CN116046879A - Method for detecting heavy metal elements in air or waste gas particulate matters - Google Patents
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4005—Concentrating samples by transferring a selected component through a membrane
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4033—Concentrating samples by thermal techniques; Phase changes sample concentrated on a cold spot, e.g. condensation or distillation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4088—Concentrating samples by other techniques involving separation of suspended solids filtration
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention belongs to the field of detection and analysis, and particularly relates to a method for detecting heavy metal elements in air or waste gas particulate matters. The method is realized by the following steps: (1) pretreatment: firstly, cutting a sampled polypropylene fiber filter membrane into a digestion tank, adding a mixed solvent of absolute ethyl alcohol and glycerol, shaking uniformly, adding mixed acid, sealing, heating and refluxing, continuously heating after uncapping, cooling, leaching the inner wall of the digestion tank by ultrapure water, leaching, filtering, leaching the filter membrane, and obtaining a solution to be measured after constant volume; (2) drawing a standard curve; (3) detection by ICP-MS. According to the invention, the dissolution of the substance to be detected can be accelerated by improving the pretreatment method of the sample, the extraction efficiency is high, and the detection accuracy is improved; the invention optimizes the detection conditions, is simple, convenient, quick and accurate, and has high recovery rate.
Description
Technical Field
The invention belongs to the field of detection and analysis, and particularly relates to a method for detecting heavy metal elements in air or waste gas particulate matters.
Background
It has been found that heavy metal elements such as lead, cadmium, manganese, arsenic, chromium, nickel, selenium, beryllium, vanadium and the like can be detected in fine particulate matter such as PM2.5 of air or exhaust gas. These elements are combined with other substances in the atmosphere to form PM2.5 and other particles which are inhaled by human body, thereby affecting the normal physiological functions of respiratory system, neovascular system, nervous system and reproductive system of human body. The heavy metal elements are mainly derived from soil, dust weathered by rocks, building dust, sea salt particles and the like; industrial coal-fired smoke dust, metallurgical dust, automobile tail gas and the like in iron and steel plants and the like.
The conventional methods for measuring the metal elements in the fine particles in the air at home include a flame atomic absorption method, a graphite furnace atomic absorption method, an X-ray fluorescence spectrometry and the like. Because the sensitivity of the flame atomic absorption method is relatively low, the content of metal elements in the sample is generally low, a large number of samples are required to be collected by a large-flow sampler, and the samples are separated and enriched, so that the pretreatment process of the samples is very time-consuming and laborious, and only single element measurement is performed; the graphite furnace atomic absorption method can generally omit an enrichment process due to low detection limit, but can not measure multiple elements at the same time, the instrument operation is relatively complicated, the analysis period is longer, and the measuring line range is relatively narrow; the X-ray fluorescence spectrometry belongs to a nondestructive analysis method, but the accuracy needs to be improved, and meanwhile, a proper particle standard sample is difficult to find, and the method is mainly used in the exploration stage of the method and the coarse screening of the sample. In the current sampling process, after the polypropylene fiber filter membrane is adopted for sampling, particles in ambient air collected by the polypropylene fiber filter membrane can not be completely dissolved out in the digestion process, and after acid is added by using a traditional digestion method, the polypropylene fiber filter membrane floats on the surface of acid, so that the acidolysis time is long and the efficiency is low.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a detection method of heavy metal elements in air or waste gas particulate matters, which can greatly improve the decomposition efficiency of a polypropylene fiber filter membrane, ensure that the particulate matters in a collected sample are completely digested, and improve the detection accuracy.
The technical scheme adopted by the invention for achieving the purpose is as follows:
the invention provides a method for detecting heavy metal elements in air or waste gas particulate matters, which comprises the following steps:
(1) Pretreatment: firstly, cutting a sampled polypropylene fiber filter membrane into a digestion tank, adding a mixed solvent of absolute ethyl alcohol and glycerol, shaking uniformly, adding mixed acid, sealing, heating and refluxing, continuously heating after uncapping, cooling, leaching the inner wall of the digestion tank by ultrapure water, leaching, filtering, leaching the filter membrane, and obtaining a solution to be measured after constant volume;
(2) Drawing a standard curve;
(3) Detection was performed using ICP-MS.
Further, in the step (1), the volume ratio of the absolute ethyl alcohol to the glycerol is 1:0.2-0.4; the volume ratio of the mixed solvent to the mixed acid is 1:2; the mixed acid is prepared by mixing nitric acid and hydrochloric acid according to a volume ratio of 3:1 and then diluting twice; the volume ratio of the mixed solvent to the ultrapure water is 1:2.
