CN115112587A - Method for detecting mercury content in industrial flue gas and dry adsorption sampling device - Google Patents
Method for detecting mercury content in industrial flue gas and dry adsorption sampling device Download PDFInfo
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- CN115112587A CN115112587A CN202210867080.5A CN202210867080A CN115112587A CN 115112587 A CN115112587 A CN 115112587A CN 202210867080 A CN202210867080 A CN 202210867080A CN 115112587 A CN115112587 A CN 115112587A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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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
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
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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
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2247—Sampling from a flowing stream of gas
- G01N1/2258—Sampling from a flowing stream of gas in a stack or chimney
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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
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2247—Sampling from a flowing stream of gas
- G01N1/2258—Sampling from a flowing stream of gas in a stack or chimney
- G01N2001/2261—Sampling from a flowing stream of gas in a stack or chimney preventing condensation (heating lines)
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
- G01N2021/3107—Cold vapor, e.g. determination of Hg
Abstract
The invention belongs to the technical field of detection of mercury in flue gas, and particularly relates to a method for detecting mercury content in industrial flue gas and a dry adsorption sampling device. The method comprises the following steps: 1) performing dry adsorption sampling to obtain two groups of parallel adsorption tubes; 2) respectively treating KCl absorption nodes to obtain a solution to be detected, and digesting the modified activated carbon absorption nodes to obtain a digestion solution to be detected; 3) analyzing the mercury content of a solution to be detected and a digestion solution to be detected by using a mercury analyzer of a CVAAS method to obtain bivalent mercury data and zero-valent mercury data, and adding the bivalent mercury data and the zero-valent mercury data to obtain total mercury data; 4) and (4) calculating to obtain the concentration of divalent mercury in the flue gas, the concentration of zero-valent mercury in the flue gas and the concentration of total mercury in the flue gas. The method adopts dry adsorption sampling, mixed acid digestion treatment and a CVAAS method for mercury detection. The method has the advantages of small sampling volume and time, simple and easily-obtained equipment and solvent required by the digestion method, high sensitivity of the cold vapor atomic absorption spectrometry and low test cost.
Description
Technical Field
The invention belongs to the technical field of detection of mercury in flue gas, and particularly relates to a method for detecting mercury content in industrial flue gas and a dry adsorption sampling device.
Background
Mercury is a heavy metal with extremely strong biological toxicity, is a well-known environmental pollutant, exists in the atmosphere, soil, water and rock stratum, circulates in an ecosystem and causes great harm to human beings and the ecological environment. The main sources of mercury emission in the atmosphere are artificial emission and natural generation, and the artificial sources are fossil energy combustion, metal smelting, garbage incineration and the like. The mercury pollutant generated by coal combustion occupies about 34% of the mercury content discharged to the atmosphere every year in China, and the emission limit value of mercury and compounds thereof is increased to 30 mu g/m in the 'emission standard of atmospheric pollutants for thermal power plants' issued by China in 2012, which is at the beginning of all industries 3 . In order to better control the emission of mercury in coal-fired flue gas, a proper method is needed to sample the flue gas and accurately detect the total mercury content in each link so as to determine proper treatment measures.
Mercury in flue gas exists in three main forms: zero-valent mercury, divalent mercury, and granular mercury. At temperatures above 800 ℃ in the coal combustion process, almost all mercury is converted to Hg 0 Is present in the flue gas, while a very small part of the mercury remains in the slag in the form of slag. The mercury generated by combustion passes through various subsequent heat exchange devices, the temperature of the flue gas is gradually reduced, the mercury in the flue gas is continuously changed, and part of the Hg 0 Through physical adsorption, chemical adsorption and chemical reaction, the mercury is absorbed by the surfaces of carbon particles or other fly ash particles in the flue gas to form granular mercury (Hg) P ) (ii) a A portion of Hg 0 When the temperature of the flue gas is reduced to a certain range, the flue gas and other components in the flue gas are subjected to homogeneous reaction to form oxidized mercury (Hg) 2+ ) Compounds, HCl, O in coal-fired flue gas 2 And NO 2 Etc. favour the conversion of mercury into Hg 2+ 。
The mercury with different chemical forms has different physical, chemical and biological properties, and in order to achieve the purpose of effective treatment, the forms of various substances of mercury in the flue gas need to be measured respectively so as to clarify the distribution rule. At present, the test methods for mercury in coal-fired flue gas can be classified into two major types, namely a manual analysis Method and an online analysis Method (such as EPA Method 30A), and the manual analysis Method can be divided into a wet chemical Method and a dry adsorbent adsorption Method: such as EPA Method 29/101A, Tris Buffer Method, Iodine Based Method, Ontario Hydro Method (Anuna abbreviation Method) of wet Method, rapid SEM Method of dry Method, EPA Method 30B, etc.
