An online preparation system and method for water-soluble anion and cation samples in the atmosphere

Abstract

The invention discloses an online preparation system and method for water-soluble anion and cation samples in the atmosphere, the system comprises an atmosphere sampling area, a particle collection area, a static oscillation area, a sample percolation area, a sample liquid storage area and a waste liquid area; the atmosphere sampling area comprises a particle size cutter, a flow controller and a sampling pump; the particle collection area comprises a multi-position turntable 1 carrying a filter membrane clip; the static oscillation area comprises a sampling tank, the upper part of the sampling tank is provided with an ultrapure water addition hole, an exhaust hole and a filter membrane clip placement inlet, the bottom is provided with a lower discharge port, and an ultrasonic vibrator is installed, and the sampling tank and the particle collection area are connected by a mechanical arm; the sample percolation area comprises a multi-position turntable 2 carrying a percolation clip; the sample liquid storage area comprises a storage tank, the upper part of the storage tank is provided with a standard solution addition port, a sample liquid inlet and a sample liquid outlet, and the bottom is provided with a waste liquid outlet. The system and method disclosed by the invention are simple to operate, efficient in preparation, can be automated, and are convenient to operate on site.

Description

Technical Field

[0001] The invention belongs to the field of ambient air detection equipment, and in particular relates to an online preparation system and method for water-soluble anion and cation samples in the atmosphere. Background Art

[0002] In recent years, ambient air particulate pollution has become increasingly serious. Atmospheric particulate matter (including total suspended particulate matter TSP, inhalable particulate matter PM10, and fine particulate matter PM2.5) is a large category of important atmospheric indicators stipulated in the "Ambient Air Quality Standard" (GB3095-2012). It has significant climate effects and is also seriously harmful to the human body.

[0003] At present, the instruments for preparing anion and cation samples in atmospheric particulate matter are mostly used for laboratory testing. Static immersion, ultrasonic vibration, filtration and other methods are mainly manual operations. The collected samples need to be immersed in ultrapure water for a certain period of time, and then ultrasonic vibration is performed to make the water-soluble anions and cations in the atmospheric particulate matter completely dissolved in the water. Finally, the extract is filtered through a 0.45μm membrane to obtain the water-soluble anion and cation preparation solution of atmospheric particulate matter. This method is cumbersome, costly, and inefficient. The external environment has a greater impact on the extraction process. It is not convenient to operate outside the laboratory and cannot meet the needs of atmospheric field testing. Summary of the invention

[0004] In order to solve the above technical problems, the present invention provides an online preparation system and method for water-soluble anion and cation samples in the atmosphere, so as to achieve the purpose of simple operation, efficient preparation, automation and convenience for on-site operation.

[0005] To achieve the above object, the technical solution of the present invention is as follows:

[0006] An online preparation system for water-soluble anion and cation samples in the atmosphere.

[0007] It includes the atmospheric sampling area, the particulate matter collection area, the static oscillation area, the sample infiltration area, the sample liquid storage area and the waste liquid area;

[0008] The atmospheric sampling area includes a particle size cutter, a flow controller and a sampling pump;

[0009] The particle collection area includes a multi-position turntable 1 carrying a filter membrane clamp, the sampling filter membrane is supported and fixed by the filter membrane clamp, the multi-position turntable 1 is connected to the particle size cutter through a sampling pipeline, and the flow controller and the sampling pump are arranged on the sampling pipeline;

[0010] The static oscillation zone includes a sampling tank, an ultrapure water adding hole, an exhaust hole and a filter membrane clamping inlet are arranged on the upper part of the sampling tank, a lower exhaust port is arranged at the bottom of the sampling tank, and an ultrasonic vibrator is installed outside the bottom of the sampling tank, the ultrapure water adding hole is connected to the ultrapure water storage tank through a pipeline, and the sampling tank is connected to the multi-position turntable through a mechanical arm;

[0011] The sample filtration area includes a multi-position turntable 2 carrying a filtration clip, the filtration membrane is supported and fixed by the filtration clip, and the multi-position turntable 2 is connected to the sampling tank through a sample pipeline 1;

[0012] The sample liquid storage area comprises a storage tank, the upper part of which is provided with a standard solution addition port, a sample liquid inlet and a sample liquid outlet, and the bottom of which is provided with a waste liquid outlet, and the sample liquid inlet is connected to a multi-position turntable 2 through a sample pipeline 2;

[0013] The waste liquid area includes a waste liquid tank, and the waste liquid outlet is connected to the waste liquid tank via a waste liquid pipeline.

