CN111829854A - On-line preparation system and method for water-soluble anion and cation samples in atmosphere - Google Patents

On-line preparation system and method for water-soluble anion and cation samples in atmosphere Download PDF

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Publication number
CN111829854A
CN111829854A CN202010784547.0A CN202010784547A CN111829854A CN 111829854 A CN111829854 A CN 111829854A CN 202010784547 A CN202010784547 A CN 202010784547A CN 111829854 A CN111829854 A CN 111829854A
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sampling
tank
sample
area
waste liquid
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付文陈
吕国亭
赵凤龙
王清泉
黄宁
任娜
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Qingdao Rongguang Electronic Technology Co ltd
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Qingdao Rongguang Electronic Technology Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
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Abstract

The invention discloses an on-line preparation system and a method of water-soluble anion and cation samples in atmosphere, wherein the system comprises an atmosphere sampling area, a particulate matter collecting area, a standing oscillation area, a sample infiltration area, a sample liquid storage area and a waste liquid area; the atmospheric sampling area comprises a particle size cutter, a flow controller and a sampling pump; the particle collection area comprises a multi-position turntable I which bears a filter membrane clamp; the standing oscillation area comprises a sampling tank, the upper part of the sampling tank is provided with an ultrapure water adding hole, an exhaust hole and a filter membrane clamping inlet, the bottom of the sampling tank is provided with a lower discharge port, an ultrasonic vibrator is arranged, and the sampling tank is connected with the particulate matter collecting area through a mechanical arm; the sample percolation region comprises a multi-position rotating disc II which carries a percolation clamp; the sample liquid storage area comprises a storage tank, a standard solution adding port, a sample liquid inlet and a sample liquid outlet are formed in the upper portion of the storage tank, and a waste liquid outlet is formed in the bottom of the storage tank. The system and the method disclosed by the invention are simple to operate, efficient in preparation, capable of realizing automation and convenient to operate on site.

Description

On-line preparation system and method for water-soluble anion and cation samples in atmosphere
Technical Field
The invention belongs to the field of environmental air detection equipment, and particularly relates to an online preparation system and method for water-soluble anion and cation samples in atmosphere.
Background
In recent years, environmental air particulate matter pollution is increasingly serious, and atmospheric particulate matters (including total suspended particulate matters TSP, inhalable particulate matters PM10 and fine particulate matters PM2.5) are a large class of important atmospheric indexes specified in environmental air quality standards (GB3095-2012), have obvious climate effect and have serious harm to human bodies.
At present, most of instruments for preparing the anion and cation samples in the atmospheric particulates are applied to laboratory detection, manual operation is mainly used in methods such as static soaking, ultrasonic oscillation, suction filtration and the like, the collected samples need to be soaked in ultrapure water for a certain time, then ultrasonic oscillation is carried out, water-soluble anions and cations in the atmospheric particulates are completely dissolved in water, and finally extraction liquid is subjected to suction filtration through a 0.45-micrometer membrane to obtain the water-soluble anion and cation preparation liquid for the atmospheric particulates. This kind of mode complex operation, with high costs, inefficiency, external environment is great to the influence of extraction process, is not convenient for operate outside the laboratory, can't satisfy the demand of atmosphere witnessed inspections.
Disclosure of Invention
In order to solve the technical problems, the invention provides an on-line preparation system and method for water-soluble anion and cation samples in the atmosphere, so as to achieve the purposes of simple operation, high preparation efficiency, automation realization and convenience for field operation.
In order to achieve the purpose, the technical scheme of the invention is as follows:
an on-line preparation system of water-soluble anion and cation samples in the atmosphere,
comprises an atmospheric sampling area, a particulate matter collecting area, a standing oscillation area, a sample infiltration area, a sample liquid storage area and a waste liquid area;
the atmospheric sampling area comprises a particle size cutter, a flow controller and a sampling pump;
the particle collection area comprises a first multi-position rotary table which bears a filter membrane clamp, a sampling filter membrane is supported and fixed through the filter membrane clamp, the first multi-position rotary table is connected with the particle size cutter through a sampling pipeline, and the flow controller and the sampling pump are arranged on the sampling pipeline;
the static oscillation area comprises a sampling tank, an ultrapure water adding hole, an exhaust hole and a filter membrane clamping inlet are formed in the upper portion of the sampling tank, a lower discharge port is formed in the bottom of the sampling tank, an ultrasonic vibrator is installed outside the bottom of the sampling tank, the ultrapure water adding hole is connected with an ultrapure water storage tank through a pipeline, and the sampling tank is connected with the first multi-position turntable through a mechanical arm;
the sample percolation area comprises a multi-position rotating disc II which bears a percolation clamp, a percolation film is supported and fixed through the percolation clamp, and the multi-position rotating disc II is connected with the sampling tank through a sample pipeline I;
the sample liquid storage area comprises a storage tank, the upper part of the storage tank is provided with a standard solution adding port, a sample liquid inlet and a sample liquid outlet, the bottom of the storage tank is provided with a waste liquid outlet, and the sample liquid inlet is connected with a multi-position turntable II through a sample pipeline II;
the waste liquid area comprises a waste liquid tank, and the waste liquid outlet is connected with the waste liquid tank through a waste liquid pipeline.
