CN102374979B - Petroleum-type pollutant detection system and detection method - Google Patents
Petroleum-type pollutant detection system and detection method Download PDFInfo
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- CN102374979B CN102374979B CN201010248795.XA CN201010248795A CN102374979B CN 102374979 B CN102374979 B CN 102374979B CN 201010248795 A CN201010248795 A CN 201010248795A CN 102374979 B CN102374979 B CN 102374979B
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- 238000001514 detection method Methods 0.000 title claims abstract description 40
- 239000003344 environmental pollutant Substances 0.000 title claims abstract description 30
- 231100000719 pollutant Toxicity 0.000 title claims abstract description 30
- 238000012545 processing Methods 0.000 claims abstract description 22
- 230000003287 optical effect Effects 0.000 claims description 19
- 230000005284 excitation Effects 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 4
- 239000002283 diesel fuel Substances 0.000 claims description 3
- 230000004907 flux Effects 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 239000010779 crude oil Substances 0.000 claims description 2
- 239000000295 fuel oil Substances 0.000 claims description 2
- 239000003502 gasoline Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000010687 lubricating oil Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 238000012544 monitoring process Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000001499 laser induced fluorescence spectroscopy Methods 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 20
- 229910001220 stainless steel Inorganic materials 0.000 description 9
- 239000010935 stainless steel Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000003321 amplification Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002480 mineral oil Substances 0.000 description 3
- 235000010446 mineral oil Nutrition 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 241000218606 Pinus contorta Species 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000002795 fluorescence method Methods 0.000 description 2
- 238000004848 nephelometry Methods 0.000 description 2
- 235000000673 shore pine Nutrition 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000000192 social effect Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a detection system and a detection method of petroleum-type pollutants. The detection system comprises an emitting unit, a receiving unit, a reference unit and a signal processing unit. The emitting unit is used for emitting laser signals, and transmitted light signals and reflected light signals are outputted; an input terminal of the reference unit receives the transmitted light signals emitted from the emitting unit. An output terminal of the reference unit is connected to an input terminal of the signal processing unit. Reference signals outputted by the reference unit are transmitted to the signal receiving unit by the output terminal of the reference unit. A sample in a sample tank is excited by the reflected light signals, such that fluorescence signals are generated. The fluorescence signals are received by the receiving unit beside the sample tank, and are outputted to the signal processing unit by the receiving unit. The fluorescence signals are processed by the signal processing unit. The system and the method provided by the invention are based on laser-induced fluorescence detection principles. Emitted signals are modulated by using a modulation technology, such that the detection sensitivity of the system is high. With the method and the system, rapid, real-time, on-line and non-contact measuring upon water body petroleum-type pollutant fluorescence signals can be realized. The system and the method can be widely applied in water body environment monitoring.
Description
Technical field:
The present invention relates to water body environment monitoring, is a kind of detection system and detection method for water body petroleum-type pollutant specifically.
Technical background:
Since entering 21 century, be accompanied by the high speed development of national economy, rivers, lake and the marine environment water quality of China have also been subjected to serious broken ring, infringement living resources, and harm humans health, hinders fishing and the mankind's activity.This situation is particularly serious in the comparatively flourishing coastal region of economy.Obviously, all kinds of waters (river, river, lake, coastal ocean) sewage petroleum class pollutants (hereinafter referred to as mineral oil) are effectively monitored and manage, and especially develop real-time dynamic monitoring technology and have great social effect and economic worth.
At present the conventional method of water body petroleum-type pollutant measurement is had to nephelometry, ultrasonic method, light scattering method, gravimetric method, NDIR (Non-Dispersive Infrared) absorption process, infrared spectrophotometer, chromatography, fluorescence method.Wherein nephelometry, ultrasonic method, light scattering method only work to the dispersed oil in water body, because they can't detect the low concentration petroleum hydrocarbon being dissolved in the water.Gravimetric method sensitivity is not high, and can cause the loss of low boiling alkane.NDIR (Non-Dispersive Infrared) absorption process is because mineral oil composition (contains in alkane, naphthenic hydrocarbon and aromatic hydrocarbon respectively at 2930cm-1 (=CH
2middle C-H stretching vibration), 2960cm-1 (CH
2middle C-H stretching vibration), 3030cm-1 (C-H stretching vibration in aromatic rings) locates the different component of absorption band, if the relative value of these components changes, be obviously difficult to survey by the NDIR (Non-Dispersive Infrared) absorption process of only measuring at a certain wave number place accurate.Infrared spectrophotometer is because the absorbance that can measure simultaneously or sequentially above-mentioned three wave number places (is A2930, A2960, A3030), and disturb littlely at these three wave number places, can easily try to achieve the total concentration of mineral oil by suitable calculating, thereby can avoid above-mentioned most of shortcoming, but this method need to be used cuvette to do transmission-type and measure, and need to carry out sample collection, and often need extraction step, only be suitable for lab analysis, be not suitable for on-line monitoring.Although chromatography can be measured multiple components, complex operation step is time-consuming, bothersome.Fluorescence method utilizes ultraviolet source as excitation source, can realize easily online, non-contact measurement to petroleum-type pollutant, is extremely potential new method.But excitation source mostly adopts the method for white light light splitting to realize at present, and fluorescence excitation efficiency is not high; And detection means is often taked the scheme of direct detection, survey signal to noise ratio (S/N ratio) lower.
