CN117538227A - Preparation equipment and method of particle quantity concentration standard substance - Google Patents
Preparation equipment and method of particle quantity concentration standard substance Download PDFInfo
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- CN117538227A CN117538227A CN202311494957.1A CN202311494957A CN117538227A CN 117538227 A CN117538227 A CN 117538227A CN 202311494957 A CN202311494957 A CN 202311494957A CN 117538227 A CN117538227 A CN 117538227A
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- 239000002245 particle Substances 0.000 title claims abstract description 218
- 239000000126 substance Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims description 23
- 239000000443 aerosol Substances 0.000 claims abstract description 78
- 238000009833 condensation Methods 0.000 claims abstract description 44
- 230000005494 condensation Effects 0.000 claims abstract description 44
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 238000000889 atomisation Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000000725 suspension Substances 0.000 claims description 10
- 238000009792 diffusion process Methods 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- 239000004793 Polystyrene Substances 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 229920002223 polystyrene Polymers 0.000 claims description 6
- 238000011282 treatment Methods 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 abstract description 18
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000011160 research Methods 0.000 description 4
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- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
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- 239000004479 aerosol dispenser Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- 238000011969 continuous reassessment method Methods 0.000 description 2
- 101150044687 crm gene Proteins 0.000 description 2
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- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 230000001225 therapeutic effect Effects 0.000 description 2
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- 239000007771 core particle Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 210000001808 exosome Anatomy 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
- G01N15/065—Investigating concentration of particle suspensions using condensation nuclei counters
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Abstract
The invention discloses a preparation device and a preparation method of a standard substance with particle number concentration, and relates to the field of measurement and detection of the standard substance, wherein the device comprises an aerosol atomization generator, a liquid drop outlet of the aerosol atomization generator is sequentially connected with a liquid drop drying device, a particle neutralizer, a differential electromigration classifier and an aerosol distributor, and an outlet of the aerosol distributor is divided into two paths, wherein one path is sequentially connected with a particle collecting impactor and a first condensation nucleus particle counter; the other branch is connected with the aerosol diluter and the second condensation nucleus particle counter in sequence. The invention can realize the preparation of the standard substance of the number concentration of nano-scale and submicron-scale particles, and the magnitude of the standard substance is calculated by the aerosol inlet concentration, the collection efficiency and the collection time, and the magnitude can be traced to SI units.
Description
Technical Field
The invention relates to the field of standard substance metering detection, in particular to equipment and a method for preparing a particle quantity concentration standard substance.
Background
In recent years, detection and characterization of particle sizes and number concentrations of nano-and submicron-sized particles have attracted strong attention in various fields. Among them, in the biomedical field, accurate measurement of nano-submicron particle parameters is a key step to recognize the intrinsic influence thereof on the life system, for example, measurement of the number of protein-loaded particles is required in the development of medical products, and measurement of cell microvesicles and exosomes as markers, concentration and phenotype are required in monitoring treatments. In the research of oral indissolvable drugs and targeted delivery for pulmonary treatment, the evaluation of the drug and therapeutic effect efficiency needs to be realized on the basis of particle number concentration measurement. In the research of the dynamic model of the generation of fibrous amyloid of neurodegenerative diseases, qualitative and quantitative analysis of nano submicron particles is needed. In the quantitative preparation of protein drugs and aggregates with biological therapeutic efficacy, the particle size and the number of particles need to be accurately obtained to meet the authority regulations and eliminate the safety problem; actual medical operation and industrial production and processing workshops, and the number and concentration of particles are used as the requirement of the cleanliness of an operation space. The particle size and concentration of solid impurities in ultrapure water and chemical reagents used in semiconductor processing are critical. Toxicity and risk assessment of the impact on the ecological environment of naturally or unintentionally produced nanoparticles produced by industrial production, etc. From the summary of the practical application situations listed above, accurate measurement of particle sizes and number concentrations of nano-sized and submicron-sized particles in different research fields is an indispensable step in scientific research in many fields in the future.
For the parameter of particle size of the particles in the liquid medium, various technologies such as an electron microscope, a laser particle size analyzer, a dynamic light scattering method and the like can be used for characterization, and standard Substances (CRMs) with the values from traceable to length measurement standards can be used for calibrating the particle size analyzer, so that the reliability of measurement results can be ensured. For the parameter of the number concentration of particles in the solution, the current measurement technology comprises a scanning electron microscope (sem) counting method, a coulter method, a particle tracking analyzer (NTA), a liquid particle counter (liquid particle counter), an ICP-MS (inductively coupled plasma-mass spectrometry) and other measurement methods, and the reliability of the concentration measurement result of the measurement instrument usually needs to be calibrated or verified by using a standard substance. However, only standard substances for the number concentration of particles having a particle diameter of 2 μm or more have been developed.
