CN114113443A - System and method for on-line continuous monitoring of aldehyde ketone compounds in gas - Google Patents
System and method for on-line continuous monitoring of aldehyde ketone compounds in gas Download PDFInfo
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- -1 aldehyde ketone compounds Chemical class 0.000 title claims abstract description 49
- 238000012544 monitoring process Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000005070 sampling Methods 0.000 claims abstract description 128
- 238000001514 detection method Methods 0.000 claims abstract description 97
- 238000002360 preparation method Methods 0.000 claims abstract description 90
- 239000000741 silica gel Substances 0.000 claims description 39
- 229910002027 silica gel Inorganic materials 0.000 claims description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 36
- 238000004140 cleaning Methods 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 5
- 238000010926 purge Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 32
- 239000007788 liquid Substances 0.000 description 16
- 238000001179 sorption measurement Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical class O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001212 derivatisation Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8804—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 automated systems
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides an on-line continuous monitoring system and a method for aldehyde ketone compounds in gas, wherein the on-line continuous monitoring system comprises a detection unit; further comprising: the bearing piece is arranged on the base and is driven by the driving module to rotate; m groups of working units, wherein M is an integer not less than 1, each group of working units comprises P working units, and P is an integer not less than 3; the working unit is arranged on the bearing piece; during the rotation of the bearing piece, each working unit is sequentially positioned at a preparation working position, a sampling working position and a detection working position; the preparation flow path is arranged at a preparation working position, the sampling flow path is arranged at a sampling working position, and the detection flow path is arranged at a detection working position; the control device is used for controlling whether the working unit at the preparation working position enters the preparation flow path, whether the working unit at the sampling working position enters the sampling flow path, and whether the working unit at the detection working position enters the detection flow path. The invention has the advantages of high working efficiency, accurate analysis result and the like.
Description
Technical Field
The invention relates to gas monitoring, in particular to an on-line continuous monitoring system and method for aldehyde ketone compounds in gas.
Background
At present, the method for sampling and analyzing the aldehyde ketone compound and the related standards are mainly based on an off-line sampling means, for example, in the national standard HJ 683-2014, after off-line sampling is performed by using a DNPH-silica gel adsorption tube, a sample is transferred to a laboratory for analysis and detection by using a high performance liquid chromatography. This off-line mode of operation has a number of disadvantages, such as:
1. the influence of human factors is large, and the requirements on storage and transportation of samples are high;
2. the material cost and the manual analysis cost are high, long-term high-frequency observation is not facilitated, and the current requirements on photochemical pollution fine control cannot be met;
3. in the manual sampling process, the DNPH-silica gel adsorption tube is greatly influenced by the environmental temperature, the adsorption derivatization efficiency of aldehyde ketone compounds on the adsorption tube is unstable, and the measurement and analysis errors are large;
4. in the analysis method, a packed column sampling tube coated with DNPH is used, the preparation process refers TO EPA TO-11A standard, the production process is complex, the storage condition is severe, and the requirement on a blank background value is high.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the automatic, high-working-efficiency and accurate-measurement online continuous monitoring system for the aldehyde ketone compound in the gas.
The purpose of the invention is realized by the following technical scheme:
the on-line continuous monitoring system for the aldehyde ketone compound in the gas comprises a detection unit; further comprising:
the bearing piece is arranged on the base and driven by the driving module to rotate;
m groups of working units, wherein M is an integer not less than 1, each group of working units comprises P working units, and P is an integer not less than 3; the working unit is arranged on the bearing piece and comprises a silica gel column, and openings are formed in two ends of the silica gel column; in the rotation of the bearing piece, when one working unit in any group of working units is in the preparation working position, the other working units are respectively in the sampling working position and the detection working position, so that each working unit is sequentially in the preparation working position, the sampling working position and the detection working position;
the preparation flow path is arranged at the preparation working position, a silica gel column entering the preparation flow path forms a sampling column for adsorbing aldehyde ketone compounds, the sampling flow path is arranged at the sampling working position, the detection flow path is arranged at the detection working position, and the detection unit is positioned in the detection flow path;
and the control device is used for controlling whether the working unit at the preparation working position enters the preparation flow path, whether the working unit at the sampling working position enters the sampling flow path and whether the working unit at the detection working position enters the detection flow path.
