CN105548507A - Device and method for measuring sulfate in atmospheric particulates - Google Patents

Device and method for measuring sulfate in atmospheric particulates Download PDF

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Publication number
CN105548507A
CN105548507A CN201610101479.7A CN201610101479A CN105548507A CN 105548507 A CN105548507 A CN 105548507A CN 201610101479 A CN201610101479 A CN 201610101479A CN 105548507 A CN105548507 A CN 105548507A
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China
Prior art keywords
sulfate
port
particle
determinator
concentration
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CN201610101479.7A
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Chinese (zh)
Inventor
杨建虎
王良
孙程
马铁成
周涛
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河北先河环保科技股份有限公司
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Priority to CN201610101479.7A priority Critical patent/CN105548507A/en
Publication of CN105548507A publication Critical patent/CN105548507A/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/6428Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N2033/0003Composite materials

Abstract

The invention belongs to the technical field of environment monitoring and particularly relates to a device and method for measuring sulfate in atmospheric particulates. The device comprises a main pipeline, a particulate cutter arranged on the main pipeline, a measuring system and a stabilizing system, wherein the measuring system and the stabilizing system are connected in parallel through a tee joint. The measuring system comprises two branch pipes, a sulfate conversion furnace, a third particle filter, a flow sensor and an SO2 detector, the two branch pipes are sequentially connected in parallel, the sulfate conversion furnace, the third particle filter, the flow sensor and the SO2 detector are sequentially connected with outlets of the branch pipes, the two ends of the two parallel-connected branch pipes are provided with a first three-way electromagnetic valve and a second three-way electromagnetic valve respectively, and the two branch pipes are provided with a second particle filter and a ventilation pipe respectively. The stabilizing system comprises a flow meter and a vacuum pump which are sequentially arranged. The measuring system further comprises a control unit. Measuring equipment used in the device is low in cost, the technical requirements for the operation environment and operators are low, and application and popularization are facilitated.