Due to the lack of a standard substance for the number concentration of nano-submicron particles, the calibration or verification of the instrument can only be performed by using some indirect method when calibrating the calibration of the relevant measuring instrument. Among them, the mass concentration-number concentration conversion method is a more common method. The quantity value of the quantity concentration is calculated according to the mass concentration information and the particle size value of the used particle size standard substance sample. However, in this method, the mass concentration value is generally derived from CRM suppliers, and the reliability of the mass concentration information cannot be ensured due to the contribution of the surfactant or the like in the solution. At the same time, the resulting particle number concentration may also present a significant problem due to the influence of the particle size distribution of the sample. Micro gold particles (GNPs) suspension drops meeting the observation requirement of a Scanning Electron Microscope (SEM) are prepared by using a micro liquid dispersing device, and the particle number of a dried sample is counted and measured by using the SEM, and the accurate NC value of the sample is calculated by combining the weight measurement result of the suspension drops. The NC parameters can be accurately obtained by the method, and the result is reliable. However, there are also significant disadvantages, such as: the measurement sample needs to be subjected to a complex pretreatment process, so that the measurement procedures are multiple to meet the accuracy and traceability requirements of the measurement result. At the same time, since the particle number concentration result is obtained by statistical measurement by a counting method, the correlation of the result with SI units has some problems
Disclosure of Invention
Based on the above problems, the invention aims to provide a preparation device and a preparation method of a standard substance with particle number concentration, and the invention adopts the following technical scheme:
the invention provides a preparation device of a particle quantity concentration standard substance, which comprises an aerosol atomization generator, wherein an air inlet of the aerosol atomization generator is connected with an air supply system, a liquid drop outlet of the aerosol atomization generator is sequentially connected with a liquid drop drying device, a particle neutralizer, a differential electromigration classifier and an aerosol distributor, the voltage and the flow of the differential electromigration classifier are controlled by a DMA (direct memory access) controller, a compressed air pipeline is connected to a pipeline between the differential electromigration classifier and the aerosol distributor, the outlet of the aerosol distributor is divided into two paths, and one path of the outlet of the aerosol distributor is sequentially connected with a particle collecting impactor and a first condensation nucleus particle counter; the other branch of the outlet of the aerosol distributor is sequentially connected with an aerosol diluter and a second condensation nucleus particle counter;
the particle collecting impactor comprises a collecting bottle, a particle inlet pipe and a particle outlet pipe are arranged at the top of the collecting bottle, the tail of the particle inlet pipe is connected with a hollow conical nozzle with a certain outlet diameter, and the hollow conical nozzle is vertically downward and is lower than the particle outlet pipe in height.
Preferably, the air supply system comprises an air compressor, a high-efficiency filter and a cold dryer, and the air compressor, the high-efficiency filter and the cold dryer are sequentially connected in series.
Preferably, the droplet drying device comprises a vertical heating dryer and a diffusion dryer, which are connected in series in sequence.
