CN105203460B - Infrared laser spectroscopy trace steam detecting system and its detection method - Google Patents
Infrared laser spectroscopy trace steam detecting system and its detection method Download PDFInfo
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Abstract
The invention belongs to Gas Thickness Detecting Technology field, more particularly to a kind of infrared laser spectroscopy trace steam detecting system and its detection method, the present invention uses biabsorption pool structure, offseted by the spectral signal difference of light path and reference path, eliminate the influence of high concentration background gas spectrum and absorption cell external environment steam, suppress optical system common-mode noise, realize the highly sensitive detection of trace steam in high-concentration industrial gas.
Description
Technical field
The invention belongs to Gas Thickness Detecting Technology field, and in particular to a kind of infrared laser spectroscopy trace steam detection system
System and its detection method.
Background technology
Industrial process is often related to high concentration process gas, such as acid manufacturing processes high concentration SO 2 gas, the semiconductor of metallurgy industry
High purity N H3 gases etc. in industry, in order to ensure product quality and equipment safety, it is necessary to improve gas purity as far as possible, reduce
Impurity component content, wherein steam are most commonly seen foreign gas, such as steam impurity meeting in acid manufacturing processes high concentration SO 2 gas
Catalyst failure and pipe-line equipment is caused to corrode, steam impurity can influence semiconductor in high purity N H3 gases in semi-conductor industry
Photoelectricity, reduce the quality of final products.Therefore, for trace steam high-sensitivity measurement method in industrial process high concentrations of gas
There is notable demand with instrument.
Dew point analysis instrument is the capital equipment of current steam measurement, but dew point analysis instrument can not be applied to industrial corrosion
The on-line checking of trace steam in property gas.Infrared laser spectroscopy method is trace steam online measuring technique newest at present, its
Non-contact, longevity advantage is particularly suitable for industrial environment trace steam on-line measurement.Patent CN104280362A proposes a kind of
Superheated vapor laser spectrum on-line detecting system, for the middle-low alloy steels problem of hot environment steam spectral detection, pass through steam
Detection is detected while realize steam temperature while two absorption lines, realizes spectroscopic simultaneous temperature adjustmemt and vapour concentration
Accurate measurement.But the infrared laser spectroscopy technology based on single line analysis is needed to steam one not by the interference of background gas composition
Spectral line is isolated, this requirement is easier to meet under usual testing conditions, but under high concentration background gas, minor background gas divides
Sub- absorption line can also be detected to trace steam and interfered, this kind of in the near of steam spectral detection especially for NH3 and SO2
In the case that infrared spectral region has higher spectrum line density as background gas, measurement accuracy is by larger limitation.Meanwhile steam
And the main component of ambient air, limited by light path design, the steam interference of light path also can be to red outside sample area
Outer laser spectrometry is applied to trace steam measurement in industrial high-purity gas and impacted.
The content of the invention
It is an object of the invention to provide one kind to be directed to the highly sensitive detection of trace steam in industrial circle high-purity process gas
Infrared laser spectroscopy trace steam detecting system and its detection method, eliminate background gas spectrum and the interference of environment steam, it is full
Trace steam impurity on-line checking application demand in sufficient industrial process high concentrations of gas.
