CN110208165B - Calibration method of split-flow aerosol diluter - Google Patents
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- 239000000443 aerosol Substances 0.000 title claims abstract description 116
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 144
- 238000005259 measurement Methods 0.000 claims abstract description 38
- 239000012895 dilution Substances 0.000 claims abstract description 34
- 238000010790 dilution Methods 0.000 claims abstract description 34
- 239000000126 substance Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 239000004793 Polystyrene Substances 0.000 claims description 7
- 229920002223 polystyrene Polymers 0.000 claims description 7
- 238000009792 diffusion process Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000009833 condensation Methods 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 4
- 230000005494 condensation Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003921 particle size analysis Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000012546 transfer Methods 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
- G01N15/10—Investigating individual particles
- G01N15/1012—Calibrating particle analysers; References therefor
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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
- G01N15/10—Investigating individual particles
- G01N2015/1022—Measurement of deformation of individual particles by non-optical means
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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
- G01N15/10—Investigating individual particles
- G01N2015/1026—Recognising analyser failures, e.g. bubbles; Quality control for particle analysers
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Abstract
The invention belongs to the field of nanoparticle metering, and particularly relates to a calibration method of a split-flow aerosol diluter. And measuring the particle concentration value by the calibrated particle counter before and after using the aerosol diluter, calculating the dilution ratio of the diluter, and comparing the dilution ratio with the nominal value to finish the calibration of the diluter. The calibration system comprises: aerosol generator, even blender, standard particle counter. The invention adopts a scientific and reasonable calibration method to ensure the accuracy and reliability of the measurement result. The calibration method can effectively calibrate the limiting aerosol diluter, improves the measurement precision of an analytical instrument such as a particle counter and the like, and provides technical support for the establishment of a traceable system of particle number concentration.
Description
Technical Field
The invention belongs to the field of nanoparticle metering, and particularly relates to a calibration method of a split-flow aerosol diluter.
Background
When the measuring instrument performs particle size analysis, the phenomenon of collision, agglomeration, coagulation and the like among particles can be caused by the excessively high concentration, and the accuracy of a measuring result is affected. The aerosol diluter has the main function of reducing the concentration of aerosol by diluting the aerosol, and solves the problems that high concentration or flow mismatch cannot be tested during particle analysis.
In the field of nano particle counting, as a traceable system of particle number concentration in a low concentration range is not established, a high-concentration sample with good traceability needs to be accurately diluted to obtain a low-concentration sample with known particle number concentration, and therefore calibration of a particle counter, an aerosol particle size spectrometer and the like is realized. In JJF1562-2016 condensation nucleus particle counter calibration standard, on-line dust particle counter calibration standard (manuscript), ISO 21501-4-2007 international standard (particle size analysis single particle optical measurement method part 4), ISO27891-2015 (aerosol particle number concentration-condensation nucleus particle counter calibration), accurate dilution of particles by aerosol diluter is required. In the above measurement and calibration, the quality of the aerosol diluter metering performance directly affects the reliability of the measurement results.
The principle of the split aerosol diluter is as follows: as shown in figure 1, when aerosol enters the inlet of the diluter, a part of aerosol particles are collected through a thin capillary tube, the flow ratio of the capillary tube is kept unchanged, the rest aerosol is filtered by a bypass high-efficiency filter, and two airflows of the capillary tube and the bypass are mixed, so that the particle concentration in the capillary tube is diluted, and a fixed particle dilution ratio can be formed by keeping a certain ratio of the capillary tube to the bypass.
Thus, the accuracy of the dilution ratio of an aerosol diluter is critical, but there is currently no certification and calibration specification for aerosol diluters and related standard regulations. The dilution ratio of the aerosol diluter is generally calibrated by adopting an aerosol photometer method, an optical particle counter method and a flow measurement method. However, the three calibration methods still have the following defects:
(1) Calibrating aerosol diluter dilution ratio using aerosol photometry
The measurement range of the aerosol photometer is (0.0001-120) mug/L, the maximum allowable error is not more than +/-5%, the aerosol diluter is specially designed for solving the problem of high concentration which cannot be tested by the dust particle counter, the particle counting is generally the best measurement range which is (3000-30000)/28.3L, and the calculated mass concentration is far less than 0.1 mug/L, so the use amount value of the aerosol diluter is the lower measurement limit of the measurement range of the aerosol photometer, the measurement indication error is larger, and the measurement uncertainty is larger.