The invention also provides a preparation method of the particle number concentration standard substance, which comprises the following steps of:
step 1: dripping standard polystyrene particles with a nominal value of Dnm into ultrapure water to prepare a suspension sample, and placing the suspension sample into the aerosol atomization generator;
step 2: preparing 100ml of surfactant solution with mass concentration of 0.3-3% by using high-purity water and sodium dodecyl sulfate with purity of more than 99.9%, and then pouring all the surfactant solution into the particle collecting impactor to be used as collecting liquid;
step 3: adjusting the generation pressure of the aerosol atomization generator so that the compressed air filtered by the 0.1 micron filter enters the aerosol atomization generator and atomizes the suspension sample into liquid drops;
step 4: adjusting the temperature of the vertical heating dryer to be above 100 ℃ so that the formed liquid drop samples are dried into solid particles, and then enabling the air flow loaded with the solid particle samples to pass through the diffusion dryer to form aerosol samples with humidity not more than 30%;
step 5: setting the voltage of the differential electromigration classifier to ensure that the classification grain diameter of the differential electromigration classifier is consistent with the nominal grain diameter of the polystyrene standard grains used in the step 1, namely Dnm;
step 6: connecting a gas circuit to ensure that aerosol samples formed in the step 4 reach Boltzmann charge balance after passing through a particle neutralizer respectively, and then passing through the differential electromigration classifier to obtain monodisperse aerosol standard particles with the known particle size of Dnm;
step 7: the aerosol standard particle sample obtained in the step 6 is diluted by compressed gas blown out of the compressed gas pipeline and then flows through the aerosol dispenser to be divided into two paths;
one path of aerosol particles with constant flow rate enter the inside of the particle collecting impactor through the particle inlet pipe and are jetted into the collecting liquid configured in the step 2 through the hollow conical nozzle, the particles are dispersed in the collecting liquid system through an impact behavior mechanism, part of particles overflow from the surface of the collecting liquid and flow out from a particle outlet pipe due to the influence of the self hydrophobicity of the particles, the acting force of fluid and the like, and the particle outlet pipe is connected with the first condensation nucleus particle counter, and the number concentration of the overflowed particles is determined by the counting of the first condensation nucleus particle counter;
the other branch is connected with a second condensation nucleus particle counter connected with the aerosol diluter in series, and the second condensation nucleus particle counter is used for measuring the number concentration of particles at the inlet of the particle collecting impactor in real time; wherein the aerosol diluter is used for properly diluting the concentration of the aerosol entering the second condensation nucleus particle counter, so as to ensure that the concentration of the entering aerosol sample is within the range of a single particle counting mode;
step 9: record the collection time t c The method comprises the steps of carrying out a first treatment on the surface of the Concentration of number of particles C in the particle collection impactor PNC Calculated by the formula:
wherein: c (C) in The number concentration of Particles flowing into the inlet of the collector recorded for the second condensation nucleus particle counter, particles/cm 3 ；Q in The sampling flow of the second condensation nucleus particle counter is L/min; c (C) out The overflow number concentration of particles at the collector outlet recorded for the first condensation nucleus particle counter, particles/cm 3 ；Q out Sampling flow for the first condensation nucleus particle counter; t is t c For particle collection time s; v (V) l The volume of liquid collected in the impactor was ml.
Preferably, the sampling flow rates of the first condensation nucleus particle counter and the second condensation nucleus particle counter are set to be 0.3L/min; setting the diameter of the outlet of the hollow conical nozzle within the range of 0.5-0.1 mm; setting the height of the outlet of the hollow conical nozzle and the liquid level within the range of 0.5-7 cm; and a magnetic stirring device is arranged at the bottom of the particle collecting impactor, and the rotating speed of the magnetic stirring device is 100rpm.
Compared with the prior art, the invention has the beneficial technical effects that:
according to the quantitative transfer method, the quantitative transfer of the particle sample in the gas to the liquid medium is realized, the traceability and the reliability are good by means of the quantitative value of the particle number concentration in the gas, the quantitative value of the particle number concentration in the liquid is obtained through calculation by accurately measuring the concentration of the entering and overflowing particles in the quantitative transfer process, the quantitative value has the characteristics of high accuracy and good traceability, and the problem that the uncertainty of the fixed value of the standard substance of the nano-scale and micro-scale particle number concentration in the liquid based on the measurement of an electron microscope is effectively solved; the invention can realize the preparation of the standard substance of the number concentration of nano-scale and submicron-scale particles, and the magnitude of the standard substance is calculated by the aerosol inlet concentration, the collection efficiency and the collection time, and the magnitude can be traced to SI units.
Drawings
The invention is further described with reference to the following description of the drawings.
FIG. 1 is a schematic diagram of a preparation apparatus for a standard substance of particle number concentration in an embodiment of the present invention;
fig. 2 is a schematic view of a particle collection impactor according to an embodiment of the invention.
Reference numerals illustrate: 1. an aerosol atomization generator; 2. an air supply system; 201. an air compressor; 202. a high-efficiency filter; 203. a cold dryer; 3. a droplet drying device; 301. a vertical heating dryer; 302. a diffusion dryer; 4. a particle neutralizer; 5. a differential electromigration classifier; 501. a DMA controller; 6. an aerosol dispenser; 7. a compressed gas line; 8. a particle collection impactor; 801. a collection bottle; 802. feeding particles into a pipe; 803. a particle outlet pipe; 804. a hollow cone nozzle; 9. a first condensation nucleus particle counter; 10. an aerosol diluter; 11. a second condensation nucleus particle counter;
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the accompanying drawings and embodiments.