The invention also aims to provide an on-line continuous monitoring method for aldehyde ketone compounds in gas by using the on-line continuous monitoring system for aldehyde ketone compounds in gas, which is realized by the following technical scheme:
the on-line continuous monitoring method of the aldehyde ketone compound in the gas by applying the on-line continuous monitoring system of the aldehyde ketone compound in the gas comprises the following steps:
the bearing piece rotates, when one working unit in any group of working units is in the preparation working position, the other working units are respectively in the sampling working position and the detection working position;
under the control of the control device, the working unit at the preparation working position enters the preparation flow path, the silica gel column forms a sampling column for adsorbing aldehyde ketone compounds, the prepared sampling column at the sampling working position enters the sampling flow path, the aldehyde ketone compounds in the environment to be detected are adsorbed, and the sampling column at the detection working position which finishes sampling enters the detection flow path;
under the control of the control device, the prepared working unit at the preparation working position is separated from the preparation flow path, the sampling column at the sampling working position is separated from the sampling flow path, and the sampling column at the detection working position is separated from the detection flow path;
and the bearing piece further rotates, so that each working unit is sequentially positioned at a preparation working position, a sampling working position and a detection working position, and the operation is circulated.
Compared with the prior art, the invention has the beneficial effects that:
1. the working efficiency is high;
through the design of the working units and the working units, one working unit in the same group of working units is in a preparation working position to prepare the sampling column on line, the other working unit of the prepared sampling column is in a sampling working position to realize on-line sampling, and the working unit after sampling is in a detection working position to realize on-line detection, namely, the preparation, sampling and detection of the sampling column corresponding to the same group of working units are carried out simultaneously, namely, the sampling and detection are carried out in parallel, so that the time consumption of the waiting process of each link is greatly reduced, and the working efficiency is remarkably improved;
the M groups of working units work simultaneously (a single-circle one-time working cycle and multiple working cycles) so that the working efficiency is further improved;
2. automation;
the working unit (including a silica gel column) automatically circulates at the preparation working position, the sampling working position and the detection working position, and automatically enters and separates from a flow path corresponding to the working position without manual intervention;
3. continuously working on line;
the preparation, sampling and detection are carried out on line, so that the working efficiency is obviously improved;
the working units continuously and circularly enter the sampling working position and the detection working is that continuous sampling and continuous detection are realized (except the time for switching the front working unit and the rear working unit, the time is short and can be ignored);
4. the detection result is accurate;
the sampling column regenerated at the preparation working position avoids the requirement of long-distance transportation, the formaldehyde derivative is less than 10 ng/root, and the sampling column has lower background blank than the existing DNPH adsorption column (the formaldehyde derivative is less than 150 ng/root) specified by the national standard, and the measurement result under low concentration is more reliable;
5. the detection cost is low;
the sampling column is regenerated and reused, the consumable materials can be automatically regenerated, and the cost of the single-sample consumable materials is reduced by more than 90%.
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 diagram of an on-line continuous monitoring system for an aldehyde ketone compound in a gas according to an embodiment of the present invention;
FIG. 2 is a schematic view of a flow path configuration of an on-line continuous monitoring system for an aldehyde ketone compound in a gas according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of an on-line continuous monitoring system for an aldehyde ketone compound in a gas according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of an on-line continuous monitoring system for an aldehyde ketone compound in a gas according to an embodiment of the present invention.
