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41 Issue by Google ACTA METROLOGICA SINICA ÿÿÿÿÿÿÿÿ ÿ ÿÿÿ
6 June 2020 ÿÿÿÿÿÿ
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
Zhang Ailiang 1 ÿ Liu Yue1 ÿ Chen Qiyue 1 ÿ Wang Tingting 2 , Shi Chanzhen 1 , Zhang Zitong 1
Abstract: The internal mechanism and working principle of aerosol photometer are introduced, and a calibration device and calibration method for mass
concentration of aerosol photometer based on filter sampling method are proposed. The concentration stability is less than 5%, and the mass concentration indication
error of the aerosol photometer is less than ±10%. The traceability of the mass concentration of the aerosol photometer is solved, which can effectively improve the
measurement accuracy of the device. Key words: metrology; aerosol photometer; mass concentration; calibration method
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ ÿÿÿÿÿÿÿÿÿÿÿÿÿ
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
Therefore, it cannot meet the demand for traceability of the testing equipment. The
1 Introduction Shanghai Institute of Metrology and Testing Technology has undertaken the task of
formulating the calibration specification for the "Aerosol Photometer" issued by the
With the gradual improvement of the cleanliness requirements of production and National Environmental Chemical Metrology Technical Committee in 2018. In this
purification areas in pharmaceutical and medical and health enterprises and institutions, specification, the technical indicators and calibration methods for the mass concentration
the challenges to clean technology will also reach an unprecedented depth and breadth of aerosol photometers need to be formulated. .
[1] . At present, aerosol photometers are widely used to detect high-efficiency filters and
filtration terminals of purification products to verify whether the relevant areas and 2 Working principle and optical measurement system
equipment meet the purification requirements. Therefore, the accuracy of the aerosol
photometric count value directly affects the final test result in a clean environment. The working principle of the aerosol photometer (hereinafter referred to as the instrument)
Compared with the previous detection of ambient air cleanliness by dust particle counters, is: the instrument extracts the air samples at the upstream and downstream ends of the filter
aerosol photometers can more intuitively and accurately reflect the leak points of the system under test at a constant flow rate, the sampling unit delivers the air sample to the
filtration system under inspection. At present, this detection method has been widely used measurement unit, and the measurement unit measures the aerosol in the air sample. The mass
by national standards and industry standards, as a widely used detection equipment, but there is no domestic is measured, and the data processing unit analyzes the measurement results and calcul
concentration
The ratio of the two calculates the leakage rate of the system under test, and finally the measurement result is output The retention efficiency of quasiparticles is not less than
by the display unit. The schematic diagram of the instrument detection principle is shown in Figure 1. 99.99%. 3.2 Polyalphaolefins
base oil and is widely used. PAO-4 (chemical code 68649-12-7) aerosol refers to the
generated by aerosol photometer fogging and mixing device. Polydisperse Aerosol. 3.3
Sampling and weighing system (1) Sampling device: the flow range is 0~50L/min, and the
stability of 4h should be less than 5%; (2) Flow standard device: The range is 0~50L/min,
the maximum
ÿÿÿÿÿ ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
light from reaching the photomultiplier tube directly. A condenser lens facing away from concentration and uniform mixing. The interior is equipped with multiple III-A
the light source directs the scattered light to the photomultiplier tube through a conical dark brushed gold nozzles, which generate polydisperse aerosols from PAO-4 oil through the
area. Its optical principle is: based on the Mie scattering theory of light, the particle size is Venturi effect. Using the filter membrane sampling method to measure the concentration
close to or larger than the wavelength of the incident light; the scattered light intensity is of the device's fog outlet, the stability of the aerosol mass concentration within 20min
asymmetric in all directions, and the forward scattering along the incident direction is the
should be less than 5% [4] . Figure 3 shows the structure of the ÿ-A wire drawing gold
strongest, and the larger the particle is. The larger the value, the stronger the forward
nozzle [5] .
