CN101782514B - Online monitoring device for concentration of hydrogen sulfide by laser - Google Patents
Online monitoring device for concentration of hydrogen sulfide by laser Download PDFInfo
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- CN101782514B CN101782514B CN2009102300207A CN200910230020A CN101782514B CN 101782514 B CN101782514 B CN 101782514B CN 2009102300207 A CN2009102300207 A CN 2009102300207A CN 200910230020 A CN200910230020 A CN 200910230020A CN 101782514 B CN101782514 B CN 101782514B
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Abstract
The invention relates to a device for detecting the concentration change of hydrogen sulfide gas in natural gas before and after the natural gas passes through a natural gas desulfurizer, and belongs to the fields of optical spectroscopy and electronics, in particular to a device for monitoring the concentration of the hydrogen sulfide gas in the natural gas by utilizing the characteristics of narrow line width, tenability and the like of a diode laser by adopting the tunable diode laser absorption spectroscopy (TDLAS). The device mainly comprises a field check unit cabinet and a signal processing unit cabinet, wherein the field check unit cabinet is provided with a gas treatment device and an optical processing device inside; and the signal processing unit cabinet is provided with a laser modulation unit, a signal processing unit and a display operation unit inside. The device detects the concentration of H2S in the natural gas on line in real time by adopting absorption spectrum technology and laser wavelength modulation technology, and generates audible and visual alarm.
Description
One, technical field
The present invention relates to a kind of device that sulfureted hydrogen gas concentration changes in the rock gas of natural-gas desulfurizer front and back that detects.Belong to spectroscopy and person in electronics, specifically adopt tunable semiconductor laser spectrum (TDLAS) technology, utilize the narrow linewidth of diode laser and characteristic such as tunable to carry out online monitoring device for concentration of hydrogen sulfide by laser before and after the natural-gas desulfurizer.
Two, background technology
At present oil gas field is under development runs into many rock gases and contains H
2The block that S is very high.Particularly the oil field height contains H
2The oil well associated gas of S.Because adopt and draw oily technology, flow process is not airtight, causes the work on the spot environment extremely abominable, the operator on duty has big life security hidden danger.Simultaneously, H
2S is a hazardous medium in the gas gathering and transportation processing procedure, can cause the heavy corrosion of pipeline and equipment under the situation that has water to exist, and especially sulfide belongs to high harm medium, and the serious harm personal safety is one of environomental pollution source of necessary strict control.Therefore the natural-gas desulfurizer that various principles occurred, but the desulfurized effect of how to evaluate natural-gas desulfurizer, this just need carry out the sulfureted hydrogen gas concentration real time on-line monitoring to the rock gas before and after the natural-gas desulfurizer.The present domestic H that is used for
2The method of S gas concentration monitoring is to adopt the method for sample examination mostly, this method must just can detect by sampling and pre-service, thereby the accuracy of measured value and real-time are reduced, its technological means is a chemical method, mainly contains iodimetric titration, methylene blue laws, lead acetate reaction rate method etc.Optical detective technology is compared major advantage with classic method be high selectivity and high sensitivity, can be in real time, dynamically, monitor fast, and system operation cost is low etc.
Three, summary of the invention
The purpose of this invention is to provide online monitoring device for concentration of hydrogen sulfide by laser before and after a kind of natural-gas desulfurizer, realize that online detection rock gas through the content of the hydrogen sulfide gas before and after the desulfurization and carry out early warning, guarantees the safe operation of gas gathering and transportation pipe network.
Technical scheme of the present invention realizes in the following manner:
Online monitoring device for concentration of hydrogen sulfide by laser is divided into concentration of hydrogen sulfide in high concentration hydrogen sulfide gas laser on-Line Monitor Device of using between 100～10000ppm and the low dense hydrogen sulfide gas on-Line Monitor Device used below the concentration of hydrogen sulfide 100ppm.
Online monitoring device for concentration of hydrogen sulfide by laser mainly is made up of on-site detecting unit rack and two unit cabinet of signal processing unit rack, and the on-site detecting unit rack is installed in the hazardous location, adopts the optical signal transmission data, and is safe and reliable.The signal processing unit rack is installed in the pulpit, functions such as the analyzing and testing of realization gas, display alarm.