Detailed Description
Fig. 1-4 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and use 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:
fig. 1 shows a schematic structural diagram of an on-line continuous monitoring system for aldehyde ketone compounds in gas according to an embodiment of the present invention, and as shown in fig. 1, the on-line continuous monitoring system for aldehyde ketone compounds in gas includes:
a detection unit, such as a liquid chromatography detection unit;
the device comprises a base, a carrier 41 and a driving module, wherein the carrier 41 is arranged on the base and driven by the driving module to rotate;
m groups of working units, wherein M is an integer not less than 1, each group of working units comprises P working units, and P is an integer not less than 3, such as a first working unit 21, a second working unit 22 and a third working unit 23; the working unit is arranged on the bearing piece 41 and comprises a silica gel column, and two ends of the silica gel column are opened; in the forward or reverse rotation of the bearing part 41, when one working unit in any group of working units is in the preparation working position, the other working units are respectively in the sampling working position and the detection working position, so that each working unit is in the preparation working position, the sampling working position and the detection working position in sequence;
a preparation flow path 11, a sampling flow path 31 and a detection flow path 51, wherein the preparation flow path 11 is arranged at the preparation working position, a silica gel column entering the preparation flow path 11 forms a sampling column for adsorbing aldehyde ketone compounds, the sampling flow path 31 is arranged at the sampling working position, the detection flow path 51 is arranged at a detection working position, and the detection unit is positioned in the detection flow path 51;
and the control device is used for controlling whether the working unit at the preparation working position enters the preparation flow path, whether the working unit at the sampling working position enters the sampling flow path and whether the working unit at the detection working position enters the detection flow path.
In order that the working units at each working position automatically enter the flow path, further, the control device comprises:
the device comprises a first moving part and a plurality of first pipelines, wherein the first pipelines are arranged on the first moving part and positioned on the upper side of a bearing part, and the preparation flow path, the sampling flow path and the detection flow path are respectively communicated with the first pipelines;
the second moving part is provided with a plurality of second pipelines, and the second pipelines are arranged on the second moving part and positioned at the lower side of the bearing part;
the first moving piece and the second moving piece are arranged on the guide rail respectively, the driving unit is used for driving the first moving piece and the second moving piece to move on the guide rail, so that the lower end of the first pipeline is connected and separated with an upper end opening of the working unit, and the upper end of the second pipeline is connected and separated with a lower end opening of the working unit.
In order to prepare (regenerate) the sampling column on line automatically, further, as shown in fig. 2, the preparation flow path includes a first container, a first pump 45, a first column 81 and a second column 82, and a second container 73, which are connected in this order; the second column 82 is connected with the first pipeline, and the second container 73 is connected with the second pipeline; DNPH powder is filled in the first column 81, and silicone gel is filled in the second column 82;
a removing unit for removing the solvent entering the working unit of the preparation flow path.
For automated cleaning and preparation (regeneration), further, the preparation flow path 11 further includes:
a first switching module 61, said first switching module 61 being adapted to selectively communicate the outlet of said first pump 45 with said first column 81 and a second conduit;
a second switching module 62, said second switching module 62 being adapted to selectively place a second column 82 in communication with said first column 81 and a second container 73.
In order to rapidly remove the solvent in the silica gel column, further, the removing unit comprises:
a gas source 75, the gas source 75 providing a purge gas;
a third switching module 63, wherein the third switching module 63 is used for selectively connecting the gas source 75 and the second column 82 to the working unit entering the preparation flow path 11.
In order to realize the automatic preparation of the sampling column, further, the first container comprises a first cleaning liquid container 71 and a coating liquid container 72;
the fourth switching module 64 is used to selectively connect the inlet of the first pump 45 to the first cleaning liquid container 71 and the coating liquid container 72.
For automated sampling, further, the sampling flow path comprises:
one end of the pretreatment unit is communicated with air, and the other end of the pretreatment unit is connected with the second pipeline;
a second pump 46, said second pump 46 being connected to said first conduit.
For automated detection, further, the detection flow path comprises:
a second cleaning liquid container 74 and a third pump 47, wherein the second cleaning liquid container 74, the third pump 47 and the first pipeline are connected in sequence;
a sample container 76, wherein the sample container 76 is connected with the second pipeline, and the detection unit 10 is connected with the sample container 76.