[0014] In the above scheme, an empty hole is left on the multi-position turntable 2 for the liquid to flow through during cleaning.

[0015] In the above scheme, the upper and lower covers of the filtration clamp are formed into a cone shape, which is used to seal the edge of the filtration membrane.

[0016] In the above solution, a flow control pump is provided on the sample pipeline.

[0017] In the above solution, the waste liquid tank is made of polytetrafluoroethylene material which is resistant to acid and alkali corrosion.

[0018] In the above solution, a control valve is provided on the waste liquid pipeline.

[0019] An online preparation method for water-soluble anions and cations in the atmosphere, using the above-mentioned online preparation system for water-soluble anions and cations in the atmosphere, includes the following process:

[0020] (1) System self-check: Before the system is put into operation, check whether there is a filter membrane clip in the particle collection area, whether there is ultrapure water in the ultrapure water storage tank, whether the multi-position turntable 2 in the sample filtration area is turned to an empty hole, and whether the waste liquid tank is full;

[0021] (2) Sampling and cleaning: After the self-test is completed, the sampling pump is started and atmospheric sampling begins; at the same time, the cleaning procedure begins, ultrapure water enters the sampling tank, and the ultrasonic vibrator starts working to ultrasonically clean the sampling tank. After the cleaning is completed, the cleaning liquid enters the storage tank through the empty holes on the multi-position turntable 2 in the sample percolation area, and is discharged into the waste liquid tank through the waste liquid outlet at the bottom of the storage tank;

[0022] (3) Sample liquid preparation: After cleaning is completed and the set sampling time is reached, the robot arm clamps the filter membrane clamp on the multi-position turntable into the sampling tank, and ultrapure water enters the sampling tank to soak the filter membrane clamp. After soaking, the ultrasonic vibrator at the lower end of the sampling tank starts to work. After a certain period of ultrasonic oscillation, the ultrasonic vibrator stops working, and the filter membrane clamp is lifted by the robot arm to above the liquid surface; the flow control pump at the lower end of the sampling tank is turned on to drip and filter the sample liquid. After the filtration starts, the control valve at the lower end of the storage tank is opened to allow the liquid passing through the filtration membrane at the front end to be discharged into the waste liquid tank; after a period of filtration, the control valve is closed to leave the leaked liquid in the storage tank for sampling by the external detection unit;

[0023] (4) System reset: After the filtration is completed, the filter membrane clamp is clamped back to the multi-position turntable by the mechanical arm. After the detection unit sampling is completed, the control valve at the lower end of the storage tank is opened to discharge the liquid into the waste liquid tank.

[0024] Through the above technical scheme, the online preparation system and method of water-soluble anion and cation samples provided by the present invention can perform real-time sampling on site, is easy to operate, and realizes automatic online preparation of water-soluble anion and cation samples, which is convenient for subsequent detection unit ion chromatography to perform sampling and detection. The system and method of the present invention are simple to operate, low in cost, high in preparation efficiency, and have good application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art are briefly introduced below.

[0026] Figure 1 A schematic diagram of an online preparation system for water-soluble anion and cation samples in the atmosphere disclosed in an embodiment of the present invention;

[0027] Figure 2 This is a schematic diagram of the structure of the atmosphere sampling area and the particulate matter collection area disclosed in the embodiment of the present invention;

[0028] Figure 3 This is a schematic diagram of the structure of the multi-position turntable 2 disclosed in an embodiment of the present invention.

