CN107179289A - Uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke - Google Patents
Uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke Download PDFInfo
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- 239000000779 smoke Substances 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000013076 uncertainty analysis Methods 0.000 title claims abstract description 15
- 238000005259 measurement Methods 0.000 claims abstract description 129
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 81
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 81
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 41
- 238000012417 linear regression Methods 0.000 claims abstract description 24
- 239000007789 gas Substances 0.000 claims description 202
- 238000004088 simulation Methods 0.000 claims description 39
- 238000010438 heat treatment Methods 0.000 claims description 37
- 238000009423 ventilation Methods 0.000 claims description 24
- 239000003546 flue gas Substances 0.000 claims description 23
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 21
- 238000010521 absorption reaction Methods 0.000 claims description 17
- 238000005070 sampling Methods 0.000 claims description 16
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- 238000002329 infrared spectrum Methods 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 13
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- 238000003556 assay Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 108010003272 Hyaluronate lyase Proteins 0.000 claims description 3
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- 230000005494 condensation Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- 230000009897 systematic effect Effects 0.000 abstract description 2
- 229960004424 carbon dioxide Drugs 0.000 description 31
- 238000011156 evaluation Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 9
- 238000001514 detection method Methods 0.000 description 6
- 235000019504 cigarettes Nutrition 0.000 description 4
- 230000008602 contraction Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
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- 239000010959 steel Substances 0.000 description 3
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
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- 239000008187 granular material Substances 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
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- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
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- 230000009467 reduction Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
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Abstract
The invention discloses a kind of uncertainty analysis method of gas concentration lwevel in industrial smoke based on infrared spectroscopic determination.This method comprises the following steps：(1) carbon dioxide measuring system is built to CO in industrial smoke2Concentration is measured；(2) determine that uncertainty is originated：The standard uncertainty that repetition measurement is introduced, the standard uncertainty that linear regression is introduced, the standard uncertainty that calibrating gas is introduced, the standard uncertainty that apparatus measures are introduced, the standard uncertainty that intercept is introduced, the standard uncertainty that slope is introduced；(3) relative standard uncertainty is synthesized；(4) relative expanded uncertainty is synthesized.This method analyzes the partial uncertainty that systematic error and random error are introduced comprehensively during analyzing and evaluating uncertainty, and finally gives carbon dioxide concentration measurement uncertainty in industrial smoke.Related data is accurately credible, and reliable method foundation is provided for the metering of industrial smoke carbon emission.
Description
Technical field
The invention belongs to carbon dioxide content detection technique field in industrial smoke, and in particular to one kind is based on infrared spectrum
Method determines the uncertainty analysis method of gas concentration lwevel in industrial smoke.
Technical background
As developing country maximum in the world, China is also coal production maximum in the world and consumption state.Coal is at me
The primary energy of state occupies main status in constituting, all kinds of burners, industry and commercial boiler can in using coal-fired process
Substantial amounts of flue gas is released, and the CO2 emission in flue gas is then the main inducing of greenhouse effects, and ecological environment is constituted
Serious threat.2008, global carbon dioxide discharge capacity reached 29,200,000,000 tons, and wherein China reaches 6,000,000,000 tons.Therefore, it is right
Carbon dioxide content in flue gas be monitored be environmental monitoring work an importance, by carbon dioxide in flue gas
The analysis of content can grasp the carbon dioxide regularity of distribution and monitoring energy consumption index situation of change.
According to State Council《" 13 " monitor greenhouse gas emission programme of work》Target：To the year two thousand twenty, the life of the unit country
Produce total value CO2 emission and declined 18% than 2015, total carbon emission will be effectively controlled.There is presently no build for China
CO2 emissions directly measure standard of tracing to the source online in vertical perfect industrial smoke, between smoke carbon dioxide discharge capacity is mostly
Connect by Coal-fired capacity measuring and calculating and indirectly measurement, because there is shortcoming in the mass measurement of coal, result that computational methods are obtained and
The difference average value of correct result is 17%, and all minus deviation, and acquired results and actual conditions differ greatly, calculating side
The data precision that method is obtained can not meet the exact requirements of carbon transaction.If dense carbon dioxide in industrial smoke can be measured accurately
Degree, directly calculates total carbon emission in conjunction with fume emission flow, greenhouse gas emission metering and monitoring system will be built
Vertical produce greatly helps.
The method of carbon dioxide concentration measurement mainly has chemical method, electrochemical process, gas chromatography, volumetric precipitation method etc.,
There is cost height, the online high-volume low defect of the poor for applicability, degree of accuracy in such method.At present there is not yet measurement range it is wide,
Response time is short, the degree of accuracy is high, strong antijamming capability, is adapted to gas concentration lwevel in the industrial smoke of online big flow detection and examines
Survey method.
Infrared spectrum technology be it is a kind of it is simple and convenient, analysis is quick, do not destroy the new analytical technology of sample, it can be same
When determine a variety of chemical compositions and physical parameter in sample, analysis result is accurately and reliably.Infrared point of FT-NIR IGS gases
Analysis system has high gas detection sensitivity and wide applicability (can be worked under high temperature and high humidity environment), detects model
Enclose width, be swift in response, be adapted to industry spot and analyzed online with side line.And uncertainty is that the tested value of embodiment is rationally dispersed,
It is the parameter being associated with measurement result, is the important indicator of contemporary error theory quantitative description measurement result quality.Therefore, originally
Dioxide component ir data sample in the industrial smoke that application passes through foundation, founding mathematical models, analysis are uncertain
Degree source, calculates uncertainty of the carbon dioxide in the range of actual industrial smoke emissioning concentration, is the industrial cigarette of Erecting and improving
CO2 emissions directly metering traces to the source standard there is provided method foundation in gas.