The on-line analytical Method EPA Method 30A comprises a flue gas sampling system, a flue gas heating and transmission system, a mercury form conversion system and a mercury detection and calibration system, wherein the flue gas is divided into two paths to respectively measure the content of element mercury and total mercury, the one-time investment is high, regular maintenance is required, and the flue gas and the Method test data of the OHM or 30B are subjected to a relative accuracy test; in the OHM method, flue gas is extracted by a smoke gun and then filtered to remove ash, granular mercury is intercepted on a filter membrane, and then divalent mercury, namely 1H, is absorbed by 3 KCl solution absorption bottles in sequence 2 O 2 SO removal by filter flask 2 And part of zero-valent mercury, 3K 2 MnO 4 The solution absorption bottle completely absorbs the zero-valent mercury, finally, the smoke is dehydrated and exhausted through the absorbent glue, and the Hg content of each part of washing and collecting liquid is analyzed.
The 30B dry method test adopts a solid sampling medium to capture gaseous mercury in the flue gas, and then the solid adsorbent is subjected to related chemical operation to analyze to obtain the mercury component in the flue gas, and the solid dry adsorbent in the 30B method has the advantages of good stability, strong operability and the like, and meanwhile, the measurement precision is equivalent to that of a wet method, and the problem of transportation of dangerous chemicals is avoided. However, the existing sampling instrument generally has the problems that the sampling field operation is complex, the phenomenon of blocking of water vapor in flue gas in the adsorbent occurs, the acquisition efficiency is low, the precision is low, the deviation is large, and the glass adsorption tube is easy to crash, so that the sampling fails and the like.
At present, the subsequent treatment method of the solid adsorbent in the dry test mostly adopts a combustion sublimation method, aqua regia microwave digestion, a direct mercury analyzer and other test methods. The combustion sublimation method is to put the activated carbon sample in a heating quartz tube, heat and volatilize the activated carbon sample by a gas lamp, enrich the mercury in the potassium permanganate-sulfuric acid absorption liquid, and determine the mercury by a colorimetric method or a titration method. The microwave digestion method is that solid sample is put into a digestion tank, then acid decomposition liquid with proper proportion is added, and then the solid sample is put into a microwave digestion instrument for digestion.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for detecting the mercury content in industrial flue gas and a dry adsorption sampling device.
The technical scheme provided by the invention is as follows:
a dry sorption sampling device, comprising:
the sampling gun is provided with two adsorption tubes in the gun mouth;
the condensing device is communicated with the gas outlet of the sampling gun through a flue gas pipeline;
and the console is provided with a heat tracing cable for tracing the sampling gun and each adsorption tube, and is also communicated with the condensing device through a pipeline.
In the above technical scheme:
the two adsorption tubes are arranged to facilitate parallel comparison, so that the error of experimental data is reduced;
the heat tracing cable is subjected to heating control by the console, and heat tracing is carried out on the adsorption pipe and the sampling gun;
the sampling gun is connected with a condensing device, and the flue gas is condensed and then enters a console to test data such as flow, vacuum degree and the like.
In the existing method, because the environmental temperature is low in the sampling process, water vapor is condensed on an adsorbent in an adsorption tube, so that the accuracy of rear detection data is influenced.
Specifically, each of the adsorption tubes comprises quartzA tube having Na sequentially disposed therein 2 CO 3 Acid absorption section, KCl puncture section, modified activated carbon absorption section and modified activated carbon puncture section, wherein quartz cotton sections are arranged at two ends of each section.