Description

The determinator of sulfate and assay method thereof in Atmospheric particulates
Technical field
The invention belongs to environmental monitoring technology field, be specifically related to determinator and the assay method thereof of sulfate in Atmospheric particulates.
Background technology
Air is one of mankind's material base of depending on for existence, and air pollution not only produces baneful influence to atmospheric visibility and physical environment, and threatens health, and the situation of China's air pollution is in recent years abnormal severe, fine particle (PM 2.5) become the primary pollutant in many cities, the composition of fine particle is more complicated, containing many kinds of substances such as heavy metal, inorganic carbon, organic carbon, sulfate, nitrate and ammonium salts, wherein sulfate, nitrate and the ammonium salt mass ratio in fine particle reaches more than 25-30%, when fine particle concentration is higher than 70 μ g/m 3time, three's proportion sum is greater than 70%, is the principal element that particle concentration raises.Sulfate in fine particle is formed by atmosphere chemically react to a great extent, SO 2can with the NH in air 3reaction, generating ammonium sulfate or ammonium hydrogen sulfate, can also there is decomposition and regenerate SO in the two 2and NH 3.In monitoring fine particle, the content of sulfate is originated for parsing fine particle and is understood its formation mechanism and has very important significance.
The main mensuration adopting chromatograph to carry out composition in Atmospheric particulates in prior art, this equipment not only cost is higher, and higher to the technical requirement of operating environment and operating personnel, is unfavorable in these field promotion and implementation.
Summary of the invention
In order to overcome the defect that above-mentioned prior art exists, the invention provides determinator and the assay method of sulfate in a kind of Atmospheric particulates, this sensing equipment cost is low, operating environment and low to the technical requirement of operating personnel, easy to use and promote.
The present invention can be achieved through the following technical solutions: the determinator of sulfate in a kind of Atmospheric particulates, key is: comprise main line and be arranged on cutter for particles on main line, threeway, the Analytical system be arranged in parallel by threeway and systems stabilisation
Described Analytical system comprises the two articles of branch roads be arranged in parallel successively, the sulfate conversion stove, the 3rd particle filter, flow sensor and the SO that are connected successively with way outlet 2detecting device, two branch road two ends in parallel are respectively arranged with the first three-way valve and the second three-way valve, and wherein a branch road is provided with the second particle filter, and another branch road is provided with ventilation duct;
Described systems stabilisation comprises the flowmeter and vacuum pump that set gradually;
Analytical system also comprises control module, flowmeter, vacuum pump, the first three-way valve, the second three-way valve, flow sensor and SO 2detecting device is connected with control module respectively.
Be provided with interference gas filtering device between described cutter for particles and threeway, systems stabilisation branch road is provided with the first particle filter.
Described cutter for particles is aerodynamic particle thing cutter, for cutting PM 1to PM 10between particle, interference gas filtering device is annular denuder.
Described annular denuder adopts the Na of 2%-4% 2cO 3solution carries out coating process.
The first described three-way valve and the second three-way valve are solenoid valve.
Described SO 2detecting device is ultraviolet fluorescence method SO 2detecting device.
The structure of described sulfate conversion stove comprises the reburner heat-preservation cotton of bridge-type structure, resistance wire, spiral helicine boiler tube and thermopair, two reburner heat-preservation cotton are symmetrical arranged the hollow cylinder structure of composition square-outside and round-inside, resistance wire genesis analysis is in the endosexine of reburner heat-preservation cotton, boiler tube is arranged on the hollow region of reburner heat-preservation cotton, be provided with catalyzer in boiler tube, thermopair is arranged on the center of boiler tube.
Described catalyzer is stainless steel, and catalytic temperature is 900-1000 DEG C.
Use the assay method of the determinator of sulfate in a kind of Atmospheric particulates, concrete steps are as follows:
The preparation of a, air sample
Air to be measured, after cutter for particles process, obtains air sample;
The concentration of b, detection gaseous sulphide and Sulfate
The a1 port of the first three-way valve, c1 port open, b1 port shutdown, the a2 port of the second three-way valve, c2 port open, b2 port shutdown, passes through SO 2air sample extracts by detecting device, and the air sample containing fine particle enters sulfate conversion stove by way of ventilation duct, remaining particle in the 3rd particle filter filtering air sample, flow sensor record air mass flow Q 1, finally enter SO 2detecting device, records the concentration of gaseous sulphide and Sulfate;
