CN110208165A - A kind of calibration method of shunt aerosol diluter - Google Patents
A kind of calibration method of shunt aerosol diluter Download PDFInfo
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- CN110208165A CN110208165A CN201910452444.1A CN201910452444A CN110208165A CN 110208165 A CN110208165 A CN 110208165A CN 201910452444 A CN201910452444 A CN 201910452444A CN 110208165 A CN110208165 A CN 110208165A
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- 239000000443 aerosol Substances 0.000 title claims abstract description 103
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 90
- 238000005259 measurement Methods 0.000 claims abstract description 33
- 239000012895 dilution Substances 0.000 claims abstract description 15
- 238000010790 dilution Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 14
- 150000001336 alkenes Chemical class 0.000 claims description 6
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 5
- 238000009792 diffusion process Methods 0.000 claims description 4
- 239000012925 reference material Substances 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 3
- 239000003085 diluting agent Substances 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 241001411320 Eriogonum inflatum Species 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000013589 supplement Substances 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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- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
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- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention belongs to nano particle metering field more particularly to a kind of calibration methods of shunt aerosol diluter.Through calibrated corpuscular counter before and after using aerosol diluter, particle concentration value is measured, calculates the dilution ratio of diluter, and the comparison with nominal value, completes the calibration to diluter.Calibration system includes: aerosol generator, uniform vortex mixer, standard particle counter.The present invention uses scientific and reasonable calibration method, guarantees the accurate and reliable of its measurement result.Calibration method of the invention can effectively calibrate limitation formula aerosol diluter, improve the measurement accuracy of the analysis instruments such as corpuscular counter, provide technical support for the traceability system foundation of amounts of particles concentration.
Description
Technical field
The invention belongs to nano particle metering field more particularly to a kind of calibration methods of shunt aerosol diluter.
Background technique
For measuring instrument when carrying out granularmetric analysis, excessive concentration can make phenomena such as the condensing that collide, reunite between particle, shadow
Ring the accuracy of measurement result.The main function of aerosol diluter is, molten by being diluted to reduce gas to aerosol
The concentration of glue solves the problems, such as to be unable to test high concentration or flow mismatch etc. when grading analysis.
Such as in nano particle counted fields, since the traceability system of low strength range endoparticle number concentration is not yet established,
The good enriched sample of traceability need to be subjected to accurate dilutions, low concentration sample known to amounts of particles concentration be obtained, thus real
Now to the calibration etc. of particle collector, aerosol partial size spectrometer.JJF1562-2016 nuclei of condensation corpuscular counter calibrating standard,
Online airborne particle counter calibrating standard (draft for deliberation), ISO 21501-4-2007 international standard (grain size analysis individual particle light
Learn the 4th part of mensuration), in ISO27891-2015 (calibration of aerosol particle number concentration-nuclei of condensation corpuscular counter),
It is required to carry out accurate dilutions to particulate matter using aerosol diluter.In above-mentioned measurement and calibration, aerosol diluter meter
The quality of amount performance directly affects the reliability of measurement result.
The principle of shunt aerosol diluter it is as follows: as shown in Figure 1, when aerosol enters diluter entrance, pass through
One thin capillary acquires a part of aerosol particle, and Capillary Flow ratio remains unchanged, and rest part aerosol is other
Road high efficiency particulate air filter filters out, and two strands of air-flows of capillary and bypass are mixed, so that the granule density in capillary is diluted, protects
The ratio of certain capillary and bypass is held, fixed particle thinner ratio can be formed.
Therefore, the accuracy of aerosol diluter thinner ratio is most important, but currently there has been no aerosol diluters
Vertification regulation and calibrating standard and relevant Standard andRegulation.It is general select aerosol photometer method, optical particle counter method,
Hydrometry calibrates the thinner ratio of aerosol diluter.But there are still following at present for above-mentioned three kinds of calibration methods
Defect:
(1) aerosol diluter thinner ratio is calibrated using aerosol photometer method
Use the measurement range of aerosol photometer for (0.0001~120) μ g/L, the limits of error be no more than ±
5%, and aerosol diluter aims at and solves this problem of high concentration for being unable to test of airborne particle counter and especially set
Meter, the general optimum measurement range of particle counting is to calculate its mass concentration much smaller than 0.1 μ in (3000~30000)/28.3L
G/L, thus aerosol diluter be using magnitude aerosol light bead metering journey measurement lower limit, the error of indication of measurement compared with
Greatly, measurement is not known larger.
