CN112577871A - Standard mass diaphragm for calibrating atmospheric particle concentration measuring instrument by beta-ray method and manufacturing method thereof - Google Patents
Standard mass diaphragm for calibrating atmospheric particle concentration measuring instrument by beta-ray method and manufacturing method thereof Download PDFInfo
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- CN112577871A CN112577871A CN202011630076.4A CN202011630076A CN112577871A CN 112577871 A CN112577871 A CN 112577871A CN 202011630076 A CN202011630076 A CN 202011630076A CN 112577871 A CN112577871 A CN 112577871A
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- 230000005250 beta ray Effects 0.000 title claims abstract description 78
- 239000002245 particle Substances 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims description 40
- 239000012528 membrane Substances 0.000 claims abstract description 99
- 230000003287 optical effect Effects 0.000 claims abstract description 57
- 229920006267 polyester film Polymers 0.000 claims abstract description 56
- 238000005070 sampling Methods 0.000 claims abstract description 39
- 239000013618 particulate matter Substances 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000005530 etching Methods 0.000 claims description 21
- 238000005259 measurement Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 3
- 239000003570 air Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000012080 ambient air Substances 0.000 description 2
- 238000003486 chemical etching Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 1
- 238000004164 analytical calibration Methods 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000008277 atmospheric particulate matter Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- G01N15/0606—Investigating concentration of particle suspensions by collecting particles on a support
- G01N15/0618—Investigating concentration of particle suspensions by collecting particles on a support of the filter type
Abstract
The invention discloses a standard mass diaphragm for calibrating a beta-ray atmospheric particle concentration measuring instrument and a manufacturing method thereof0The value of/I) and the mass of the first blank filter membrane after trapping the particulate matter; obtaining an initial measured beta-ray dose I using a second blank filter1(ii) a Arranging an optical polyester film on the second blank filter membrane; the measured beta-ray dose I was obtained using Structure A2Calculating ln (I)1/I2) A value of (d); using ln (I)0The value of/I) and ln (I)1/I2) Judging whether the used optical polyester film can be used as a standard mass diaphragm for calibrating equivalent mass after sampling with the first blank filter membrane; if the judgment is not successful, the optical polyester film is processed until the optical polyester film can be used as a standard quality film for calibration, and the optical polyester film is taken down. The invention can combine experiments locally, and eliminates the use of other standard diaphragmsOn time, errors due to different composition states of particulate matter in the atmosphere.
Description
Technical Field
The invention relates to the technical field of atmospheric particulate matter concentration detection, in particular to a standard mass diaphragm for calibrating an atmospheric particulate concentration measuring instrument by a beta-ray method and a manufacturing method thereof.
Background
In the field of atmospheric particle concentration detection, common methods are a light scattering method and a beta-ray method, wherein the beta-ray method has the advantages of higher measurement precision, stable measurement and the like, and is commonly used for measuring atmospheric particles in a state-controlled environmental air quality monitoring station. Beta-ray methods rely on the change in radiation as it passes through the enriched particles being measured to calculate the equivalent concentration, and therefore a set of membranes equivalent to the amount of particulate matter must be present to perform prior instrument calibration. The standard diaphragms commonly used at present can only be supplied by foreign instrument manufacturers along with instrument quota, the selling price is high, the number of the available diaphragms is small, the purchasing is inconvenient, the time period is long, and the working efficiency of the measuring work is seriously influenced. Meanwhile, due to different composition states of particles in the atmosphere, errors can be generated in calibration of the purchased standard diaphragm.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a standard mass diaphragm for calibrating an atmospheric particle concentration measuring instrument by a beta-ray method and a manufacturing method thereof.