In the scheme, a vacancy hole is reserved on the second multi-position rotating disc and is used for flowing through of liquid during cleaning.
In the scheme, the upper cover and the lower cover of the infiltration clamp are tapered and used for sealing the edge of the infiltration membrane.
In the above scheme, the first sample pipeline is provided with a flow control pump.
In the scheme, the waste liquid tank is made of acid-base corrosion resistant polytetrafluoroethylene.
In the above scheme, a control valve is arranged on the waste liquid pipeline.
An online preparation method of water-soluble anion and cation samples in the atmosphere adopts the online preparation system of the water-soluble anion and cation samples in the atmosphere, and comprises the following processes:
(1) system self-checking: before the system runs, whether a filter membrane clamp is arranged in a particulate matter collecting area or not, whether ultrapure water exists in an ultrapure water storage tank or not, whether a multi-position turntable of a sample percolation area is rotated to an empty hole or not and whether a waste liquid tank is full or not are checked;
(2) sampling and cleaning: after the self-checking is finished, starting a sampling pump to start atmospheric sampling; simultaneously, starting a cleaning program, enabling ultrapure water to enter a sampling tank, enabling an ultrasonic vibrator to start working, carrying out ultrasonic cleaning on the sampling tank, enabling cleaning liquid to enter the storage tank through a vacancy hole in a multi-position turntable II of the sample infiltration area after cleaning is finished, and discharging the cleaning liquid into a waste liquid tank through a waste liquid outlet in the bottom of the storage tank;
(3) preparing a sample solution: after cleaning is finished and the set sampling time is reached, the mechanical arm clamps a filter membrane clamp on the first multi-position turntable into a sampling tank, ultrapure water enters the sampling tank to soak the filter membrane clamp, an ultrasonic vibrator at the lower end of the sampling tank starts to work after soaking is finished, the ultrasonic vibrator stops working after ultrasonic oscillation for a certain time, and the filter membrane clamp is lifted to be above the liquid level by the mechanical arm; opening a flow control pump at the lower end of the sampling tank, carrying out leakage percolation on the sample liquid, and opening a control valve at the lower end of the storage tank after the percolation starts, so that the liquid with the front end passing through the percolation membrane is discharged into a waste liquid tank; after a period of percolation, closing the control valve to leave the percolate in the storage tank for sampling by the external detection unit;
(4) resetting the system: after the infiltration is finished, the filter membrane clamp is clamped back to the first multi-position turntable by the mechanical arm, and after the sampling of the detection unit is finished, the control valve at the lower end of the storage tank is opened to discharge liquid into the waste liquid tank.
Through the technical scheme, the on-line preparation system and the method for the water-soluble anion and cation sample can carry out on-site real-time sampling, are convenient to operate, realize automatic on-line preparation of the water-soluble anion and cation sample, and facilitate the subsequent sampling detection of the detection unit ion chromatogram. The system and the method provided by the invention are simple to operate, low in cost, high in preparation efficiency and good in application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a schematic diagram of an on-line preparation system for water-soluble anion and cation samples in the atmosphere according to an embodiment of the present invention;
FIG. 2 is a schematic view of an atmospheric sampling region and a particulate collection region according to an embodiment of the disclosure;
fig. 3 is a schematic structural diagram of a multi-position turntable according to an embodiment of the present invention.