The content of the invention
In order to achieve the above object, it is based on carbon dioxide in infrared spectroscopic determination industrial smoke the invention provides one kind
(CO2) concentration uncertainty analysis method.This method can determine carbon dioxide (CO in industrial smoke2) measurement of concetration is true
Surely the main source spent, takes measures for main source, could further improve carbon dioxide (CO2) measurement accuracy, be
Carbon emission accurate measurement provides reliable method.
The present invention is achieved by the following technical solutions
The uncertainty analysis method of gas concentration lwevel, this method in a kind of industrial smoke based on infrared spectroscopic determination
Comprise the following steps：
1) CO in industrial smoke is built2Concentration measurement system；
2) use step 1) described in CO2Concentration measurement system is to CO in industrial smoke2Concentration is measured, and step is as follows：
1. use step 1) build system to a series of known CO2The simulation industrial smoke of standard gas concentration is carried out
Measurement, according to CO in simulation industrial smoke2The series concentration content and its corresponding measurement result of calibrating gas set up standard work
Make curve, and standard fit working curve y=a+bx is obtained through over-fitting；
In formula, y：Metering absorbs peak area (PA*S)；x：Gas concentration lwevel (vol.%)；a：The intercept of regression equation；
b：The slope of regression equation；
2. gathers actual industrial flue gas, using step 1) constructed by system measure, it is and 1. described according to step
Standard fit working curve obtains CO in industrial smoke to calculate2The measured value of concentration；
Described simulation industrial smoke：Refer to using actual industrial carbon dioxide in flue gas levels as foundation, using many
Plant calibrating gas and use CO2Concentration measurement system control calibrating gas flow, be formulated as it is identical with industrial smoke composition, contain
The close mixed gas of amount, prepares a series of known CO2The simulation industrial smoke mixed gas of standard gas concentration；Then use
Step 1) build system measure, pass through known serial CO2Standard gas concentration and its corresponding measurement result are built
Vertical standard working curve；
3) CO in statistics influence measurement industrial smoke2Every partial uncertainty of concentration measurement,
CO in industrial smoke2Concentration measurement C combined standard uncertainty u (C) and its variance is as follows：
Wherein, propagation coefficient
In above-mentioned formula, u (C)：Represent CO2The combined standard uncertainty of assay；u(y)：Represent metering absworption peak
The standard uncertainty that area change is introduced；u(a)：Represent the standard uncertainty that intercept is introduced；u(b)：Represent that slope is introduced
Standard uncertainty；Represent that repeatedly measurement gained absorbs the average value of peak area；uR：Represent the mark that repetition measurement is introduced
Quasi- uncertainty；u1：Represent the standard uncertainty that linear regression is introduced；u2：Represent CO2The standard that calibrating gas is introduced is not true
Fixed degree；u3：Represent the standard uncertainty that apparatus measures are introduced；
It can obtain, CO in influence measurement industrial smoke2The items of concentration measurement do not know component：
(1)uR：The standard uncertainty that repetition measurement is introduced；
(2)u1：The standard uncertainty that linear regression is introduced；
(3)u2：CO2The standard uncertainty that calibrating gas is introduced；
(4)u3：The standard uncertainty that apparatus measures are introduced；
(5)u(a)：The standard uncertainty that intercept is introduced；
(6)u(b)：The standard uncertainty that slope is introduced；
4) relative standard uncertainty is synthesized
Combined standard uncertainty
It can obtain, synthesize relative standard uncertainty
5) relative expanded uncertainty
Spreading factor k=2 is taken, then CO in industrial smoke2Measurement of concetration is with respect to expanded uncertainty Urel=2 × urel(C)。
The described uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke, step
1) CO in the industrial smoke described in2Concentration measurement system includes calibrating gas storage tank, is deposited by ventilation line with calibrating gas
The gas that storage tank is connected mixes heating bath, and infrared point of the IGS gases that heating bath is connected are mixed by gas line and gas
Analyzer, described IGS gases infrared spectrum analyser is electrically connected with the signal input part of data acquisition device；In the industrial smoke
CO2Concentration measurement system also include flue gas generation system, the sampling gun being connected with flue gas generation system, by ventilation line with
The dust filter unit that sampling gun is connected, the condenser being connected by ventilation line with dust filter unit, passes through ventilation line
The sampling pump being connected with condenser, the gas being connected by ventilation line with sampling pump mixes heating bath；Described industry
CO in flue gas2Concentration measurement system also includes controller；
Described calibrating gas storage tank gas outlet is provided with gas mass flow gauge, and described gas mixes heating
Pond and connection gas mix heating bath and cladding is provided with heat tape in the ventilation line of IGS gas infrared spectrum analysers；
Described gas mass flow gauge and heat tape are electrically connected with the signal output part of controller.