[0029] In the figure, A, atmospheric sampling area; B, particle collection area; C, static oscillation area; D, sample percolation area; E, sample liquid storage area; F, waste liquid area; 1, particle size cutter; 2, flow controller; 3, sampling pump; 4, filter membrane clamp; 5, multi-position turntable 1; 6, sampling filter membrane; 7, sampling pipeline; 8, sampling tank; 9, ultrapure water addition hole; 10, exhaust hole; 11, filter membrane clamp inlet; 12, lower outlet; 13, ultrasonic vibrator; 14 , ultrapure water storage tank; 15, filtration clamp; 16, multi-position turntable 2; 17, empty hole; 18, filtration membrane; 19, sample pipeline 1; 20, flow control pump; 21, storage tank; 22, standard solution addition port; 23, sample solution inlet; 24, sample solution outlet; 25, pump; 26, detection unit; 27, waste liquid tank; 28, waste liquid pipeline; 29, control valve; 30, robotic arm; 31, waste liquid outlet; 32, sample pipeline 2. DETAILED DESCRIPTION

[0030] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0031] The present invention provides an online preparation system for water-soluble anion and cation samples in the atmosphere, such as Figure 1 As shown, the system includes an atmosphere sampling area A, a particulate matter collection area B, a static oscillation area C, a sample filtration area D, a sample liquid storage area E and a waste liquid area F.

[0032] The atmospheric sampling area A includes a particle size cutter 1, a flow controller 2 and a sampling pump 3; the particle size cutter 1 is used to cut particles of different sizes such as TSP, PM2.5 and PM10, and the flow controller 2 is used to set the sampling flow rate, which can switch between low, medium and high flow rates according to different standards; the sampling pump 3 provides power for collecting atmospheric samples.

[0033] like Figure 2 As shown, the particle collection area B includes a multi-position turntable 5 carrying a filter membrane clamp 4, which can be used for continuous sampling. The sampling filter membrane 6 is supported and fixed by the filter membrane clamp 4, and the multi-position turntable 5 is connected to the particle size cutter 1 through a sampling pipeline 7, and the flow controller 2 and the sampling pump 3 are arranged on the sampling pipeline 7.

[0034] The static oscillation zone C includes a sampling tank 8 made of polyethylene material, with an ultrapure water adding hole 9, an exhaust hole 10 and a filter membrane clamp inlet 11 on the upper part of the sampling tank 8, a lower outlet 12 at the bottom of the sampling tank 8, and an ultrasonic vibrator 13 installed outside the bottom of the sampling tank 8. The ultrapure water adding hole 9 is connected to the ultrapure water storage tank 14 through a pipeline for adding ultrapure water. Ultrapure water is quantitatively added to the sampling tank 8 through a pump 25 for cleaning the sampling tank 8 and soaking the sampling filter membrane 6; the exhaust hole 10 is used for exhaust during ultrasonic oscillation; the sampling tank 8 is connected to the turntable 5 through a mechanical arm 30, and the filter membrane clamp 4 is placed by the mechanical arm 30 through the filter membrane clamp inlet 11 into the ultrapure water that has been pre-added to the sampling tank 8 for soaking. After soaking for a certain period of time, the ultrasonic vibrator 13 at the lower end of the sampling tank 8 starts to work, ultrasonically oscillates the liquid in the sampling tank 8, and the water-soluble anions and cations are completely dissolved in the ultrapure water.

[0035] The sample filtration area D includes a multi-position turntable 16 carrying a filtration clip 15, which is used for filtration of the sample liquid after pretreatment. Since the aperture of the ion chromatographic injection valve body of the detection unit 26 is required to be less than 0.45μm, the sample needs to be filtered through a 0.45μm filter membrane to avoid clogging the injection valve. Figure 3 As shown, a vacant hole 17 is left on the multi-position turntable 2 16 for the liquid to flow through during cleaning. The filtration membrane 18 is supported and fixed by the filtration clamp 15. The upper and lower covers of the filtration clamp 15 are conical and used to seal the edge of the filtration membrane 18. The multi-position turntable 2 16 is connected to the sampling tank 8 through the sample pipeline 19. The sample pipeline 19 is provided with a flow control pump 20. When the sample is pre-treated in the static oscillation zone C, the flow control pump 20 is in a closed state.