Further, in the step (1), the heating reflux adopts sectional heating, specifically: firstly, refluxing for 30min at 50-60 ℃; then heating to 110 ℃ and refluxing for 90min; continuously heating for 1h; standing for 30min; the leaching time is 30min.
Further, in the step (2), the standard curve is drawn as follows: sequentially preparing standard solutions of elements to be detected in a volumetric flask, wherein the concentrations of the standard solutions are respectively 0.00 mug/L, 0.50 mug/L, 1.00 mug/L, 5.00 mug/L, 10.0 mug/L, 50.0 mug/L, 100.0 mug/L and 500.0 mug/L, and the medium is 1% nitric acid; adding an internal standard solution along with the sample before atomization; the measurement was performed by ICP-MS, and a standard curve was drawn.
The element to be measured of the present invention includes, but is not limited to Be, cr, co, ni, cu, zn, cd, sn, ba, pb.
Further, in the step (2), the internal standard is 20 mug/L of Rh and Re standard solution.
Further, in the step (3), the parameters of the ICP-MS are:
the beneficial effects of the invention are as follows:
(1) According to the invention, the dissolution of the substance to be detected can be accelerated by improving the pretreatment method of the sample, the extraction efficiency is high, and the detection accuracy is improved;
(2) The invention optimizes the detection conditions, is simple, convenient, quick and accurate, and has high recovery rate.
Drawings
Fig. 1 is a standard graph.
Detailed Description
The technical scheme of the invention is further explained and illustrated by specific examples.
Example 1
(1) Pretreatment: firstly, cutting a whole 47mm polypropylene fiber filter membrane to be digested into a digestion tank, firstly adding 5ml of absolute ethyl alcohol and glycerin, shaking uniformly, fully contacting with the filter membrane, then adding 10ml of nitric acid-hydrochloric acid mixed acid (50% of antipWANG water: nitric acid: hydrochloric acid volume ratio 3:1, mixing, diluting twice), then covering, and firstly refluxing for 30min on an electric hot plate at 50-60 ℃; then heating to 110 ℃ and refluxing for 90min, opening the cover and continuing to heat for 1 hour, cooling, leaching the inner wall of the digestion tank by using about 5mL of ultrapure water, standing for half an hour for leaching, filtering, and fixing the volume to 50.0mL for measurement.
(2) Inductively coupled plasma: instrument tuning: after igniting the plasma, after the instrument is ready, the sample tube is put into tuning liquid, whether the signal intensity and stability of Li, co, in, U are normal or not is observed, and in the standard mode, the Li signal intensity is more than 5 multiplied by 10 4 Co signal intensity is greater than 10×10 4 In signal intensity is greater than 22×10 4 The U signal intensity is more than 30 multiplied by 10 4 The method comprises the steps of carrying out a first treatment on the surface of the The device is then switched to KED mode, tuned again, co signal strength greater than 3X 10 4 A Co/ClO ratio of greater than 18. If the value is not reached, performing quality correction on the instrument, and if the difference between the quality correction result and the true value exceeds more than 0.1amu, correcting the instrument to a correct value; the specific parameters are shown in table 1.
TABLE 1
(3) Standard curve drawing
A series of standard solutions of elements to be detected are sequentially prepared in a volumetric flask, wherein the concentrations are respectively 0.00 mug/L, 0.50 mug/L, 1.00 mug/L, 5.00 mug/L, 10.0 mug/L, 50.0 mug/L, 100.0 mug/L and 500.0 mug/L, and the medium is 1% nitric acid. The internal standard is Rh and Re standard solution, and the internal standard solution is added on line with the sample in real time before atomization, so that the internal standard solution is fully mixed with the sample. The measurement was performed by ICP-MS, and a standard curve was drawn, and the standard curve is shown in FIG. 1. The concentration range of the calibration curve can be adjusted according to the measurement requirement.
(4) Sample measurement
Before each sample is measured, the device is rinsed again (30 seconds) to begin measuring the sample, and the signal is minimized (typically 30 seconds) by rinsing with a wash blank solution. Standard curve drawing and sample measurement require real-time addition of internal standard solutions.
(5) Blank test
The preparation and measurement methods of the blank film and the sample are completely the same, the used reagent amount is the same, and the blank test is carried out simultaneously when the sample is measured, and the blank is the blank of the laboratory reagent.