Described gas, which mixes heating bath, to be included being filled with cylindrical shell and the cylindrical shell rear end of bulk steel wire lump
Rear gas chamber, in described rear gas chamber axially pivot joint be provided with disturbance impeller and including being located at the expansion arc at two ends and being located in
The contraction section in portion, is sufficiently mixed so that air-flow expands compressed transform realization by swift current；After corresponding with contraction section
Heating muff is provided with gas chamber outer wall, provided with heating medium and electrical heating wire between the heating muff and rear gas chamber's outer wall.
The described uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke, step
2) the use step 1) CO2Concentration measurement system is to CO in industrial smoke2Concentration is measured, and step is as follows：
A. according to step 1) build CO2Concentration measurement system, measures a series of known CO2The simulation of standard gas concentration
Industrial smoke calibrating gas, the CO of each concentration2Calibrating gas obtains corresponding measurement result, after measuring, root respectively
According to known CO in simulation industrial smoke2Standard gas concentration and its corresponding measurement result set up standard working curve；
B. the regression equation of standard working curve described in least square method calculation procedure a is used：Y=a+bx；Through fitting meter
Calculate：A=0.0254；B=1.25501；R=0.99965；Produce standard fit working curve regression equation：Y=a+bx=
0.0254+1.25501x；
In formula, y：Metering absorbs peak area (PA*S)；x：Gas concentration lwevel (vol.%)；a：The intercept of regression equation；
b：The slope of regression equation；
C. actual industrial flue gas is gathered, using step 1) constructed by system measure, and the mark according to step b
Quasi- fitting operations curve obtains CO in industrial smoke to calculate2The measured value of concentration.
The described uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke, step
3) standard uncertainty that the measurement reproducibility described in is introduced, using type A evaluation method,
The standard deviation of wherein single measurement result is calculated as with Bessel Formula：(in formula, sR1
Represent the standard deviation of absworption peak area result obtained by single measurement, yjRepresent to measure CO in sample every time2The single absorption of gained
Peak area test value,Represent CO in repeatedly measurement sample2The average value of the absorption peak area of gained, n represents that absorbing peak area surveys
Measure number of times, j represent absorb peak area measurement sequence number, j=1,2,3 ... n),
So the standard uncertainty introduced by repetition measurement is as follows：(in formula,Represent multiple
The average value of measurement gained absworption peak area result standard deviation).
The described uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke, step
3) standard uncertainty that the linear regression described in is introduced, using type A evaluation method, in measurement process, by least square
Method carries out the standard fit working curve obtained by linear regression to measure CO in industrial smoke2Institute in concentration, linear regression procedure
The standard uncertainty that the standard deviation of introducing, i.e. linear regression are introduced：
(in formula, s1Represent the standard uncertainty that linear regression is introduced, yiRepresent measurement every time
Simulation industrial smoke in CO2Single absorption peak area test value obtained by calibrating gas；Represent measurement CO every time2Calibrating gas
The single match value for absorbing peak area of gained, n represents absorption peak area measurement number of times, and i represents to absorb peak area measurement sequence number, i
=1,2,3 ... n).
The described uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke, step
3) CO described in2The standard uncertainty that calibrating gas is introduced is, using type B evaluation method：
(in formula, UrelRepresent CO2The relative expanded uncertainty of calibrating gas content,Represent repeatedly to survey
CO in amount simulation industrial smoke2The average value of peak area is absorbed obtained by calibrating gas).
The described uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke, step
3) standard uncertainty that the apparatus measures described in are introduced, using type B evaluation method, CO2Absorb peak area quantification and determine used
The maximum tolerance of infrared spectrometer is 1%, by being uniformly distributed consideration, and the relative standard uncertainty of apparatus measures is：
Then corresponding standard uncertainty is：(in formula, u3relRepresent that the relative standard of apparatus measures is not true
Fixed degree,Represent CO in repeatedly measurement simulation industrial smoke2The average value of peak area is absorbed obtained by calibrating gas).
The described uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke, step
3) standard uncertainty that the intercept described in is introduced is, using type A evaluation method：
In formula, s1Represent the standard uncertainty that linear regression is introduced；xiRepresent the industrial cigarette of the used simulation of measurement every time
CO in gas2The concentration of calibrating gas,Represent that repeatedly measurement uses CO in simulation industrial smoke2Calibrating gas series concentration
Average value, n represents CO in simulation industrial smoke2The pendulous frequency of calibrating gas, i represents the sequence number of pendulous frequency, i=1,2,
3……n。
The described uncertainty analysis method based on gas concentration lwevel in infrared spectroscopic determination industrial smoke is to walk
It is rapid 3) described in slope introduce standard uncertainty be, using type A evaluation method：
In formula, s1Represent the standard uncertainty that linear regression is introduced；xiRepresent the industrial cigarette of the used simulation of measurement every time
CO in gas2The concentration of calibrating gas,Represent that repeatedly measurement uses CO in simulation industrial smoke2Standard gas concentration is averaged
Value, n represents CO in simulation industrial smoke2Calibrating gas pendulous frequency, i represents the sequence number of pendulous frequency, i=1,2,3 ... n.