The technical scheme adopted by the invention is as follows:
a method for manufacturing a standard mass diaphragm for calibrating a beta-ray atmospheric particle concentration measuring instrument comprises the following steps:
s1, sampling the sampling point by the atmospheric particle concentration measuring instrument by the beta-ray method by using the first blank filter membrane, and calculating ln (I) after the measurement is finished0The value of/I) and the mass of the first blank filter membrane after trapping the particulate matter, wherein I0The beta ray quantity is initially measured before sampling, and I is the beta ray quantity measured after sampling;
s2, the atmospheric particle concentration measuring instrument by the beta-ray method obtains the initially measured beta-ray quantity I by utilizing the second blank filter membrane1(ii) a Arranging an optical polyester film on the second blank filter membrane to form a structure A; the measured beta-ray dose I was obtained using Structure A2Calculating ln (I)1/I2) A value of (d); the second blank filter membrane is the same as the first blank filter membrane;
s3, using ln (I)0The value of/I) and ln (I)1/I2) Judging whether the used optical polyester film can be used as a standard mass diaphragm for calibrating equivalent mass after sampling with the first blank filter membrane;
s4, if the structure A cannot be judged, taking down the optical polyester film on the structure A, etching the optical polyester film by using etching liquid, gradually reducing the thickness of the optical polyester film, assembling the optical polyester film into a new structure A, and measuring the thickness of the optical polyester film;
s5, repeating S3-S4 until the optical polyester film used in the new structure A can be used as a standard mass film for calibration with equivalent mass after sampling the first blank filter membrane, and removing the optical polyester film.
Preferably, when the first blank filter and the second blank filter are mounted, the rough surfaces of the first blank filter and the second blank filter face the direction of the air inlet, and the optical polyester film is arranged on the rough surface side of the second blank filter.
Preferably, I0The average value of the beta ray amount in a preset time period after the sampling starts to be measured; i is the average value of beta ray amount in the last preset period of time before the sampling is finished; i is1The average value of the beta ray quantity in a preset time period after the start of the measurement is obtained by utilizing a second blank filter membrane for the beta ray method atmospheric particle concentration measuring instrument; i is2The beta-ray atmospheric particle concentration measuring instrument utilizes the average value of beta-ray quantity of the structure A in a preset time period after the measurement is started.
Preferably, the first blank filter and the second blank filter used in S1 and S2 are both isothermal and isowet; before the first blank filter membrane and the second blank filter membrane are used, the first blank filter membrane and the second blank filter membrane are placed in a constant-temperature constant-humidity environment for a preset time, and the first blank filter membrane and the second blank filter membrane are made to be isothermal and equal-humidity.
Preferably, in S3, ln (I) is calculated0I) minus ln (I)1/I2) Is divided by ln (I)0Obtaining an error, and judging that the used optical polyester film can be used as a standard quality diaphragm for calibration when the error is within a preset range value; and when the error exceeds a preset range value, judging that the used optical polyester film cannot be used as a standard quality diaphragm for calibration.
Preferably, the preset range value is ln (I)0/I) a range between plus and minus 1%.
Preferably, in S4, the etching solution is a sodium hydroxide solution.
Preferably, the concentration of solute in the sodium hydroxide solution is 5-8mol/L, and the etching temperature is 35-80 ℃.
The invention also provides a standard mass diaphragm for calibrating the atmospheric particle concentration measuring instrument by the beta-ray method, which is manufactured by the manufacturing method.
Preferably, the standard quality diaphragm for calibrating the beta-ray atmospheric particle concentration measuring instrument further comprises a diaphragm plate, a circular hole is formed in the diaphragm plate, and the optical polyester film is arranged in the circular hole.