Described on-site detecting unit rack is divided into two kinds of high concentration and low concentration on-site detecting unit racks.
In the high concentration on-site detecting unit rack gas treatment equipment and optical processing system are housed.Wherein gas treatment equipment comprises dry filter device, decompression stable-pressure device, measuring apparatus, gas sampler.Optical processing system comprises automatic focus lens and fiber coupler.Detected gas in the gathering line is passed through
Stainless-steel tube introduce on the gas path joint of on-site detecting unit rack, detected gas enters gas sampler through decompression voltage stabilizing, dry filter after handling, two ends at gas sampler are equipped with automatic focus lens and fiber coupler respectively, laser enters gas sampler by Optical Fiber Transmission after the line focus of automatic focus lens, be coupled in the single-mode fiber by opposite window outgoing and by fiber coupler, be transferred to demodulation and processing that the signal processing unit rack carries out signal, obtain detected gas concentration in real time.
In the low concentration on-site detecting unit rack gas treatment equipment and optical processing system are housed.Wherein gas treatment equipment comprises dry filter device, decompression stable-pressure device, measuring apparatus, and optical processing system comprises automatic focus lens, repeatedly reflection tank and fiber coupler.Detected gas in the gathering line is passed through
Stainless-steel tube introduce on the gas path joint of on-site detecting unit rack, detected gas enters the repeatedly reflection tank that has transparent window through decompression voltage stabilizing, dry filter after handling.One end of reflection tank has air admission hole, and the other end has venthole; Repeatedly one side secondary mirror is respectively installed in the inner air admission hole of reflection tank both sides, the other end is equipped with principal reflection mirror, the both sides of venthole have the laser of assembling transparent window film and go into perforation and perforation hole, and tested gas enters repeatedly reflection tank from air admission hole, leaves reflection tank from venthole.Secondary mirror and principal reflection mirror are the spherical mirror that radius is R, and the relative distance of placement is R, and laser enters from going into perforation, and repeatedly reflection is penetrated from perforation hole again between secondary mirror and principal reflection mirror.By adjusting the wherein position of a secondary mirror, this secondary mirror is rotated to another secondary mirror direction, and the spot number that projects on the principal reflection mirror increases, and can constantly adjust the increase light path, maximum light path can reach 30m, reaches the purpose that improves systematic survey sensitivity.Laser penetrates from perforation hole and is coupled to the single-mode fiber by fiber coupler, is transferred to demodulation and processing that the signal processing unit rack carries out signal, obtains detected gas concentration in real time.
The signal processing unit rack of the sulfuretted hydrogen laser on-Line Monitor Device of high concentration and low concentration is basic identical, and Laser Modulation unit, signal processing unit, display unit etc. are housed in its cabinet.Adopting centre wavelength in the Laser Modulation unit is that the near infrared dfb semiconductor laser instrument of 1576nm is as H
2The detection laser source of S, utilize laser temperature and current control module with the laser instrument output center wavelength be tuned near the 1576.37nm H
2S absorbs the line center, and the 50Hz sawtooth signal that signal generating circuit produces is superimposed upon on the drive current of laser instrument and makes the slow scanned H of optical maser wavelength
2S absorption lines of gases, signal generating circuit produce on the drive current that the 5KHz sine wave signal is superimposed upon laser instrument simultaneously carries out high frequency modulated to laser output wavelength.Laser is by optical fiber the gas sampler in the detecting unit rack (or repeatedly reflection tank) of reaching the spot, there is the micro-optical sensor of link input single-mode fiber and output single-mode fiber at gas sampler (or repeatedly reflection tank) two ends, light signal through gas absorption passes through the output single-mode fiber to the signal processing unit rack, the laser that absorbs enters gas and demarcates the pond, and gas is demarcated the H that has been full of normal concentration under the atmospheric pressure in the pond
2S gas is used for the real-time calibration to the detection absorption signal, and contrast standard gas wavelength and actual measurement laser wavelength, by laser temperature and current control module optical maser wavelength is drifted about and carries out the self-adaptation adjustment, realizes H