Special absorption peak shape can be left in infrared spectrogram after the energy of gas with various molecule absorption different wave length,
The absorption spectrum curve shape of material of the same race is identical, and the size that concentration difference only will result only in absorption spectrum changes,
Existence function relation i.e. between the area and concentration of absorption spectrum.It is referred to as " the light of gas based on this kind of unique absorbing structure
Compose fingerprint ", the different gas of analysis and identification and determine its concentration according to this；
Each asymmetric gas molecule has the absworption peak of uniqueness in Fourier infrared absorption region, is absorbed by these
Information is that can carry out quantitative or qualitative analysis, and the selection rule of characteristic wavelength scope is：Include component gas characteristic absorpting spectrum
Line；The absorption intensity of characteristic wavelength scope and mixture gas component concentration be linear or non-linear relation；In the range of characteristic wavelength
There is larger absorption coefficient；
Based on above-mentioned consideration, (2400~2200) cm is chosen by testing-1In the range of a small characteristic absorption peak be two
The optimal quantitative characteristic absworption peak of carbonoxide, as shown in figure 3, its specific scope is (2240~2238) cm-1, as shown in figure 4, its peak
Size and gas concentration lwevel height direct proportionality, it is possible thereby to by testing (2240~2238) cm-1In region
The small peak area that absorbs of carbon dioxide obtains gas concentration lwevel indirectly.
Compared with prior art, the present invention has following positive beneficial effect
(1) present invention has carried out dust granules and water steaming in preceding processing, flue gas to flue gas first in data acquisition
Gas is removed, and eliminates the interference of dust and vapor to measurement result, and not only ensuring this method uninterruptedly can continuously grasp
Make, and improve the repeatability and measurement accuracy of measurement data；
(2) most direct-reading quasi-instruments can not retain carbon dioxide initial data at present, and the present invention can not only show two in real time
Carbonoxide concentration value, moreover it is possible to record quantitative carbon dioxide and absorb peak area original spectrum diagram data, related data can be protected for a long time
Deposit, meet carbon emission data values and trace to the source requirement.The present invention analyzes system mistake comprehensively during analyzing and evaluating uncertainty
The partial uncertainty that difference and random error are introduced, the uncertainty related data of final gained is accurately credible, is industrial smoke
Carbon emission metering provides reliable method foundation.
Brief description of the drawings
Fig. 1 is the schematic diagram of constructed carbon dioxide detecting system；
The meaning that symbol is represented in figure is：1 is calibrating gas accumulator tanks, and 2 be gas mass flow gauge, and 3 be that gas is mixed
Heating bath, 4 be heat tape, and 5 be IGS gas infrared spectrum analysers, and 6 be data acquisition device, and 7 be industrial smoke generation system, 8
It is dust filter unit for sampling gun, 9,10 be condenser, and 11 be sampling pump, and 12 be controller；
Fig. 2 is the structural representation that gas mixes heating bath；
The meaning that symbol is represented in figure is：301 be cylindrical shell, and 302 be bulk steel wire lump, and 303 be rear gas chamber, and 304 are
Impeller is disturbed, 305 be heating muff, and 306 be electrical heating wire；
Fig. 3 is that carbon dioxide infrared signature absorbs spectrogram；
Fig. 4 is quantitative carbon dioxide characteristic absorption spectrogram；
Fig. 5 is standard fit working curve used in carbon dioxide concentration measurement in industrial smoke；
Fig. 6 is carbon dioxide concentration measurement uncertainty source cause-and-effect diagram in industrial smoke.
Embodiment
The present invention is described in more details below by embodiment, but is not intended to limit the invention
Protection domain.
Embodiment 1
The uncertainty analysis method of gas concentration lwevel in a kind of industrial smoke based on infrared spectroscopic determination, including with
Lower step：
1) structure and measuring process of carbon dioxide measuring system are as follows：
1. the structure of carbon dioxide measuring system：
The measuring system of carbon dioxide as shown in figure 1, the system includes calibrating gas storage tank 1, by ventilation line with
The gas that calibrating gas storage tank 1 is connected mixes heating bath 3, mixes what heating bath 3 was connected by gas line and gas
IGS gases infrared spectrum analyser 5, described IGS gases infrared spectrum analyser 5 is electrically connected with the signal input part of data acquisition device 6；
The system also includes flue gas generation system 7, and the sampling gun 8 being connected with flue gas generation system 7 passes through ventilation line and sampling gun
8 dust filter units 9 being connected, the condenser 10 being connected by ventilation line with dust filter unit 9, by ventilation line with
The sampling pump 11 that condenser 10 is connected, the gas being connected by ventilation line with sampling pump 11 mixes heating bath 3；It is (described
Dust filter unit 9 be mainly used in being filtered to remove dust granules in flue gas；Described condenser 10 is mainly used in removing flue gas
In vapor, in order to avoid impacted to carbon dioxide measurement)；The system also includes controller 12；
The gas outlet of described calibrating gas storage tank 1 is provided with gas mass flow gauge 2, and described gas is mixed
Heating bath 3 and connection gas mix heating bath 3 and cladding is provided with electricity in the ventilation line of IGS gases infrared spectrum analyser 5
Heating tape 4；Signal output part of the described gas mass flow gauge 2 and heat tape 4 with controller 12 is electrically connected；
Described gas mixes heating bath 3 as shown in Fig. 2 the cylindrical shell including being filled with bulk steel wire lump 302
301 and the rear gas chamber 303 of cylindrical shell rear end, axially pivot joint is provided with disturbance impeller 304 and bag in described rear gas chamber 303
The expansion arc and the contraction section positioned at middle part positioned at two ends are included, is realized so that air-flow expands compressed transform by swift current
It is sufficiently mixed；Heating muff 305, the heating muff 305 and rear gas chamber are provided with rear gas chamber corresponding with contraction section outer wall
Provided with heating medium and electrical heating wire 306 between 303 outer walls；
