CN112747975A - Device and method for collecting atmospheric fine particulate concentrated solution on line and measuring heavy metal elements - Google Patents
Device and method for collecting atmospheric fine particulate concentrated solution on line and measuring heavy metal elements Download PDFInfo
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Abstract
The invention belongs to the technical field of environmental protection, and particularly relates to a device and a method for collecting atmospheric fine particulate concentrated solution and measuring heavy metal elements on line. The device of the invention comprises: the device comprises a float flowmeter, a concentrated airflow vacuum pump, a main airflow vacuum pump, a drying pipe, a mass flow controller, a collision type PM2.5 cutting head, a condensing system machine, a water tank, an electric heating rod, a virtual cutter, a biological sampling bottle, two micro-injection pumps, an automatic sample injector, an inductively coupled plasma mass spectrum and the like. The device fuses the particles into the liquid through links such as sampling, condensation, concentration and the like, so that the concentration of the particles is improved by one order of magnitude, the concentration effect is better than that of similar products, and the problems of sample pollution, high reagent loss and the like existing in the traditional filter membrane collection monitoring method are effectively avoided; the concentration technology and the inductively coupled plasma mass spectrometry are used for measuring the heavy metal, so that the detection rate can be greatly improved, the sampling time can be reduced, the realization of the artificial intelligent on-line detection of the atmospheric particulates can be realized, and the method can be widely applied to environmental monitoring.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a device and a method for concentration collection and online measurement of particulate matters.
Background
PM2.5 refers to particles having an aerodynamic equivalent diameter of less than or equal to 2.5 microns in the atmosphere, also known as respirable particles. Although PM2.5 is only a component that is present in small amounts in the earth's atmospheric constituents, it has a significant effect on air quality and visibility, among other things. The atmospheric PM2.5 has small particle size, large specific surface area, contains a large amount of toxic and harmful substances, has long suspension time in the atmosphere and long transmission distance, thereby having no negligible negative effects on human health and atmospheric environmental quality.
In recent years, the atmospheric PM2.5 pollution in China is serious, so that the diagnosis rate is increased rapidly and susceptible people die prematurely. Particularly, the toxic and harmful chemical components carried by the haze aerosol particles endanger the health of people, and cause high social attention. There has been a great deal of epidemiological evidence that PM2.5 has acute and chronic health effects. Toxic and harmful heavy metals such as Pb, Cd, Ni, Mn, V, Zn and the like are mainly adsorbed on the particles with the particle size of less than 2.5 microns. Research shows that heavy metals can directly enter alveoli of a human body along with PM2.5 through respiration and are greatly enriched in the human body. As, Cr, Ni and Cd have certain carcinogenic effect on human body, and Zn, Cu and Pb accumulation can increase teratogenic effect of human body. High concentration PM2.5 exposure can increase the risk of suffering from acute respiratory diseases and cardiovascular and cerebrovascular diseases, and PM2.5 can induce chronic diseases such as lung cancer, COPD (chronic obstructive pneumonia), cardiovascular and cerebrovascular diseases and the like, and influence the immune system, the nervous system and the like of a human body. Therefore, the research on the biotoxicity of the haze aerosol particles also becomes one of the research hotspots and frontiers. However, the determination of the biotoxicity of the atmospheric particulates is limited by detection technologies and instruments (such as a higher detection limit), and currently, the determination still remains in an off-line detection stage, and needs to be performed under the conditions of heavy pollution and a longer continuous sampling time, and the requirements of monitoring the concentration of the atmospheric particulates and the characteristics of toxic chemical components in real time cannot be met.
In order to fill the technical blank, and in order to fill the technical blank, the on-line concentration and collection device for the PM2.5 in the medium-flow atmosphere, which is developed by the invention, can concentrate and enrich aerosol to a level which is enough to obviously detect the toxicity of the aerosol on the premise of not changing any physicochemical characteristics except concentration. Meanwhile, the device can be used together with an online toxicity detection device, particles are fused into liquid through links such as sampling, saturation, condensation, concentration and collection, the concentration of the particles can be increased by one order of magnitude, the concentration effect is better than that of similar products, the problems of sample pollution, high loss of samples and reagents and the like existing in the traditional filter membrane collection monitoring method are effectively avoided, the organic components are easily determined by using a flight time mass spectrometry technology, the inorganic components are determined by using an ion chromatograph, the heavy metals are determined by using an inductive coupling plasma mass spectrometry, the air flow demand is greatly reduced, and the air flow is reduced to 50 liters/min from the original 1000 liters/min. The realization of artificial intelligent atmospheric particulate matter on-line detection in the future becomes possible, and the method can be widely applied to environmental monitoring and health risk assessment.