To achieve the above object, the invention provides following technical scheme:A kind of infrared laser spectroscopy trace steam detection
System, including infrared semiconductor laser, the light beam that the infrared semiconductor laser is sent are beamed into beam intensity ratio through beam splitter
Example is 1:1 detection light and reference light, the detection light and reference light incide detection absorption cell and with reference to absorption cell, institutes respectively
It is two multiple reflections optical absorption ponds of light path identical to state detection absorption cell and reference absorption cell, and the detection absorption cell is provided with
Air inlet and gas outlet, detection sample gas enters absorption cell by air inlet, and is flowed out by gas outlet, described with reference to close in absorption cell
The high-purity calibrating gas of background gas species identical with examining sample measuring device of Feng Youyi atmospheric pressure, detection light and reference light pass through
After absorption cell, opto-electronic conversion is carried out by the first photodetector and the second photodetector respectively, and send the signal to signal
Acquisition processing module obtains detecting spectral signal and reference spectra signal;System also includes signal generating circuit and semiconductor laser
Device control module, the signal generating circuit is respectively to semiconductor laser control module and signal acquisition process module output saw
Tooth ripple signal, the semiconductor laser control module drive the laser of the sawtooth signal and infrared semiconductor laser
Electric current is superimposed, and realizes that output wavelength continuously scans in setting wave-length coverage periodically;
And a kind of detection method detected using said system, comprise the following steps:
Spectral normalization, respectively with detection spectral signal S0And reference spectra signal R (n)0(n) top does not have gas absorption
N0Individual data point carries out average acquiring signal strength parameter value S0mAnd R0m, for detecting spectral signal S0And reference light (n)
Spectrum signal R0(n) normalization calculates, and obtains normalization detection spectral signal S (n) and reference spectra signal R (n):
Spectrum difference is offseted, and difference processing is carried out to normalization detection spectral signal S (n) and reference spectra signal R (n),
Obtain detecting spectral signal D (n) only:
D (n)=R (n)-S (n);
Spectral line linear fit, spectrum linear fitting is carried out to net detection spectral signal D (n), and fitting linear function is taken as Lip river
Hereby function, fitting function are for human relations:
Wherein, Φ0For direct current background, nLFor Lorentz half-breadth, n0It is the center of spectral line, A is steam target absorption line
Integration Absorption Line is strong, and A is directly proportional to vapour concentration;
Vapour concentration inverting, the strong A of calibration steam target absorption line integral Absorption Line is obtained first0:It will detect in absorption cell
It is filled with known steam concentration C0A standard atmospheric pressure steam calibration gas, record detection absorption cell calibration spectrum signal X0
(n), with calibration spectrum signal X0(n) top does not have the n that gas absorbs0Individual data point carries out average acquiring signal strength parameter value
X0m, for calibration spectrum signal X0(n) normalization calculates, and obtains normalizing calibration spectrum signal X (n):
There is no the data point fitting background signal (B of water vapor absorption using calibration spectrum signal (X (n)) both ends are normalized
(n)), fitting function is:
B (n)=a0+a1n+a2n2;
Wherein:a0、a1、a2For fitting parameter;
Normalization calibration spectrum signal X (n) subtracts fitting background signal B (n) and obtains net calibration spectrum signal (Y (n)):
Y (n)=X (n)-B (n)
Spectrum linear fitting is carried out to net calibration spectrum signal (Y (n)), fitting linear function is taken as Lorentzian, intended
Closing function is:
Wherein, Φ '0For net calibration spectrum signal direct current background, n'LFor net calibration spectrum signal spectrum Lorentz half-breadth,
n'0It is the center of net calibration spectrum signal spectrum, A0Steam calibration gas target absorption line integral Absorption Line is strong;
Utilize A0Sample gas reclaimed water can be obtained with the strong A ratio relations of steam target absorption line integral Absorption Line in detection sample gas
Vapour concentration C0, calibration relation is:
C is the vapour concentration data detected.
The technical effects of the invention are that:The present invention uses biabsorption pool structure, passes through light path and reference path
Spectral signal difference offsets, and eliminates the influence of high concentration background gas spectrum and absorption cell external environment steam, suppresses optical system
Common-mode noise, realize the highly sensitive detection of trace steam in high-concentration industrial gas.
Brief description of the drawings
Fig. 1 is the infrared laser spectroscopy trace gas detection system pie graph that the present invention is offseted based on double light path difference;
Fig. 2 is the infrared laser spectroscopy Trace gas detection data processing method stream that the present invention is offseted based on double light path difference
Cheng Tu;
Fig. 3 is the infrared laser spectroscopy Trace gas detection data processing method letter that the present invention is offseted based on double light path difference
Number figure.
Label in Fig. 1:1 infrared semiconductor laser, 2 semiconductor laser control modules, 3 signal generating circuits, 41 ×
2 fiber optic splitters, 5 first fiber collimating lenses, 6 first fiber collimating lenses, 7 air inlets, 8 detection absorption cells, 9 gas outlets,
10 heating tapes, 11 temperature sensors, 12 first photodetectors, 13 temperature controllers, 14 first LPF amplifying circuits, 17
With reference to absorption cell, 18 second photodetectors, 20 second LPF amplifying circuits, 21 signal acquisition process modules.