The invention has the following beneficial effects:
in the manufacturing method of the standard quality diaphragm for calibrating the beta-ray atmospheric particle concentration measuring instrument, the beta-ray atmospheric particle concentration measuring instrument utilizes the first blank filter membrane to sample at the sampling point, and the beta-ray quantity before and after sampling at the actual sampling point and the quality of particulate matters trapped by the first blank filter membrane are obtained, so that errors caused by different component states of particulate matters in the atmosphere when other standard diaphragms are used for calibration can be eliminated; using ln (I)0The value of/I) and ln (I)1/I2) The value of (A) is used for judging whether the used optical polyester film can be used as a standard quality diaphragm for calibrating equivalent quality after sampling with the first blank filter membrane, so that errors caused by different blank filter membranes in the standard film manufacturing process are eliminated. In addition, the equivalent quality of the diaphragm is controlled by utilizing chemical etching, the process requirement is low, the standard quality diaphragm can be manufactured in a general-grade chemical laboratory, the cost of the medicine and the material required by manufacturing is low, the acquisition is convenient, the diaphragm can be manufactured at any time when the measurement is needed, the diaphragm does not need to be imported from foreign countries, and the working efficiency of the measurement work is ensured.
Detailed Description
The present invention will be further described with reference to the following examples.
The invention relates to a method for manufacturing a standard quality diaphragm for calibrating a beta-ray atmospheric particle concentration measuring instrument, which comprises the following steps:
1) cutting the blank filter membrane into a circular blank filter membrane with the area of S by using a circular cutter (S is the effective dust deposition area), and putting the blank filter membrane into a container with constant temperature and constant humidityThe test chamber was left for 24h and the blank filter was isothermally wetted. Measuring the mass of the blank filter membrane for multiple times by using a balance with the precision of one ten-thousandth, recording effective values for 10 times, and taking the average value of the effective values for 10 times as the mass m of the blank filter membrane before particulate matters are deposited0(unit: mg);
2) correctly clamping the blank filter membrane obtained in the step 1) by using a serrated forceps and placing the blank filter membrane into a beta-ray method atmospheric particle concentration measuring instrument, enabling the rough surface of the blank filter membrane to face the air inlet direction, recording the count value of a beta-ray detector per minute, taking the average value of five minutes before the sampling begins, and counting the average value as the initially measured beta-ray quantity I0。
3) The method comprises the steps of placing a beta-ray atmospheric particle concentration measuring instrument at a place needing to be measured for sampling, and setting sampling time T (unit: min), the sampling flow rate Q (unit: l/min), sampling is started. After sampling is finished, the counting value of a beta-ray detector per minute is recorded, the average value of the last five minutes before sampling is taken as the beta-ray quantity I measured after particulate matters are trapped, and ln (I) is calculated after measurement is finished0The value of/I.
4) Taking out the blank filter membrane deposited with the particulate matters in the step 3) by using the same tweezers immediately, placing the blank filter membrane in a constant-temperature constant-humidity laboratory for 24 hours, weighing the blank filter membrane in a balance used before under the same conditions after the blank filter membrane is subjected to constant temperature and humidity, measuring the mass of the filter membrane after sampling for multiple times, recording effective values for 10 times, and taking the average value of the recorded values for 10 times as the mass m of the filter membrane after sampling1(unit: mg);
5) calculating the mass difference value delta m before and after sampling the blank filter membrane as m1-m0And calculating the concentration of the particulate matter in the ambient air at the measurement point
(unit: μ g/m)3)；
6) Taking a cut blank filter membrane again, wherein the blank filter membrane is the same as the blank filter membrane in the step 1), and a plurality of blank filter membranes can be cut out simultaneously in the step 1) and are subjected to the same treatment for subsequent use; non-serrated forceps for the blank filter membraneCorrectly clamping the filter membrane, placing the filter membrane into an atmospheric particle concentration measuring instrument adopting a beta-ray method, enabling the rough surface of the blank filter membrane to face the direction of an air inlet, recording the count value of a beta-ray detector per minute, taking the average value of five minutes before sampling begins, and calculating the initial measured beta-ray quantity I1。