As shown in fig. 1 and 2, the embodiment discloses a preparation device of a standard substance of particle quantity concentration, which comprises an aerosol atomization generator 1, wherein an air inlet of the aerosol atomization generator 1 is connected with an air supply system 2, a liquid drop outlet of the aerosol atomization generator 1 is sequentially connected with a liquid drop drying device 3, a particle neutralizer 4, a differential electromigration classifier 5 and an aerosol distributor 6, the voltage and the flow rate of the differential electromigration classifier 5 are controlled by a DMA controller 501, a compressed gas pipeline 7 is connected on a pipeline between the differential electromigration classifier 5 and the aerosol distributor 6, an outlet of the aerosol distributor 6 is divided into two paths, and one path of the outlet of the aerosol distributor 6 is sequentially connected with a particle collecting impactor 8 and a first condensation nucleus particle counter 9; the other branch of the outlet of the aerosol distributor 6 is sequentially connected with an aerosol diluter 10 and a second condensation nucleus particle counter 11;
the particle collecting impactor 8 comprises a collecting bottle 801, a particle inlet pipe 802 and a particle outlet pipe 803 are arranged at the top of the collecting bottle 801, a hollow conical nozzle 804 with a certain outlet diameter is connected to the tail of the particle inlet pipe 802, and the hollow conical nozzle 804 faces downwards vertically and is lower than the particle outlet pipe 803 in height.
In this embodiment, the air supply system 2 includes an air compressor 201, a high-efficiency filter 202, and a chiller-dryer 203, where the air compressor 201, the high-efficiency filter 202, and the chiller-dryer 203 are sequentially connected in series. The droplet drying apparatus 3 includes a vertical heating dryer 301 and a diffusion dryer 302, and the vertical heating dryer 301 and the diffusion dryer 302 are connected in series in this order.
Based on the preparation equipment, the embodiment also discloses a preparation method of the standard substance with the particle number concentration, which comprises the following steps:
step 1: a suspension sample was prepared by dropping polystyrene standard particles having a nominal value of Dnm into ultrapure water, and the obtained sample was placed in the aerosol atomization generator 1.
Step 2: 100ml of a surfactant solution having a mass concentration of 0.3 to 3% was prepared using high purity water and sodium dodecyl sulfate having a purity of 99.9% or more, and then all of the surfactant solution was poured into the particle collecting impactor 8 as a collection liquid.
Step 3: the generation pressure of the aerosol atomization generator 1 was adjusted so that the compressed air filtered through the 0.1 μm filter entered the aerosol atomization generator 1 and atomized the suspension sample into droplets.
Step 4: the temperature of the vertical heat dryer 301 is adjusted to above 100 ℃ so that the formed droplet sample dries to solid particles, after which the gas stream carrying the solid particle sample passes through the diffusion dryer 302 to form an aerosol sample having a humidity of not more than 30%.
Step 5: the voltage of the differential electromigration classifier 5 is set so that the classified particle size thereof is identical to the nominal particle size of the polystyrene standard particles used in step 1, i.e. Dnm.
Step 6: and (3) connecting the gas paths to ensure that the aerosol sample formed in the step (4) reaches Boltzmann charge balance after passing through the particle neutralizer (4) respectively, and then passing through the differential electromigration classifier (5) to obtain the monodisperse aerosol standard particles with the known particle size of Dnm.
Step 7: the aerosol standard particle sample obtained in the step 6 is diluted by compressed gas blown out of a compressed gas pipeline 7 and then flows through an aerosol distributor 6 to be divided into two paths; the compressed gas blown out from the compressed gas line 7 also needs to be filtered.
One path of aerosol particles with constant flow rate enter the inside of the particle collecting impactor through the particle inlet pipe 802 and are jetted into the collecting liquid configured in the step 2 through the hollow conical nozzle 804, the particles are dispersed in the collecting liquid system through an impact behavior mechanism, part of particles overflow from the surface of the collecting liquid and flow out from the particle outlet pipe 803 due to the influence of the self hydrophobicity of the particles, the acting force of fluid and the like, the particle outlet pipe 803 is connected with the first condensation nucleus particle counter 9, and the number concentration of the overflowed particles is determined by counting of the first condensation nucleus particle counter 9.