Embodiment
As shown in figure 1, a kind of infrared laser spectroscopy trace steam detecting system, including infrared semiconductor laser 1, it is described
The light beam that infrared semiconductor laser 1 is sent is beamed into light intensity ratio as 1 through beam splitter 4:1 detection light and reference light, it is described
Detection light and reference light incide detection absorption cell 8 and refer to absorption cell 17 respectively, described to detect absorption cell 8 and with reference to absorption cell
17 be two multiple reflections optical absorption ponds of light path identical, and the detection absorption cell 8 is provided with air inlet 7 and gas outlet 9, detects
Sample gas enters absorption cell by air inlet 7, and is flowed out by gas outlet 9, and an atmospheric pressure is sealed with the reference absorption cell 17
The high-purity calibrating gas of background gas species identical with examining sample measuring device, after detection light and reference light are by absorption cell, respectively
Opto-electronic conversion is carried out by the first photodetector 12 and the second photodetector 18, and sends the signal to signal acquisition process mould
Block 21 obtains detecting spectral signal and reference spectra signal;System also includes signal generating circuit 3 and semiconductor laser controls
Module 2, the signal generating circuit 3 is respectively to semiconductor laser control module 2 and the output saw of signal acquisition process module 21
Tooth ripple signal, the semiconductor laser control module 2 drive the laser of the sawtooth signal and infrared semiconductor laser 1
Streaming current is superimposed, and realizes that output wavelength continuously scans in setting wave-length coverage periodically.
Pass through temperature and electric current control using near-infrared semiconductor laser as detection light source, semiconductor laser control module
System by the output center wavelength of semiconductor laser be tuned to steam target absorption core, setting signal occur circuit, with
Sawtooth signal caused by the signal generating circuit, which is superimposed upon in semiconductor laser control module, is setting its output wavelength
Wavelength range periodically is continuously scanned, and the laser beam beam splitting of semiconductor laser output is divided into for detection by fiber optic splitter
Light and reference light
Detection light and reference light by photodetector by carrying out opto-electronic conversion and LPF amplification respectively after absorption cell
Obtain detecting spectral signal S by analog-to-digital conversion and signal acquisition0And reference spectra signal R (n)0(n), such as Fig. 3 (a), (b) institute
Show, wherein n counts for Temporal Sampling.Detect spectral signal S0(n) water vapor absorption spectral signal, inspection in detection absorption cell are included
Survey the outer water vapor absorption spectral signal of absorption cell, background gas absorption spectrum signal, and optical noise etc.;Reference spectra signal R
(n) include with reference to water vapor absorption spectral signal, background gas absorption spectrum signal outside absorption cell, and optical noise etc..
Further, heating tape 10 and temperature sensor are mounted on the detection absorption cell 8 and reference absorption cell 17
11, temperature controller 13 will detect absorption cell 8 and the temperature control with reference to absorption cell 17 by heating tape 10 and temperature sensor 11
System is more than moisture condensation temperature, to prevent from detecting absorption cell 8 and with reference to the moisture condensation in absorption cell 17, influence testing result
Accuracy.As the preferred embodiments of the present invention, temperature controller 13 will detect absorption cell 8 and the temperature with reference to absorption cell 17
Control is at 50 DEG C.
Further, the detection absorption cell 8 and the external circuits with reference to absorption cell 17 are also consistent, with further true
Protect the accuracy of testing result.
Further, it is respectively equipped between first, second photodetector 12,18 and signal acquisition process module 21
First LPF amplifying circuit 14 and the second LPF amplifying circuit 20.The detection light is emitted after absorption cell 8 after testing
Output light is formed, the output light reaches converted electrical number after the first photodetector 12, first photodetector 12
It is communicated to the first LPF amplifying circuit 14 progress signal filter and amplification, the first LPF amplification to export electric signal
The output signal of circuit 14 carries out data acquisition as detection spectral signal by signal acquisition process module 21;The reference light warp
Outgoing forms output light after detection absorption cell 17, and the output light reaches converted electrical number after the second photodetector 18, described
The output electric signal of second photodetector 18 is communicated to the second LPF amplifying circuit 20 progress signal filter and amplification, institute
The output signal for stating the first LPF amplifying circuit 20 carries out data acquisition as reference light by signal acquisition process module 21
Spectrum signal.
Preferably, the beam splitter 4 is 1 × 2 fiber optic splitter, and the detection light and reference light that the beam splitter 4 is sent are divided
Do not enter detection absorption cell 8 after the first optical fiber collimator 5 and the second optical fiber collimator 6 collimation and refer to absorption cell 9.