(2) Calibrating aerosol diluter dilution ratio directly using range of optical particle counter
The repeatability of the measurement value of the particle concentration of the particle counter is not more than 10% fs, and the error of the indication value of the particle concentration is less than ±30%, as specified in the JJF1190-2008 dust particle counter calibration specification. Therefore, when the particle counter is used for measuring the concentration of the aerosol generator before and after the diluter, the particle counter can work at two gears with high concentration and low concentration simultaneously, if the uncertainty of the indication error of the particle counter at the two gears is excessive, the indication error of the dilution ratio of the diluter is measured to be more than +/-30%, and the error of the indication value of the dilution ratio of the diluter is generally not more than +/-10%, so that the measured data is meaningless. In the step-by-step traceability chain of internationally recognized laser particle counter (OPC) -condensation nucleus particle counter (CPC) -aerosol electrometer (FCE), namely, the calibration of the measurement result of the laser particle counter is realized through the condensation nucleus particle counter (CPC), the measurement result of the calibrated laser particle counter can be traceable to the national current standard, the aerosol diluter is used as an important ring from the middle to the bottom of the traceability chain, and if the diluter is traceable to the particle counter again, the traceability chain is disordered.
3. Calibrating aerosol diluter dilution ratio using flow measurement
Only the flow of the original particle counter and the flow of the supplementary clean compressed gas are measured, then the dilution ratio is calculated, the condition that the variation value of the particle concentration in the diluter cannot be truly measured at all is ignored, and whether the aerosol particles have condensation, adhesion and other factors in the diluter is ignored.
Thus, there is a need for a method of calibrating an aerosol diluter that has small measurement errors and reliable results.
Disclosure of Invention
The invention aims to solve the technical problem of providing a calibration method of a split-flow aerosol diluter, which adopts a scientific and reasonable calibration method to ensure the accuracy and reliability of a measurement result.
The invention is realized in the following way:
The invention relates to a calibration method of a split-flow aerosol diluter, which specifically comprises the following steps:
(2) Preparing a calibration sample: the standard substance is a monodisperse particle with the particle diameter of 0.5 mu m, single-point measurement is selected for a diluter with fixed dilution ratio, and upper, middle and lower 3 points are selected as measurement points in the range of the maximum dilution ratio for a diluter with dynamic dilution ratio; the standard sample is diluted to obtain 2 samples, wherein the concentration of the 2# sample is f times that of the 1# sample, and f is a fixed dilution multiple of the diluter or a measurement point in calibration, and then the calibration is performed according to the rest steps.
(5) The calibration system comprises an aerosol generator, a uniform mixing box and a standard particle counter which are sequentially connected, when the calibration system is used, a No. 1 sample is atomized by the aerosol generator, the flow of aerosol is regulated to be smaller than that of the standard particle counter, the aerosol enters the standard particle counter through the uniform mixing box, the required flow of the standard particle counter is not supplied by the aerosol generator, and insufficient flow is automatically sucked into the uniform mixing box through a HEPA or ULPA filter and enters the standard particle counter, so that the flow of the aerosol and the flow of the standard particle counter are matched.
When the sample No. 1 is used, setting parameters of an aerosol generator are adjusted, so that the particle concentration measured by a standard particle counter is in the range of (3000-30000)/28.3L, the measurement is repeated for 3 times, and the concentration of the standard particle counter, namely C 1, is recorded;
(6) When the No. 2 sample is used for calibration, the flow of the standard particle counter is ensured to be matched with the nominal flow of the split-flow type aerosol diluter to be calibrated, the aerosol input port of the split-flow type aerosol diluter to be calibrated is connected with the aerosol output port of the uniform mixing box, and the aerosol output port of the split-flow type aerosol diluter to be calibrated is connected with the input port of the standard particle counter. And measuring the measured value of the No. 2 sample in a standard particle counter, and repeating the measurement for 3 times, namely a particle concentration value C 2;
Typically, the standard particle counter is set to sample for 1 minute, i.e., C 1、C2 is the total number of aerosol particles collected within one minute of the standard particle counter.
(7) Finally, the dilution ratio f 0.5 of the split-flow aerosol diluter is calculated according to the following formula, compared with a nominal value, and the indication error delta f,0.5 is calculated to finish the calibration of the split-flow aerosol diluter:
Further:
In the step (1), the standard substance of the monodisperse particles is a standard substance of monodisperse Polystyrene (PSL) particles, and the particle size of the standard substance is 0.5 mu m.