2. using gas concentration lwevel in above-mentioned carbon dioxide measuring system measurement industrial smoke：
A. controller is opened, the flow number of every kind of calibrating gas in heating-up temperature and measuring system is set on the controller
(being set according to actual industrial flue gas constituent measurement range), by heat tape by gas concentration lwevel detecting system
The uniform heating bath of gas and the ventilation line of the connection uniform heating bath of gas and IGS gas infrared spectrum analysers be heated to 155 ± 5
DEG C constant temperature, and the detection temperature of IGS gas infrared spectrum analysers is set as identical temperature, i.e., 155 ± 5 DEG C；
By the control of controller in the step, a series of the mixed of different carbon dioxide standard gas concentrations can must be made
Close gas；
b.CO2、NO、SO2、N2Calibrating gas stores the gas that tank valve and calibrating gas storage tank gas outlet are set
Mass flowmenter is opened, and flow that each calibrating gas is set according to step a controllers, by whole ventilation line is passed through gas
Mix in heating bath, mixing is heated in gas mixes heating bath, gas mixing heating bath is heated to 155 ± 5 DEG C；Then will
The gaseous sample that heating is mixed is passed through IGS gases infrared spectrum analyser (the IGS gas by the ventilation line under the conditions of 155 ± 5 DEG C
Body infrared spectrum analyser model：ANTARIS；Test temperature is set as 155 DEG C during the instrument use) in tested；
C. in measurement process, during mixed gas is passed through, IGS infrared-gas point is passed through with 3000ml/min flow velocity
Tested in analyzer, a series of known CO are tested successively2The simulation industrial smoke calibrating gas of standard gas concentration, Mei Geyi
Know that concentration obtains corresponding metering and absorbs peak area respectively (result is as shown in table 1)；Each concentration carry out three replications it
After average, according to known CO2The concentration of calibrating gas and corresponding absworption peak area average, drafting are corresponded to
Standard working curve；Then the regression equation of standard working curve is calculated using least square method：
Y=a+bx
In formula, y：Peak area (PA*S) is absorbed for metering；x：For gas concentration lwevel (vol.%)；a：For regression equation
Intercept；b：For the slope of regression equation；
By the Fitting Calculation, a=0.0254；B=1.25501；R=0.99965；I.e. regression equation is：Y=a+bx=
0.0254+1.25501x, gained standard fit working curve is as shown in Figure 5；
Known CO2The simulation industrial smoke calibrating gas test result of standard gas concentration is as shown in table 1：
The CO of table 12Standard gas concentration-metrology features absorb peak area corresponding relation
It can be obtained by the above results：Linearity error≤± 1%, shows that the test system linearity is good, can be completely used for reality
The measurement of gas concentration lwevel in the industrial smoke of border；
D. the step gas that 2. calibrating gas storage tank valve and calibrating gas storage tank gas outlet described in b are set is closed
Weight flowmeter, opens the valve (industrial chimney sampling gas circuit in be provided with valve) of industrial smoke production system, using adopting
Industrial smoke in sample rifle and sampling pump collection flue gas generation system, the industrial smoke of collection is respectively by dust filter unit and cold
Condenser (condensation temperature of condenser is 2 DEG C in the course of work) is filtered, except water process, and the industrial smoke after the completion of processing leads to
Cross ventilation line and be passed through gas and mix in heating bath and be heated to 155 DEG C, then by the ventilation line under the conditions of 155 DEG C, with 3000ml/
Min flow velocity is passed through IGS infrared gas analysers and tested, and the absworption peak face of carbon dioxide in industrial smoke is obtained in real time
Product, then the standard fit working curve according to step 2. c can calculate the CO obtained in industrial smoke2Concentration；
2) count and calculate CO in influence measurement industrial smoke2Concentration measurement every partial uncertainty (its not
Degree of certainty source cause-and-effect diagram is as shown in Figure 6)：
CO in industrial smoke2Concentration measurement C Composite Seismogram u (C) and its variance is as follows：
Propagation coefficient：
In above-mentioned formula, u (C)：For CO2The combined standard uncertainty of assay；u(y)：Represent metering absworption peak face
The standard uncertainty that product change is introduced；u(a)：Represent the standard uncertainty that intercept is introduced；u(b)：Represent what slope was introduced
Standard uncertainty；Represent that repeatedly measurement gained absorbs the average value of peak area；uR：Represent the standard that repetition measurement is introduced
Uncertainty；u1：Represent the standard uncertainty that linear regression is introduced；u2：Represent CO2The stardard uncertairty that calibrating gas is introduced
Degree；u3：Represent the standard uncertainty that apparatus measures are introduced；
So, CO in influence measurement industrial smoke2Every partial uncertainty of concentration measurement is specially：
(1) the standard uncertainty u that repetition measurement is introducedR, using type A evaluation method：
The main inconsistency, environment temperature, pressure by sample gas in standard uncertainty source that repetition measurement is introduced
What the factors such as power, human users were introduced；Under the conditions of repeatability, surveyed according to the assay method of establishment is parallel to same gaseous sample
Fixed 6 times, to investigate measurement reproducibility, measurement result is as shown in table 2：
The sample gas horizontal survey result of table 2
The standard deviation of wherein single measurement result is calculated with Bessel Formula：
In formula, sR1Represent the standard deviation of absworption peak area result obtained by single measurement, yjRepresent CO in sample2It is single to inhale
The test value of peak area is received,Represent CO in repeatedly measurement sample2The average value of peak area is absorbed, n represents to absorb peak area measurement
Number of times, j represents that measurement absorbs peak area sequence number, j=1,2,3 ... n；Following result can be obtained by bringing the data of table 2 into formula (III)：
The detection number of times of each sample is 3 times in an experiment, and takes the average value of 3 testing results；That is, replication work
CO in industry flue gas2The standard uncertainty of content is：
(Represent being averaged for absworption peak area standard deviation obtained by 3 measurements
Value).