In the figure, A, an atmosphere sampling area; B. a particulate matter collection zone; C. standing the oscillation area; D. a sample percolation region; E. a sample liquid storage region; F. a waste liquid zone; 1. a particle size cutter; 2. a flow controller; 3. a sampling pump; 4. filter membrane clamping; 5. a first multi-position rotating disc; 6. sampling a filter membrane; 7. a sampling pipeline; 8. a sampling tank; 9. an ultrapure water addition hole; 10. an exhaust hole; 11. the filter membrane clamps the inlet; 12. a lower discharge port; 13. an ultrasonic vibrator; 14. an ultra-pure water storage tank; 15. percolating and clamping; 16. a second multi-position rotating disc; 17. a void hole; 18. filtering the membrane; 19. a first sample pipeline; 20. a flow control pump; 21. storing the tank; 22. a standard solution addition port; 23. a sample fluid inlet; 24. a sample liquid outlet; 25. a pump; 26. a detection unit; 27. a waste liquid tank; 28. a waste liquid line; 29. a control valve; 30. a mechanical arm; 31. a waste liquid outlet; 32. and a second sample pipeline.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
The invention provides an on-line preparation system of water-soluble anion and cation samples in atmosphere, which comprises an atmosphere sampling area A, a particulate matter collecting area B, a standing oscillation area C, a sample infiltration area D, a sample liquid storage area E and a waste liquid area F, as shown in figure 1.
The atmospheric sampling area A comprises a particle size cutter 1, a flow controller 2 and a sampling pump 3; the particle size cutter 1 is used for cutting particles with different particle sizes of TSP, PM2.5 and PM10, the flow controller 2 is used for setting sampling flow, and low, medium and high flows can be switched according to different standards; the sampling pump 3 provides the collection power of the atmospheric sample.
As shown in FIG. 2, the particulate collection zone B comprises a multi-position rotating disk 5 carrying filter holders 4 for sequential sampling. The sampling filter membrane 6 is supported and fixed through the filter membrane clamp 4, the multi-position rotating disc I5 and the particle size cutter 1 are connected through the sampling pipeline 7, and the flow controller 2 and the sampling pump 3 are arranged on the sampling pipeline 7.
The standing oscillation area C comprises a sampling tank 8 made of polyethylene, an ultrapure water adding hole 9, an exhaust hole 10 and a filter membrane clamping inlet 11 are formed in the upper portion of the sampling tank 8, a lower discharge port 12 is formed in the bottom of the sampling tank 8, an ultrasonic vibrator 13 is installed outside the bottom of the sampling tank 8, the ultrapure water adding hole 9 is connected with an ultrapure water storage tank 14 through a pipeline and used for adding ultrapure water, and the ultrapure water is quantitatively added into the sampling tank 8 through a pump 25 and used for cleaning the sampling tank 8 and soaking the sampling filter membrane 6; the exhaust hole 10 is used for exhausting gas during ultrasonic oscillation; the sampling tank 8 is connected with the first position rotating disc 5 through a mechanical arm 30, the filter membrane clamp 4 is placed into ultrapure water which is added into the sampling tank 8 in advance through a filter membrane clamp inlet 11 by the mechanical arm 30 to be soaked, after the ultrapure water is soaked for a certain time, the ultrasonic vibrator 13 at the lower end of the sampling tank 8 starts to work, liquid in the sampling tank 8 is subjected to ultrasonic oscillation, and water-soluble anions and cations are completely dissolved in the ultrapure water.
The sample infiltration region D comprises a second multi-position rotating disc 16 which carries an infiltration clamp 15 and is used for infiltration of pretreated sample liquid, and because the aperture of the ion chromatography injection valve body of the detection unit 26 is required to be less than 0.45 mu m, a sample needs to be infiltrated by a filter membrane with the diameter of 0.45 mu m so as not to block the injection valve. As shown in FIG. 3, the second multi-position rotary plate 16 is provided with a hole 17 for allowing the liquid to flow through during the cleaning process. The infiltration membrane 18 is supported and fixed by the infiltration clamp 15, and the infiltration clamp 15 is provided with a conical upper cover and a conical lower cover for sealing the edge of the infiltration membrane 18. The second multi-position rotating disc 16 is connected with the sampling tank 8 through a first sample pipeline 19, a flow control pump 20 is arranged on the first sample pipeline 19, and when the sample is preprocessed in the standing oscillation area C, the flow control pump 20 is in a closed state.
The sample liquid reservoir E is used to collect the diafiltered sample and provide a sample for ion chromatography in the detection unit 26. The sample liquid storage area E comprises a storage tank 21, the upper part of the storage tank 21 is provided with a standard solution adding port 22, a sample liquid inlet 23 and a sample liquid outlet 24, and the bottom part is provided with a waste liquid outlet 31; the standard solution adding port 22 is used for adding a standard solution and is used for timing calibration or standard addition comparison; the sample liquid inlet 23 is connected with the second multi-position rotating disc 16 through a second sample pipeline 32, and the sample liquid outlet 24 is connected with the sample injection unit of the detection unit 26 through a pump 25.