(2) aerosol diluter thinner ratio is directly calibrated using the range of optical particle counter
According to " JJF1190-2008 airborne particle counter calibrating standard " in regulation corpuscular counter particle concentration
The repeatability of measured value is not more than 10%FS, and the error of indication of particle concentration is less than ± 30%.Therefore it is surveyed using corpuscular counter
When amount makes to make the concentration of the aerosol generator before and after diluter, corpuscular counter can be made to work at the same time in high concentration and low concentration
Two gears on, and particle counting makes to measure dilute if the uncertainty of the error of indication in two gears is all excessive
The error of indication for releasing the thinner ratio of device is greater than ± 30%, and general diluter thinner ratio show the error of title value be usually no more than ±
10%, the data that measurement obtains so just lose meaning." the laser particle counter (the OPC)-nuclei of condensation generally acknowledged in the world at present
In the chain of tracing to the source step by step of corpuscular counter (CPC)-aerosol electrostatic meter (FCE) ", that is, pass through nuclei of condensation corpuscular counter (CPC)
Realize the calibration of the measurement result of laser particle counter, the laser particle counter measurement result after calibration can trace to the source to country
Current standard, aerosol diluter as in chain of tracing to the source to it is lower and on an important ring, if diluter is allowed to trace to the source to particle again
Counter will result in chain confusion of tracing to the source.
3. calibrating aerosol diluter thinner ratio using hydrometry
The flow for only measuring the flow of predecessor counter and the clean compressed gas of supplement, then calculates its dilution
Than can not really measure the changing value situation in diluter of particle concentration at all, have ignored aerosol particle in diluter
It inside whether there is the factors such as cohesion, attachment.
Therefore, the calibration method of the reliable aerosol diluter of and result small there is an urgent need for a kind of measurement error at present.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of calibration method of shunt aerosol diluter, use
Scientific and reasonable calibration method guarantees the accurate and reliable of its measurement result.
The present invention is implemented as follows:
A kind of calibration method of shunt aerosol diluter of the invention, specifically comprises the following steps:
(2) calibration sample is prepared: the monodisperse particle certified reference material that calibration is 0.5 μm of partial size using standard substance,
Spot measurement is selected for the diluter of fixed dilution ratio, for the diluter of dynamic dilution ratio, in maximum dilution than in range
Select 3 points of upper, middle and lower as measurement point；Standard substance sample is diluted, obtains 2 samples, wherein the concentration of 2# sample
It should be f times of 1# sample concentration, the measurement point when f is the fixed extension rate of diluter or calibration, then according to remaining
Lower step is calibrated.
(5) calibration system includes sequentially connected aerosol generator, uniform mixing tank, standard particle counter, is used
When, 1# sample is atomized in the aerosol generator, and adjust the stream that aerosol flow is less than standard particle counter
Amount, by uniform mixing tank, into standard particle counter, flow needed for standard particle counter is supplied in addition to aerosol generator
Except giving, insufficient flow independently sucks uniform mixing tank by HEPA or ulpa filter, into standard particle counter, makes
The two flow matches.
When using 1# sample, the setting parameter of aerosol generator is adjusted, keeps the particle of standard particle counter measures dense
Degree is within the scope of (3000~30000)/28.3L, and duplicate measurements 3 times, the concentration of record standard corpuscular counter, i.e. C1；
(6) when being calibrated using 2# sample, it is ensured that the flow of standard particle counter and shunt aerosol to be calibrated are dilute
The rated flow for releasing device coincide, and the aerosol input port of shunt aerosol diluter to be calibrated is connected uniform mixing tank
Aerosol outlet, aerosol delivery outlet connect the input port of standard particle counter.And 2# sample is measured in standard particle meter
The measured value of number device, duplicate measurements 3 times, i.e. particle concentration value C2；
Under normal conditions, the sampling time of standard particle counter setting is 1 minute, i.e. C1、C2For standard particle counter
Within one minute, collected aerosol total particle number.