The concentration of c, detection gaseous sulphide
The a1 port of the first three-way valve, b1 port open, c1 port shutdown, the a2 port of the second three-way valve, b2 port open, c2 port shutdown, passes through SO 2air sample extracts by detecting device, air sample containing fine particle is by way of the second particle filter, after particle is removed and then by sulfate conversion stove, remaining particle in the 3rd particle filter filtering air sample, flow sensor record air mass flow Q 2, finally enter SO 2detecting device, records the concentration of gaseous sulphide;
The concentration of d, count particles state sulfate
The concentration of the gaseous sulphide in step b and Sulfate is deducted the concentration of gaseous sulphide in step c, finally obtain the concentration of the Sulfate in air to be measured.
In step a, air to be measured first passes into interference gas filtering device after cutter for particles process, obtains air sample by after interference gas filtering.
Beneficial effect of the present invention:
In this determinator, each ingredient syndeton is simple, cost is lower, during operation also more for convenience, higher technical requirement is not had to operating personnel, and this device is low to the requirement of environment in use, can uses in any occasion, greatly facilitate the mensuration of Atmospheric particulates sulfate concentration, carried out the control of cycling by control module, thus calculate air particle sulfate concentration comparatively accurately by multi-group data.In addition, compared with the Ion Chromatographic Method of routine, the present invention can not only monitor water miscible Sulfate, can also monitor water insoluble component;
The aerodynamic particle thing cutter that cutter for particles is selected can carry out PM 1to PM 10particle cutting, filtered out the air of the particle containing PM2.5 by the cutting head choosing PM2.5;
Interference gas filtering device is annular denuder, preferably adopts the Na of 2% 2cO 3solution carries out coating process, and effective filtering interfering gas, mainly comprises SO 2and H 2s;
Sulfate conversion stove is used for gaseous sulphide in air sample and Sulfate to be converted into SO 2, catalyzer used during conversion is stainless steel, and catalytic temperature is 900-1000 DEG C;
Systems stabilisation is for ensureing that total sampling flow of whole determinator meets the design discharge requirement of cutting head in aerodynamic particle thing cutter, the real time measurement deducting flow sensor by the design discharge of cutter for particles obtains a calculated flow rate value, and this calculated flow rate value is set to flowmeter;
In this device, the state being controlled the first three-way valve and the second three-way valve by control module is switched, a valve state is switched at interval of 20 minutes, carry out the operation of step b, step c respectively, after a cycle period terminates, just can obtain one group of concentration data and be used for the calculating of the Sulfate concentration of carrying out in Step d, employing multi-group data calculates, degree of accuracy is higher, and the Sulfate concentration values obtained is more accurate, effectively can reduce the error of testing result.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is the profile figure of sulfate conversion stove in Fig. 1.
Fig. 3 is the cross-sectional view of sulfate conversion stove in Fig. 1.
In accompanying drawing, 1 is cutter for particles, and 2 is interference gas filtering devices, 3 is threeways, and 4 is first particle filters, and 5 is flowmeters, 6 is vacuum pumps, 7 is first three-way valves, and 8 is second particle filters, and 9 is second three-way valves, 10 is sulfate conversion stoves, 11 is the 3rd particle filters, and 12 is flow sensors, and 13 is SO 2detecting device, 14 is control modules, and 15 is reburner heat-preservation cotton, and 16 is resistance wires, and 17 is boiler tubes, and 18 is thermopairs.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described.
Specific embodiment, as shown in Figure 1, the determinator of sulfate in a kind of Atmospheric particulates, comprises main line and is arranged on the cutter for particles 1 on main line, and cutter for particles 1 is aerodynamic particle thing cutter, can carry out PM 1to PM 10particle cutting, main line is connected with interference gas filtering device 2 in cutter for particles 1 rear end, and interference gas filtering device 2 be annular denuder, preferably employing 2%-4% or Na 2cO 3carry out coating process, be connected with threeway 3 in interference gas filtering device 2 rear end, threeway 3 is connected with main line, Analytical system, systems stabilisation respectively.