Disclosure of Invention
The invention aims to provide a device and a method for collecting atmospheric fine particles and measuring heavy metal elements in an online concentration manner, so that the concentration degree of the particles is greatly improved, and the problems of sample pollution, high reagent loss and the like are effectively avoided.
The invention provides a device for collecting atmospheric fine particles and measuring heavy metal elements in an online concentration manner, which comprises: the device comprises a float flowmeter, a concentrated airflow vacuum pump, a main airflow vacuum pump, a drying pipe, a mass flow controller, a condensing agent circulating pipe, a collision type PM2.5 cutting head, a condenser, a water tank heat insulation layer, a visual window, an electric heating rod with a temperature sensor, a temperature control digital display device, a condensation inner pipe, a condensation outer spiral pipe, a heat insulation layer, a virtual cutter, a main airflow outlet, a nozzle connecting pipe, a biological sampling bottle, a micro-injection pump, an automatic sample injector and an inductively coupled plasma mass spectrum; wherein:
the water tank is externally sleeved with a heat insulation layer, and two thirds of the upper left part of the front wall of the water tank is provided with a quartz glass visual window;
the U-shaped heating rod is arranged at the bottom end inside the water tank, and an external power line of the U-shaped heating rod is connected with the temperature control digital display device;
the upper part of the water tank is provided with two ports, one of which is connected with a cyclone PM2.5 cutting head and an erosion device by a quick-connection flange; secondly, connecting a coaxially arranged condensation inner pipe by using a quick-connection flange;
a soft copper spiral pipe is tightly wound outside the condensation inner pipe, a heat insulation layer is wrapped outside the spiral pipe, and an inlet at the upper part and an outlet at the lower part of the spiral pipe are respectively connected to an outlet and an inlet of a condensation machine through anti-freezing hoses; forming a circulating flow of condensate;
the upper end of the condensation inner pipe is connected with the virtual cutter through a quick connection flange, the lower end of the interior of the condensation inner pipe is provided with a nozzle which is coaxial with the inner pipe, and the upper end of the condensation inner pipe is provided with a nozzle connecting pipe which is coaxial with the nozzle and is spaced at a certain distance;
a main air outlet is arranged beside the outlet of the nozzle connecting pipe, and is connected with a drying pipe, then connected with a high-flow mass flow controller and then connected with a main air flow vacuum pump to form a main air path; the upper part of the outlet of the nozzle connecting pipe is connected with the air inlet of the biological sampling bottle;
the gas outlet of the biological sampling bottle is connected with a float flowmeter and then connected with a concentrated gas flow vacuum pump to form a concentrated gas path;
the bottom of the biological sampling bottle is provided with a sample inlet and a sample outlet which are respectively connected with the sample outlet and the sample inlet of the two channels of the two micro-injection pumps; one channel at the other end of the concentrated gas flow vacuum pump is connected with a sample inlet of the sampling bottle, and the other channel is connected with the inductively coupled plasma mass spectrum.