The other branch is connected with a second condensation nucleus particle counter 11 connected in series with an aerosol diluter 10, and the second condensation nucleus particle counter 11 is used for measuring the number concentration of particles at the inlet of the particle collecting impactor 8 in real time; wherein the aerosol diluter 10 is used for properly diluting the concentration of the aerosol entering the second condensation nucleus particle counter 11, so as to ensure that the concentration of the aerosol sample entering the aerosol diluter is within the range of a single particle counting mode; the first condensation nucleus particle counter 9 and the second condensation nucleus particle counter 11 are measured and calibrated, and the measurement values can be traced to the international system of units (SI units).
Step 9: record the collection time t c The method comprises the steps of carrying out a first treatment on the surface of the Particle number concentration C in particle collection impactor 8 PNC Calculated by the formula:
wherein: c (C) in The number concentration of the inflowing Particles at the inlet of the particle collecting impactor 8 recorded for the second condensation nucleus particle counter 9, particles/cm 3 ；Q in The sampling flow rate of the second condensation nucleus particle counter 9 is L/min; c (C) out The overflow number concentration of particles at the outlet of the impactor 8, particles/cm, is collected for the particles recorded by the first condensation nucleus particle counter 11 3 ；Q out For the first coagulationThe sampling flow rate of the core particle counter 11; t is t c For particle collection time s; v (V) l The volume of liquid collected in the impactor was ml.
In this embodiment, the sampling flow rates of the first condensation nucleus particle counter 9 and the second condensation nucleus particle counter 11 may be set to 0.3L/min; setting the diameter of the outlet of the hollow conical nozzle 804 within the range of 0.5-0.1 mm; setting the height of the outlet of the hollow conical nozzle 804 and the liquid level to be in the range of 0.5-7 cm; a magnetic stirring device is arranged at the bottom of the particle collecting impactor 8, and the rotating speed of the magnetic stirring device is 100rpm.
By adopting the technical scheme, the standard substance samples of the number and concentration of the particles in the liquid with the nominal particle diameters of 100nm and 500nm are respectively prepared, wherein important monitoring parameters and calculated and measured C are obtained PNC See the table below for values.
In the method, parameters such as nozzle size, nozzle position state and the like in the system are designed and optimized, so that quantitative transfer or collection of particles in aerosol into a liquid medium is realized, and the collection efficiency of aerosol samples reaches more than 90%. By adopting the method, the preparation of the standard substances of the number concentration of the nano-scale particles and the submicron-scale particles can be realized, the quantity value is calculated through the aerosol inlet concentration, the collection efficiency and the collection time, and the quantity value can be traced to SI units.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (5)
1. The preparation equipment of the standard substance of the number concentration of the particles is characterized in that: the device comprises an aerosol atomization generator (1), wherein an air inlet of the aerosol atomization generator (1) is connected with an air supply system (2), a liquid drop outlet of the aerosol atomization generator (1) is sequentially connected with a liquid drop drying device (3), a particle neutralizer (4), a differential electromigration classifier (5) and an aerosol distributor (6), the voltage and the flow of the differential electromigration classifier (5) are controlled by a DMA (direct memory access) controller (501), a compressed air pipeline (7) is connected on a pipeline between the differential electromigration classifier (5) and the aerosol distributor (6), an outlet of the aerosol distributor (6) is divided into two paths, and one path of the outlet of the aerosol distributor (6) is sequentially connected with a particle collecting impactor (8) and a first condensation nucleus particle counter (9); the other branch of the outlet of the aerosol distributor (6) is sequentially connected with an aerosol diluter (10) and a second condensation nucleus particle counter (11);
the particle collecting impactor (8) comprises a collecting bottle (801), a particle inlet pipe (802) and a particle outlet pipe (803) are arranged at the top of the collecting bottle (801), the tail of the particle inlet pipe (802) is connected with a hollow conical nozzle (804) with a certain outlet diameter, and the hollow conical nozzle (804) is vertically downward and is lower than the particle outlet pipe (803).
2. The apparatus for producing a standard substance for quantitative concentration of particles according to claim 1, wherein: the air supply system (2) comprises an air compressor (201), a high-efficiency filter (202) and a cold dryer (203), wherein the air compressor (201), the high-efficiency filter (202) and the cold dryer (203) are sequentially connected in series.
3. The apparatus for producing a standard substance for quantitative concentration of particles according to claim 2, wherein: the liquid drop drying device (3) comprises a vertical heating dryer (301) and a diffusion dryer (302), wherein the vertical heating dryer (301) and the diffusion dryer (302) are sequentially connected in series.
