end of a deactivated quartz capillary column 35 through a Dean-Switch switching system 33, and the outlet end of the VOCs chromatographic column 34 and the outlet end of the deactivated quartz capillary column 35 are connected with a mass spectrum detector 37 through a three-way valve 36.
The utility model discloses during the specific use, adopt following step to VOCs and IVOCs simultaneous on-line collection and detection:
and step S1, allowing a standard sample or ambient air to enter the TD system through the temperature-controlled sampling channel, allowing a group of sampling tube groups in the TD system to simultaneously perform adsorption sampling on the target substance, wherein the same group of sampling tube groups comprises sampling tubes containing VOCs adsorbent and sampling tubes containing IVOCs adsorbent.
When sampling is carried out, a TD system is adopted, and TD on-line sampling and sample introduction are completed by a temperature control sampling channel and a sampling tube. When the sampling tube adsorbs a sampling target substance, the sampling duration is set to be 0-999min, and the temperature of the sampling tube is controlled to be-40-20 ℃.
The sampling pipe group in the TD system consists of VOCs and IVOCs sampling pipes, namely two sampling pipes filled with VOCs and IVOCs adsorbents. Two sampling pipes in every group sampling nest of tubes pass through three-way connection, realize gathering VOCs and IVOCs simultaneously through the reposition of redundant personnel of tee bend.
When the two sampling pipes in the same group adsorb a target substance, the same mass flow meter is adopted to respectively control the two sampling pipes to sample at different sampling flow rates. Specifically, a flow rate control valve can be installed at the tail end of each sampling tube, and when two sampling tubes are respectively controlled by a mass flow meter to sample at different sampling flow rates at the same time, the sampling tube filled with the VOCs adsorbent is controlled to sample at the low sampling flow rate of 0-100ml/min and the sampling tube filled with the IVOCs adsorbent is controlled to sample at the high sampling flow rate of 100-500ml/min at the same time, so that the total amount of target substances meeting the detection requirements of an analysis system on VOCs and IVOCs can be collected within the same sampling time.
And step S2, desorbing the target substance by using inert gas by the sampling tube group after the target substance is adsorbed, and loading the desorbed target substance into the GC/MS analysis system by the inert gas through a sample transmission pipeline connected with the GC/MS analysis system.
The target substance is desorbed by inert gas at 150-350 ℃, and the inert gas adopts 99.999% of high-purity helium. When the target substance is desorbed in the step, the temperature is preferably raised to 300 ℃ at the speed of 1-40 ℃/s for 5min under the high-purity helium flow, and then the temperature is raised to 350 ℃ at the speed of 1-40 ℃/s and is kept for 5-15 min to desorb the target substance.
The TD system comprises two groups of sampling tube groups, namely a sampling tube group A and a sampling tube group B, when one group of sampling tube groups is used for simultaneously adsorbing and sampling the target substance, the other group of sampling tube groups is subjected to the following step S2 of desorbing the target substance by using inert gas, and the two groups of sampling tube groups are alternately subjected to sampling and desorbing steps. Namely: sampling and thermal desorption work are alternately carried out on the sampling pipe group A and the sampling pipe group B, when sampling of the sampling pipe group B is completed, VOCs and IVOCs in ambient air are collected by the sampling pipe group A under a set sampling condition, and meanwhile, target substances are analyzed by the sampling pipe group B under a set thermal desorption condition.
The temperature control sampling channel, the two groups of three-way pipes and the sample transmission pipeline connected with the GC/MS analysis system are connected through the four-way valve, and the two groups of sampling pipe groups are switched to alternately perform sampling and desorption steps through the four-way valve.