7) Cutting an optical polyester film (such as a PET film) into a membrane with the area of S by using a circular die, then putting the membrane into a sodium hydroxide solution for etching (because the existing optical polyester film which is bought at present has larger thickness (the thickness is 50 mu m) and can not be directly used, the etching needs to be carried out firstly, if the optical polyester film with the smaller thickness can be directly obtained, the etching can be directly used without etching firstly), after etching for a period of time, taking out the membrane and putting the membrane on a blank filter membrane which is obtained in the step 6), then putting the integral structure of the optical polyester film and the blank filter membrane inside a beta-ray method atmospheric particle concentration measuring instrument for measuring, continuously measuring for 5 minutes, recording the average value of 5 minutes, and calculating the beta-ray quantity I which is measured after the optical polyester film and the blank filter membrane pass through2Calculating ln (I)1/I2) A value of (d); wherein the etching temperature of the sodium hydroxide solution is 35-80 ℃, and the concentration of sodium hydroxide in the sodium hydroxide solution is 5-8 mol/L;
8) the ln (I) obtained by calculating after passing through an optical polyester film sheet and a blank filter film sheet1/I2) Calculating the value and the obtained ln (I) after trapping particulate matter0The value of/I is compared, i.e. ln (I) is calculated0I) minus ln (I)1/I2) The difference of (a). If there is an error (ln (I) between the two0I) minus ln (I)1/I2) Is divided by ln (I)0Percentage after/I)) exceeds +/-1%, taking the optical polyester film piece down, putting the optical polyester film piece into a sodium hydroxide solution again for etching, taking out for testing, repeatedly etching and testing until the obtained ln (I) is calculated1/I2) Value of (d) and ln (I)0If the error between the values of/is within. + -. 1%, an optical polyester film having an equivalent mass of rho is obtained.
9) And finally, tightly fixing the optical polyester film sheet obtained in the step 8) on a film plate, and attaching an equivalent mass label.
Examples
The process of the manufacturing method of the standard quality diaphragm for calibrating the beta-ray atmospheric particle concentration measuring instrument comprises the following steps:
cutting the blank filter membrane into 3.14cm area by using a circular cutter2The blank filter membrane is placed in a constant temperature and humidity laboratory for 24 hours to be isothermal and equal humidity. Measuring the mass of the blank filter membrane for multiple times by using a balance with the precision of one ten-thousandth, recording 10 effective values, and taking the average value of the 10 recorded values as the mass m of the filter membrane before depositing the particulate matters0209.6 mg; correctly clamping the blank filter membrane by using a pair of jagged tweezers, placing the blank filter membrane into a beta-ray atmospheric particle concentration measuring instrument, enabling the rough surface of the filter membrane to face the air inlet direction, recording the count value of a beta-ray detector per minute, taking the average value of the five minutes before the sampling begins, and counting the average value as the beta-ray quantity I initially measured0＝91080。
The beta-ray method atmospheric particle concentration measuring instrument is placed at a place needing to be measured for sampling, the sampling time is set to be 300min, the sampling flow is set to be 16.7L/min, and the instrument starts to sample. After sampling is finished, the counting value of a beta-ray detector per minute is recorded, the average value of the last five minutes before sampling is finished is taken, and the beta-ray quantity I measured after particulate matters are trapped is 73582, ln (I)0I ═ ln (91080/73582) ═ 0.2133. Taking out the blank filter membrane deposited with the particulate matters by using the same tweezers at once, placing the filter membrane in a constant-temperature constant-humidity laboratory for 24 hours, weighing the filter membrane in a balance used before under the same conditions after the filter membrane is subjected to constant temperature and constant humidity, measuring the mass of the sampled filter membrane for multiple times, recording 10 effective values, and taking the average value of the 10 recorded values as the mass m of the sampled filter membrane1211.4 mg; calculating mass difference Δ m ═ m1-0-211.4-209.6-1.8 mg, calculating the concentration of particulate matter in the ambient air