In the above technical scheme:
the adsorption tube is made of quartz, so that the strength of the adsorption tube is enhanced, and the possibility of sampling failure caused by crushing is reduced; the adsorbent filling length and filling amount in the adsorption tube are larger;
the adsorption tube is filled with sodium carbonate, potassium chloride and halogen modified activated carbon, and after acid is adsorbed, bivalent mercury and zero-valent mercury in the flue gas can be respectively adsorbed by the potassium chloride and the halogen modified activated carbon. The sampling method is simple to operate, the form of mercury in gas can be detected while the basis of measurement accuracy is ensured, and the adsorption tube after sampling is convenient to store and transport.
Specifically, the modified activated carbon is activated carbon modified by halogen compounds.
In the technical scheme, the halogen compound modification can increase the mercury adsorption capacity.
Specifically, the activated carbon is modified by an impregnation method by using a modifier, wherein the modifier comprises but is not limited to HCl, HBr, KI, NaBr and I 2 、CaBr 2 Any one or more of them.
The invention also provides a method for detecting the mercury content in the industrial flue gas, which comprises the following steps:
1) by adopting the dry adsorption sampling device provided by the invention, two groups of parallel adsorption tubes are obtained;
2) respectively processing KCl breakdown sections in the adsorption tubes and digesting the modified activated carbon breakdown sections, then detecting, and under the condition that no mercury is detected in the two breakdown sections, respectively processing the KCl absorption sections to obtain a solution to be detected, and digesting the modified activated carbon absorption sections to obtain a digestion solution to be detected;
3) analyzing the mercury content of the solution to be detected and the digestion solution to be detected obtained in the step 2) by using a mercury analyzer of a CVAAS method to respectively obtain bivalent mercury data and zero-valent mercury data, and adding the bivalent mercury data and the zero-valent mercury data to obtain total mercury data;
4) and (2) calculating the corresponding divalent mercury concentration in the flue gas, the zero-valent mercury concentration in the flue gas and the total mercury concentration in the flue gas by using the divalent mercury data, the zero-valent mercury data and the total mercury data obtained in the step 3) and combining the flue gas sampling volume recorded by the control console in the step 1).
In the technical scheme, dry adsorption sampling, mixed acid digestion treatment and mercury detection by a CVAAS method are adopted. The method has the advantages of simple operation, small sampling volume and time, convenient transportation of sampling equipment, simple and easily-obtained equipment solvent required by the digestion method, high sensitivity of Cold Vapor Atomic Absorption Spectrometry (CVAAS) and low test cost.
Specifically, in the step 2): and under the condition that mercury is detected in any one of the KCl breakdown section or the modified activated carbon breakdown section, reducing the sampling time and/or reducing the sampling flow rate to reduce the collected mercury amount until no mercury is detected in the two breakdown sections.
Specifically, in the step 2): and treating the KCl absorption section or the KCl puncture section by using 1mol/L HCl solution, wherein the mass ratio of the volume of HCl to KCl is about 20mL:1 g.
Specifically, in the step 2), the digestion specifically comprises the following steps: adding the mixed acid into a conical flask filled with modified activated carbon in a fume hood, heating the conical flask by using a heating plate, heating the conical flask to 55-65 ℃ for 2 hours, cooling the conical flask to room temperature, slowly adding a BrCl solution with equivalent concentration of 0.01 and volume ratio of 5%, wherein the mixed acid is mixed acid of nitric acid and sulfuric acid with concentration ratio of 7:3, and the ratio of the mixed acid to the activated carbon is (30-40) mL:1 g.
In the technical scheme, a large amount of harmful and irritant gases are generated in the whole digestion process and the BrCl treatment process, and the whole experimental treatment process is carried out in a fume hood.
Specifically, in the step 1), the heat tracing temperature of the adsorption tube and the sampling gun is higher than 100 ℃.
In the technical scheme, the temperature of the heat tracing cable can be controlled by the console, the heat tracing temperature of the adsorption tube and the sampling gun is higher than 100 ℃, and the condensation phenomenon of water vapor at the adsorption tube can be reduced.