2The locking of S gas near infrared absorption line.Accept by infrared photoelectric detector through the laser signal of demarcating the pond, after opto-electronic conversion, export electric signal, one the tunnel send lock-in amplifier to carry out second harmonic signal detects, the reference signal of lock-in amplifier comes from the sinusoidal modulation signal that described signal generating circuit produces, the data acquisition of the direct feed signals processing unit in another road, handle and control module, at first carry out digital low-pass filtering, then it is made linear fit as the laser intensity signal, the second harmonic signal of lock-in amplifier output utilizes the match light intensity signal to carry out normalized to eliminate the influence that light-intensity variation detects concentration.Second harmonic signal after the normalization obtains one through progressive mean repeatedly and detects absorption spectra, the standard absorption signal that utilizes the gas of preserving in advance to demarcate the pond carries out the light path IC that the match of minimum secondary product obtains the check point hydrogen sulfide gas to the absorption spectra that detects, or obtains light path average gas concentration divided by total optical path.Signal processing unit is sent to the concentration value of detected gas on the LCD of display unit, carries out real-time display density value and concentration curve on liquid crystal display, and realizes sound and light alarm.Adopt 2 optical fiber to be connected between on-site detecting unit rack and the signal processing unit rack, can realize safe and reliable operation.
The present invention has adopted advanced tunable infrared diode laser as light source, utilizes absorption spectrum technology and optical maser wavelength modulation technique real-time online to detect H in the rock gas
2S concentration, and carry out sound and light alarm.Overcome the traditional experiment chamber and detected H
2The S concentration sensitivity is low, accuracy is low, the periodic calibrating maintenance is big, cost is high and can not realize shortcomings such as precise real-time detection.The present invention has the following advantages:
1, highly sensitive: instrument adopts on hardware that length scanning, high frequency modulated, phase-locked amplification, background offset, higher hamonic wave input and balance Detection Techniques, improved the detection sensitivity of this technology effectively, monitoring sensitivity is higher than the sensitivity index of other sensor far away less than the ppm magnitude.
2, accuracy: utilize the absorption line of molecule to realize measurement, eliminated the interference of other any gas, realized accurate measurement to its concentration.
3, rapidity: the wavelength tuning limit of laser instrument is about 1ms, that is to say, the fastest concentration value of a ms measurement of realizing.
4, reliability:, can trust fully aspect the reliability of life-span and performance because use is employed laser instrument and other parts in the optical communication.
5, security: a remarkable advantages near infrared spectrum district is exactly to mate with the low loss window of optical fiber, and the single mode Si optical fiber of this instrument utilization commercialization transmits at a distance, adopts optical fiber transmission signal to guarantee the essential safety of gas gathering and transportation station field device.
6, demarcation is convenient and swift: need not designing from calibration system of gas calibration.
Four, description of drawings
Fig. 1 is a structural representation of the present invention
Fig. 2 is the wavelength-modulated systematic schematic diagram
Fig. 3 is repeatedly the reflection tank structural drawing
Fig. 4 is the tuning live width of infrared tuning diode laser instrument and the relation of absorption peak width
Fig. 5 is the second-harmonic detection principle schematic
Fig. 6 is on-site detecting unit rack process of gas path figure
Five, embodiment
For further disclosing technical scheme of the present invention,, elaborate by embodiment below in conjunction with Figure of description.
Among Fig. 1: 1, the Laser Modulation unit cabinet of signal processing unit rack, 2, main power switch, 3, gas is demarcated the pond, 4, general supply socket, 5, laser output flange, 6, laser input flange, 7, electrical signal output interface, 8, fan, 9, D.C. regulated power supply, 10, semiconductor laser current control module, 11, semiconductor laser temperature control modules, 12,1576nm near infrared semiconductor laser, 13, signal generator, 14, lock-in amplifier, above element are installed in the Laser Modulation unit cabinet of signal processing unit rack.15, output single-mode fiber, 24, the input single-mode fiber.Following element is installed in the site disposal unit cabinet, and 16, the site disposal unit cabinet, 17, the input optical fibre flange, 18, input optical fibre, 19, the automatic focus lens, 20, gas sampler (repeatedly reflection tank), 21, fiber coupler, 22, output optical fibre, 23, the output optical fibre flange.