Summary of the invention:
For there being the weak points such as fluorescence excitation efficiency is not high, detection noise is low in prior art, the technical problem to be solved in the present invention is to provide a kind of to be had fluorescence excitation efficiency height and surveys the good petroleum-type pollutant levels detection system of signal to noise ratio (S/N ratio), another object of the present invention is to provide a kind of detection method of utilizing petroleum-type pollutant levels detection system of the present invention to detect petroleum-type pollutant levels.
For solving the problems of the technologies described above, technical scheme of the present invention is as follows:
A kind of petroleum-type pollutant detection system, is characterized in that comprising transmitter unit, receiving element, reference unit and signal processing unit; Wherein: described transmitter unit Emission Lasers signal, is output as optical signal transmissive and reflected light signal by output terminal; The input end of described reference unit is accepted the optical signal transmissive of this transmitter unit transmitting, and the output terminal of described reference unit connects the input end of described signal processing unit;
Sample in reflected light signal irradiation the excited sample pond of described transmitter unit produces fluorescence signal, described receiving element is positioned at sample cell this fluorescence signal of other reception and described fluorescence signal is processed, and the output terminal of described receiving element connects described signal processing unit.
Described transmitter unit comprises coaxial laser instrument, chopper and the spectroscope of placing in turn, and the excitation source of wherein said laser instrument adopts laser diode.
Described receiving element comprises diaphragm, optical filter, detector and housing, in its middle shell, coaxially have three penetrating holes, in described hole, place in turn diaphragm, optical filter and detector, described diaphragm is positioned at the input end of described receiving unit, and described detector is positioned at the output terminal of described receiving unit.
Described optical filter adopts the bandpass filter that centre wavelength is 500hm-800nm.
Described diaphragm is diameter of phi 1-12mm continuous variable adjustable diaphragm.
The detector of described receiving element is photomultiplier.
Described signal processing unit comprises lock-in amplifier and host computer, wherein the input end of this lock-in amplifier connects the output terminal of described receiving element, the output terminal of this lock-in amplifier connects the input end of host computer, and the reference signal input end of described lock-in amplifier connects the chopper of transmitter unit.
Described reference unit comprises reference detector, and described reference detector is photomultiplier.
The centre wavelength of the laser that described excitation source is launched is 405nm or 355nm.
Described sample cell is labware or outdoor open liquid level, with detection system be contactless.
Described petroleum-type pollutant detection system is surveyed for crude oil, diesel oil, gasoline, lubricating oil or other HC fuel oil.
A detection method that uses described petroleum-type pollutant detection system, comprising:
The laser diode Emission Lasers of transmitter unit, is modulated to " interchange " signal through chopper, is output as transmitted light and reflected light through spectroscope;
Transmitted light enters in the detector of reference unit, and detector light signal is converted in the host computer that electric signal is sent to signal processing unit;
Reflected light is irradiated to sample cell, and excited sample produces fluorescence signal, and receiving element gathers fluorescence signal, regulates the luminous flux of fluorescence signal via diaphragm, by the interference of background signal in optical filter filtering fluorescence signal, exports lock-in amplifier to through detector;
Lock-in amplifier inputs to host computer after fluorescence signal is further amplified;
The output signal of lock-in amplifier signal and reference unit is compared computing by host computer, the impact bringing to eliminate light source fluctuation;
The output signal of lock-in amplifier, the output signal of reference unit input in host computer, calculate the concentration of petroleum-type pollutant with this.