Sulfate conversion stove 10, the 3rd particle filter 11, flow sensor 12 and SO that Analytical system is provided with two articles of branch roads in parallel successively, is connected with two articles way outlets 2detecting device 13, two branch road two ends in parallel are connected with respectively and comprise a1 port, b1 port, first three-way solenoid valve 7 of c1 port and comprise a2 port, b2 port, second three-way solenoid valve 9 of c2 port, a1 port exports with one of threeway on main line 3 and is connected, a2 port is connected with the entrance of sulfate conversion stove 10, article two, the entrance of branch road respectively with b1 port, c1 port connects, outlet respectively with b2 port, c2 port connects, wherein, the second particle filter 8 is provided with between b1 port and b2 port, ventilation duct is provided with between c1 port and c2 port.
Another of systems stabilisation and threeway on main line 3 exports and is connected, and is disposed with the first particle filter 4, flowmeter 5 and vacuum pump 6.
Control module 14 is also provided with, flowmeter 5, vacuum pump 6, first three-way solenoid valve 7, second three-way solenoid valve 9, flow sensor 12 and SO in determinator 2detecting device 13 is connected with control module 14 respectively.
Above three-way valve is preferably three-way solenoid valve, SO 2detecting device 13 is ultraviolet fluorescence method SO 2detecting device.
As shown in Figures 2 and 3, sulfate conversion stove 10 comprises reburner heat-preservation cotton 15, resistance wire 16, boiler tube 17 and thermopair 18, reburner heat-preservation cotton 15 is bridge-type structure, two reburner heat-preservation cotton 15 symmetries connect to form the hollow cylinder structure of square-outside and round-inside, resistance wire 16 genesis analysis is in the endosexine of reburner heat-preservation cotton 15, boiler tube 17 is helical structure and is arranged on the hollow region of reburner heat-preservation cotton 15, is provided with catalyzer in boiler tube 17, and thermopair 18 inserts the center of boiler tube 17.
Use this determinator to carry out the assay method of sulfate in Atmospheric particulates, step is as follows:
The preparation of a, air sample
Cutter for particles 1 is aerodynamic particle thing cutter, chooses PM 2.5cutting head, air to be measured filters out PM after treatment 2.5particle, then interference gas (is mainly comprised SO by interference gas filtering device 2 2and H 2s) filtering, obtains air sample;
The concentration of b, detection gaseous sulphide and Sulfate
The a1 port of the first three-way solenoid valve 7, c1 port open, b1 port shutdown, the a2 port of the second three-way solenoid valve 9, c2 port open, b2 port shutdown, passes through SO 2air sample extracts by detecting device 13, containing PM 2.5the air sample of particle directly enters sulfate conversion stove 10 by way of ventilation duct, and gaseous sulphide and Sulfate are converted into SO by sulfate conversion stove 10 2, remaining particle in the 3rd particle filter 11 filtering air sample, flow sensor 12 records air mass flow Q 1, finally enter SO 2detecting device 13, records the concentration of gaseous sulphide and Sulfate;
The concentration of c, detection gaseous sulphide
The a1 port of the first three-way solenoid valve 7, b1 port open, c1 port shutdown, the a2 port of the second three-way solenoid valve 9, b2 port open, c2 port shutdown, passes through SO 2air sample extracts by detecting device 13, containing PM 2.5particle in air sample, by way of the second particle filter 8, all filters out by the air sample of particle, and then by sulfate conversion stove 10, gaseous sulphide is converted into SO by sulfate conversion stove 10 2, remaining particle in the 3rd particle filter 11 filtering air sample, flow sensor 12 records air mass flow Q 2, finally enter SO 2detecting device 13, records the concentration of gaseous sulphide;
The concentration of d, count particles state sulfate
The concentration of the gaseous sulphide in step b and Sulfate is deducted the concentration of gaseous sulphide in step c, finally obtain the concentration of the Sulfate in air to be measured.
In step b and step c, sulfate conversion stove 10 is for being converted into SO by gaseous sulphide in air sample and Sulfate 2, catalyzer used during conversion is stainless steel, and catalytic temperature is 950 DEG C, and wherein gaseous sulphide comprises sulphuric dioxide SO 2, sulfuretted hydrogen H 2s, mercaptan and thioether etc., Sulfate comprises ammonium sulfate (NH 4) 2sO 4, ammonium hydrogen sulfate NH 4hSO 4, sodium sulphate Na 2sO 4, potassium sulfate K 2sO 4, magnesium sulfate MgSO 4, calcium sulphate CaSO 4; SO 2ultraviolet fluorescence method SO selected by detecting device 13 2detecting device.
In this device, the state switching of the first three-way solenoid valve 7 and the second three-way solenoid valve 9 can also be controlled by control module 14, a valve state is switched at interval of 20 minutes, carry out the operation of step b, step c respectively, after a cycle period terminates, just can obtain one group of concentration data and be used for the calculating of the Sulfate concentration of carrying out in Step d, effectively can reduce the error of testing result.