The method for continuously monitoring the aldehyde ketone compound in the gas on line provided by the embodiment of the invention, that is, according to the working method of the system for continuously monitoring the aldehyde ketone compound in the gas on line provided by the embodiment of the invention, the method for continuously monitoring the aldehyde ketone compound in the gas on line comprises the following steps:
the bearing part 41 rotates, when one working unit in any group of working units is in the preparation working position, the other working units are respectively in the sampling working position and the detection working position;
under the control of the control device, the working unit at the preparation working position enters the preparation flow path 11, the silica gel column forms a sampling column for adsorbing aldehyde ketone compounds, the prepared sampling column at the sampling working position enters the sampling flow path 31 for adsorbing aldehyde ketone compounds in the environment to be detected, and the sampling column at the detection working position which finishes sampling enters the detection flow path 51;
under the control of the control device, the prepared working unit at the preparation working position is separated from the preparation flow path 11, the sampling column at the sampling working position is separated from the sampling flow path 31, and the sampling column at the detection working position is separated from the detection flow path 51;
the carrier 41 is further rotated so that each working unit is sequentially in the preparation working position, the sampling working position and the inspection working position, and is circulated, thereby completing the preparation, sampling and inspection automatically on line.
In order to realize online and automated preparation of the sampling column, in the preparation flow path 11, the way of the silica gel column forming the sampling column is as follows:
the cleaning solution sequentially passes through a silica gel column and a second column 82, and organic silica gel is filled in the second column 82;
the coating liquid sequentially passes through a first column 81, a second column 82 and a silica gel column, and DNPH powder is filled in the first column 81;
and removing the solvent in the silica gel column, wherein the silica gel column forms a sampling column.
Example 2:
the system and the method for continuously monitoring the aldehyde ketone compound in the gas on line are applied to air monitoring according to the embodiment 1 of the invention.
In the present application example, as shown in fig. 1, the bearing member 41 is a disk, and through holes are uniformly formed on the circumference of the disk; a group of working units is arranged on the bearing piece 41, the only group of working units comprises three working units, the three working units (the first working unit 21, the second working unit 22 and the third working unit 23) are respectively arranged in the through holes, and the central angle corresponding to the adjacent working units is 120 degrees; the working unit comprises a silica gel column (filled with pure silica gel), and the upper end and the lower end of the silica gel column are provided with openings; the driving module adopts a motor and is used for driving the bearing piece 41 to rotate;
in the control device, a first moving member and a second moving member are respectively in a disc shape and are arranged on a vertical guide rail, and a driving unit adopts a screw rod driven by a motor and is used for respectively and independently driving the first moving member and the second moving member to move up and down (only move up and down) on the vertical guide rail; the three first pipelines are uniformly arranged on the circumference of the first moving member, when the first moving member vertically moves downwards, the lower end of each first pipeline is respectively connected and sealed with the upper end opening of the working unit on the bearing member 41, and when the first moving member vertically moves upwards, the lower end of each first pipeline is respectively separated from the upper end opening of the working unit on the bearing member 41; the three second pipelines are uniformly arranged on the circumference of the second moving member, when the first moving member vertically moves upwards, the upper end of each second pipeline is respectively connected and sealed with the lower end opening of the working unit on the bearing member 41, and when the second moving member vertically moves downwards, the upper end of each second pipeline is respectively separated from the lower end opening of the working unit on the bearing member 41, so that whether the working unit enters the flow path or not is automatically controlled;
as shown in fig. 2, the preparation flow path 11 is in a preparation working position, and includes a first container, a fourth switching module 64, a first pump 45, a first switching module 61, a first column 81, a second switching module 62, a second column 82, and a third switching module 63, which are connected in sequence, and a fifth switching module 65 and a second container 63, which are connected in sequence, and the purging unit employs an air source 75; the third switching module 63 is connected with the first pipeline, the fifth switching module 65 is connected with the second pipeline, the first container comprises a first cleaning liquid container 71 and a coating liquid container 72, the cleaning liquid adopts acetone, the coating liquid adopts isopropanol (or methanol, ethyl acetate) and acid solution, and hydrochloric acid, boric acid and the like can be adopted; the switching modules all adopt electromagnetic three-way valves, one outlet of the first switching module 61 is connected with a second pipeline, one outlet of the second switching module 62 is communicated with the second container 73, and an inlet of the third switching module 63 is sequentially communicated with the first MFC91 and the gas source 75, such as a nitrogen cylinder; the first column 81 is filled with DNPH powder, and the second column 82 is filled with organic silica gel, such as Phenyl silica gel;