Based on the device, the method comprises the following specific steps:
(1) introducing original atmosphere into a cyclone PM2.5 cutting head, screening out atmospheric particulate matters with aerodynamic equivalent diameter less than or equal to 2.5 micrometers by the PM2.5 cutting head, then realizing gas-solid separation of atmospheric aerosol through an erosion apparatus by means of system suction, and enabling separated particulate matters to enter a water tank;
(2) under the observation of a visual window, adding deionized water to two thirds of the height of the water tank, heating the deionized water by using an electric heating rod with a temperature sensor, and controlling the temperature to be 45 +/-2 ℃ by using a temperature control digital display device;
(3) heating the generated water vapor to enable the particles to reach a saturated state, and then flowing through the condensation inner pipe; circulating to make the condensate condense and grow the saturated particles; wherein the aerodynamic diameter of most PM2.5 particles can be increased to 3-4 microns; the external circulation temperature control mode of the condenser controls the temperature to be minus 19 +/-1 ℃; wherein the condensate is 80% ethanol;
(4) condensing the grown particles into a virtual cutter, and accelerating at a nozzle; the accelerating power comes from two gas paths: a main gas path and a concentration gas path; in the main gas path, the flow is controlled to be 50 +/-2 liters/minute and is accurately controlled by a mass flow controller with the flow rate of 0-200 liters/minute; the concentration gas path is the main path for the particles to pass through; in the concentration gas path, the flow of the concentration gas is controlled to be 5 +/-0.2 liter/min and is controlled by a float flowmeter of 0-10 liters/min;
(5) in the virtual cutter, the particles accelerated by the nozzle are received by a nozzle connecting pipe which is coaxially arranged and is arranged above the nozzle with a certain gap; under the condition that the concentration of the particulate matters is the same, the gas flow is changed into one tenth of the original gas flow, and the concentration of the particulate matters in the original atmosphere is changed into ten times of the original concentration, so that the concentration effect is achieved; collecting the concentrated saturated particles on line by a biological sampling bottle, wherein the collecting solvent is deionized water or other organic solvents;
(6) one of the two micro-injection pumps is used for injecting a solvent into the biological sampling bottle, the solvent injection speed is 5-10 ml/min, the operation lasts for 1 min, and the dormancy lasts for 59 min; the other is used for extracting the collected concentrated solution from the biological sampling bottle, the extraction speed of the concentrated solution is 5-10 ml/min, the operation lasts for 1 min, and the dormancy lasts for 59 min;
(7) the concentrated solution pumped by the micro-injection pump is collected into an automatic sample injector on line, and finally, the concentrated solution is injected into an inductively coupled plasma mass spectrum (24) to analyze the heavy metals.
In the invention, the diameter of the condensation inner pipe is 2.5 cm, and the length is 80 cm; the condensate is ethanol with a certain concentration (for example, the concentration can be 70-90%, and the condensate can be adjusted, and only the effects of refrigerating and reducing the volatilization amount are achieved).
In the invention, the diameter of the nozzle is 0.37 +/-0.01 cm, the spacing gap between the nozzle and the nozzle connecting pipe is 0.45 +/-0.01 cm, and the diameter of the connecting pipe is 2.5 +/-0.1 cm.
The invention has the beneficial effects that:
(1) the device can concentrate actual atmospheric particulates by 7 to 10 times (the size of the particulates is related), the concentration efficiency is high and can reach 75 to 99 percent (the size of the particulates is related), and the concentration performance is stable;
(2) the device has low requirements on the flow of sampled inlet air, and the actual atmospheric particulate matters can be efficiently concentrated when the medium flow is 50 liters/minute;
(3) the particles concentrated by the device do not need to be dried, and can be directly collected and used for subsequent on-line or off-line analysis;
(4) the device realizes the on-line collection of the concentrated sample, and meanwhile, the semi-on-line inductively coupled plasma mass spectrum is highly automated, and the whole device is simple and convenient to operate, reliable, stable and easy to maintain.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for on-line concentration collection of atmospheric fine particulate matter and measurement of heavy metals.