In the step (2), the aerosol generator comprises a gas mass flowmeter with a precise controller, an aerosol atomizer and a diffusion dryer. Wherein the diffusion dryer ensures that the humidity of the sol particles produced is below 30%.
In the step (2), the uniform mixing box is provided with an aerosol inlet, a clean dilution air inlet and an aerosol outlet, wherein the aerosol inlet is connected with the aerosol generator, and the aerosol outlet is connected with the standard particle counter.
In the step (2), the requirements of the aerosol generator are as follows: standard particles with particle sizes in the range of 0.1 μm to 5 μm are atomized.
In the step (2), the requirements of the uniform mixing box are as follows: the stability of the aerosol concentration within 10 minutes should be better than 1%.
In the step (2), the standard particle counter has the following requirements: should have particle size ranges of 0.3 μm, 0.5 μm, 1 μm, 5 μm and be able to measure particle number concentrations in the range of (3000-30000)/28.3L with reproducibility better than 3%.
The invention has the following advantages: the calibration method can effectively calibrate the split-flow aerosol diluter, improves the measurement precision of an analytical instrument such as a particle counter and the like, and provides technical support for the establishment of a traceable system of particle number concentration.
Drawings
The invention will be further described with reference to examples of embodiments with reference to the accompanying drawings.
Fig. 1 is a schematic diagram of a split aerosol diluter, wherein 1 bypasses the air inlet, 2 high efficiency filters, 3 trim valves, 4 capillaries.
Fig. 2 is a schematic diagram of the components of the calibration system.
Fig. 3 is a schematic diagram of a calibration process of the calibration system.
Detailed Description
Example 1
Firstly, preparing two monodisperse Polystyrene (PSL) particle standard solutions with different concentrations, wherein the volumes of the solutions are 100mL, a 1# sample is a dilution of high-concentration polystyrene with the particle size of 0.5 mu m and purified water, and the concentration of the polystyrene solution prepared by a 2# sample is f times of that of the 1# sample, namely the dilution multiple of a diluter, as shown in table 1.
TABLE 1 calibration of standard substances for the desired concentration ratio
* The concentration ratio of the monodisperse particle diluent can be prepared separately according to the actual measurement point.
The preparation method of the monodisperse particle diluent comprises the following steps:
(1) The high-concentration polystyrene stock solution is directly dripped into a clean micro beaker to avoid the pollution of the stock solution.
(2) A sample No. 1 is prepared, and a 50uL microsampler is used to transfer 50uL stock solution from a microshutter to a 100mL volumetric flask. And (3) injecting pure water into the volumetric flask, when the pure water approaches to a 100mL score line, closing the volumetric flask stopper, reversing the volumetric flask stopper back and forth for 3 times to fully mix the solution, and then injecting the pure water until the pure water reaches the 100mL score line.
(4) Sample #2 was prepared by transferring f 50uL (here 500uL if the dilution ratio was 10 nominal) stock solution from a microsampler of 500uL into a 100mL solution flask. And (3) injecting pure water into the volumetric flask, when the pure water approaches to a 100mL score line, closing the volumetric flask stopper, reversing the volumetric flask stopper back and forth for 3 times to fully mix the solution, and then injecting the pure water until the pure water reaches the 100mL score line.
The calibration method is that the particle concentration value is measured by the calibrated particle counter before and after the aerosol diluter is used, the dilution ratio of the diluter is calculated, and the dilution ratio is compared with the nominal value, so that the calibration of the diluter is completed. The method comprises the following steps:
(1) Firstly, a No. 1 sample is selected, an aerosol generator (the flow and particle generation rate are controlled by a gas mass flowmeter with a precise controller and an aerosol atomizer to form stable aerosol particles, the humidity of the generated aerosol particles is guaranteed to be lower than 30 percent by a dryer) is arranged in a solution bottle, a generator power supply is started, clean compressed air filtered by an efficient filter enters the aerosol generator, standard solution in the device is atomized, aerosol generation amount is regulated to obtain aerosol particles with proper concentration and stable concentration, the flow is smaller than the nominal flow of a particle counter, the aerosol particles pass through a uniform mixing box and are connected to the particle counter, and insufficient flow required by the particle counter is independently sucked into the uniform mixing box through a HEPA or ULPA filter except the generator supply, so that the two flows are matched. The working principle is shown in figure 2. According to the connection of fig. 2, the particle counter is turned on, preheated, self-cleaned, zeroed, and set to the appropriate particle size range and sampling time. The concentration of the particle counter was calculated to be C 1.