The infrared laser spectroscopy trace steam detecting system offseted in the present invention based on double light path difference is structurally characterized in that:
The system includes detection absorption cell 8 and refers to absorption cell 17, detects absorption cell 8 and has identical light with reference to absorption cell 17
Road and light path, the air inlet 7 for detecting absorption cell 8 samples gas circuit with detection sample gas and is connected, with reference to being sealed with one in absorption cell 17
Standard atmospheric pressure background gas;
The laser beam that the semiconductor laser 1 exports is by 1 through fiber coupling in 1 × 2 fiber optic splitter:1 light intensity
Ratio beam splitting is detection light and reference light;
Heating tape 10 and temperature sensor 11 are installed on the detection absorption cell 8 and reference absorption cell 17, by temperature control
Device 13 processed will detect absorption cell 8 and with reference to the temperature control of absorption cell 17 in identical temperature.
A kind of detection method detected using said system, comprises the following steps:
Step 1:Spectral normalization, respectively with detection spectral signal S0And reference spectra signal R (n)0(n) top does not have gas
The n that body absorbs0Individual data point carries out average acquiring signal strength parameter value S0mAnd R0m, for detecting spectral signal S0(n) and
Reference spectra signal R0(n) normalization calculates, and obtains normalization detection spectral signal S (n) and reference spectra signal R (n):
As shown in Fig. 3 (c), (d), normalization detection spectral signal (S (n)) equally includes steam in detection absorption cell and inhaled
The collection of letters number, the outer water vapor absorption signal of detection absorption cell, background gas absorption signal, and optical noise etc.;Normalize reference light
Spectrum signal (R (n)) equally includes with reference to water vapor absorption signal, background gas absorption signal outside absorption cell, and optical noise
Deng;
Step 2:Spectrum difference is offseted, and difference is carried out to normalization detection spectral signal S (n) and reference spectra signal R (n)
Processing, obtains detecting spectral signal D (n) only:
D (n)=R (n)-S (n);
As shown in Fig. 3 (e), spectral signal (D (n)) is detected only and only includes water vapor absorption spectrum letter in detection absorption cell
Number;
Step:3:Spectral line linear fit, spectrum linear fitting is carried out to net detection spectral signal D (n), is fitted linear function
Lorentzian is taken as, fitting function is:
Wherein, Φ0For direct current background, nLFor Lorentz half-breadth, n0It is the center of spectral line, A is steam target absorption line
Integration Absorption Line is strong, and A is directly proportional to vapour concentration;
Step 4:Vapour concentration inverting:
The strong A of calibration steam target absorption line integral Absorption Line is obtained first0:It is dense by known steam is filled with detection absorption cell
Spend C0A standard atmospheric pressure steam calibration gas, record detection absorption cell calibration spectrum signal X0(n), believed with calibration spectrum
Number X0(n) top does not have the n that gas absorbs0Individual data point carries out average acquiring signal strength parameter value X0m, for calibrating light
Spectrum signal X0(n) normalization calculates, and obtains normalizing calibration spectrum signal X (n):
There is no the data point fitting background signal B (n) of water vapor absorption using calibration spectrum signal X (n) both ends are normalized, intend
Closing function is:
B (n)=a0+a1n+a2n2;
Wherein:a0、a1、a2For fitting parameter;
Normalization calibration spectrum signal X (n) subtracts fitting background signal B (n) and obtains net calibration spectrum signal Y (n):
Y (n)=X (n)-B (n)
Spectrum linear fitting is carried out to net calibration spectrum signal Y (n), fitting linear function is taken as Lorentzian, is fitted
Function is:
Wherein, Φ '0For net calibration spectrum signal direct current background, n'LFor net calibration spectrum signal spectrum Lorentz half-breadth,
n'0It is the center of net calibration spectrum signal spectrum, A0Steam calibration gas target absorption line integral Absorption Line is strong;
Then, A is utilized0Sample can be obtained with the strong A ratio relations of steam target absorption line integral Absorption Line in detection sample gas
Steam concentration C in gas0, calibration relation is:
C is the vapour concentration data detected.
The present invention uses biabsorption pool structure, is offseted by the spectral signal difference of light path and reference path, eliminates
The influence of high concentration background gas spectrum and absorption cell external environment steam, suppress optical system common-mode noise, realize high concentration work
The highly sensitive detection of trace steam in industry gas.