Specifically, the specific steps of step 3) are as follows: respectively preparing hydroxylamine hydrochloride solution with mass volume concentration of 0.1g/mL and SnCl 2 The method comprises the steps of carrying out calibration curve on an instrument, starting detection operation, diluting the solution to be detected or the digestion solution to be detected to the appropriate detection concentration, putting 10ml of the diluted solution into a reaction bottle of an analyzer, dropping a few drops of prepared hydroxylamine hydrochloride solution into the reaction bottle, reducing redundant oxidant in the solution, finally adding 0.5ml of prepared stannous chloride solution, installing and fixing the reaction bottle on a reaction unit, starting testing the concentration of mercury by using a photometer unit after a safety buckle is fastened, wherein the solution to be detected corresponds to bivalent mercury data, the digestion solution to be detected corresponds to zero-valent mercury data, automatically sending a prompt tone by the instrument after the measurement is finished, and displaying an analysis result on a connected computer terminal.
Based on above-mentioned technical scheme, after the sample operation, under clean experimental environment, cut the adsorption tube, avoid dust pollution, take out four sections adsorbents after the absorption and put into the clean container that the size is suitable. Treating KCl adsorption nodes by using a hydrochloric acid solution, heating and digesting the modified activated carbon by using a mixed acid of nitric acid and sulfuric acid, reducing redundant oxidizing agent by using a hydroxylamine hydrochloride solution, and finally adding SnCl 2 The solution reduced the mercury to elemental form and was detected using a mercury analyzer. The digestion detection method simplifies the traditional microwave digestion and sublimation digestion methods, has simple and common experimental reagents and equipment, and is suitable for operation under simple laboratory conditions.
For the testing process of the mercury analyzer, a mercury standard solution is used for calibration before the testing is started, sample detection is carried out after a calibration curve is obtained, the concentration of the mercury standard solution is selected according to the measuring range of a specific instrument, and the mercury standard solution needs to be prepared on the testing day.
The hydroxylamine hydrochloride solution and SnCl 2 The mass volume concentration of the solution is 0.1g/mL, and the hydroxylamine hydrochloride solution is used for reducing redundant oxidant, SnCl 2 The solution is used for converting valence state in the solutionThe mercury is reduced to elemental form.
The invention has the beneficial effects that: the total mercury detection method has the advantages of simple sampling system equipment, easy operation, low cost, small equipment volume and convenient transportation and packaging. And the quartz adsorption tube is not easy to break, so that the sampling failure rate is reduced. The smoke gun and the adsorbent are subjected to heat tracing, so that the condensation of water vapor in the adsorption pipe is reduced, and the data detection accuracy is improved; the KCl section after adsorption is treated by the hydrochloric acid solution, the modified activated carbon is digested by a heating method of mixing nitric acid and sulfuric acid with strong acid, the operation is simple, the consumed time is short, the digestion solution and equipment are simple and easy to obtain, the operation cost is reduced, and the method is suitable for operation under simple laboratory conditions; the method for detecting mercury by adopting the CVAAS method has the advantages of low equipment cost, high sensitivity, accurate test data and low error.
Drawings
Fig. 1 is a schematic structural diagram of a dry adsorption sampling device provided by the invention.
Fig. 2 is a schematic structural diagram of an adsorption tube of the dry adsorption sampling device provided by the invention.
Fig. 3 is a schematic flow chart of the method for detecting mercury content in industrial flue gas provided by the invention.
In fig. 1, 2 and 3, the structures represented by the reference numerals are listed as follows:
1. the device comprises an adsorption tube, 2, a sampling gun, 3, a condensing device, 4, a console, 5, a heat tracing cable, 6, a flue gas pipeline, 7, a fume hood, 8, a heating plate, 9, a conical flask, 10, a reaction unit, 11, a reaction bottle, 12, a photometer unit, 13, a computer end, 21, a quartz cotton section, 22, a modified activated carbon breakdown section, 23, a modified activated carbon absorption section, 24, a KCl breakdown section, 25, a KCl absorption section, 26, Na 2 CO 3 Acid absorption joint, 27 and quartz tube.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
In one embodiment, as shown in fig. 1, a dry adsorption sampling device includes: the sampling gun 2 is provided with two adsorption tubes 1 in the gun mouth; the condensing device 3 is communicated with the gas outlet of the sampling gun 2 through a flue gas pipeline 6; and a console 4 provided with a heat tracing cable 5 for tracing the sampling gun 2 and each adsorption tube 1, and further communicated with the condensing unit 3 through a pipeline.