The waste liquid area F comprises a waste liquid tank 27 for containing all waste liquid generated by the instrument, a waste liquid outlet 31 is connected with the waste liquid tank 27 through a waste liquid pipeline 28, and a control valve 29 is arranged on the waste liquid pipeline 28. The waste liquid tank 27 is made of acid-base corrosion-resistant polytetrafluoroethylene.
An online preparation method of water-soluble anion and cation samples in the atmosphere adopts the online preparation system of the water-soluble anion and cation samples in the atmosphere, and comprises the following processes:
(1) system self-checking: before the system runs, whether the filter membrane clamp 4 is arranged in the particle collection area or not, whether ultrapure water exists in the ultrapure water storage tank 14 or not, whether the multi-position turntable II 16 of the sample infiltration area D rotates to the vacancy hole 17 or not and whether the waste liquid tank 27 is full or not are checked; if all is normal, the system starts sampling after 10s after the self-checking passes, and if the self-checking item does not pass, the system displays an alarm prompt.
(2) Sampling and cleaning: after the self-checking is finished, starting a sampling pump to start atmospheric sampling; and simultaneously, starting a cleaning program, enabling ultrapure water to enter the sampling tank 8 through the pump 25, enabling the ultrasonic vibrator 13 to work, carrying out ultrasonic cleaning on the sampling tank 8, and after the cleaning is finished, enabling the cleaning liquid to directly enter the storage tank 21 through the vacancy hole 17 on the second multi-position rotating disc 16 of the sample infiltration area D and be discharged into the waste liquid tank 27 through the waste liquid outlet 31 at the bottom of the storage tank 21.
(3) Preparing a sample solution: after the cleaning is finished, the set sampling time is reached, and the sampling time can be set according to the actual situation. Specifically, reference can be made to HJ799-2016 (F) water-soluble anions in ambient air particles-、Cl-、Br-、NO2-、NO3-、PO4 3-、SO3 2-、SO4 2-) To measureFixed ion chromatography and HJ800-2016 (Li) water-soluble cations in ambient air particulate matter+、Na+、NH4 +、K+、Ca2+、Mg2+) Measurement of ion chromatography (CRLC). The mechanical arm 30 clamps the filter membrane clamp 4 on the multi-position rotating disc I5 into the sampling tank 8, ultrapure water enters the sampling tank 8 through the pump 25 to soak the filter membrane clamp 4, the ultrasonic vibrator 13 at the lower end of the sampling tank 8 starts to work after soaking is finished, the ultrasonic vibrator 13 stops working after ultrasonic oscillation for a certain time, and the filter membrane clamp 4 is lifted to the position above the liquid level by the mechanical arm 30; after the sampling filter membrane 6 is soaked and ultrasonically oscillated, water-soluble anions and cations in the particulate matters are completely dissolved in the solution in the sampling tank 8, and the pretreated sample liquid is obtained. Opening the flow control pump 20 at the lower end of the sampling tank 8 to perform leakage percolation on the sample liquid, and opening the control valve 29 at the lower end of the storage tank 21 after the percolation starts, so that the liquid with the front end passing through the percolation membrane is discharged into the waste liquid tank 27; after a certain time of percolation, the control valve 29 is closed to store the percolating fluid in the storage tank 21 for sampling by the external detection unit.