The present invention has following good effect and advantage:
1. the present invention adopts laser diode as excitation source, has volume small and exquisite, the advantage that launching efficiency is high.
2. the present invention adopts chopper to modulate transmitting illuminant, but not direct detection can effectively improve detection signal to noise ratio (S/N ratio).
3. the present invention is provided with reference unit light source, can effectively eliminate the impact that light source fluctuation brings.
4. to adopt Stainless Steel Shell to form integrated, light tight for receiving element of the present invention, and anti-electromagnetic interference capability is strong.
5. the present invention utilizes lock-in amplifier to realize the amplification processing to weak signal, has greatly improved detection signal to noise ratio (S/N ratio).
6. the present invention adopts laser-induced fluorescence (LIF) measuring technique, avoided that lab analysis brings loaded down with trivial details, simple to operate, save time, to survey signal to noise ratio (S/N ratio) high, hardly with safeguarding, and is not vulnerable to external interference, easy to use.
Brief description of the drawings
Fig. 1 is the structured flowchart of detection system of the present invention;
Fig. 2 is the structural representation of detection system of the present invention;
Fig. 3 is the probe unit structural representation of detection system of the present invention;
Fig. 4 is for adopting detection system measurement result schematic diagram of the present invention;
Wherein:
1, laser instrument; 2, chopper; 3, spectroscope; 4, optical filter; 5, detector; 6, reference detector; 7, diaphragm; 8, lock-in amplifier; 9, computing machine; 10, sample cell; 501, multiplier tube high-pressure modular; 502, multiplier tube receives forms; 503, the 1st Stainless Steel Shell; 504, the 2nd Stainless Steel Shell; 505, the 3rd Stainless Steel Shell.
Embodiment
Below in conjunction with embodiment, the present invention will be described in detail.
As shown in Figure 1-2, petroleum-type pollutant detection system comprises transmitter unit, receiving element, reference unit, signal processing unit, described transmitter unit comprises coaxial laser instrument 1, chopper 2, the spectroscope 3 of placing in turn, wherein laser instrument 1 adopts laser diode as excitation source, the centre wavelength of the laser that laser diode is launched is 405nm, also the LASER Light Source of optional other centre wavelength, for example LASER Light Source of centre wavelength 355nm.The laser of launching is modulated to " interchange " signal of 1kHz through chopper 2, be transmitted light and the reflected light that energy respectively accounts for half through spectroscope 3 light splitting again, wherein transmitted light enters reference unit, the signal output part of reference unit connects the signal input part of signal processing unit by ISA capture card, reflected light is irradiated on the sample in sample cell 10, excited sample produces fluorescence signal, the contiguous sample cell 10 of receiving element receives the fluorescence signal producing, and wherein the signal output part of receiving element connects the signal input part of signal processing unit.
Described signal processing unit is made up of lock-in amplifier 8 and host computer 9, wherein the signal input part of lock-in amplifier 8 connects the signal output part of receiving element, the output terminal of lock-in amplifier 8 connects the input end of host computer by GPIB capture card, the model of GPIB capture card is PCI-82350B, for realizing the communication between lock-in amplifier and host computer.The reference signal input end of lock-in amplifier 8 connects the chopper 2 of transmitter unit, and the signal after chopper 2 modulation also inputs to the reference signal input end of lock-in amplifier 8 as the reference signal of lock-in amplifier 8 by signal wire.
Reference unit comprises reference detector 6, in the present embodiment, reference detector 6 adopts photomultiplier to change electric signal into the light signal of input, and be sent to the host computer 9 of signal processing unit by ISA capture card, the model PCL-711S that ISA capture card adopts, reference detector 6 models are shore pine CR114.
As shown in Figure 3, the receiving element of detection system of the present invention comprises diaphragm 7, optical filter 4, detector 5 and housing; In its middle shell, coaxially have three mutually penetrating holes, in hole, place in turn diaphragm 7, optical filter 4 and detector 5, diaphragm 7 is positioned at the input end of receiving unit, detector 5 is positioned at the output terminal of described receiving unit, communicate with the external world so that receiving optical signals for the hole of placing diaphragm 7, closed states for hole and the external world of placing detector 5, for increasing opaqueness and anti-electromagnetic interference (EMI).Detector 5 adopts photomultiplier, this photomultiplier receives forms 502 by multiplier tube high-pressure modular 501, multiplier tube and forms, be positioned at the output terminal of receiving element, diaphragm 7 is positioned at the receiving end of receiving element, first fluorescence signal from sample cell enters into receiving element by diaphragm 7, optical filter 4 is between diaphragm 7 and detector 5, for the interference of the background signal of filtering fluorescence signal; Housing is stainless steel material, by the 1st Stainless Steel Shell the 503, the 2nd Stainless Steel Shell 504 and the 3rd Stainless Steel Shell 505, successively by screw thread the becoming one that closely link together.Adopt Stainless Steel Shell processing to make whole receiving element light tight, and have the effect of anti-electromagnetic interference (EMI), the model of the detector 5 of receiving element is shore pine CR131.