In one embodiment, as shown in FIG. 2, the adsorption tube 1 comprises a quartz tube 27 in which Na is sequentially disposed 2 CO 3 Acid absorption section 26, KCl absorption section 25, KCl puncture section 24, modified activated carbon absorption section 23 and modified activated carbon puncture section 22, wherein quartz cotton sections 21 are arranged at two ends of each section.
In one embodiment, as shown in fig. 3, the method for detecting the mercury content in the industrial flue gas comprises the following steps:
firstly, a dry adsorption sampling device is adopted to obtain two groups of adsorption tubes in parallel, and the heat tracing temperature in the adsorption process is higher than 100 ℃.
Next, under the clean test conditions, each adsorption tube 1 was treated with a cutter. Under the condition that no mercury is detected in the KCl breakdown section 24 and the modified activated carbon breakdown section 22, treating the KCl adsorption section by using 1mol/L HCl solution, wherein the mass ratio of the volume of HCl to the mass of the KCl adsorption section is about 20mL:1g, to obtain a treated solution to be detected. Then, digesting the adsorbed modified activated carbon by using a mixed acid with a concentration ratio of nitric acid to sulfuric acid of 7:3 in a fume hood 7, wherein the ratio of the mixed acid to the activated carbon is about 30-40 mL:1g, adding the mixed acid into a conical flask filled with the modified activated carbon, heating the mixture by using a heating plate 8, heating the mixture to about 55-65 ℃ and continuously heating the mixture for 2 hours, cooling the mixture to room temperature, and slowly adding a BrCl solution with the equivalent concentration of 0.01 and the volume ratio of the BrCl solution to be detected being 5% to obtain the digestion solution to be detected.
Then, the solution to be detected and the digestion solution to be detected were separately tested using a mercury analyzer of CVAAS method. Respectively preparing hydroxylamine hydrochloride solution with mass volume concentration of 0.1g/mL and SnCl 2 Solutions, and standard solutions of mercury of different suitable concentrations. After the instrument is calibrated, the detection operation is started, the digestion solution is diluted to proper detection concentration, 10ml of the diluted solution is put into a reaction bottle 11 of an analyzer, and the diluted solution is dripped into the reaction bottleAdding a few drops of prepared hydroxylamine hydrochloride solution into a reaction bottle, reducing redundant oxidant in the solution, finally adding 0.5ml of prepared stannous chloride solution, installing and fixing the reaction bottle on a reaction unit 10, starting to test the concentration of mercury by using a photometer unit 12 after a safety buckle is buckled, automatically giving out prompt sound by an instrument after the measurement is finished, and presenting an analysis result on a connected computer end 13.
And finally, calculating the corresponding concentration of divalent mercury in the flue gas, the concentration of zero-valent mercury in the flue gas and the concentration of total mercury in the flue gas by a conventional technical scheme based on the divalent mercury data, the zero-valent mercury data and the total mercury data and by combining the flue gas sampling volume recorded by the console.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A dry adsorption sampling device, comprising:
a sampling gun (2), two adsorption tubes (1) are arranged in the muzzle of the sampling gun;
the condensing device (3) is communicated with the gas outlet of the sampling gun (2) through a flue gas pipeline (6);
and the console (4) is provided with a heat tracing cable (5) for tracing the sampling gun (2) and each adsorption tube (1), and is also communicated with the condensing device (3) through a pipeline.
2. The dry adsorption sampling device of claim 1, wherein: each adsorption tube (1) comprises a quartz tube (27) in which Na is sequentially arranged 2 CO 3 Acid absorption joint (26), KCl absorption joint (25), KCl puncture joint (24), modified activated carbon absorption joint (23) and modified activated carbon puncture joint (22), wherein quartz cotton small joints (21) are arranged at two ends of each joint.