the sampling flow path 31 is positioned at a sampling working position and comprises a pretreatment unit, a second MFC92 and a second pump 46, wherein the pretreatment unit comprises a filter 56 and an ozone column 57, the ozone column 57 is connected with a second pipeline, and the second pump 46, the second MFC92 and the first pipeline are sequentially connected;
the detection flow path 51 is in a detection operation, and includes the second cleaning liquid container 74, the third pump 47, and the sixth switching module 66, the sample container 76, and the detection unit 10, which are connected in this order; the third pump 74 adopts a syringe pump, the sixth switching module 66 is connected with the first pipeline, the sample container 76 is connected with the second pipeline, and the detection unit 10 adopts a liquid chromatography detection unit; the gas source 75 is connected to the sixth switching module 66 through a third MFC 93; the second cleaning liquid container 74 contains acetone.
The method for continuously monitoring the aldehyde ketone compound in the gas on line provided by the embodiment of the invention, that is, according to the working method of the system for continuously monitoring the aldehyde ketone compound in the gas on line provided by the embodiment of the invention, the method for continuously monitoring the aldehyde ketone compound in the gas on line comprises the following steps:
the driving module drives the bearing part 41 to rotate in the forward direction, the first working unit 21 is in the preparation working position, meanwhile, the second working unit 22 is in the sampling working position, and the third working unit 23 is in the detection working position;
the driving unit drives the first moving piece to move downwards and the second moving piece to move upwards, the upper end opening of each first pipeline and the upper end opening of the working unit are connected and sealed, the upper end opening of the second pipeline and the lower end opening of the working unit are connected and sealed, so that the first working unit 21 enters the preparation flow path 11, namely the third switching module 63, the first pipeline, the first working unit (silica gel column) 21, the second pipeline and the fifth switching module 65 are communicated, meanwhile, the second working unit 22 enters the sampling flow path 31, that is, the second pump 46, the second MFC92, the first pipeline, the second working unit (prepared sampling column) 22, the second pipeline, the ozone removal column 57 and the filter 56 are communicated, and the third working unit 23 enters the detection flow path 51, that is, the sixth switching module 66, the first pipeline, the third working unit (sampled sampling column) 23, the second pipeline and the sample container 76 are communicated;
in the preparation flow path, with the first-fifth switching module switching, first, the cleaning liquid flows through the fourth switching module 64, the first pump 45, the first switching module 61, the fifth switching module 65, the first working unit (silica gel column) 21, the third switching module 63, the second column 82, and the second switching module 62 in this order, and then enters the second container 73, thereby cleaning the first working unit (silica gel column) 21 and the second column 82; next, the coating liquid flows through the fourth switching module 64, the first pump 45, the first switching module 61, the first column 81, the second switching module 62, the second column 82, the third switching module 63, the first working unit (silica gel column) 21, and the fifth switching module 65 in this order, and then enters the second container 73; then, the nitrogen provided by the gas source 75 flows through the third switching module 63, the first working unit (silica gel column) 21 and the fifth switching module 65 in sequence, so that the automatic online preparation of the sampling column is realized;
in the sampling flow path 31, the second pump 46 is operated, and the air flows through the filter 56, the ozone removal column 57, the second operation unit (prepared sampling column) 22, the second MFC92, and the second pump 46 in this order, and the aldehyde-ketone compound in the air is adsorbed in the sampling column;
in the detection flow path 51, by switching the sixth switching module 66, firstly, the cleaning solution flows through the third pump 47, the sixth switching module 66, the third working unit (sampled sampling column) 23 and the sample container 76 in sequence, the DNPH derivative adsorbed in the third working unit (sampled sampling column) 23 enters the sample container 76, and then, the unit provided by the gas source 75 flows through the third MFC93, the sixth switching module 66, the third working unit (sampled sampling column) 23 and the sample container 76 in sequence, so that the purging and the bubbling in the sample container 76 are uniformly mixed; then, the liquid in the sample container 76 enters the detection unit 10 for detection; the preparation, the sampling and the detection are carried out simultaneously;