scattering [2] . The scattered light intensity is proportional to the particle number
concentration. If the relative density of the particles is known, the ratio of the particle
number to the mass is a constant, so the scattered light intensity is proportional to the
can be achieved by measuring the scattered light intensity caused by aerosol under a
specific light path [3] . The schematic diagram of the optical measurement system of the
ÿÿÿÿÿ ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
3.1 Filter
Membrane The filter membrane is circular with a diameter of (37 ± 0.25) mm; the
4. Calibration method of mass concentration indication error
pore size is less than 2 ÿm; the thickness is 0.2 to 0.25 ÿm; at a clean air flow rate of 0.45
m/s, the pressure It should be less than 3kPa; the mass increase value after exposure to
4.1 Preparation before calibration (1)
35% RH air for 24h should not exceed 10ÿg; glass fiber filter membrane, quartz filter
The visual inspection of the filter membrane should ensure that the edges are flat, the thickness is uniform,
membrane and other inorganic filter membranes can be selected.
Machine Translated by Google
Volume 41 Issue 6 Zhang Ailiang et al.: A Calibration Method for Mass Concentration of Aerosol Photometer ÿÿÿ
(2) Before sampling, the filter membrane should be balanced and weighed 5 Verification of calibration results
in a constant temperature and humidity environment, that is, 15-30 °C, (50±5)% RH,
5.1 Stability verification of the mist outlet of the aerosol misting and mixing device
and the filter membrane should be placed for at least 24 hours; The wet equipment
Since the stability of the mass concentration of the misting port of the aerosol
remains the same; after the filter is equilibrated, the filter is weighed using an
misting and mixing device is directly related to the calibration result of the mass
analytical balance.
concentration of the aerosol photometer, it is necessary to verify the stability of the
4.2 Mass concentration calibration
aerosol concentration of the misting port [7] . By adjusting the relevant parameters of
Set the internal reference value of the instrument to be calibrated to 100 mg/m3 . Perform the aerosol fogging and mixing device, a stable aerosol can be generated.
the calibration according to the calibration system shown in Figure 4. Select an aerosol photometer with a repeatability better than 1.5% and connect it to
the fogging port of the aerosol fogging and mixing device. After the instrument is
stable, read the initial value of the aerosol photometer and start timing. The
concentration value was read once every 5 min, for a total of 5 times. Take the
maximum and minimum values of the five readings, and calculate the 20-min stability
Figure 4 Schematic diagram of the instrument concentration indication error calibration system
ÿÿÿÿÿÿÿÿÿ ×
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r
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
In the formula: ÿÿ is the stability of the aerosol fogging mixing device; ÿmax is the maximum value
Use the aerosol fogging and mixing device to generate PAO-4 aerosol with a mass concentration
of the five concentration values, mg/m3 ; ÿmin is the minimum value of the five concentration
of 1 to 100 mg/m3 . Connect the fogging ports I and II of the aerosol photometer fogging and mixing
values, mg/m3 ; ÿ is the maximum value of the five concentration values. Average, mg/m3 .
device to the filter membrane respectively through hoses. The sampling port of the sampling device and
Three kinds of aerosols with different mass concentrations were generated
the downstream sampling port of the instrument to be calibrated shall conduct equal flow sampling at the
by using the aerosol fogging and mixing device.
same time, and the measured value Cs1 of the filter membrane sampling device shall be calculated
ÿÿÿ
And record the concentration measurement value Cm1 of the instrument being calibrated .
according to formula (1).