It is that the near infrared semiconductor laser 12 of 1576nm is as H that the present invention adopts centre wavelength as shown in Figure 1, 2
2The detection laser light source of S, utilize laser temperature control module 11 and current control module 10 output center wavelengths be tuned near the 1576.37nm H
2S absorbs the line center, and the 50Hz sawtooth signal that signal generator 13 produces is superimposed upon on the drive current of laser instrument and makes the slow scanned H of optical maser wavelength
2S absorption lines of gases, signal generator 13 produce on the drive current that the 5KHz sine wave signal is superimposed upon laser instrument simultaneously carries out high frequency modulated to optical maser wavelength.Laser is by laser output flange 5 and output single-mode fiber 15, be transferred in the field check unit cabinet 16 laser input flange 17, input optical fibre 18 is delivered to automatic focus lens 19 places to laser, laser enters in the gas sampler (repeatedly reflection tank) 20 that gas to be measured is housed through automatic focus, by the fiber coupler 21 that is installed in gas sampler (repeatedly reflection tank) 20 other ends laser coupled in output optical fibre 22, the output optical fibre flange 23 by being installed in the on-site detecting unit rack combines with input single-mode fiber 24 sends the laser that absorbed back in the Laser Modulation unit cabinet in the signal processing unit rack laser input flange 6 places.The laser that absorbed enters gas and demarcates pond 3, and gas is demarcated the H that is full of an atmospheric pressure normal concentration in the pond 3
2S gas is used to check the real-time calibration of absorption signal, and contrast standard gas wavelength and actual measurement laser wavelength, carries out the self-adaptation adjustment by laser temperature control module 11 and 10 pairs of optical maser wavelengths drifts of current control module, realizes H
2The locking of S gas near infrared absorption line.Accept by infrared photoelectric detector through the laser signal of demarcating pond 3, after opto-electronic conversion, export electric signal, one the tunnel send lock-in amplifier 14 to carry out second harmonic signal detects, the reference signal of lock-in amplifier 14 comes from the sinusoidal modulation signal that described signal generating circuit produces, the data acquisition of the direct feed signals processing unit in another road, handle and control module, at first carry out digital low-pass filtering, then it is made linear fit as the laser intensity signal, the second harmonic signal of lock-in amplifier 14 outputs utilizes the match light intensity signal to carry out normalized to eliminate the influence that light-intensity variation detects concentration.Second harmonic signal after the normalization obtains one through progressive mean repeatedly and detects absorption spectra, the standard absorption signal that the gas that utilization is preserved is in advance demarcated pond 3 carries out the match of minimum secondary product and deducts the light path IC that the calibration gas concentration obtains gas the absorption spectra that detects, or obtains light path average gas concentration divided by total optical path.Signal processing unit is sent to the concentration value of detected gas on the LCD of display unit, carries out real-time display density value and concentration curve on liquid crystal display, and realizes sound and light alarm.
Among Fig. 3,1 '-air admission hole, 2 '-holder, 3 ' A-secondary mirror, 4 ' B-secondary mirror, 5 '-the column type cloche, 6 '-principal reflection mirror, 7 '-the inlet lens, 8 '-venthole, 9 '-the outlet lens, 10 '-holder, 11 '-4 pull bars.
Laser sees through inlet lens 7 ' be mapped on secondary mirror 4 ' B, secondary mirror 4 ' B with beam reflection focus on principal reflection mirror 6 ' on, again by principal reflection mirror 6 ' with beam reflection to secondary mirror 3 ' A, secondary mirror 3 ' A light beam by outlet lens 9 ' reflect away.The position of modulation secondary mirror 3 ' A makes secondary mirror 3 ' A rotate around the axle perpendicular to paper plane, project principal reflection mirror 6 ' on spot number increase, constantly adjust light path.Gas enters into repeatedly reflection tank by air intake opening 1, from venthole 8 ' go out.