the driving unit drives the first moving piece to move upwards and the second moving piece to move downwards, the upper end openings of the first pipelines and the working unit are separated, and the upper end openings of the second pipelines and the lower end openings of the working unit are separated;
the driving module drives the bearing part 41 to rotate forward by 120 degrees, the detected third working unit 23 is in the preparation working position, meanwhile, the sampled second working unit 22 is in the detection working position, and the prepared first working unit 21 is in the sampling working position;
under the action of the control device, the third working unit 23 enters the preparation flow path 11, meanwhile, the second working unit 22 enters the detection flow path 51, and the first working unit 21 enters the sampling flow path 31 in the same way as the above; the third working unit 23 completes the preparation (regeneration) of the sampling column automatically on line, meanwhile, the second working unit 22 automatically detects on line, and the first working unit 21 automatically samples on line; the preparation, sampling and detection modes are the same as the above;
under the action of the control device, the third working unit 23 is separated from the preparation flow path 11, meanwhile, the second working unit 22 is separated from the detection flow path 51, the first working unit 21 is separated from the sampling flow path 31, and the separation mode of the first working unit and the second working unit is the same as the above;
the driving module drives the bearing part 41 to rotate forward by 120 degrees, the prepared third working unit 23 is in the sampling working position, meanwhile, the detected second working unit 22 is in the preparation working position, and the sampled first working unit 21 is in the detection working position;
under the action of the control device, the third working unit 23 enters the sampling flow path 31, meanwhile, the second working unit 22 enters the preparation flow path 11, and the first working unit 21 enters the detection flow path 51 in the same way as the above; the second working unit 22 completes the preparation (regeneration) of the sampling column automatically on line, meanwhile, the third working unit 23 automatically samples on line, and the first working unit 21 automatically detects on line;
under the action of the control device, the third working unit 23 is separated from the sampling flow path 31, meanwhile, the second working unit 22 is separated from the preparation flow path 11, and the first working unit 21 is separated from the detection flow path 51;
repeating the cycle; it can be seen that, by the rotation of the bearing member 41, each working unit is sequentially located at the preparation working position, the sampling working position and the detection working position, and the operation is repeated, so that the preparation, the sampling and the detection are automatically completed on line.
Example 3:
the application example of the system and the method for continuously monitoring the aldehyde ketone compound in the gas on line in the air monitoring according to the embodiment 1 of the invention is different from the embodiment 2 in that:
as shown in fig. 3, there are two groups of working units, each group of working units includes three working units, the first group of working units includes a first working unit 21, a second working unit 22 and a third working unit 23, the second group of working units includes a fourth working unit 27, a fifth working unit 28 and a sixth working unit 29, the six working units of the two groups of working units are uniformly arranged in the whole circumference direction of the bearing member 41, and the corresponding central angles of the two adjacent working units are 60 degrees; corresponding to the two sets of working units, the first preparation flow path 11 and the second preparation flow path 12 are respectively in preparation working positions, the first sampling flow path 31 and the second sampling flow path 32 are respectively in sampling working positions, and the first detection flow path 51 and the second detection flow path 52 are respectively in detection working positions;
correspondingly to the number of the working units, the first moving piece is provided with six first pipelines, the second moving piece is provided with six second pipelines, and when the first moving piece and the second moving piece move up and down, the first pipelines (the second pipelines) are connected and separated from the corresponding working units;
when the bearing member 41 rotates for one circle, each working unit undergoes a secondary working cycle, such as being located in a preparation working position, a sampling working position, a detection working position, a preparation working position, a sampling working position, and a detection working position in sequence; at the same time, two working units (such as a first working unit 21 and a fourth working unit 27) are prepared on line, two working units (such as a second working unit 22 and a fifth working unit 28) are sampled on line, and two working units (such as a third working unit 23 and a sixth working unit 29) are detected on line; the working unit is changed to the working position every 60 degrees of rotation of the carrier 41.