Referring to fig. 2, after passing through a temperature-controlled sampling channel and through a four-way valve and a three-way valve, ambient air enters two sampling tubes of a sampling tube group a for adsorption sampling, and target substances are respectively enriched in the two sampling tubes of the sampling tube group a (during sampling, the temperature of the sampling tubes is controlled to be-40-20 ℃); meanwhile, the sampling tube group B is used for carrying out thermal desorption, the desorbed target substance is transported by carrier gas (helium gas, 99.999 percent), and after passing through the three-way valve and the four-way valve in sequence, under the set flow dividing condition, a part of the target substance is sent to the GC/MS analysis system through the sample transmission pipeline, and the other part of the target substance is discharged into the ambient air through the flow dividing pipeline.
Referring to fig. 3, the sampling pipe group A completes adsorption sampling, after the sampling pipe group B completes thermal desorption, the sampling pipe group A performs thermal desorption, and the sampling pipe group B performs adsorption sampling, so that two groups of sampling pipe groups alternately perform sampling and thermal desorption.
Step S3, in a GC/MS analysis system, switching VOCs target substances separated out firstly by an IVOCs gas chromatographic column into the VOCs gas chromatographic column by adopting a Dean-Switch switching system for secondary separation to obtain target substances VOCs; after the separation of VOCs target substances is completed within a set time, a Dean-Switch switching system is adopted to Switch subsequently separated IVOCs target substances to a deactivated quartz capillary column to obtain target substances IVOCs, and the secondarily separated target substances VOCs and the target substances IVOCs passing through the quartz capillary column are converged by a three-way valve and then enter a mass spectrum detector for simultaneous detection and analysis.
In the step, a Dean-Switch switching system (commercial system) is adopted for accurate control, VOCs target substances enter a DB624 chromatographic column for secondary separation, and IVOCs enter a deactivated quartz capillary column. And finally, connecting the ends of the DB624 chromatographic column and the deactivated quartz capillary column by a three-way valve, allowing the chromatographic column to enter a mass spectrum detector, realizing simultaneous detection of VOCs and IVOCs by the mass spectrum detector, and identifying and quantitatively analyzing organic matters according to the difference of the peak-out time (namely, the retention time) and the ion fragment characteristics of each target substance.
Referring to fig. 4, a target substance in the TD system is sent to a GC sample inlet through a sample transmission pipeline from high-purity helium, enters a DB-5MS gas chromatographic column first, and a target substance of VOCs separated from the DB-5MS gas chromatographic column first passes through a Dean-Switch switching system and is switched to a DB624 chromatographic column for secondary separation, at this time, an electromagnetic valve in the Dean-Switch switching system is in an "ON" open state, and the VOCs split by the DB624 chromatographic column pass through a three-way valve and then enter mass spectrometry detection;
referring to fig. 5, after a certain set time, the target substances of the IVOCs subsequently separated from the DB-5MS gas chromatographic column are switched to the deactivated quartz capillary column by the Dean-Switch system, at this time, the electromagnetic valve in the Dean-Switch system is in an "OFF" closed state, and the high purity helium gas is transported through the deactivated quartz capillary column and the three-way valve and enters mass spectrometry detection.
The utility model discloses a device is through two sets of sampling nest of tubes A of TD system and sampling nest of tubes B and is lasted sampling in turn and thermal desorption, and the target material through thermal desorption sends to GC MS system analysis, realizes VOCs and IVOCs's online function of collecting simultaneously and analyzing.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above embodiments, and that the foregoing embodiments and descriptions are provided only to illustrate the principles of the present invention without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

  1. The device for simultaneously collecting and detecting VOCs and IVOCs on line comprises a temperature control sampling channel, a TD system connected with the temperature control sampling channel and a GC/MS analysis system connected with the TD system, and is characterized in that the TD system comprises at least one group of sampling tube groups, each sampling tube group comprises a sampling tube filled with a VOCs adsorbent and a sampling tube filled with an IVOCs adsorbent, and the temperature control sampling channel is respectively connected with two sampling tubes through a tee joint;
    the GC/MS analysis system comprises a sample transmission pipeline connected with the TD system, a sample injection port and an IVOCs gas chromatographic column communicated with the sample injection port, wherein the outlet end of the IVOCs gas chromatographic column is respectively connected with the inlet end of the VOCs chromatographic column and the inlet end of the deactivated quartz capillary column through a Dean-Switch switching system, and the outlet end of the VOCs chromatographic column and the outlet end of the deactivated quartz capillary column are connected with a mass spectrum detector through a three-way valve.