Taking a blank filter membrane which is cut out and is the same as the previous filter membrane, correctly clamping the blank filter membrane by using a pair of jagged tweezers, and putting the blank filter membrane into the beta-rayThe rough surface of the filter membrane faces the direction of the air inlet, the count value of a beta ray detector per minute is recorded, the average value of the five minutes before the sampling begins is taken, and the initially measured beta ray quantity I is measured189886. Cutting an optical polyester film base film with the thickness of 50 mu m into a film with the area of 3.14cm by using a circular die2Then placing the membrane into 6mol/L sodium hydroxide solution for etching at the etching temperature of 60 ℃, taking out the membrane to place on a blank filter membrane with the same area after etching for a period of time, then placing the optical polyester film sheet and the blank filter membrane in an instrument for measurement, continuously testing for 5 minutes, recording the average value of five minutes, and calculating the beta ray quantity I measured after passing through the optical polyester film sheet and the blank filter membrane277686, ln (I) is calculated1/I2) Ln (89886/77686) 0.1458. The ln (I) obtained by calculating after passing through an optical polyester film sheet and a blank filter film sheet1/I2) Calculating the value and the obtained ln (I) after trapping particulate matter0The I/values are compared. The error between the two exceeds +/-1 percent, taking down the optical polyester film piece, putting the optical polyester film piece into sodium hydroxide solution again for etching, taking out the optical polyester film piece for testing, repeatedly carrying out etching test until the obtained ln (I) is calculated after the optical polyester film piece and the blank filter membrane1/I2) Calculating the value and the obtained ln (I) after trapping particulate matter0The error between the/I values is-0.75%, the error is within + -1%, and the obtained optical polyester film piece has an equivalent mass of 359.2 μ g/ml3The standard membrane of (1).
And finally, tightly fixing the optical polyester film sheet on a film plate, and attaching an equivalent mass label.
And obtaining the optical polyester standard film with other concentration equivalent mass concentration by the same method.
In conclusion, the invention can calculate the mass concentration of the beta-ray atmospheric particle concentration measuring instrument by combining a manual weighing method with an experiment, then uses the optical polyester film as a base material, controls the thickness of the optical polyester film by using the mass concentration of the beta-ray atmospheric particle concentration measuring instrument, the beta-ray quantity initially measured and the beta-ray quantity measured after particulate matters are trapped, and adopts a chemical etching method to control the thickness of the optical polyester film so that the beta-ray quantity measured after the optical polyester film with a certain thickness is the same as the beta-ray quantity measured after the particulate matters are trapped, thereby obtaining the standard mass diaphragm with specific equivalent mass concentration. The invention has simple preparation requirement and convenient and fast operation, can be manufactured at any time when in measurement, does not need to be imported from foreign countries, and ensures the working efficiency of measurement work. Because the method is based on a standard manual weighing method, the accuracy of the manufactured diaphragm is relatively high. Meanwhile, due to the fact that the composition states of the particles in the atmosphere of each place are different, the method can be manufactured in a local experiment, and errors caused by the fact that the composition states of the particles in the atmosphere of each place are different when other standard diaphragms are used for calibration are eliminated.
Claims (10)
1. A method for manufacturing a standard mass diaphragm for calibrating a beta-ray atmospheric particle concentration measuring instrument is characterized by comprising the following steps:
s1, sampling the sampling point by the atmospheric particle concentration measuring instrument by the beta-ray method by using the first blank filter membrane, and calculating ln (I) after the measurement is finished0The value of/I) and the mass of the first blank filter membrane after trapping the particulate matter, wherein I0The beta ray quantity is initially measured before sampling, and I is the beta ray quantity measured after sampling;
s2, the atmospheric particle concentration measuring instrument by the beta-ray method obtains the initially measured beta-ray quantity I by utilizing the second blank filter membrane1(ii) a Arranging an optical polyester film on the second blank filter membrane to form a structure A; the measured beta-ray dose I was obtained using Structure A2Calculating ln (I)1/I2) A value of (d); the second blank filter membrane is the same as the first blank filter membrane;
s3, using ln (I)0The value of/I) and ln (I)1/I2) Judging whether the used optical polyester film can be used as a standard mass diaphragm for calibrating equivalent mass after sampling with the first blank filter membrane;
s4, if the structure A cannot be judged, taking down the optical polyester film on the structure A, etching the optical polyester film by using etching liquid, reducing the thickness of the optical polyester film, assembling the optical polyester film into a new structure A, and measuring the thickness of the optical polyester film;
s5, repeating S3-S4 until the optical polyester film used in the new structure A can be used as a standard mass film for calibration with equivalent mass after sampling the first blank filter membrane, and removing the optical polyester film.
