CN119086203A - A device and method for preparing filter membrane substrate particle standard material - Google Patents
A device and method for preparing filter membrane substrate particle standard material Download PDFInfo
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- CN119086203A CN119086203A CN202411187439.XA CN202411187439A CN119086203A CN 119086203 A CN119086203 A CN 119086203A CN 202411187439 A CN202411187439 A CN 202411187439A CN 119086203 A CN119086203 A CN 119086203A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0272—Investigating particle size or size distribution with screening; with classification by filtering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0076—Hardness, compressibility or resistance to crushing
- G01N2203/0083—Rebound strike or reflected energy
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Abstract
The invention provides a preparation device and a preparation method of a filter membrane substrate particulate standard substance, which belong to the technical field of standard substance metering detection and comprise an aerosol generator, wherein an air outlet of the aerosol generator is connected with an air inlet of a dryer, an air outlet of the dryer is connected with an air inlet of a two-stage mixer, an air outlet of the two-stage mixer is connected with an air inlet of a multi-stage aerosol splitter, an air outlet of the multi-stage aerosol splitter is connected with an air inlet of a filter membrane parallel sampler, an air outlet of the filter membrane parallel sampler is connected with an air inlet of a leakage detector, the leakage detector is also connected with a vacuum pump, and the aerosol generator, the two-stage mixer, the multi-stage aerosol splitter, the filter membrane parallel sampler, the leakage detector and the vacuum pump are all electrically connected with a computer control unit. The invention can realize the rapid batch preparation of the standard substance of the filter membrane substrate particles, the deposition amount of the particles on the surface of the filter membrane and the chemical components can be regulated and controlled, and the loaded particle substance amount has good consistency.
Description
Technical Field
The invention relates to the technical field of standard substance metering detection, in particular to a device and a method for preparing a filter membrane substrate particle standard substance.
Background
Atmospheric particulate pollution monitoring is one of the key tasks in the field of environmental monitoring. Among them, particulate component measurement is a key basis for contaminant source resolution and causative analysis. Various manual and automatic methods of component measurement, such as manual measurement of water-soluble ions, organic carbon/elemental carbon and metallic elements, and on-line measurement of organic carbon/elemental carbon and elemental analysis, all use filters to collect and analyze particulates in the atmosphere. The particulate standard substance based on the filter membrane is an indispensable standard substance for instrument calibration and whole-flow verification.
At present, particulate standard substances of a filter membrane substrate are mainly prepared by sampling environmental samples, such as SRM 2783 and RM 8785 developed by National Institute of Standards and Technology (NIST), ERM-CZ110 developed by European Union and the like. The filter membrane substrate standard substance prepared by the method has long sampling time, can not ensure that any two filter membranes have similar sample quantity and chemical composition, and has independent fixed value for each filter membrane, and the quantity value can not be actively regulated. In addition, the single-piece filter membrane has little sample amount and large uncertainty of weighing and chemical analysis results.
Disclosure of Invention
The invention aims to provide a device and a method for preparing a standard substance of filter membrane substrate particles, which can realize the rapid batch preparation of the standard substance of filter membrane substrate particles, the deposition amount and chemical components of the particles on the surface of the filter membrane can be regulated and controlled, and the loaded particle substance has good consistency.
In order to achieve the above purpose, the invention provides a filter membrane substrate particulate standard substance preparation device and method, comprising an aerosol generator, wherein an air outlet of the aerosol generator is connected with an air inlet of a dryer, an air outlet of the dryer is connected with an air inlet of a two-stage mixer, an air outlet of the two-stage mixer is connected with an air inlet of a multi-stage aerosol splitter, an air outlet of the multi-stage aerosol splitter is connected with an air inlet of a filter membrane parallel sampler, an air outlet of the filter membrane parallel sampler is connected with an air inlet of a leakage detector, the leakage detector is also connected with a vacuum pump, and the aerosol generator, the two-stage mixer, the multi-stage aerosol splitter, the filter membrane parallel sampler, the leakage detector and the vacuum pump are all electrically connected with a computer control unit.