(7) the thinner ratio f of the shunt aerosol diluter is finally calculated as follows0.5, and and nominal value into
Row comparison, calculates its error of indication Δ δf,0.5, complete the calibration to shunt aerosol diluter:
Further:
In step (1), the monodisperse particle certified reference material is monodisperse polyphenyl alkene (PSL) particles levels object
Matter, partial size are 0.5 μm.
In step (2), the aerosol generator includes gas mass flow meter, aerosol atomizing with micromanipulator
Device and diffusion dryer.Wherein diffusion dryer guarantees the humidity for the sol particles that it is generated lower than 30%.
In step (2), the uniform mixing tank is equipped with an aerosol entrance, a clean diluent air entrance, one
Aerosol outlet, the aerosol entrance connect the aerosol generator, and the aerosol outlet connects the standard particle
Counter.
In step (2), the requirement of the aerosol generator are as follows: by standard particle of the partial size in 0.1 μm~5 μ ms
Atomization.
In step (2), the requirement of the uniform mixing tank are as follows: the stability of the aerosol concentration in 10 minutes should be better than
1%.
In step (2), the requirement of the standard particle counter are as follows: should have 0.3 μm, 0.5 μm, 1 μm, 5 μm of partial size gears,
And it is capable of measuring the amounts of particles concentration within the scope of (3000~30000)/28.3L, repeatability is better than 3%.
The present invention has the advantage that calibration method of the invention effectively can carry out school to shunt aerosol diluter
Standard improves the measurement accuracy of the analysis instruments such as corpuscular counter, provides technology branch for the traceability system foundation of amounts of particles concentration
Support.
Detailed description of the invention
The present invention is further illustrated in conjunction with the embodiments with reference to the accompanying drawings.
Fig. 1 is the schematic diagram of shunt aerosol diluter, wherein 1 bypass air inlet, 2 high efficiency particulate air filters, 3 reset valves, 4
Capillary.
Fig. 2 is the composition schematic diagram of calibration system.
Fig. 3 is the calibration process schematic diagram of calibration system.
Specific embodiment
Embodiment 1
Alkene (PSL) particles levels solution, the volume of solution are the monodisperse polyphenyl of two kinds of various concentrations of preparation first
100mL, 1# sample are the dilution of the high concentration polystyrene that partial size is 0.5 μm and pure water, the polyphenyl second of 2# sample preparation
The concentration of alkene solution is f times of 1#, the i.e. extension rate of diluter, as shown in table 1.
Table 1. calibrates the standard substance of required concentration ratio
* the concentration ratio of monodisperse particle dilution can also separately be prepared according to actual spot of measurement.
The preparation method of monodisperse particle dilution is as follows:
(1) the polystyrene stoste of high concentration is directly dripped in clean micro beaker, to avoid stoste pollution.
(2) 1# sample is prepared, selects the microscale sampler of 50uL by the stoste of 50uL by moving into 100mL's in micro beaker
In molten measuring bottle.Pure water is injected into volumetric flask, when close to 100mL groove, covers tightly capacity bottle stopper, is inverted 3 times back and forth, is filled solution
Divide mixing, then pure water is injected, until reaching at 100mL groove.
(4) 2# sample is prepared, selects the microscale sampler of 500uL by f*50uL (if thinner ratio nominal value is 10, herein
For 500uL) stoste by micro beaker move into 100mL molten measuring bottle in.Pure water is injected into volumetric flask, is carved close to 100mL
When line, capacity bottle stopper is covered tightly, inverts 3 times back and forth, is sufficiently mixed solution, then pure water is injected, until reaching 100mL groove
Place.