Claims (10)

1. the determinator of sulfate in Atmospheric particulates, it is characterized in that: comprise main line and be arranged on cutter for particles (1) on main line, threeway (3) and the Analytical system be arranged in parallel by threeway (3) and systems stabilisation
Described Analytical system comprises the two articles of branch roads be arranged in parallel successively, the sulfate conversion stove (10), the 3rd particle filter (11), flow sensor (12) and the SO that are connected successively with way outlet 2detecting device (13), two branch road two ends in parallel are respectively arranged with the first three-way valve (7) and the second three-way valve (9), wherein a branch road is provided with the second particle filter (8), and another branch road is provided with ventilation duct;
Described systems stabilisation comprises the flowmeter (5) and vacuum pump (6) that set gradually;
Analytical system also comprises control module (14), flowmeter (5), vacuum pump (6), the first three-way valve (7), the second three-way valve (9), flow sensor (12) and SO 2detecting device (13) is connected with control module (14) respectively.
2. the determinator of sulfate in a kind of Atmospheric particulates according to claim 1, it is characterized in that: between described cutter for particles (1) and threeway (3), be provided with interference gas filtering device (2), systems stabilisation branch road is provided with the first particle filter (4).
3. the determinator of sulfate in a kind of Atmospheric particulates according to claim 2, is characterized in that: described cutter for particles (1) is aerodynamic particle thing cutter, for cutting PM 1to PM 10between particle, interference gas filtering device (2) is annular denuder.
4. the determinator of sulfate in a kind of Atmospheric particulates according to claim 3, is characterized in that: described annular denuder adopts the Na of 2%-4% 2cO 3solution carries out coating process.
5. the determinator of sulfate in a kind of Atmospheric particulates according to claim 1, is characterized in that: described the first three-way valve (7) and the second three-way valve (9) are solenoid valve.
6. the determinator of sulfate in a kind of Atmospheric particulates according to claim 1, is characterized in that: described SO 2detecting device (13) is ultraviolet fluorescence method SO 2detecting device.
7. the determinator of sulfate in a kind of Atmospheric particulates according to claim 1, it is characterized in that: the structure of described sulfate conversion stove (10) comprises the reburner heat-preservation cotton (15) of bridge-type structure, resistance wire (16), spiral helicine boiler tube (17) and thermopair (18), two reburner heat-preservation cotton (15) are symmetrical arranged the hollow cylinder structure of composition square-outside and round-inside, resistance wire (16) genesis analysis is in the endosexine of reburner heat-preservation cotton (15), boiler tube (17) is arranged on the hollow region of reburner heat-preservation cotton (15), boiler tube is provided with catalyzer in (17), thermopair (18) is arranged on the center of boiler tube (17).
8. the determinator of sulfate in a kind of Atmospheric particulates according to claim 7, it is characterized in that: described catalyzer is stainless steel, catalytic temperature is 900-1000 DEG C.
9. use the assay method of the determinator of sulfate in the Atmospheric particulates described in claim 1, it is characterized in that, concrete steps are as follows:
The preparation of a, air sample
Air to be measured, after cutter for particles (1) process, obtains air sample;
The concentration of b, detection gaseous sulphide and Sulfate
The a1 port of the first three-way valve (7), c1 port open, b1 port shutdown, the a2 port of the second three-way valve (9), c2 port open, b2 port shutdown, passes through SO 2air sample extracts by detecting device (13), air sample containing fine particle enters sulfate conversion stove (10) by way of ventilation duct, remaining particle in 3rd particle filter (11) filtering air sample, flow sensor (12) record air mass flow Q 1, finally enter SO 2detecting device (13), records the concentration of gaseous sulphide and Sulfate;
The concentration of c, detection gaseous sulphide
The a1 port of the first three-way valve (7), b1 port open, c1 port shutdown, the a2 port of the second three-way valve (9), b2 port open, c2 port shutdown, passes through SO 2air sample extracts by detecting device (13), air sample containing fine particle is by way of the second particle filter (8), after particle is removed and then by sulfate conversion stove (10), remaining particle in 3rd particle filter (11) filtering air sample, flow sensor (12) record air mass flow Q 2, finally enter SO 2detecting device (13), records the concentration of gaseous sulphide;
The concentration of d, count particles state sulfate
The concentration of the gaseous sulphide in step b and Sulfate is deducted the concentration of gaseous sulphide in step c, finally obtain the concentration of the Sulfate in air to be measured.
10. the assay method of the determinator of sulfate in use Atmospheric particulates according to claim 9, in step a, air to be measured first passes into interference gas filtering device (2) after cutter for particles (1) process, obtains air sample by after interference gas filtering.
CN201610101479.7A 2016-02-25 2016-02-25 Device and method for measuring sulfate in atmospheric particulates CN105548507A (en)

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CN106644966A (en) * 2016-12-28 2017-05-10 武汉三众和光电科技有限公司 Self-calibration rising dust measuring method and self-calibration rising dust measuring device

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