(4) Resetting the system: and after the percolation is finished, the filter membrane clamp 4 is clamped back to the multi-position turntable I5 through the mechanical arm 30, after the sampling of the detection unit 26 is finished, the control valve 29 at the lower end of the storage tank 21 is opened, the liquid is discharged into the waste liquid tank 27, and the system finishes one-time operation. The system can set the cycle number to continuously run.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (7)

1. An on-line preparation system of water-soluble anion and cation samples in atmosphere is characterized by comprising an atmosphere sampling area, a particulate matter collecting area, a standing oscillation area, a sample infiltration area, a sample liquid storage area and a waste liquid area;
the atmospheric sampling area comprises a particle size cutter, a flow controller and a sampling pump;
the particle collection area comprises a first multi-position rotary table which bears a filter membrane clamp, a sampling filter membrane is supported and fixed through the filter membrane clamp, the first multi-position rotary table is connected with the particle size cutter through a sampling pipeline, and the flow controller and the sampling pump are arranged on the sampling pipeline;
the static oscillation area comprises a sampling tank, an ultrapure water adding hole, an exhaust hole and a filter membrane clamping inlet are formed in the upper portion of the sampling tank, a lower discharge port is formed in the bottom of the sampling tank, an ultrasonic vibrator is installed outside the bottom of the sampling tank, the ultrapure water adding hole is connected with an ultrapure water storage tank through a pipeline, and the sampling tank is connected with the first multi-position turntable through a mechanical arm;
the sample percolation area comprises a multi-position rotating disc II which bears a percolation clamp, a percolation film is supported and fixed through the percolation clamp, and the multi-position rotating disc II is connected with the sampling tank through a sample pipeline I;
the sample liquid storage area comprises a storage tank, the upper part of the storage tank is provided with a standard solution adding port, a sample liquid inlet and a sample liquid outlet, the bottom of the storage tank is provided with a waste liquid outlet, and the sample liquid inlet is connected with a multi-position turntable II through a sample pipeline II;
the waste liquid area comprises a waste liquid tank, and the waste liquid outlet is connected with the waste liquid tank through a waste liquid pipeline.
2. The system for the in-situ preparation of samples of water-soluble anions and cations in the atmosphere of claim 1, wherein the second multi-position rotating disc is provided with a hole for allowing the liquid to flow through during cleaning.
3. The system for on-line preparation of samples of water-soluble anions and cations in the atmosphere of claim 1, wherein the percolation clamp is tapered at the top and bottom for edge sealing of the percolation membrane.
4. The system for the on-line preparation of samples of water-soluble anions and cations in the atmosphere as claimed in claim 1, wherein the first sample pipeline is provided with a flow control pump.
5. The system for on-line preparation of samples of water-soluble anions and cations in the atmosphere according to claim 1, wherein the waste liquid tank is made of acid and alkali corrosion resistant polytetrafluoroethylene.
6. The system for the on-line preparation of samples of water-soluble anions and cations in the atmosphere according to claim 1 or 5, wherein the waste liquid pipeline is provided with a control valve.
7. An online preparation method of water-soluble anion and cation samples in the atmosphere, which adopts the online preparation system of water-soluble anion and cation samples in the atmosphere as claimed in claim 2, and is characterized by comprising the following steps:
(1) system self-checking: before the system runs, whether a filter membrane clamp is arranged in a particulate matter collecting area or not, whether ultrapure water exists in an ultrapure water storage tank or not, whether a multi-position turntable of a sample percolation area is rotated to an empty hole or not and whether a waste liquid tank is full or not are checked;
(2) sampling and cleaning: after the self-checking is finished, starting a sampling pump to start atmospheric sampling; simultaneously, starting a cleaning program, enabling ultrapure water to enter a sampling tank, enabling an ultrasonic vibrator to start working, carrying out ultrasonic cleaning on the sampling tank, enabling cleaning liquid to enter the storage tank through a vacancy hole in a multi-position turntable II of the sample infiltration area after cleaning is finished, and discharging the cleaning liquid into a waste liquid tank through a waste liquid outlet in the bottom of the storage tank;
(3) preparing a sample solution: after cleaning is finished and the set sampling time is reached, the mechanical arm clamps a filter membrane clamp on the first multi-position turntable into a sampling tank, ultrapure water enters the sampling tank to soak the filter membrane clamp, an ultrasonic vibrator at the lower end of the sampling tank starts to work after soaking is finished, the ultrasonic vibrator stops working after ultrasonic oscillation for a certain time, and the filter membrane clamp is lifted to be above the liquid level by the mechanical arm; opening a flow control pump at the lower end of the sampling tank, carrying out leakage percolation on the sample liquid, and opening a control valve at the lower end of the storage tank after the percolation starts, so that the liquid with the front end passing through the percolation membrane is discharged into a waste liquid tank; after a period of percolation, closing the control valve and leaving the percolating liquid in the storage tank for sampling by the external detection unit;
(4) resetting the system: after the infiltration is finished, the filter membrane clamp is clamped back to the first multi-position turntable by the mechanical arm, and after the sampling of the detection unit is finished, the control valve at the lower end of the storage tank is opened to discharge liquid into the waste liquid tank.
CN202010784547.0A 2020-08-06 2020-08-06 On-line preparation system and method for water-soluble anion and cation samples in atmosphere Pending CN111829854A (en)

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