Preferably, the two-stage mixer comprises a first-stage mixer and a second-stage mixer, wherein an air inlet of the first-stage mixer is connected with an air outlet of the dryer, an air inlet of the second-stage mixer is connected with an air outlet of the first-stage mixer, and the first-stage mixer is also connected with an electrostatic neutralizer.
Preferably, the outlets of the multi-stage aerosol flow divider are divided into multiple paths, and each path is connected with a filter membrane parallel sampler.
Preferably, the aerosol flow divider adopts a rotationally symmetrical structure to divide one aerosol sample into multiple paths.
The invention also provides a preparation method of the filter membrane substrate particulate standard substance, which comprises the following steps:
S1, generating aerosol by an aerosol generator to a dryer;
s2, removing the moisture of the aerosol by a dryer to obtain dried aerosol;
s3, enabling the dried aerosol to enter a first-stage mixer, mixing the aerosol with charged ion wind generated by an electrostatic neutralizer, and removing charges on the surfaces of particles in the dried aerosol to obtain the aerosol after static removal;
s4, the aerosol after static electricity removal enters a second-stage mixer to be mixed with clean air, so that the aerosol for preparing the standard substance is obtained;
s5, enabling the aerosol for preparing the standard substance to enter an aerosol diverter so as to achieve diversion of the aerosol;
s6, enabling the split aerosol to enter different filter membrane parallel samplers respectively;
S7, an air outlet of the filter membrane parallel sampler is connected with a leakage detector, a measurement result of the leakage detector is transmitted into a computer control unit, and whether the filter membrane parallel sampler leaks or not is judged.
When the outlet of the leakage detector is connected with a vacuum pump and standard substances are prepared, the computer control unit starts the vacuum pump to pump air to generate negative pressure, so that aerosol is driven to pass through a filter membrane arranged in the filter membrane parallel sampler, particles in the aerosol are trapped by the filter membrane, and gas is discharged through the vacuum pump.
Preferably, in step S6, the filter membrane parallel sampler is mounted with the filter membrane before use, and the mounting steps are as follows:
numbering the filter membrane, standing for 24 hours in an environment with the temperature of 15-25 ℃ and the humidity of 30-60% RH, wherein the fluctuation of the temperature is not more than +/-1 ℃ and the fluctuation of the humidity is not more than +/-5% RH in the standing process, continuously weighing at least 3 times every 1 hour in the same environment by using a balance, calculating an average value as a weighing result at the moment, and recording the last weighing result as the mass of the filter membrane before sampling until the difference value between the weighing result at the current moment and the weighing result before 1 hour is within +/-10 mug.
Preferably, in step S7, when it is determined that the filter membrane parallel sampler leaks, the computer control unit controls the aerosol generator, the electrostatic neutralizer, the second-stage mixer, the filter membrane parallel sampler, and the vacuum pump to be stopped in an emergency.
When judging that the filter membrane parallel sampler does not leak, the filter membrane parallel sampler can be started and stopped according to the preset sampling time or sampling volume or manual operation
Therefore, the preparation device and the preparation method of the filter membrane substrate particulate standard substance have the beneficial technical effects that:
(1) The rapid batch preparation of the standard substances of the particles on the filter membrane substrate can be realized, the deposition amount of the particles on the surface of the filter membrane and the chemical components can be regulated and controlled, and the loaded particle substances have good consistency;
(2) The two-stage mixer is adopted, and a particle size screening device such as a PM 2.5 cutter or a PM 10 cutter can be added between the first-stage mixer and the second-stage mixer so as to meet the requirement of collecting aerosol with specific particle size. Because the particle screening device generally has fixed working flow, for example, the working flow of a common PM 2.5 cutter and a PM 10 cutter is 16.7L/min, and when the filter membrane substrate particle standard substance is prepared in batches, a plurality of filter membrane parallel samplers can be simultaneously used, the total sampling flow can be far more than 16.7L/min, and the problem of flow mismatch exists. Through the use of two-stage mixing, guarantee that the outlet flow is 16.7L/min when first level, satisfy the requirement of particulate matter screening plant, continue to supply clean air at the second level, satisfy the requirement of filter membrane parallel sampling, can solve above-mentioned problem.