Claims (5)
- A kind of 1. detection method of infrared laser spectroscopy trace steam detecting system, it is characterised in that:Swash including infrared semiconductor Light device(1), the infrared semiconductor laser(1)The light beam sent is through beam splitter(4)Light intensity ratio is beamed into as 1:1 detection Light and reference light, the detection light and reference light incide detection absorption cell respectively(8)With with reference to absorption cell(17), the detection Absorption cell(8)With with reference to absorption cell(17)For two multiple reflections optical absorption ponds of light path identical, the detection absorption cell(8) Provided with air inlet(7)And gas outlet(9), detect sample gas and pass through air inlet(7)Into absorption cell, and by gas outlet(9)Outflow, institute State and refer to absorption cell(17)In be sealed with the high-purity Standard Gases of background gas species identical with examining sample measuring device of atmospheric pressure After body, detection light and reference light are by absorption cell, respectively by the first photodetector(12)With the second photodetector(18)Enter Row opto-electronic conversion, and send the signal to signal acquisition process module(21)Obtain detecting spectral signal and reference spectra signal; System also includes signal generating circuit(3)With semiconductor laser control module(2), the signal generating circuit(3)Respectively to Semiconductor laser control module(2)And signal acquisition process module(21)Export sawtooth signal, the semiconductor laser Control module(2)By the sawtooth signal and infrared semiconductor laser(1)Laser drive current superposition, realize output wave Grow and continuously scanned in setting wave-length coverage periodically;Comprise the following steps:Step 1:Spectral normalization, respectively with detection spectral signalWith reference spectra signalTop does not have gas absorption 'sIndividual data point carries out average acquiring signal strength parameter valueWith, for detecting spectral signalAnd reference light Spectrum signalNormalization calculates, and obtains normalization detection spectral signalWith reference spectra signal:,;Step 2:Spectrum difference is offseted, and spectral signal is detected to normalizationWith reference spectra signalCarry out difference processing, Obtain detecting spectral signal only:;Step 3:Spectral line linear fitting, to net detection spectral signalSpectrum linear fitting is carried out, fitting linear function is taken as Lorentzian, fitting function are:;Wherein,For direct current background,For Lorentz half-breadth,It is the center of spectral line,It is steam target absorption line product Divide Absorption Line strong,It is directly proportional to vapour concentration;Step 4:Vapour concentration inverting:It is strong that calibration steam target absorption line integral Absorption Line is obtained first:Known vapour concentration will be filled with detection absorption cell A standard atmospheric pressure steam calibration gas, record detection absorption cell calibration spectrum signal, with calibration spectrum signalTop does not have what gas absorbedIndividual data point carries out average acquiring signal strength parameter value, for calibration spectrum SignalNormalization calculates, and obtains normalizing calibration spectrum signal:;Using normalizing calibration spectrum signalBoth ends do not have the data point fitting background signal of water vapor absorption, it is fitted letter Number is:;Wherein:、、For fitting parameter;Normalize calibration spectrum signalSubtract fitting background signalObtain net calibration spectrum signal:To net calibration spectrum signalSpectrum linear fitting is carried out, fitting linear function is taken as Lorentzian, fitting function For:Wherein,For net calibration spectrum signal direct current background,For net calibration spectrum signal spectrum Lorentz half-breadth,It is net The center of calibration spectrum signal spectrum,Steam calibration gas target absorption line integral Absorption Line is strong;Then, utilizeIt is strong with steam target absorption line integral Absorption Line in detection sample gasRatio relation can be obtained in sample gas Vapour concentration C, calibration relation are:;C is the vapour concentration data detected;Steps 1 and 2, the n appeared in 3,4 are all Temporal Sampling points.
- 2. detection method according to claim 1, it is characterised in that:The detection absorption cell(8)With with reference to absorption cell (17)On be mounted on heating tape(10)And temperature sensor(11), temperature controller(13)Pass through heating tape(10)Passed with temperature Sensor(11)Absorption cell will be detected(8)With with reference to absorption cell(17)Temperature control more than moisture condensation temperature.
- 3. detection method according to claim 1, it is characterised in that:The detection absorption cell(8)With with reference to absorption cell (17)External circuits be also consistent.
- 4. detection method according to claim 1, it is characterised in that:First, second photodetector(12、18)With Signal acquisition process module(21)Between be respectively equipped with the first LPF amplifying circuit(14)Amplify electricity with the second LPF Road(20).
- 5. detection method according to claim 1, it is characterised in that:The beam splitter(4)For 1 × 2 fiber optic splitter, institute State beam splitter(4)The detection light and reference light sent is respectively through the first optical fiber collimator(5)With the second optical fiber collimator(6)Collimation Enter detection absorption cell afterwards(8)With with reference to absorption cell(17).
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CN108827906A (en) * | 2018-04-20 | 2018-11-16 | 合肥工业大学 | A kind of near infrared spectrum multicomponent gas on-line detecting system and method |
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