Example 4:
the application example of the system and the method for continuously monitoring the aldehyde ketone compound in the gas on line in the air monitoring according to the embodiment 1 of the invention is different from the embodiment 3 in that:
as shown in fig. 4, there are two sets of work units, each set of work units including three work units, the first set of work units including the first work unit 21, the second work unit 22, and the third work unit 23, and the second set of work units including the fourth work unit 27, the fifth work unit 28, and the sixth work unit 29; the three working units of each group of working units are uniformly arranged in the whole circumferential direction of the carrier 41, the central angle corresponding to two adjacent working units in each group is 120 degrees, that is, any working unit in the second group of working units is located between the adjacent working units of the first group of working units, and the central angle between the working units of the adjacent first group of working units and the working units of the second group of working units is less than 120 degrees, such as 30 degrees, 45 degrees, 60 degrees and 90 degrees; that is, the six working units are uniformly or non-uniformly arranged over the entire circumference of the carrier 41; the number and the positions of the first moving parts and the second moving upper pipelines are matched with the positions of the working units on the bearing parts;
every time the bearing member 41 rotates 120 degrees, the working units in each group of working units are shifted, but the working units in each group are not shifted, for example, the working units in the first group of working units are not shifted to the working positions corresponding to the second group of working units.
It can be seen that, for each rotation of the carrier 41, the same working unit undergoes a working cycle, i.e. is located at the preparation working position, the sampling working position and the detection working position at different times; at the same time, two working units are prepared on line, two working units are sampled on line, and two working units are detected on line.
The above embodiment shows the case of one or two groups of working units, but of course, there may be more groups, such as three, four or more groups, in which case, more preparation flow paths, sampling flow paths and detection flow paths need to be configured, and more pipelines need to be configured for the first moving member and the second moving member.
Claims (10)
1. The on-line continuous monitoring system for the aldehyde ketone compound in the gas comprises a detection unit; characterized in that the on-line continuous monitoring system for the aldehyde ketone compound in the gas further comprises:
the bearing piece is arranged on the base and driven by the driving module to rotate;
m groups of working units, wherein M is an integer not less than 1, each group of working units comprises P working units, and P is an integer not less than 3; the working unit is arranged on the bearing piece and comprises a silica gel column, and openings are formed in two ends of the silica gel column; in the rotation of the bearing piece, when one working unit in any group of working units is in the preparation working position, the other working units are respectively in the sampling working position and the detection working position, so that each working unit is sequentially in the preparation working position, the sampling working position and the detection working position;
the preparation flow path is arranged at the preparation working position, a silica gel column entering the preparation flow path forms a sampling column for adsorbing aldehyde ketone compounds, the sampling flow path is arranged at the sampling working position, the detection flow path is arranged at the detection working position, and the detection unit is positioned in the detection flow path;
and the control device is used for controlling whether the working unit at the preparation working position enters the preparation flow path, whether the working unit at the sampling working position enters the sampling flow path and whether the working unit at the detection working position enters the detection flow path.