Comparative example 1
(1) Pretreatment: firstly, cutting a whole polypropylene fiber filter membrane with the thickness of 47mm to be digested into a digestion tank, adding 10ml of nitric acid-hydrochloric acid mixed acid (50% of antipWANG water: nitric acid: hydrochloric acid volume ratio is 3:1, mixing, diluting twice), then covering, and refluxing on an electric heating plate at 50-60 ℃ for 30min; heating to 110deg.C, refluxing for 90min, opening cover, heating for 1 hr, cooling, eluting the inner wall of digestion tank with about 5ml ultrapure water, standing for half an hour for leaching, filtering, eluting the filter membrane, and fixing volume to 50.0ml, and testing
The other steps are the same as in example 1.
Comparative example 2
(1) Pretreatment: firstly cutting a whole polypropylene fiber filter membrane of 47mm to be digested into a digestion tank, firstly adding 5mL of absolute ethyl alcohol and glycerin, shaking uniformly, fully contacting with the filter membrane, then adding 10mL of nitric acid-hydrochloric acid mixed acid (50% of antiphlogistic water: nitric acid: hydrochloric acid volume ratio is 3:1, mixing, diluting twice), then covering, heating to 110 ℃ on an electric plate, refluxing for 120min, continuously heating for 1h after covering, cooling, leaching the inner wall of the digestion tank by using about 5mL of ultrapure water, standing for half an hour, leaching, filtering, leaching the filter membrane, fixing the volume to 50.0mL, and measuring.
Effect examples
(1) And (3) marking and recycling test: preparing a marked filter membrane in a constant temperature and humidity weighing box: and (3) dropwise adding 0.25mL of standard mixed standard solution with the concentration of 0.50mL of 10mg/L on the filter membrane by using a sample injection needle, naturally airing, calculating that the theoretical standard concentration after digestion and volume fixing is respectively 50.0 mug/L and 100.0 mug/L, and manufacturing 9 filter membranes with each concentration. Respectively digesting by three digestion methods: table 2 shows the test results of the method provided in comparative example 1; table 3 shows the test results of the method provided in comparative example 2; table 4 shows the test results obtained by the method provided in example 1.
TABLE 2
TABLE 3 Table 3
TABLE 4 Table 4
Claims (6)
1. The method for detecting the heavy metal elements in the air or exhaust gas particulate matters is characterized by comprising the following steps of:
(1) Pretreatment: firstly, cutting a sampled polypropylene fiber filter membrane into a digestion tank, adding a mixed solvent of absolute ethyl alcohol and glycerol, shaking uniformly, adding mixed acid, sealing, heating and refluxing, continuously heating after uncapping, cooling, leaching the inner wall of the digestion tank by ultrapure water, leaching, filtering, leaching the filter membrane, and obtaining a solution to be measured after constant volume;
(2) Drawing a standard curve;
(3) Detection was performed using ICP-MS.
2. The method according to claim 1, wherein in the step (1), the volume ratio of the absolute ethanol to the glycerol is 1:0.2-0.4; the volume ratio of the mixed solvent to the mixed acid is 1:2; the mixed acid is prepared by mixing nitric acid and hydrochloric acid according to a volume ratio of 3:1 and then diluting twice; the volume ratio of the mixed solvent to the ultrapure water is 1:2.
3. The detection method according to claim 1 or 2, wherein in step (1), the heating reflux adopts a sectional heating, specifically: firstly, refluxing for 30min at 50-60 ℃; then heating to 110 ℃ and refluxing for 90min; continuously heating for 1h; standing for 30min; the leaching time is 30min.
4. The method according to claim 1, wherein in the step (2), the standard curve is drawn as follows: sequentially preparing standard solutions of elements to be detected in a volumetric flask, wherein the concentrations of the standard solutions are respectively 0.00 mug/L, 0.50 mug/L, 1.00 mug/L, 5.00 mug/L, 10.0 mug/L, 50.0 mug/L, 100.0 mug/L and 500.0 mug/L, and the medium is 1% nitric acid; adding an internal standard solution along with the sample before atomization; the measurement was performed by ICP-MS, and a standard curve was drawn.
5. The method according to claim 4, wherein in the step (2), the internal standard is 20. Mu.g/L of Rh, re standard solution.
6. The method according to any one of claims 1 to 5, wherein in step (3), the parameters of the ICP-MS are:
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