Drawings
FIG. 1 is a schematic diagram of the air path structure of a filter membrane substrate particulate standard substance preparation device according to the present invention;
FIG. 2 is a schematic diagram of the circuit control structure of a filter membrane substrate particulate standard substance preparation device according to the present invention;
FIG. 3 is a schematic view of the rotational symmetry axis of an aerosol dispenser;
FIG. 4 is a schematic diagram of a method of using the outlet portion of the aerosol dispenser, wherein (a) in FIG. 4 is that any 2 outlets can be used, (b) in FIG. 4 is that 3 outlets form rotational symmetry and can be used, (c) in FIG. 4 is that 4 outlets form rotational symmetry and can be used, and (d) in FIG. 4 is that 3 outlets do not form rotational symmetry and cannot be used;
FIG. 5 is a graph of 16-way filter sampling consistency data.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
Example 1
As shown in FIG. 1, the air path structure schematic diagram of the filter membrane substrate particulate standard substance preparation device comprises an aerosol generator, wherein an air outlet of the aerosol generator is connected with an air inlet of a dryer, an air outlet of the dryer is connected with an air inlet of a two-stage mixer, an air outlet of the two-stage mixer is connected with an air inlet of a multi-stage aerosol splitter, an air outlet of the multi-stage aerosol splitter is connected with an air inlet of a filter membrane parallel sampler, an air outlet of the filter membrane parallel sampler is connected with an air inlet of a leakage detector, and the leakage detector is also connected with a vacuum pump.
Fig. 2 is a schematic diagram of a circuit control structure of a filter membrane substrate particulate standard substance preparation device according to the present invention, wherein an aerosol generator, a two-stage mixer, a multi-stage aerosol diverter, a filter membrane parallel sampler, a leak detector and a vacuum pump are all electrically connected with a computer control unit.
The function of each component will be described in detail below.
The aerosol generator can generate aerosol in the form of dry powder or liquid drops, has an air inlet pressure or flow control function, and can adjust the air inlet pressure or flow of the aerosol generator by using a computer control unit.
The dryer may remove moisture by diffusion drying or heating to convert the droplets into solid particulate matter.
The dried aerosol enters a first-stage mixer and is mixed with charged ion wind generated by an electrostatic neutralizer, so that the charges on the surfaces of particles in the aerosol are eliminated. The aerosol after static removal enters a second-stage mixer and is mixed with clean air to obtain the aerosol for preparing standard substances.
The second-stage mixer has a clean air flow rate condition function, and the air inflow of clean air can be regulated by using a computer control unit. In addition, the second-stage mixer has temperature, humidity and particulate concentration monitoring functions. The computer control unit can collect the temperature, the humidity and the concentration of the particulate matters in the second-stage mixer, and can adjust the working parameters of the aerosol generator and the air inflow of the second-stage mixer according to the concentration of the particulate matters so as to maintain the concentration of the aerosol sample. The second stage mixer has an exhaust port with a high efficiency filter cartridge, and when the intake air flow is greater than the sampling flow, excess air is vented through the exhaust port. Therefore, the sampling flow does not need to be controlled to be completely consistent with the intake air flow during sampling.