  2. 2. The device for simultaneously collecting and detecting VOCs and IVOCs according to claim 1, wherein the TD system comprises two sets of the sampling tube sets, the temperature-controlled sampling channel and the two sets of the sampling tube sets are respectively connected to two inlet ends of a four-way valve through an I end of a three-way interface, and an outlet end of the four-way valve is connected to a sample inlet of the GC/MS analysis system through the sample transmission line.
  3. 3. The device for the simultaneous on-line collection and detection of VOCs and IVOCs of claim 1, wherein the temperature controllable range of the temperature controlled sampling channel is between 220 ℃ and 350 ℃.
  4. 4. The device for simultaneously collecting and detecting VOCs and IVOCs according to claim 1, wherein the sampling tube is a temperature-controllable sampling tube, and the temperature of the sampling tube is controllable within a range of-40 to 20 ℃.
  5. 5. The device for the simultaneous on-line collection and detection of VOCs and IVOCs according to claim 2, wherein said three-way valve and said four-way valve are temperature-controllable solenoid valves, and the temperature of said three-way valve and said four-way valve is controlled within a range of room temperature to 350 ℃.
  6. 6. The apparatus for the simultaneous on-line collection and detection of VOCs and IVOCs of claim 2, wherein the sample transfer line is a temperature-controlled transfer line, and the temperature of the sample transfer line is controlled within a range of room temperature to 300 ℃.
  7. 7. The apparatus for simultaneous on-line collection and detection of VOCs and IVOCs of claim 2, wherein a shunt line is further provided downstream of the outlet end of the four-way valve.
  8. 8. The simultaneous online collection and detection device of VOCs and IVOCs as claimed in any one of claims 1 to 7, wherein the sampling inlet end of each of the sampling tubes is connected to the interface II end of the tee, and the sampling outlet end of each of the sampling tubes is connected to an external or inert gas line through a flow rate control valve;
    and the two flow rate control valves in the same group are connected with the same mass flow meter.
  9. 9. The apparatus for the simultaneous online collection and detection of VOCs and IVOCs of claim 8, wherein the inert gas in the inert gas line is 99.999% high purity helium.
  10. 10. The device for simultaneous online collection and detection of VOCs and IVOCs of claim 8, wherein the flow rate control valve is in communication with an external or inert gas line through a flow switching valve.
CN202020926809.8U 2020-05-28 2020-05-28 VOCs and IVOCs are online collection and detection device simultaneously Active CN212301457U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111579315A (en) * 2020-05-28 2020-08-25 上海市环境科学研究院 VOCs and IVOCs simultaneous on-line collecting and detecting method
CN114019038A (en) * 2021-10-09 2022-02-08 长鑫存储技术有限公司 Device and method for monitoring organic matters in environmental gas
CN115326997A (en) * 2022-09-13 2022-11-11 广州禾信仪器股份有限公司 Double-channel chromatographic detector and organic pollutant detection method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111579315A (en) * 2020-05-28 2020-08-25 上海市环境科学研究院 VOCs and IVOCs simultaneous on-line collecting and detecting method
CN111579315B (en) * 2020-05-28 2023-06-02 上海市环境科学研究院 VOCs and IVOCs simultaneous online collection and detection method
CN114019038A (en) * 2021-10-09 2022-02-08 长鑫存储技术有限公司 Device and method for monitoring organic matters in environmental gas
CN114019038B (en) * 2021-10-09 2024-01-02 长鑫存储技术有限公司 Device and method for monitoring organic matters in environmental gas
CN115326997A (en) * 2022-09-13 2022-11-11 广州禾信仪器股份有限公司 Double-channel chromatographic detector and organic pollutant detection method

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