50MHz is tuning live width among Fig. 4, the 500MHz correspondence be the absorption peak width.
A is direct absorption spectrum among Fig. 5, and B is the first harmonic spectral line, and C is the second harmonic spectral line.
In Fig. 6,16-on-site detecting unit rack, 1 "
The threading inlet union, 2 " two pass ball valves, 3 " filtrator, 4 " tensimeter; 5 "-reduction valve, 6 " sample flow meter, 7 " sampling thief imported valve, 20-gas sampler, 8 " sampling thief outlet valve, 9 " safety valve, 10 " threading outlet connection, 11 " safety vent pipeline.
Detected gas in the natural gas line is passed through
Stainless-steel tube introduce on-site detecting unit rack 16
Inlet union 1 " on; detected gas " enters filtrator 3 " through two pass ball valves 2 detected gas is filtered; tensimeter 4 " shows the gaseous tension after filtering, the set pressure that detected gas was through reduction valve 5 after dry filter was handled " handling; sample flow meter 6 " metering is by gas admittance valve 7 " enters gas sampler 20 then; during the gases in the gas sampler 20 " are discharged to blow-down pipe 11 " by sampling thief outlet valve 8; if the interior pressure of trunk line surpasses safety valve 9 simultaneously ", during safety valve 9 " can be opened; gas directly enters blow-down pipe 11 ", " discharge by the outlet connection 10 of on-site detecting unit rack 16 then.
Claims (2)
1. online monitoring device for concentration of hydrogen sulfide by laser is mainly used in the device of hydrogen sulfide gas content in the rock gas that detects before and after the natural-gas desulfurizer, it is characterized in that
A, high-concentration hydrogen sulfide laser on-Line Monitor Device are by high-concentration hydrogen sulfide on-site detecting unit rack, and signal Processing rack two parts are formed.High-concentration hydrogen sulfide on-site detecting unit rack profile is a rectangle, and gas treatment equipment and optical processing system are housed in the cabinet; Wherein gas treatment equipment comprises dry filter device, decompression stable-pressure device, measuring apparatus, gas sampler; Optical processing system comprises automatic focus lens and fiber coupler; Detected gas in the gathering line is passed through
Stainless-steel tube introduce in the high-concentration hydrogen sulfide on-site detecting unit rack, link to each other with the joint of high-concentration hydrogen sulfide on-site detecting unit rack gas circuit, detected gas is through the decompression voltage stabilizing, dry filter enters gas sampler after handling, two ends at gas sampler are equipped with automatic focus lens and fiber coupler respectively, laser enters an end of gas sampler after the line focus of automatic focus lens by Optical Fiber Transmission, be coupled in the single-mode fiber by the window outgoing of the gas sampler other end and by fiber coupler, be transferred to demodulation and processing that the signal processing unit rack carries out signal, obtain detected gas concentration in real time.
B, low concentration hydrogen sulphide laser on-Line Monitor Device are by low concentration hydrogen sulphide on-site detecting unit rack, and signal Processing rack two parts are formed.Low concentration hydrogen sulphide on-site detecting unit rack is made as rectangle: gas treatment equipment and optical processing system are housed in the cabinet; Wherein gas treatment equipment comprises dry filter device, decompression stable-pressure device, measuring apparatus, and optical processing system comprises automatic focus lens, repeatedly reflection tank and fiber coupler; Detected gas in the gathering line is passed through
Stainless-steel tube introduce in the low concentration hydrogen sulphide on-site detecting unit rack, link to each other with the joint of low concentration hydrogen sulphide on-site detecting unit rack gas circuit, detected gas enters the repeatedly reflection tank that has transparent window after through decompression voltage stabilizing, dry filter processing; Repeatedly an end of reflection tank has air admission hole, and the other end has venthole; Repeatedly one side secondary mirror is respectively installed in the inner air admission hole of reflection tank both sides, the other end is equipped with principal reflection mirror, the both sides of venthole have the laser of assembling transparent window film and go into perforation and perforation hole, and detected gas enters repeatedly reflection tank from air admission hole, leaves repeatedly reflection tank from venthole; Two sides secondary mirror and principal reflection mirror are the spherical mirror that radius is R, and the relative distance that principal reflection mirror and two sides secondary mirror are placed is R, and laser enters from going into perforation, and repeatedly reflection is penetrated from perforation hole again between two sides secondary mirror and principal reflection mirror; By adjusting the wherein position of a secondary mirror, this secondary mirror is rotated to another secondary mirror direction, the spot number that projects on the principal reflection mirror increases, can constantly adjust the increase light path, improve the sensitivity of systematic survey, laser penetrates from perforation hole and is coupled to the single-mode fiber by fiber coupler, is transferred to demodulation and processing that the signal processing unit rack carries out signal, obtains detected gas concentration in real time.