Calibration method is, through calibrated corpuscular counter before and after using aerosol diluter, measures particle concentration
Value calculates the dilution ratio of diluter, and the comparison with nominal value, completes the calibration to diluter.It is specific as follows:
(1) select 1# sample first, be added aerosol generator (by the gas mass flow meter with micromanipulator and
Aerosol atomizing device forms stable particulate to control flow and particle generation rate.Guarantee its generation by drier
Sol particles humidity lower than in solution bottle 30%), open generator power, clean by high efficiency particulate air filter filtering is pressed
After contracting air enters aerosol generator, the standard solution in device is atomized, it is appropriate that adjusting aerosol occurrence quantity obtains concentration
And the molten particle of gas that concentration is stable, and its flow is less than corpuscular counter rated flow, by uniform mixing tank, accesses particle meter
Device is counted, for flow needed for corpuscular counter other than generator supply, insufficient flow is autonomous by HEPA or ulpa filter
Uniform mixing tank is sucked, the two flow matches are made.Working principle is as shown in Figure 2.According to the connection type of Fig. 2, particle meter is opened
Number devices, allow its preheating, self-cleaning, zeroing, and corpuscular counter was arranged to suitable particle size range and sampling time.Calculate grain
The concentration of sub-count device is C1。
(2) it is constant to save aerosol generator equipment, 2# sample is changed in the solution bottle of aerosol generator.
(3) flow value of corresponding corpuscular counter and the rated flow of diluter is selected to match, and by shunt
Aerosol diluter accesses between uniform mixing tank and corpuscular counter, as shown in figure 3, re-measuring according to the method described above, counts
The concentration for calculating corpuscular counter is C2。
Note: in Fig. 3, the working flow and aerosol diluter working flow point Ying Xiangtong of corpuscular counter.
So calculate the thinner ratio f of aerosol diluter are as follows:
Wherein:
C1The concentration of -1# solution, standard particle counter measures value；
C2The concentration of -2# solution, standard particle counter measures value；
C1#The concentration of PSL particle in -1# solution；
C2#The concentration of PSL particle in -2# solution.
The technical requirements of calibration system of the present invention are as follows:
1) aerosol generator
Standard particle of the partial size in (0.1~5) μ m can be atomized.
2) uniform mixing tank
The stability of aerosol concentration in 10 minutes should be better than 1%.
3) corpuscular counter
Should have 0.3 μm, 0.5 μm of partial size gear, the amounts of particles that can measure within the scope of (3000~30000)/28.3L is dense
Degree, repeatability are better than 3%, if diluter flow is 2.83L/min, then selecting flow is the corpuscular counter of 2.83L/min,
If diluter flow is 28.3L/min, then selecting flow is the corpuscular counter of 28.3L/min.
Calibration method and result: select certain brand (III 110) corpuscular counter standard, have from
0.1 μm to 5.0 μm of 8 partial size channels, flow 1.0CFM, uncertainty of measurement MPEG: ± 10%, repeatability is
0.4%, certain brand particle concentration diluter (ATI aerosol particle concentration diluter TDA-D10) is selected, flow is
1.0CFM, thinner ratio nominal value are 10.
The aerosol generator of use, controls its flow and constant concentration, and stability is better than 2%/h.Preparing partial size is
The monodisperse polyphenyl of two kinds of concentration of 500nm alkene (PSL) particles levels solution, wherein 2# solution concentration is the 10 of 1# solution concentration
Times.
Conventional calibration method directly selects 2# standard substance to be calibrated (method 1), and the gas for adjusting particle generator is dense
Degree, and controlling its aerosol concentration is 36288 (stability is better than 2%/h), the dilution of the aerosol diluter of measurement such as table 2
It is shown.
The present invention is calibrated (method 2) using 1# and 2# standard substance respectively, and aerosol occurs when replacing standard substance
The setting of device is constant, when using 1# standard substance, is directly measured with corpuscular counter, when using 2# standard substance, in particle meter
Before number device plus diluter measures, as shown in table 3.
Table 2. measures the thinner ratio of diluter using 2# standard substance
Table 3. uses 1# standard substance and 2# standard substance respectively, measures the thinner ratio of aerosol diluter
From table 2 and table 3 it will be seen that method 2 with the measurement result of method 1 compared with the nominal value of diluter, side
The relative error of method 2 is smaller.And since the uncertainty of measurement of standard particle counter is MPEG: ± 10%, repeatability is
0.4%, method 1 measure it is uncertain be greater than 10, method 2 measure it is uncertain be then better than 3, because of 2 measurement result of the method can
It is far longer than the reliability of 1 measurement result of method by property.
Although specific embodiments of the present invention have been described above, those familiar with the art should be managed
Solution, we are merely exemplary described specific embodiment, rather than for the restriction to the scope of the present invention, it is familiar with this
The technical staff in field should be covered of the invention according to modification and variation equivalent made by spirit of the invention
In scope of the claimed protection.