The aerosol flow divider adopts a rotationally symmetrical structure to uniformly divide one aerosol sample into multiple paths. The feature of the rotationally symmetrical structure is that the line where the center of the inlet is located along the direction of the air flow is taken as the rotationally symmetrical axis, so that the internal cavity of the aerosol diverter can completely coincide with the rotation before rotating after rotating around the axis by a certain angle (more than 0 DEG and less than 360 DEG), as shown in figure 3. For aerosol dispensers having more than 2 outlets, all of the outlets may not be used, and the unused outlets may be closed by plugging the outlets. The aerosol splitters may be used in cascade, i.e. the outlet of a previous stage aerosol splitter is connected to the inlet of a next stage aerosol splitter.
In order to ensure that the aerosol concentration of each outlet of the aerosol splitter is consistent, the condition that all outlets of the aerosol splitter which are used in a single way have the same flow rate is satisfied in use, and when more than 2 outlets are used in a single way, each outlet is in a rotationally symmetrical structure, as shown in figure 4. If multiple aerosol splitters are used in cascade, each aerosol splitter should meet the above conditions.
The filter membrane parallel sampler has a flow control function, can set sampling flow through a computer control unit, controls sampling start and stop, and transmits real-time flow and accumulated volume back to the computer control unit.
The leak detector measures the concentration of particulates in the gas after passing through the filter using a particle count or mass concentration sensing module. And the computer control unit collects the measurement result of the leakage detector and judges whether leakage occurs to the filter membrane parallel sampler according to the result. If leakage occurs, the computer control unit can control the aerosol generator, the static neutralizer, the second-stage mixer, the filter membrane parallel sampler and the vacuum pump to stop in an emergency.
The invention will be further illustrated by means of specific examples.
The invention relates to a filter membrane substrate particulate matter standard substance preparation device which comprises a computer control unit, an aerosol generator, a dryer, a first-stage mixing device, an electrostatic neutralizer, a second-stage mixing device, a multi-stage aerosol shunt, a filter membrane parallel sampler, a leakage detector and a vacuum pump. The multi-stage aerosol flow divider is a two-stage cascade flow divider, each flow divider is provided with 1 inlet and 4 outlets, and the 4 outlets of the first-stage flow divider are respectively connected with the inlets of the 4 second-stage flow dividers, so that the aerosol flow dividing effect of 1 minute and 16 minutes is realized overall. The total number of filter membrane parallel samplers is 16, a round filter membrane with the diameter of 47mm is used for sampling, and the sampling flow of a single filter membrane is 10L/min.
The filters were individually numbered before being attached to the parallel sampler, allowed to stand for 24 hours in an environment at a temperature of (20.+ -. 0.5) °c and a humidity of (50.+ -. 5)%RH, then continuously weighed 3 times with a balance at 1 hour intervals in the same environment, and the average value of the 3 times of weighing was calculated as the weighing result at that time until the difference between the weighing result at the current time and the weighing result before 1 hour was within.+ -. 10. Mu.g. The last weighing result was recorded as the mass of the filter before sampling.
Aerosol is generated by using an aerosol generator based on an atomization principle and aqueous solution of sodium chloride, the atomization generation flow of the aerosol generator is regulated to be about 5L/min, the neutralization flow of the electrostatic neutralizer is 10L/min, the clean air flow of the first-stage mixer is 25L/min, the clean air flow of the second-stage mixer is 125L/min, and the temperature, the humidity and the concentration of particles in the second-stage mixer are monitored. After the concentration of particulate matter in the second-stage mixer is stabilized, determining a baseline fluctuation standard deviation of the leak detector according to the following method:
In the embodiment, the baseline fluctuation standard deviation of the leak detector is calculated by adopting a method of directly connecting a clean air pipeline to an air inlet of the leak detector, purging the clean air and simultaneously reading the measurement result of the leak detector according to the need. Starting at 0 seconds per minute, 1 measurement was recorded per second, and measurements were continuously recorded for 1min, to obtain 60 measurements, and 1min average and standard deviation were calculated according to the following formula.