[0036] The sample liquid storage area E is used to collect samples after diafiltration and provide samples for the ion chromatograph of the detection unit 26. The sample liquid storage area E includes a storage tank 21, the upper part of which is provided with a standard solution addition port 22, a sample liquid inlet 23 and a sample liquid outlet 24, and the bottom of which is provided with a waste liquid outlet 31; the standard solution addition port 22 is used for adding a standard solution, for timed calibration or standard addition comparison; the sample liquid inlet 23 is connected to the multi-position turntable 2 16 through a sample pipeline 2 32, and the sample liquid outlet 24 is connected to the sample injection unit of the detection unit 26 through a pump 25.

[0037] The waste liquid area F includes a waste liquid tank 27 for containing all waste liquid generated by the instrument. The waste liquid outlet 31 is connected to the waste liquid tank 27 via a waste liquid pipeline 28, and a control valve 29 is provided on the waste liquid pipeline 28. The waste liquid tank 27 is made of polytetrafluoroethylene material that is resistant to acid and alkali corrosion.

[0038] An online preparation method for water-soluble anions and cations in the atmosphere, using the above-mentioned online preparation system for water-soluble anions and cations in the atmosphere, includes the following process:

[0039] (1) System self-check: Before the system is put into operation, check whether there is a filter membrane clip 4 in the particle collection area, whether there is ultrapure water in the ultrapure water storage tank 14, whether the multi-position turntable 2 16 in the sample filtration area D is turned to the empty hole 17, and whether the waste liquid tank 27 is full. If everything is normal, the system will start sampling 10 seconds after the self-check passes. If any of the self-check items fail, the system will display an alarm prompt.

[0040] (2) Sampling and cleaning: After the self-test is completed, the sampling pump is started and atmospheric sampling begins. At the same time, the cleaning procedure begins. Ultrapure water enters the sampling tank 8 through the pump 25. The ultrasonic vibrator 13 starts working to perform ultrasonic cleaning on the sampling tank 8. After the cleaning is completed, the cleaning liquid directly enters the storage tank 21 through the empty hole 17 on the multi-position turntable 2 16 in the sample filtration area D, and is discharged into the waste liquid tank 27 through the waste liquid outlet 31 at the bottom of the storage tank 21.

[0041] (3) Sample solution preparation: After cleaning is completed and the set sampling time is reached, the sampling time can be set according to the actual situation. For details, please refer to HJ799-2016 "Water-soluble anions (F - , Cl - Br - 、NO 2- 、NO 3- PO4 3- 、SO3 2- 、SO4 2- ) Determination of Ion Chromatography" and HJ800-2016 "Water-soluble Cations (Li + 、Na + NH4 + , K + , Ca 2+ Mg 2+ ) Determination of ion chromatography. The mechanical arm 30 clamps the filter membrane clamp 4 on the multi-position turntable 5 into the sampling tank 8, and ultrapure water enters the sampling tank 8 through the pump 25 to soak the filter membrane clamp 4. After soaking, the ultrasonic vibrator 13 at the lower end of the sampling tank 8 starts to work. After a certain period of ultrasonic oscillation, the ultrasonic vibrator 13 stops working, and the filter membrane clamp 4 is lifted above the liquid surface by the mechanical arm 30; after the sampling filter membrane 6 is soaked and ultrasonically oscillated, the water-soluble anions and cations in the particles are completely dissolved in the solution of the sampling tank 8 to obtain a pretreated sample liquid. The flow control pump 20 at the lower end of the sampling tank 8 is turned on to drip and filter the sample liquid. After the filtration starts, the control valve 29 at the lower end of the storage tank 21 is opened to allow the liquid passing through the filtration membrane at the front end to be discharged into the waste liquid tank 27; after a period of filtration, the control valve 29 is closed to store the leaked liquid in the storage tank 21 for sampling by the external detection unit.

[0042] (4) System reset: After the filtration is completed, the filter membrane clamp 4 is clamped back to the multi-position turntable 5 by the mechanical arm 30. After the detection unit 26 finishes sampling, the control valve 29 at the lower end of the storage tank 21 is opened to discharge the liquid into the waste liquid tank 27. The system ends one operation. The system can set the number of cycles for continuous operation.