(2) The device of the aerosol generator is kept unchanged, and the solution bottle of the aerosol generator is replaced by a No.2 sample.
(3) The corresponding particle counter flow value is selected to match the nominal flow of the diluter and the split aerosol diluter is inserted between the homogeneous mixing tank and the particle counter, as shown in fig. 3, and re-measured as described above, with the particle counter concentration calculated as C 2.
Note that: in fig. 3, the particle counter operating flow rate should be the same as the aerosol diluter operating flow rate point.
Then the dilution ratio f of the aerosol diluter is calculated as:
wherein:
concentration of C 1 -1 # solution, standard particle counter measurement;
concentration of C 2 -2 # solution, standard particle counter measurement;
concentration of PSL particles in C 1# -1 # solution;
Concentration of PSL particles in C 2# -2 # solution.
The technical requirements of the calibration system of the invention are as follows:
1) Aerosol generator
Standard particles having a particle size in the range of (0.1 to 5) μm can be atomized.
2) Uniform mixing box
The stability of the aerosol concentration within 10 minutes should be better than 1%.
3) Particle counter
The particle size range of 0.3 μm and 0.5 μm is adopted, the particle number concentration in the range of (3000-30000)/28.3L can be measured, the repeatability is better than 3%, for example, the flow rate of the diluter is 2.83L/min, then a particle counter with the flow rate of 2.83L/min is selected, for example, the flow rate of the diluter is 28.3L/min, and then the particle counter with the flow rate of 28.3L/min is selected.
Calibration method and results: selecting a brand of%III 110) an etalon for particle counters with 8 particle size channels ranging from 0.1 μm to 5.0 μm at a flow rate of 1.0CFM with a measurement uncertainty of MPEG: + -10% and a repeatability of 0.4%, a brand of particle concentration diluter (ATI aerosol particle concentration diluter TDA-D10) was selected at a flow rate of 1.0CFM with a dilution ratio of 10 nominal.
The aerosol generator is adopted, the flow and the concentration are controlled to be constant, and the stability is better than 2%/h. A standard solution of monodisperse Polystyrene (PSL) particles with a particle size of 500nm and two concentrations is prepared, wherein the concentration of the 2# solution is 10 times that of the 1# solution.
The conventional calibration method directly selects the No. 2 standard substance for calibration (method 1), adjusts the gas concentration of the particle generator, controls the aerosol concentration to 36288 (stability is better than 2%/h), and the measured dilution ratio of the aerosol diluter is shown in Table 2.
The present invention uses standard substances 1# and 2# for calibration (method 2), the setting of the aerosol generator is unchanged when the standard substances are replaced, the measurement is directly performed by a particle counter when the standard substance 1# is used, and the measurement is performed by adding a diluter before the particle counter when the standard substance 2# is used, as shown in table 3.
TABLE 2 measurement of dilution ratio of diluter using No. 2 Standard substance
TABLE 3 dilution ratio of aerosol diluter measured using # 1 standard and # 2 standard, respectively
From tables 2 and 3 we can see that the relative error of method 2 is smaller compared to the nominal value of the diluter for the measurement of method 2 and method 1. And the uncertainty of the standard particle counter is MPEG: + -10%, the repeatability is 0.4%, the uncertainty of the measurement of the method 1 is more than 10, and the uncertainty of the measurement of the method 2 is better than 3, so the reliability of the measurement result of the method 2 is far more than that of the measurement result of the method 1.
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that the specific embodiments described are illustrative only and not intended to limit the scope of the invention, and that equivalent modifications and variations of the invention in light of the spirit of the invention will be covered by the claims of the present invention.