(2) the standard uncertainty u that linear regression is introduced1, using type A evaluation method：
In actual measurement process, carry out the standard fit working curve obtained by linear regression to count by least square method
Calculate CO in industrial smoke gas2The standard that the standard deviation introduced in concentration, linear regression procedure, i.e. linear regression are introduced is not true
Fixed degree：
In formula, s1The standard uncertainty introduced for linear regression, yiCO in the simulation industrial smoke that expression is measured every time2
Single absorption peak area test value obtained by calibrating gas,Represent CO in measurement simulation industrial smoke every time2It is single obtained by calibrating gas
It is individual absorb peak area match value, n represent absorb peak area measurement number of times, i represent absorb peak area measurement sequence number, i=1,
2,3 ... n；
Bringing the data of table 1 into formula (IV), can to obtain result as follows：
(3)CO2The standard uncertainty u that calibrating gas is introduced2, using type B evaluation method：
Calibrating gas used during carbon dioxide concentration measurement standard working curve is fitted in the embodiment by Henan Province
Measure engineering center to provide, establishing criteria material certificate, CO2The relative expanded uncertainty U of contentrelAll be 2%, extension because
Sub- k=2, then testing the standard uncertainty that Plays gas introduces is：
In formula, UrelRepresent CO2The relative expanded uncertainty of calibrating gas content,Represent the repeatedly industrial cigarette of measurement simulation
CO in gas2The average value of peak area is absorbed obtained by calibrating gas, the data of table 1 are substituted into formula (V) can obtain following result：
In formula, yiRepresent CO in measurement simulation industrial smoke every time2Single absorption peak area test value, i obtained by calibrating gas
Represent to absorb peak area measurement sequence number, i=1,2,3 ... n).
(4) the standard uncertainty u that apparatus measures are introduced3, using type B evaluation method：
The standard uncertainty calculation formula that described apparatus measures are introduced is as follows：
In formula, u3relThe relative standard uncertainty of apparatus measures is represented,Represent in repeatedly measurement simulation industrial smoke
CO2The average value of peak area is absorbed obtained by calibrating gas；
CO2It is 1% to absorb peak area quantification to determine the maximum tolerance of infrared spectrometer used, by being uniformly distributed consideration, its
Relative standard uncertainty is：The data and the data of table 1 are substituted into formula (VI) to obtain：Institute is right
The standard uncertainty answered is：
(5) the standard uncertainty u (a) that intercept is introduced, using type A evaluation method：
The standard uncertainty that the intercept is introduced is calculated as follows：
In formula, s1Represent the standard uncertainty that linear regression is introduced, xiRepresent that measurement every time uses simulation industrial smoke
Middle CO2The concentration of calibrating gas；Represent CO in repeatedly measurement simulation industrial smoke2Calibrating gas uses CO2Standard Gases system
The average value of row concentration, n represents CO in simulation industrial smoke2Calibrating gas pendulous frequency, i represents the sequence number of pendulous frequency, i=
1,2,3 ... n；The data of table 1 substitution formula (VII) can be obtained into result as follows：
The standard uncertainty that intercept is introduced is calculated as follows：
(6) the standard uncertainty u (b) that slope is introduced, using type A evaluation method：
The standard uncertainty that the slope is introduced is calculated as follows：
In formula, s1Represent the standard uncertainty that linear regression is introduced；xiRepresent that measurement every time uses simulation industrial smoke
Middle CO2The concentration of calibrating gas,Represent CO in repeatedly measurement simulation industrial smoke2Calibrating gas uses CO2Standard Gases system
The average value of row concentration, n represents CO in simulation industrial smoke2Calibrating gas pendulous frequency, i represents the sequence number of pendulous frequency, i=
1,2,3 ... ... n；The public formula (VIII) of the data of table 1 substitution can be obtained into result as follows：
The standard uncertainty that slope is introduced is calculated as follows：
By all standard uncertainty of above-mentioned calculating, following form can be obtained：
CO in the industrial smoke of table 32Measurement of concetration uncertainty concludes table
3) synthesis relative standard uncertainty is calculated
By step 1) b calculate data can obtain：
Propagation coefficient：
Then combined standard uncertainty
So, synthesize relative standard uncertainty
4) relative expanded uncertainty is calculated
Spreading factor k=2 is taken, then CO in industrial smoke2Measurement of concetration is with respect to expanded uncertainty Urel=2 × urel(C)
=2.3%.