Claims (7)
1. a kind of calibration method of shunt aerosol diluter, characterized by the following steps:
(1) calibration sample is prepared: the monodisperse particle certified reference material that calibration is 0.5 μm of partial size using standard substance, for
The diluter of fixed dilution ratio selects spot measurement, for the diluter of dynamic dilution ratio, in maximum dilution than selecting in range
3 points of upper, middle and lower are used as measurement point；Standard substance sample is diluted, obtains 2 samples, wherein the concentration of 2# sample should be
F times of 1# sample concentration, the measurement point when f is the fixed extension rate of diluter or calibration, then walks according to remainder
Suddenly it is calibrated；
(2) calibration system includes sequentially connected aerosol generator, uniform mixing tank, standard particle counter, in use, will
1# sample is atomized in the aerosol generator, and adjusts the flow that aerosol flow is less than standard particle counter, warp
Uniform mixing tank is crossed, into standard particle counter, flow needed for standard particle counter supplies it in addition to aerosol generator
Both outside, insufficient flow independently sucks uniform mixing tank by HEPA or ulpa filter, into standard particle counter, make
Flow matches；
When using 1# sample, the setting parameter of aerosol generator is adjusted, the granule density of standard particle counter measures is made to exist
Within the scope of 3000~30000/28.3L, duplicate measurements 3 times, the concentration of record standard corpuscular counter, i.e. C1；
(3) when being calibrated using 2# sample, it is ensured that the flow of standard particle counter and shunt aerosol diluter to be calibrated
Rated flow coincide, the gas that the aerosol input port of shunt aerosol diluter to be calibrated is connected uniform mixing tank is molten
Gel outlet, aerosol delivery outlet connect the input port of standard particle counter.And 2# sample is measured in standard particle counter
Measured value, duplicate measurements 3 times, i.e. particle concentration value C2；
Under normal conditions, the sampling time of standard particle counter setting is 1 minute, i.e. C1、C2Divide for standard particle counter one
Within clock, collected aerosol total particle number；
(4) the thinner ratio f of the shunt aerosol diluter is finally calculated as follows0.5, and carried out pair with nominal value
Than calculating its error of indication Δ δf,0.5, complete the calibration to shunt aerosol diluter:
2. the calibration method of shunt aerosol diluter according to claim 1, it is characterised in that: in step (1), institute
Stating monodisperse particle certified reference material is monodisperse polyphenyl alkene (PSL) particles levels substance, and partial size is 0.5 μm.
3. the calibration method of shunt aerosol diluter according to claim 1, it is characterised in that: in step (2), institute
Stating aerosol generator includes the gas mass flow meter with micromanipulator, aerosol atomizing device and diffusion dryer,
Middle diffusion dryer guarantees the humidity for the sol particles that it is generated lower than 30%.
4. the calibration method of shunt aerosol diluter according to claim 1, it is characterised in that: in step (2), institute
Uniform mixing tank is stated equipped with an aerosol entrance, clean diluent air entrance, an aerosol outlet.
5. the calibration method of shunt aerosol diluter according to claim 1, it is characterised in that: in step (2), institute
State the requirement of aerosol generator are as follows: be atomized standard particle of the partial size in 0.1 μm~5 μ ms.
6. the calibration method of shunt aerosol diluter according to claim 1, it is characterised in that: in step (2), institute
State the requirement of uniform mixing tank are as follows: the stability of the aerosol concentration in 10 minutes should be better than 1%.
7. the calibration method of shunt aerosol diluter according to claim 1, it is characterised in that: in step (2), institute
State the requirement of standard particle counter are as follows: should have 0.3 μm, 0.5 μm, 1 μm, 5 μm of partial size gears, and be capable of measuring (3000~
30000) the amounts of particles concentration within the scope of/28.3L, repeatability are better than 3%.
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| CN113252372B (en) * | 2021-03-30 | 2023-04-18 | 湘潭市计量测试检定所 | Calibration method of medical compression atomizer |
| CN114112866A (en) * | 2021-12-28 | 2022-03-01 | 苏州苏信环境科技有限公司 | Testing device and method for verifying consistency of particle counter sensor |
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