Reference numbers in the figures: the device comprises a float flowmeter 1, a concentrated airflow vacuum pump 2, a main airflow vacuum pump 3, a drying pipe 4, a mass flow controller 5, a condensing agent circulating pipe 6, a collision type PM2.5 cutting head 7, a condenser 8, a water tank 9, a water tank thermal insulation layer 10, a visible window 11, an electric heating rod with a temperature sensor 12, a temperature control digital display device 13, a condensation inner pipe 14, a condensation outer spiral pipe 15, a thermal insulation layer 16, a virtual cutter 17, a main airflow outlet 18, a nozzle 19, a nozzle adapter 20, a biological sampling bottle 21, a micro-injection pump 22, an automatic sample injector 23 and an inductively coupled plasma mass spectrum 24.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Example 1:
atmospheric particulates are screened by a cyclone type PM2.5 cutting head 7, particulates with the particle size smaller than 2.5 micrometers enter an erosion device 7 to remove acid-base gas, the passing particulates enter a water tank 9 set to be at a constant temperature of 45 +/-2 ℃ to wrap water vapor and reach a supersaturation state, saturated ions ascend to a condensation pipe 14 set to be at a constant temperature of-19 +/-1 ℃ to condense droplets growing to 3-4 micrometers under the control of a mass flow controller 5 under the suction force of a main airflow vacuum pump 3 of 50 +/-2 liters/minute, the droplets pass through a nozzle 19 in a virtual cutter 17 to enter a concentration gas path at an accelerated speed, and gas enters a bypass gas outlet to be discharged, so that the concentration of the particulates is ten times improved. The concentrated liquid drops are pumped to a biological sampling bottle 21 by a concentrated gas flow vacuum pump 2 which is controlled by 5 +/-0.2 liters/minute through a float flow meter 1, and are sprayed on the wall of the bottle in a radial mode from three needle eye nozzles to be captured by liquid phase solvent which is vigorously swirled. Notably, the droplet-like particulate matter trapping efficiency is higher, and therefore, the concentrated particulate matter does not need to be dried. The concentrated solution collected by the liquid phase is periodically pumped into a sample tube in a fraction collector 23 for storage by two microinjection pumps 22 controlled by online software. And then, pumping a water sample into the instrument for an automatic sample introduction system of the inductively coupled plasma mass spectrometry, and carrying out online analysis on the heavy metal according to a set program and a sample list. Through the above process and operation, the online analysis of heavy metals in atmospheric particulates is realized, and compared with the traditional filter membrane analysis, the detection rate is improved, and the complexity, pollution and loss of pretreatment are effectively avoided. See table 1 for details.
Table 1 uranium concentration (ppb) in samples of particles concentrated and not concentrated in real atmospheric environment
Claims (4)
1. The utility model provides an on-line concentration gathers atmospheric fine particles thing and measures heavy metal element's device which characterized in that includes: the device comprises a float flowmeter (1), a concentrated air flow vacuum pump (2), a main air flow vacuum pump (3), a drying pipe (4), a mass flow controller (5), a condensing agent circulating pipe (6), a collision type PM2.5 cutting head (7), a condensing machine (8), a water tank (9), a water tank heat insulation layer (10), a visible window (11), an electric heating rod (12) with a temperature sensor, a temperature control digital display device (13), a condensation inner pipe (14), a condensation outer spiral pipe (15), a heat insulation layer (16), a virtual cutter (17), a main air flow outlet (18), a nozzle (19), a nozzle connecting pipe (20), a biological sampling bottle (21), two micro-injection pumps (22), an automatic sample injector (23) and an inductive coupling plasma mass spectrum (24); wherein:
a heat insulation layer (10) is sleeved outside the water tank (9), and a quartz glass visible window (11) is arranged at the upper left two thirds of the front wall of the water tank;
the U-shaped heating rod (12) is arranged at the bottom end inside the water tank (9), and an external power line of the U-shaped heating rod (12) is connected with the temperature control digital display device (13);
the upper part of the water tank (9) is provided with two ports, one of which is connected with a cyclone PM2.5 cutting head and an erosion device (7) by a quick-connection flange; secondly, a condensing inner pipe (14) which is coaxially arranged is connected by a quick-connection flange;
a soft copper spiral pipe (15) is tightly wound outside the condensation inner pipe (14), a heat insulation layer (16) is wrapped outside the spiral pipe (15), and an inlet at the upper part and an outlet at the lower part of the spiral pipe (15) are respectively connected to an outlet and an inlet of a condensation machine (8) through anti-freezing hoses; forming a circulating flow of condensate;
the upper end of the condensation inner pipe (14) is connected with a virtual cutter (17) by a quick-connection flange, the lower end of the interior of the condensation inner pipe is provided with a nozzle (19) which is coaxial with the inner pipe, and the upper end of the condensation inner pipe is provided with a nozzle connecting pipe (20) which is coaxial with the nozzle (19) and is spaced at a certain distance;
an air outlet is arranged beside the outlet of the nozzle connecting pipe (20), and is connected with a drying pipe (4), then connected with a mass flow controller (5) with large flow and then connected with a main air flow vacuum pump (3); the upper part of the outlet of the nozzle connecting pipe (20) is connected with the air inlet of the biological sampling bottle (21);
an air outlet of the biological sampling bottle (21) is connected with a float flowmeter (1), and then is connected with a concentrated airflow vacuum pump (2) to form a concentrated air path;
the bottom of the biological sampling bottle (21) is provided with a sample inlet and a sample outlet which are respectively connected with the sample outlet and the sample inlet of the two channels of the two micro-injection pumps (22); one channel at the other end of the concentrated gas flow vacuum pump (2) is connected with a sample inlet of the sampling bottle (21), and the other channel is connected with the auto-sampler (23) and then is connected with the inductively coupled plasma mass spectrum (24).