From above-mentioned experimental result, using Fourier transform infrared spectrometry to CO in the industrial smoke of simulation2Concentration is carried out
The main source of uncertainty in measurement, measurement process is by calibrating gas and standard working curve introducing, therefore, in reality
Should try one's best reduction systematic error in the detection process of border, could further improve CO2The precision of measurement of concetration, is that carbon emission is accurately counted
Amount provides reliable method.
Claims (9)
1. a kind of uncertainty analysis method of gas concentration lwevel in industrial smoke based on infrared spectroscopic determination, its feature exists
In this method comprises the following steps：
1) CO in industrial smoke is built2Concentration measurement system；
2) use step 1) described in CO2Concentration measurement system is to CO in industrial smoke2Concentration is measured；
3) CO in statistics influence measurement industrial smoke2Every partial uncertainty of concentration measurement,
CO in industrial smoke2Concentration measurement C combined standard uncertainty u (C) and its variance is as follows：
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In above-mentioned formula, u (C)：For CO2The combined standard uncertainty of assay；u(y)：Represent that metering absorbs peak area and become
Change the standard uncertainty introduced；u(a)：Represent the standard uncertainty that intercept is introduced；u(b)：Represent the standard that slope is introduced
Uncertainty；Represent that repeatedly measurement gained absorbs the average value of peak area；uR：Represent that the standard that repetition measurement is introduced is not true
Fixed degree；u1：Represent the standard uncertainty that linear regression is introduced；u2：Represent the stardard uncertairty that carbon dioxide calibrating gas is introduced
Degree；u3：Represent the standard uncertainty that apparatus measures are introduced；
It can obtain, CO in influence measurement industrial smoke2Every partial uncertainty of concentration measurement is specially：
(1)uR：The standard uncertainty that repetition measurement is introduced；
(2)u1：The standard uncertainty that linear regression is introduced；
(3)u2：The standard uncertainty that carbon dioxide calibrating gas is introduced；
(4)u3：The standard uncertainty that apparatus measures are introduced；
(5)u(a)：The standard uncertainty that intercept is introduced；
(6)u(b)：The standard uncertainty that slope is introduced；
4) relative standard uncertainty is synthesized
Combined standard uncertainty
Synthesize relative standard uncertainty
5) relative expanded uncertainty is synthesized
Spreading factor k=2 is taken, then CO in industrial smoke2Measurement of concetration is with respect to expanded uncertainty Urel=2 × urel(C)。
2. the uncertainty of gas concentration lwevel point in the industrial smoke according to claim 1 based on infrared spectroscopic determination
Analysis method, it is characterised in that step 1) described in industrial smoke in CO2Concentration measurement system includes calibrating gas storage tank, leads to
The gas mixing heating bath that ventilation line is connected with calibrating gas storage tank is crossed, passes through ventilation line and gas mixes heating bath
The IGS gas infrared spectrum analysers being connected, described IGS gases infrared spectrum analyser and the signal input part electricity of data acquisition device
Connection；CO in described industrial smoke2Concentration measurement system also includes flue gas generation system, is connected with flue gas generation system
Sampling gun, the dust filter unit being connected by ventilation line with sampling gun, is connected by ventilation line with dust filter unit
Condensation dehydrater, by ventilation line and the sampling pump that is connected of condensation dehydrater, be connected by ventilation line with sampling pump
Logical gas mixes heating bath；CO in described industrial smoke2Concentration measurement system also includes controller；
Described calibrating gas storage tank gas outlet is provided with gas mass flow gauge, described gas mix heating bath with
And the connection uniform heating bath of gas is provided with heat tape with being coated in the ventilation line of IGS gas infrared spectrum analysers；It is described
Gas mass flow gauge and heat tape electrically connected with the signal output part of controller.
3. gas concentration lwevel is uncertain in the industrial smoke according to claim 1 or 2 based on infrared spectroscopic determination
Spend analysis method, it is characterised in that step 2) the use CO2Concentration measurement system is to CO in industrial smoke2Concentration is surveyed
Amount, step is as follows：
A. according to step 1) build CO2Concentration measurement system, measures a series of known CO2The simulation industry of standard gas concentration
Flue gas calibrating gas, the CO of each concentration2Calibrating gas obtains corresponding measurement result respectively, after measuring, according to mould
Intend known CO in industrial smoke2Standard gas concentration and its corresponding measurement result set up standard working curve；
B. the regression equation of standard working curve described in least square method calculation procedure a is used：Y=a+bx；Through the Fitting Calculation：a
=0.0254；B=1.25501；R=0.99965；Produce standard fit working curve regression equation：Y=a+bx=0.0254+
1.25501x；
In formula, y：Metering absorbs peak area (PA*S)；x：Gas concentration lwevel (V/V)；a：The intercept of regression equation；b：Recurrence side
The slope of journey；
C. actual industrial flue gas is gathered, using step 1) constructed by system measure, and standard according to step b is intended
Close working curve and obtain CO in industrial smoke to calculate2The measured value of concentration.