3. The dry adsorption sampling device of claim 1, wherein: the modified activated carbon is activated carbon modified by halogen compounds.
4. The dry adsorption sampling device of claim 3, wherein: the activated carbon is modified by an impregnation method by using a modifier, wherein the modifier comprises HCl, HBr, KI, NaBr and I 2 、CaBr 2 Any one or more of them.
5. The method for detecting the mercury content in the industrial flue gas is characterized by comprising the following steps:
1) using the dry adsorption sampling device according to any one of claims 1 to 4, two sets of parallel adsorption tubes (1) are obtained;
2) respectively processing KCl breakdown sections in the adsorption tubes (1) and digesting the modified activated carbon breakdown sections, then detecting, and respectively processing KCl absorption sections under the condition that no mercury is detected in the two breakdown sections to obtain a solution to be detected, and digesting the modified activated carbon absorption sections to obtain a digestion solution to be detected;
3) analyzing the mercury content of the solution to be detected and the digestion solution to be detected obtained in the step 2) by using a mercury analyzer of a CVAAS method to respectively obtain bivalent mercury data and zero-valent mercury data, and adding the bivalent mercury data and the zero-valent mercury data to obtain total mercury data;
4) and (3) calculating the corresponding divalent mercury concentration in the flue gas, the zero-valent mercury concentration in the flue gas and the total mercury concentration in the flue gas by using the divalent mercury data, the zero-valent mercury data and the total mercury data obtained in the step 3) and combining the flue gas sampling volume recorded by the console (4) in the step 1).
6. The method for detecting the mercury content in the industrial flue gas according to claim 5, wherein in the step 2): and under the condition that mercury is detected in any one of the KCl breakdown section or the modified activated carbon breakdown section, reducing the sampling time and/or reducing the sampling flow rate to reduce the collected mercury amount until no mercury is detected in the two breakdown sections.
7. The method for detecting the mercury content in the industrial flue gas according to claim 5, wherein in the step 2): and treating the KCl absorption section or the KCl puncture section by using 1mol/L HCl solution, wherein the mass ratio of the volume of HCl to KCl is about 20mL:1 g.
8. The method for detecting the mercury content in the industrial flue gas according to claim 5, wherein in the step 2), the digestion specifically comprises the following steps: adding the mixed acid into a conical flask (9) filled with modified activated carbon in a fume hood (7), heating by using a heating plate (8), heating to 55-65 ℃, continuously heating for 2h, cooling to room temperature, slowly adding a BrCl solution with equivalent concentration of 0.01 and with volume ratio of 5%, wherein the mixed acid is mixed acid with nitric acid and sulfuric acid in a concentration ratio of 7:3, and the ratio of the mixed acid to the activated carbon is (30-40) mL:1 g.
9. The method for detecting the mercury content in the industrial flue gas according to the claim 5, wherein in the step 1), the heat tracing temperature of the adsorption tube (1) and the sampling gun (2) is higher than 100 ℃.
10. The method for detecting the mercury content in the industrial flue gas according to claim 5, wherein the specific steps in the step 3) are as follows: respectively preparing hydroxylamine hydrochloride solution with mass volume concentration of 0.1g/mL and SnCl 2 The method comprises the steps of carrying out calibration curve on an instrument, starting detection operation, diluting the solution to be detected or the digestion solution to be detected to the appropriate detection concentration, putting 10ml of the diluted solution into a reaction bottle (11) of an analyzer, dropping a few drops of prepared hydroxylamine hydrochloride solution into the reaction bottle, reducing redundant oxidant in the solution, finally adding 0.5ml of prepared stannous chloride solution, installing and fixing the reaction bottle on a reaction unit (10), starting measurement on the concentration of mercury by using a photometer unit (12) after a safety buckle is made, enabling the solution to be detected to correspond to bivalent mercury data and the digestion solution to be detected to correspond to zero-valent mercury data, automatically sending prompt tone by the instrument after the measurement is finished, and displaying an analysis result on a connected computer end (13).
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