2. The device according to claim 1, characterized in that the condensation inner tube (14) has a diameter of 2.5 cm and a length of 80 cm, the condensate being a concentration of ethanol.
3. The device according to claim 1, characterized in that the diameter of the nozzle (19) is 0.37 ± 0.01 cm, the spacing gap between the nozzle (19) and the nozzle adapter (20) is 0.45 ± 0.01 cm, and the diameter of the adapter (20) is 2.5 ± 0.1 cm.
4. A method for collecting atmospheric fine particles and measuring heavy metal elements by on-line concentration based on the device of any one of claims 1 to 3 is characterized by comprising the following specific steps:
(1) the original atmosphere is introduced into a collision type PM2.5 cutting head (7), the PM2.5 cutting head (7) screens out atmospheric particulate matters with aerodynamic equivalent diameter less than or equal to 2.5 micrometers, and the atmospheric particulate matters enter a water tank (9) through system suction;
(2) under the observation of a visual window (11), adding deionized water to two thirds of the height of a water tank (9), heating the deionized water by an electric heating rod (12) with a temperature sensor, and controlling the temperature to be 45 +/-2 ℃ by a temperature control digital display device (13);
(3) the water vapor generated by heating leads the particles to reach a saturated state and then flows through the condensation inner pipe (14); condensing saturated particles by circulating and circulating condensate to grow, wherein the aerodynamic diameter of most PM2.5 particles can be increased to 3-4 microns; in addition, the temperature is controlled to be minus 19 +/-1 ℃ in an external circulation temperature control mode of the condenser;
(4) condensing the grown particles into a virtual cutter (17) to obtain acceleration at a nozzle (19); the accelerating power comes from two gas paths: a main gas path and a concentration gas path; an outlet (18) of the main gas path is connected with a drying pipe (4) and then connected with a large-flow vacuum pump (3) so as to prevent the pump body from being damaged by excessive water vapor of the system; wherein, the flow of the main gas path is controlled to be 50 +/-2 liters/minute, and is accurately controlled by a mass flow controller (5) with the flow of 0-200 liters/minute; the concentration gas path is a main path through which the particles pass, and the flow of the concentration gas in the concentration gas path is controlled to be 5 +/-0.2 liters/minute and is controlled by a float flowmeter (1) of 0-10 liters/minute;
(5) in the virtual cutter (17), the particles accelerated by the nozzle (19) are received by a nozzle connecting pipe (20) which is arranged coaxially and is arranged above the nozzle with a certain gap; under the condition that the concentration of the particulate matters is the same, the gas flow is changed into one tenth of the original gas flow, and the concentration of the particulate matters in the original atmosphere is changed into ten times of the original concentration, so that the concentration effect is achieved; collecting the concentrated saturated particles on line by a biological sampling bottle (21), wherein the collecting solvent is deionized water or other organic solvents;
(6) one of the two micro-injection pumps (22) is used for injecting a solvent into the biological sampling bottle (21), the injection speed of the solvent is 5-10 ml/min, the operation lasts for 1 min, and the dormancy lasts for 59 min; the other is used for extracting the collected concentrated solution from the biological sampling bottle, the extraction speed of the concentrated solution is 5-10 ml/min, the operation lasts for 1 min, and the dormancy lasts for 59 min;
(7) the concentrated solution pumped by the micro-injection pump (22) is collected in an automatic sample injector (23) on line, and finally injected into an on-line inductively coupled plasma mass spectrum (24) to analyze the heavy metal components.
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| CN114414651A (en) * | 2022-01-17 | 2022-04-29 | 大连诚泽检测有限公司 | Method for determining heavy metal in PM2.5 by inductively coupled plasma mass spectrometry |
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