4. A method for preparing a standard substance for particle number concentration using the apparatus for preparing a standard substance for particle number concentration according to claim 3, comprising the steps of:
step 1: dripping standard polystyrene particles with a nominal value of Dnm into ultrapure water to prepare a suspension sample, and placing the suspension sample into the aerosol atomization generator (1);
step 2: preparing 100ml of surfactant solution with mass concentration of 0.3-3% by using high-purity water and sodium dodecyl sulfate with purity of more than 99.9%, and then pouring all the surfactant solution into the particle collecting impactor (8) to be used as collecting liquid;
step 3: adjusting the generation pressure of the aerosol atomization generator (1) so that compressed air filtered by a 0.1 micron filter enters the aerosol atomization generator (1) and atomizes a suspension sample into liquid drops;
step 4: adjusting the temperature of the vertical heating dryer (301) to be above 100 ℃ so that the formed liquid drop sample is dried into solid particles, and then forming an aerosol sample with humidity not more than 30% after the air flow loaded with the solid particle sample passes through the diffusion dryer (302);
step 5: setting the voltage of the differential electromigration classifier (5) to ensure that the classification grain diameter of the differential electromigration classifier is consistent with the nominal grain diameter of the polystyrene standard grains used in the step 1, namely Dnm;
step 6: connecting a gas circuit to ensure that aerosol samples formed in the step 4 reach Boltzmann charge balance after passing through a particle neutralizer (4) respectively, and then passing through a differential electromigration classifier (5) to obtain monodisperse aerosol standard particles with a known particle size of Dnm;
step 7: the aerosol standard particle sample obtained in the step 6 is diluted by compressed gas blown out of the compressed gas pipeline (7) and then flows through the aerosol distributor (6) to be divided into two paths;
one path of aerosol particles with constant flow rate enter the inside of the particle collecting impactor (8) through the particle inlet pipe (802) and are jetted into the collecting liquid configured in the step 2 through the hollow conical nozzle (804), the particles are dispersed in the collecting liquid system through an impact behavior mechanism, part of particles overflow from the surface of the collecting liquid due to the influence of the hydrophobicity of the particles, the acting force of fluid and the like, and flow out of the particle outlet pipe (803), the particle outlet pipe (803) is connected with the first condensation nucleus particle counter (9), and the number concentration of overflowed particles is determined by counting by the first condensation nucleus particle counter (9);
the other branch is connected with a second condensation nucleus particle counter (11) connected with the aerosol diluter (10) in series, and the second condensation nucleus particle counter (11) is used for measuring the number concentration of particles at the inlet of the particle collecting impactor (8) in real time; wherein the aerosol diluter (10) is operative to appropriately dilute the aerosol concentration entering the second condensation nucleus particle counter (11) to ensure that the incoming aerosol sample concentration is within its single particle count mode range;
step 9: record the collection time t c The method comprises the steps of carrying out a first treatment on the surface of the The particle number concentration C in the particle collection impactor (8) PNC Calculated by the formula:
wherein: c (C) in The number concentration of Particles flowing into the inlet of the collector recorded by the second condensation nucleus particle counter (9), particles/cm 3 ；Q in The sampling flow of the second condensation nucleus particle counter (9) is L/min; c (C) out The concentration of the number of overflows of particles at the outlet of the collector, recorded for the first condensation nucleus particle counter (11), particles/cm 3 ；Q out Sampling flow for a first condensation nucleus particle counter (11); t is t c For particle collection time s; v (V) l The volume of liquid collected in the impactor was ml.
5. The method for preparing the standard substance for the quantitative concentration of particles according to claim 4, wherein: setting the sampling flow rates of the first condensation nucleus particle counter (9) and the second condensation nucleus particle counter (11) to be 0.3L/min; setting the diameter of the outlet of the hollow conical nozzle (804) within the range of 0.5-0.1 mm; setting the height of the outlet of the hollow conical nozzle (804) and the liquid level to be in the range of 0.5-7 cm; and a magnetic stirring device is arranged at the bottom of the particle collecting impactor (8), and the rotating speed of the magnetic stirring device is 100rpm.
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| CN202311494957.1A CN117538227A (en) | 2023-11-10 | 2023-11-10 | Preparation equipment and method of particle quantity concentration standard substance |
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| CN202311494957.1A CN117538227A (en) | 2023-11-10 | 2023-11-10 | Preparation equipment and method of particle quantity concentration standard substance |
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