2. The system for on-line continuous monitoring of aldehyde ketone compounds in a gas according to claim 1, wherein the control means comprises:
the device comprises a first moving part and a plurality of first pipelines, wherein the first pipelines are arranged on the first moving part and positioned on the upper side of a bearing part, and the preparation flow path, the sampling flow path and the detection flow path are respectively communicated with the first pipelines;
the second moving part is provided with a plurality of second pipelines, and the second pipelines are arranged on the second moving part and positioned at the lower side of the bearing part;
the first moving piece and the second moving piece are arranged on the guide rail respectively, the driving unit is used for driving the first moving piece and the second moving piece to move on the guide rail, so that the lower end of the first pipeline is connected and separated with an upper end opening of the working unit, and the upper end of the second pipeline is connected and separated with a lower end opening of the working unit.
3. The system for on-line continuous monitoring of an aldehyde ketone compound in a gas according to claim 2, wherein the production flow path comprises a first vessel, a first pump, a first column and a second column, and a second vessel connected in series; the second column is connected with the first pipeline, and the second container is connected with the second pipeline; DNPH powder is filled in the first column, and organic silica gel is filled in the second column;
a removing unit for removing the solvent entering the working unit of the preparation flow path.
4. The system for on-line continuous monitoring of an aldehyde ketone compound in a gas of claim 3, wherein the production flow path further comprises:
a first switching module for selectively communicating an outlet of the first pump with the first column and a second conduit;
a second switching module for selectively communicating the second column with the first column and a second vessel.
5. The system for on-line continuous monitoring of aldehyde ketone compounds in a gas according to claim 3, wherein the purge unit comprises:
a gas source providing a purge gas;
and the third switching module is used for enabling the working unit entering the preparation flow path to be selectively communicated with the gas source and the second column.
6. The system for on-line continuous monitoring of aldehyde ketone compounds in a gas of claim 3, wherein the first container comprises a cleaning solution container and a coating solution container;
the fourth switching module is used for enabling the inlet of the first pump to be selectively communicated with the cleaning solution container and the coating solution container.
7. The system for on-line continuous monitoring of an aldehyde ketone compound in a gas of claim 2, wherein the sampling flow path comprises:
one end of the pretreatment unit is communicated with air, and the other end of the pretreatment unit is connected with the second pipeline;
a second pump connected to the first conduit.
8. The system for on-line continuous monitoring of an aldehyde ketone compound in a gas of claim 2, wherein the detection flow path comprises:
the cleaning solution container, the third pump and the first pipeline are sequentially connected;
the sample container is connected with the second pipeline, and the detection unit is connected with the sample container.
9. A method for on-line continuous monitoring of an aldehyde ketone compound in a gas using the system for on-line continuous monitoring of an aldehyde ketone compound in a gas according to any one of claims 1 to 8, the method for on-line continuous monitoring of an aldehyde ketone compound in a gas comprising:
the bearing piece rotates, when one working unit in any group of working units is in the preparation working position, the other working units are respectively in the sampling working position and the detection working position;
under the control of the control device, the working unit at the preparation working position enters the preparation flow path, the silica gel column forms a sampling column for adsorbing aldehyde ketone compounds, the prepared sampling column at the sampling working position enters the sampling flow path, the aldehyde ketone compounds in the environment to be detected are adsorbed, and the sampling column at the detection working position which finishes sampling enters the detection flow path;
under the control of the control device, the prepared working unit at the preparation working position is separated from the preparation flow path, the sampling column at the sampling working position is separated from the sampling flow path, and the sampling column at the detection working position is separated from the detection flow path;
and the bearing piece further rotates, so that each working unit is sequentially positioned at a preparation working position, a sampling working position and a detection working position, and the operation is circulated.
10. The method according to claim 9, wherein the silica gel column forms a sampling column in the preparation flow path by:
the cleaning solution sequentially passes through a silica gel column and a second column, and organic silica gel is filled in the second column;
the coating solution sequentially passes through a first column, a second column and a silica gel column, and DNPH powder is filled in the first column;
and removing the solvent in the silica gel column, wherein the silica gel column forms a sampling column.
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