2. The method for manufacturing a standard mass diaphragm for calibration of a β -ray atmospheric particle concentration measuring instrument according to claim 1, wherein when the first blank filter membrane and the second blank filter membrane are mounted, the rough surface sides of the first blank filter membrane and the second blank filter membrane are directed toward the air inlet, and the optical polyester film is provided on the rough surface side of the second blank filter membrane.
3. The method for manufacturing the standard mass diaphragm for calibrating the beta-ray atmospheric particle concentration measuring instrument according to claim 1, wherein I is0The average value of the beta ray amount in a preset time period after the sampling starts to be measured; i is the average value of beta ray amount in the last preset period of time before the sampling is finished; i is1The average value of the beta ray quantity in a preset time period after the start of the measurement is obtained by utilizing a second blank filter membrane for the beta ray method atmospheric particle concentration measuring instrument; i is2The beta-ray atmospheric particle concentration measuring instrument utilizes the average value of beta-ray quantity of the structure A in a preset time period after the measurement is started.
4. The method for manufacturing the standard mass diaphragm for calibrating the beta-ray atmospheric particle concentration measuring instrument according to claim 1, wherein the first blank filter membrane and the second blank filter membrane used in S1 and S2 are both isothermal and isowet; before the first blank filter membrane and the second blank filter membrane are used, the first blank filter membrane and the second blank filter membrane are placed in a constant-temperature constant-humidity environment for a preset time, and the first blank filter membrane and the second blank filter membrane are made to be isothermal and equal-humidity.
5. The method for manufacturing a standard mass diaphragm for calibration of a β -ray atmospheric particle concentration measurement instrument according to claim 1, wherein in S3, ln (I) is calculated0I) reductionDeln (I)1/I2) Is divided by ln (I)0Obtaining an error, and judging that the used optical polyester film can be used as a standard quality diaphragm for calibration when the error is within a preset range value; and when the error exceeds a preset range value, judging that the used optical polyester film cannot be used as a standard quality diaphragm for calibration.
6. The method for manufacturing a standard mass diaphragm for calibrating a beta-ray atmospheric particle concentration measuring instrument according to claim 5, wherein the preset range value is ln (I)0/I) a range between plus and minus 1%.
7. The method for manufacturing a standard mass diaphragm for calibrating a beta-ray atmospheric particle concentration measuring instrument according to claim 1, wherein in S4, a sodium hydroxide solution is used as the etching solution.
8. The method for manufacturing the standard mass diaphragm for calibrating the beta-ray atmospheric particle concentration measuring instrument according to claim 7, wherein the concentration of solute in the sodium hydroxide solution is 5-8mol/L, and the etching temperature is 35-80 ℃.
9. A standard mass diaphragm for calibrating a beta-ray atmospheric particle concentration measuring instrument, which is obtained by the manufacturing method of any one of claims 1 to 8.
10. The standard mass diaphragm for calibrating the beta-ray method atmospheric particle concentration measuring instrument according to claim 9, further comprising a diaphragm plate, wherein a circular hole is formed in the diaphragm plate, and an optical polyester film is arranged in the circular hole.
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Cited By (1)
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| CN117054305A (en) * | 2023-10-11 | 2023-11-14 | 广东盈峰科技有限公司 | Monitor, calibration method and device thereof and storage medium |
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