4. the uncertainty of gas concentration lwevel point in the industrial smoke according to claim 1 based on infrared spectroscopic determination
Analysis method, it is characterised in that step 3) described in measurement reproducibility introduce standard uncertainty：
The standard deviation of its single measurement result is calculated as with Bessel Formula：
In formula, sR1Represent the standard deviation of single measurement absworption peak area result, yjRepresent to measure CO in sample every time2Gained
Single absorption peak area test value,Represent CO in repeatedly measurement sample2The average value of the absorption peak area of gained, n is represented
Peak area measurement number of times is absorbed, j represents to absorb peak area measurement sequence number, j=1,2,3 ... n；
After the measurement of multiplicating property, the standard uncertainty introduced by measurement reproducibility is：
5. the uncertainty of gas concentration lwevel point in the industrial smoke according to claim 1 based on infrared spectroscopic determination
Analysis method, it is characterised in that step 3) described in linear regression introduce standard uncertainty be calculated as follows：
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In formula, s1Represent the standard uncertainty that linear regression is introduced, yiCO in the simulation industrial smoke that expression is measured every time2
Single absorption peak area test value obtained by calibrating gas；Represent the CO measured every time2Single absorption peak area obtained by calibrating gas
Match value, n represent absorb peak area measurement number of times, i absorb peak area measurement sequence number, i=1,2,3 ... n.
6. the uncertainty of gas concentration lwevel point in the industrial smoke according to claim 1 based on infrared spectroscopic determination
Analysis method, it is characterised in that step 3) described in carbon dioxide calibrating gas introduce standard uncertainty be calculated as follows：
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Middle CO2The average value of peak area is absorbed obtained by calibrating gas.
7. the uncertainty of gas concentration lwevel point in the industrial smoke according to claim 1 based on infrared spectroscopic determination
Analysis method, it is characterised in that step 3) described in apparatus measures introduce standard uncertainty be calculated as follows：
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CO2The average value of peak area is absorbed obtained by calibrating gas.
8. the uncertainty of gas concentration lwevel point in the industrial smoke according to claim 1 based on infrared spectroscopic determination
Analysis method, it is characterised in that step 3) described in intercept introduce standard uncertainty be calculated as follows：
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CO2The concentration of calibrating gas,Represent that repeatedly measurement uses CO in simulation industrial smoke2The series concentration of calibrating gas it is flat
Average, n represents CO in simulation industrial smoke2Calibrating gas pendulous frequency, i represents the sequence number of pendulous frequency, i=1,2,3 ...
n。
9. the uncertainty of gas concentration lwevel point in the industrial smoke according to claim 1 based on infrared spectroscopic determination
Analysis method, it is characterised in that step 3) described in slope introduce standard uncertainty be calculated as follows：
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Value, n represents CO in simulation industrial smoke2Calibrating gas pendulous frequency, i represents the sequence number of pendulous frequency, i=1,2,3 ... n.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111413291A (en) * | 2020-04-09 | 2020-07-14 | 中国科学院上海应用物理研究所 | Infrared spectrum quantitative analysis method of gas fluoride |
| CN112505215A (en) * | 2020-11-19 | 2021-03-16 | 广东中认华南检测技术有限公司 | Method for evaluating uncertainty of content of octabromodiphenyl ether in sample |
| CN112650740A (en) * | 2020-12-24 | 2021-04-13 | 华电电力科学研究院有限公司 | Method and system for reducing uncertainty of online monitoring carbon emission data |
| CN113188613A (en) * | 2021-03-05 | 2021-07-30 | 深圳市联恒星科技有限公司 | Multiphase flow measurement method and system based on uncertainty analysis |
| US20230266235A1 (en) * | 2022-02-24 | 2023-08-24 | Thalo Labs, Inc. | Systems and Methods for Measuring Emissions from a Building |
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| CN2854600Y (en) * | 2005-12-31 | 2007-01-03 | 索纪文 | Smoke on-line analyzer |
| CN205483934U (en) * | 2016-02-01 | 2016-08-17 | 河南省计量科学研究院 | Particulate matter measuring apparatu calibration system |
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| CN111413291A (en) * | 2020-04-09 | 2020-07-14 | 中国科学院上海应用物理研究所 | Infrared spectrum quantitative analysis method of gas fluoride |
| CN112505215A (en) * | 2020-11-19 | 2021-03-16 | 广东中认华南检测技术有限公司 | Method for evaluating uncertainty of content of octabromodiphenyl ether in sample |
| CN112650740A (en) * | 2020-12-24 | 2021-04-13 | 华电电力科学研究院有限公司 | Method and system for reducing uncertainty of online monitoring carbon emission data |
| CN112650740B (en) * | 2020-12-24 | 2023-04-18 | 华电电力科学研究院有限公司 | Method and system for reducing uncertainty of online monitoring carbon emission data |
| CN113188613A (en) * | 2021-03-05 | 2021-07-30 | 深圳市联恒星科技有限公司 | Multiphase flow measurement method and system based on uncertainty analysis |
| CN113188613B (en) * | 2021-03-05 | 2024-04-05 | 深圳市联恒星科技有限公司 | Multi-phase flow measurement method and system based on uncertainty analysis |
| US20230266235A1 (en) * | 2022-02-24 | 2023-08-24 | Thalo Labs, Inc. | Systems and Methods for Measuring Emissions from a Building |
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