[0043] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. An online preparation method for water-soluble anion and cation samples in the atmosphere, using an online preparation system for water-soluble anion and cation samples in the atmosphere, characterized in that: The online preparation system includes an atmospheric sampling area, a particle collection area, a static oscillation area, a sample filtration area, a sample liquid storage area, and a waste liquid area; The atmospheric sampling area includes a particle size cutter, a flow controller and a sampling pump; The particle collection area includes a multi-position turntable 1 carrying a filter membrane clamp, the sampling filter membrane is supported and fixed by the filter membrane clamp, the multi-position turntable 1 is connected to 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 zone includes a sampling tank, an ultrapure water adding hole, an exhaust hole and a filter membrane clamping inlet are arranged on the upper part of the sampling tank, a lower exhaust port is arranged at the bottom of the sampling tank, and an ultrasonic vibrator is installed outside the bottom of the sampling tank, the ultrapure water adding hole is connected to the ultrapure water storage tank through a pipeline, and the sampling tank is connected to the multi-position turntable through a mechanical arm; The sample filtration area includes a multi-position turntable 2 carrying a filtration clip, the filtration membrane is supported and fixed by the filtration clip, and the multi-position turntable 2 is connected to the sampling tank through a sample pipeline 1; The sample liquid storage area comprises a storage tank, the upper part of which is provided with a standard solution addition port, a sample liquid inlet and a sample liquid outlet, and the bottom of which is provided with a waste liquid outlet, and the sample liquid inlet is connected to a multi-position turntable 2 through a sample pipeline 2; The waste liquid area includes a waste liquid tank, and the waste liquid outlet is connected to the waste liquid tank via a waste liquid pipeline; An empty hole is left on the multi-position turntable 2 for the liquid to flow through during cleaning; The online preparation method includes the following steps: (1) System self-check: Before the system is put into operation, check whether there is a filter membrane clip in the particle collection area, whether there is ultrapure water in the ultrapure water storage tank, whether the multi-position turntable 2 in the sample filtration area is turned to an empty hole, and whether the waste liquid tank is full; (2) Sampling and cleaning: After the self-test is completed, the sampling pump is started and atmospheric sampling begins; at the same time, the cleaning procedure begins, ultrapure water enters the sampling tank, and the ultrasonic vibrator starts working to ultrasonically clean the sampling tank. After the cleaning is completed, the cleaning liquid enters the storage tank through the empty holes on the multi-position turntable 2 in the sample percolation area, and is discharged into the waste liquid tank through the waste liquid outlet at the bottom of the storage tank; (3) Sample liquid preparation: After cleaning is completed and the set sampling time is reached, the robot arm clamps the filter membrane clamp on the multi-position turntable into the sampling tank, and ultrapure water enters the sampling tank to soak the filter membrane clamp. After soaking, the ultrasonic vibrator at the lower end of the sampling tank starts to work. After a certain period of ultrasonic oscillation, the ultrasonic vibrator stops working, and the filter membrane clamp is lifted by the robot arm to above the liquid surface; the flow control pump at the lower end of the sampling tank is turned on to drip and filter the sample liquid. After the filtration starts, the control valve at the lower end of the storage tank is opened to allow the liquid passing through the filtration membrane at the front end to be discharged into the waste liquid tank; after a period of filtration, the control valve is closed to leave the leaked liquid in the storage tank for sampling by the external detection unit; (4) System reset: After the filtration is completed, the filter membrane clamp is clamped back to the multi-position turntable by the mechanical arm. After the detection unit sampling is completed, the control valve at the lower end of the storage tank is opened to discharge the liquid into the waste liquid tank.

2. The online preparation system for water-soluble anion and cation samples in the atmosphere according to claim 1, characterized in that: The upper and lower covers of the filtration clamp are formed into a cone shape and are used for sealing the edge of the filtration membrane.

3. The online preparation system for water-soluble anion and cation samples in the atmosphere according to claim 1, characterized in that: A flow control pump is arranged on the sample pipeline.

4. The online preparation system for water-soluble anion and cation samples in the atmosphere according to claim 1, characterized in that: The waste liquid tank is made of polytetrafluoroethylene material which is resistant to acid and alkali corrosion.

5. The online preparation system for water-soluble anion and cation samples in the atmosphere according to claim 1 or 4, characterized in that: A control valve is arranged on the waste liquid pipeline.

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