The leak detector reading is considered stable when the difference between the average values of the preceding and following 2min satisfies the following condition:
wherein, The average value of j min, sj is the standard deviation of j min, i is the number of the measurement result within 1min, and q ij is the i measurement result of j min; is the average value of j+1min; s j+1 is the standard deviation of j+1min;
At this time, the measurement results were recorded for another 1min, and the standard deviation was calculated as the baseline fluctuation standard deviation.
After the baseline fluctuation standard deviation measurement is completed, the 16 outlets of the second-stage aerosol flow divider are respectively connected with 16 parallel samplers, the outlets of the parallel samplers are connected with the air inlet of the leakage detector, and the computer control unit is used for starting sampling simultaneously. The sampling duration is set to 1h.
In this embodiment, the computer control unit reads the measurement results of the acquisition leak detector at 1s intervals and compares them with the baseline results. And when the concentration of the particulate matters exceeds 10 times of the standard deviation of the baseline fluctuation, judging that the filter membrane sampler leaks. If the continuous measurement results are leakage for at least 5 seconds, the computer control unit controls the aerosol generation and sampling to be stopped, and meanwhile prompts are carried out on a software interface.
And when the sampling time reaches the set time length, the computer control unit simultaneously stops the sampling of the 16 parallel samplers. Stopping the aerosol generator, the static neutralizer, the first-stage mixer and the second-stage mixer, disconnecting the parallel samplers and the aerosol flow divider, taking out the filter membrane from the 16 parallel samplers, standing for 24 hours in an environment with the temperature of (20+/-0.5) DEG C and the humidity of (50+/-5) RH, continuously weighing 3 times in the same environment by using a balance every 1 hour, and calculating the average value of 3 times of weighing as the weighing result at the moment until the difference value between the weighing result at the current moment and the weighing result before 1 hour is within +/-10 mug. The last weighing result is recorded as the mass of the filter after sampling.
And sequentially calculating the mass difference before and after sampling of each filter membrane, namely the mass of the particulate matter sample collected by the surface of the filter membrane. The results are shown in Table 1:
table 1 filter membrane sampling weighing results
| Filter membrane numbering | Mass before sampling (μg) | Quality after sampling (μg) | Particulate matter amount (μg) |
| 1 | 1333526 | 1334992 | 1466 |
| 2 | 1365271 | 1366724 | 1453 |
| 3 | 1381695 | 1383154 | 1459 |
| 4 | 1354487 | 1355949 | 1462 |
| 5 | 1312528 | 1313983 | 1455 |
| 6 | 1346698 | 1348158 | 1460 |
| 7 | 1376658 | 1378117 | 1459 |
| 8 | 1360868 | 1362325 | 1457 |
| 9 | 1358086 | 1359548 | 1462 |
| 10 | 1377633 | 1379089 | 1456 |
| 11 | 1390028 | 1391486 | 1458 |
| 12 | 1375884 | 1377345 | 1461 |
| 13 | 1369790 | 1371253 | 1463 |
| 14 | 1378532 | 1379985 | 1453 |
| 15 | 1342077 | 1343528 | 1451 |
| 16 | 1333695 | 1335152 | 1457 |
| Average value of | / | / | 1458 |
As can be seen from table 1 and fig. 5, the amount of particulate matter collected by the 16 filter membranes had good consistency. The maximum relative deviation between the mass of the particles collected on the single-piece filter membrane and the average value of 16 pieces is within +/-0.6%, so that the uniformity requirement of the standard substance fixed value is met.
Therefore, the preparation device and the preparation method of the filter membrane substrate particulate standard substance can realize the rapid batch preparation of the filter membrane substrate particulate standard substance, the deposition amount and the chemical components of the particulate matters on the surface of the filter membrane can be regulated and controlled, and the loaded particulate matters have good consistency.
It should be noted that the above-mentioned embodiments are merely for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted by the same, and the modified or substituted technical solution may not deviate from the spirit and scope of the technical solution of the present invention.
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