Claims (7)
1.A method of calibrating a split aerosol diluter, comprising: the method comprises the following steps:
(1) Preparing a calibration sample: the standard substance is a monodisperse particle with the particle diameter of 0.5 mu m, single-point measurement is selected for a diluter with fixed dilution ratio, and upper, middle and lower 3 points are selected as measurement points in the range of the maximum dilution ratio for a diluter with dynamic dilution ratio; diluting a standard substance sample to obtain 2 samples, wherein the concentration of the 2# sample is f times that of the 1# sample, f is the nominal value of the dilution ratio of the split-flow aerosol diluter, and then calibrating according to the rest steps;
(2) The calibration system comprises an aerosol generator, a uniform mixing box and a standard particle counter which are sequentially connected, when the system is used, a No. 1 sample is atomized in the aerosol generator, the flow of aerosol is regulated to be smaller than that of the standard particle counter, the aerosol enters the standard particle counter through the uniform mixing box, the required flow of the standard particle counter is not supplied by the aerosol generator, and insufficient flow is automatically sucked into the uniform mixing box through a HEPA or ULPA filter and enters the standard particle counter to enable the flow of the aerosol and the flow of the standard particle counter to be matched;
When the sample No. 1 is used, setting parameters of an aerosol generator are adjusted, so that the particle concentration measured by a standard particle counter is in a range of 3000-30000/28.3L, the measurement is repeated for 3 times, and the concentration of the standard particle counter, namely C 1#, namely the concentration of monodisperse particles with the standard substance particles in the sample No. 1 is recorded;
(3) When the No. 2 sample is used for calibration, ensuring that the flow of the standard particle counter is consistent with the nominal flow of the split-flow type aerosol diluter to be calibrated, connecting an aerosol input port of the split-flow type aerosol diluter to be calibrated with an aerosol output port of the uniform mixing box, connecting an aerosol output port of the split-flow type aerosol diluter to the input port of the standard particle counter, measuring the measured value of the No. 2 sample in the standard particle counter, and repeating the measurement for 3 times, namely, a particle concentration value C 2#, namely, the concentration of monodisperse particles in the No. 2 sample with the standard substance particles;
(4) Finally, the dilution ratio f 0.5 of the split-flow aerosol diluter is calculated according to the following formula, and is compared with the nominal value f, and the indication error is calculated Calibration of the split aerosol diluter is completed:；；
wherein:
-solution concentration of sample # 1;
-solution concentration of sample # 2;
-1 # sample in which the monodisperse particles have a concentration of particles of the standard substance;
the monodisperse particles in sample # 2 demonstrate the concentration of standard particles.
2. The method of calibrating a split-flow aerosol diluter according to claim 1, wherein: in the step (1), the standard substance of the monodisperse particles is a standard substance of monodisperse polystyrene particles, and the particle size of the standard substance is 0.5 mu m.
3. The method of calibrating a split-flow aerosol diluter according to claim 1, wherein: in the step (2), the aerosol generator comprises a gas mass flowmeter with a precise controller, an aerosol atomizer and a diffusion dryer, wherein the diffusion dryer ensures that the humidity of sol particles generated by the aerosol generator is lower than 30%.
4. The method of calibrating a split-flow aerosol diluter according to claim 1, wherein: in the step (2), the uniform mixing box is provided with an aerosol inlet, a clean dilution air inlet and an aerosol outlet.
5. The method of calibrating a split-flow aerosol diluter according to claim 1, wherein: in the step (2), the requirements of the aerosol generator are as follows: standard particles with the particle size ranging from 0.1 μm to 5 μm are atomized.
6. The method of calibrating a split-flow aerosol diluter according to claim 1, wherein: in the step (2), the requirements of the uniform mixing box are as follows: the stability of the aerosol concentration within 10 minutes should be better than 1%.
7. The method of calibrating a split-flow aerosol diluter according to claim 1, wherein: in the step (2), the standard particle counter has the following requirements: the particle size ranges of 0.3 μm, 0.5 μm, 1 μm and 5 μm are required, and the particle number concentration in the range of (3000-30000)/28.3L can be measured, and the repeatability is better than 3%.
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| CN106054237A (en) * | 2016-07-28 | 2016-10-26 | 中国船舶重工集团公司第七〇九研究所 | System platform for calibrating radioactive aerosol monitoring equipment and working method thereof |
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| GB201311097D0 (en) * | 2013-06-21 | 2013-08-07 | Particle Measuring Syst | A method and apparatus for dilution of aerosols |
| US9254500B2 (en) * | 2013-10-09 | 2016-02-09 | Massachusetts Institute Of Technology | Aerosol generation for stable, low-concentration delivery |
| CN109357928B (en) * | 2018-11-13 | 2024-04-09 | 上海市计量测试技术研究院 | Device and method for calibrating dilution ratio of aerosol diluter |
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| CN103889488A (en) * | 2011-10-28 | 2014-06-25 | 皇家飞利浦有限公司 | Analysis and control of aerosol flow |
| CN106054237A (en) * | 2016-07-28 | 2016-10-26 | 中国船舶重工集团公司第七〇九研究所 | System platform for calibrating radioactive aerosol monitoring equipment and working method thereof |
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