2. online monitoring device for concentration of hydrogen sulfide by laser according to claim 1 is characterized in that being equipped with in the signal processing unit rack Laser Modulation unit, signal generating circuit, signal processing unit, display unit etc.; Adopting centre wavelength in the Laser Modulation unit is the detection laser source of the near infrared dfb semiconductor laser instrument of 1576nm as sulfuretted hydrogen, utilize laser temperature and current control module with the laser instrument output center wavelength be tuned near the 1576.37nm hydrogen sulfide absorption line center, the 50Hz sawtooth signal that signal generating circuit produces is superimposed upon the absorption line that makes the slow scanned hydrogen sulfide gas of optical maser wavelength on the driving circuit of laser instrument, and signal generating circuit produces simultaneously on the driving circuit that the 5KHz sine wave signal is superimposed upon laser instrument laser output wavelength is carried out high frequency modulated; Laser is by gas sampler in the optical fiber arrival high-concentration hydrogen sulfide on-site detecting unit rack or the repeatedly reflection tank in the low concentration hydrogen sulphide on-site detecting unit rack, gas sampler or repeatedly the reflection tank two ends micro-optical sensor that connects input single-mode fiber and output single-mode fiber is arranged, the light signal of output single-mode fiber output process gas absorption is to the signal processing unit rack, laser through surveyed area enters gas demarcation pond, gas is demarcated the hydrogen sulfide gas that has been full of normal concentration under the atmospheric pressure in the pond, be used for detecting the real-time calibration of absorption signal, and contrast standard gas wavelength and actual measurement laser wavelength, by laser temperature and current control module the self-adaptation adjustment is carried out in the optical maser wavelength drift, realized the locking of hydrogen sulfide gas near infrared absorption line; The laser signal of demarcating the pond through gas is received by infrared photoelectric detector, after opto-electronic conversion, export electric signal, one the tunnel send lock-in amplifier to carry out second harmonic signal detects, the reference signal of lock-in amplifier comes from the sinusoidal modulation signal that described signal generating circuit produces, the data acquisition of the direct feed signals processing unit in another road, handle and control module, at first carry out digital low-pass filtering, then it is made linear fit as the laser intensity signal, the second harmonic signal of lock-in amplifier output utilizes match laser intensity signal to carry out normalized to eliminate the influence that light-intensity variation detects concentration; Second harmonic signal after the normalization obtains one through progressive mean repeatedly and detects absorption spectra, and the standard absorption signal that utilizes the gas of preserving in advance to demarcate the pond carries out the light path IC that the match of minimum secondary product obtains the check point hydrogen sulfide gas to detecting absorption spectra; Signal processing unit is sent to the concentration value of detected gas on the LCD of display unit, carries out real-time display density value and concentration curve on liquid crystal display, and realizes sound and light alarm; All adopt optical fiber to be connected between high-concentration hydrogen sulfide on-site detecting unit rack and the signal processing unit rack or between low concentration hydrogen sulphide on-site detecting unit rack and the signal processing unit rack, can realize safe and reliable operation.
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| US10156516B2 (en) | 2015-01-27 | 2018-12-18 | Arkema France | Portable device for the in-line measurement of the hydrogen sulfide concentration of an off-gas |
| EP3488225A4 (en) * | 2016-07-25 | 2020-03-04 | MKS Instruments, Inc. | Gas measurement system |
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|---|---|
| CN101782514A (en) | 2010-07-21 |
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