ÿÿÿÿÿÿÿÿ ÿÿÿ
V
Where: Cs is the measured value of the filter membrane sampling device, mg/m3 ; w1 is the mass of the
filter membrane before sampling, mg; w2 is the mass of the filter membrane after sampling, mg; V is the
sampling volume, m3 . The sampling port of the exchange filter sampling device is connected to the
downstream sampling port of the instrument to be calibrated, and the misting port of the aerosol
mist mixing device is connected. At the same time, equal flow sampling is carried out, the measured value
Cs2 of the membrane sampling device is calculated and the concentration measurement of the instrument
Fig.5 Stability curve of misting port I
under calibration is recorded. value Cm2 . Calculate the ith single concentration indication error ÿi of the
ÿÿÿÿÿ ÿÿÿÿÿÿÿÿ ÿÿÿÿÿÿÿÿÿ
instrument according to formula (2), mg/m3 . (Cm1 + Cm2 ) - (Cs1 + Cs2 ) ÿi=
ÿÿÿ
ÿ
In the formula: Cs1 is the calculated value of the filter membrane sampling device connected to the misting
port I, mg/m3 ; Cs2 is the calculated value of the filter membrane sampling device connected to the misting
port II, mg/m3 ; Cm1 is the instrument to be calibrated connected to the misting port. The measured value
of ÿ, mg/ m3 ; Cm2 is the measured value of the instrument to be calibrated connected to the fogging port
ÿ, mg/m3 . Repeat the above operation 4 times, and calculate the mass concentration indication
Table 1 Stability of the mass concentration of the mist nozzle at different concentrations The stability of the fog concentration of the fog mixing device is better than 5%, and the
ÿÿÿÿÿ ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ The error of the mass concentration indication value of the glue photometer is less than ±10%. thus effective
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
Solve the problem of traceability of mass concentration of aerosol photometer
Aerosol fog concentration Mist mouth I Mist mouth II It ensures the accuracy of mass concentration measurement of aerosol photometer and can improve the
ÿÿ ÿÿÿ ÿÿÿ
[ references]
ÿÿ ÿÿÿ ÿÿÿ
[1] Huang Tinglei, Li Min, Chen Yazhu. Development of Optical Particle Counting Device
ÿÿÿ ÿÿÿ ÿÿÿ
[J]. Chinese Journal of Metrology, 2006, 27(1): 88-90.
From the data in Table 1, it can be seen that there are two aerosol mist mixing devices.
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
The stability of the concentration of the fogging port within 20min is less than 5%, which is in line with the technical requirements.
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
technical requirements. Therefore, the misting port of the aerosol misting and mixing device is unstable ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
The systematic error introduced by the property is under control, the device can be used for gas [2] Wang Shimin, Zhu Zhen, Ye Mao, et al. Mie theory in light scattering particle size measurement
Sol photometer mass concentration calibration work. On two improved numerical calculation methods [J]. Journal of Metrology, 1999,
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
5.2 Verification of filter sampling calibration results
Table 2 Calibration results of aerosol mass concentration [3] Wang Zhengqi, Hu Guangyong, Zhang Yuchen. Aerosol Photometer R&D Analysis
ÿÿÿ·ÿÿÿ ÿÿÿ·ÿÿÿ ÿÿÿ·ÿÿÿ ÿÿÿÿ [4] Zhang Ailiang, Gu Lingling, Gao Zheng, et al. Aerosol for leak detection of high efficiency filter
Research on the calibration method of glue photometer [J]. Cleaning and Air Conditioning Technology, 2016,
ÿÿÿÿÿ ÿÿÿÿÿ ÿÿÿÿ ÿÿÿ
ÿÿÿÿÿÿÿÿ ÿÿÿÿÿÿÿÿÿÿÿÿ
ÿÿÿÿÿ ÿÿÿÿÿ ÿÿÿÿ ÿÿÿ
ÿÿÿÿÿÿÿÿ ÿÿÿÿ ÿÿÿÿ ÿ ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ on
ÿÿÿÿÿ ÿÿÿÿÿ ÿÿÿ ÿÿÿ
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
The development of reference material [J]. Chinese Journal of Metrology, 2019, 40(1): 159-
From the data in Table 2, it can be found that the aerosol hair mist is used for mixing.
ÿÿÿÿ
The device and filter sampling method were used to calibrate the aerosol photometer and were calibrated
ÿÿhangÿ ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿationÿÿÿÿÿ
The relative indication error of the mass concentration of the aerosol photometer is less than
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
±10%. The calibration results meet the technical requirements of these three types of instruments
ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ
Therefore, this method can effectively solve the problem of traceability of such instruments.
need.
In this paper, an aerosol photometer mass concentration parameter is given. Metrology calibration technology and standardization research.
Calibration device and calibration method, and experimentally verified aerosol emission ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