The embodiment of the present invention is in the time of work, the laser diode Emission Lasers of transmitter unit, be modulated to " interchange " signal through chopper 2, be divided into transmitted light and reflected light two-way through spectroscope 3 outputs, wherein transmitted light and catoptrical energy respectively account for half, transmitted light enters in the detector 6 of reference unit, and detector 6 is converted to electric signal by light signal and is sent in the host computer 9 of signal processing unit through ISA capture card, " interchange " signal being modulated into through chopper 2 also inputs to the reference signal input end of lock-in amplifier 8 as the reference signal of lock-in amplifier 8 by signal wire, the reflected light being separated by spectroscope 3 is irradiated on the sample in sample cell 10, excited sample produces fluorescence signal, receiving element gathers the fluorescence signal from sample, first enter receiving element by diaphragm 7, in this enforcement, diaphragm 7 is diameter of phi 1-12mm continuous variable adjustable diaphragm, as required by regulating diaphragm 7 to regulate the luminous flux of fluorescence signal, fluorescence signal through overregulating is by the jamming pattern signal in optical filter 4 filtering fluorescence signals, in the present embodiment, to adopt centre wavelength be the bandpass filter 4 of 500nm-800nm to optical filter 4, the fluorescence signal of removing undesired signal inputs in lock-in amplifier 8 through detector 5, faint fluorescence signal is carried out phase sensitive detection by lock-in amplifier 8, after amplification, input to host computer 9, the collection of the output signal of host computer 9 responsible lock-in amplifiers 8, the output signal of reference unit, further compares the output signal of the reference unit of lock-in amplifier 8 signals and collection the impact that computing brings to eliminate light source fluctuation.Host computer 9 is processed the signal gathering, and calculates the concentration of water outlet petroleum class pollutant through software analysis.In the embodiment of the present invention, process the signal gathering according to host computer, adopt visualBasic to write upper computer software, by the concentration of linear regression method analytical calculation water outlet petroleum class pollutant.
In the present embodiment taking-10# diesel oil as sample, centre wavelength is the laser diode of 405nm is measured variable concentrations to oil sample petroleum-type pollutant as LASER Light Source, measurement result is shown in Fig. 4, horizontal ordinate represents the concentration of oil pollutant, ordinate represents relative light intensity, from measurement result, between the concentration of petroleum-type pollutant and fluorescence intensity, there is good linear relationship, can be used as the foundation of concentration monitor.
Petroleum-type pollutant detection system of the present invention adopts laser as excitation source, and the impact that reference unit brings in order to eliminate light source fluctuation is set, and adopts chopper to realize the modulation to incident light, realizes the amplification to hypofluorescence signal by phase lock amplifying technology.Whole measuring system is measured convenient, can realize real-time, the non-contact monitoring of petroleum-type pollutant, and highly sensitive, reliability high detection, can be used as boat-carrying, airborne equipment, for water body environment monitoring provides strong technological means.
Claims (5)
1. a petroleum-type pollutant detection system, is characterized in that comprising transmitter unit, receiving element, reference unit and signal processing unit; Wherein:
Described transmitter unit Emission Lasers signal, is output as optical signal transmissive and reflected light signal by output terminal; Transmitted light and energy of reflection light respectively account for half;
The input end of described reference unit receives the optical signal transmissive of this transmitter unit transmitting, and the output terminal of described reference unit connects the input end of described signal processing unit;
Sample in reflected light signal irradiation the excited sample pond of described transmitter unit produces fluorescence signal, described receiving element is positioned at sample cell this fluorescence signal of other reception and described fluorescence signal is processed, and the output terminal of described receiving element connects described signal processing unit;
Described receiving element comprises diaphragm, optical filter, detector and housing, in its middle shell, coaxially have three penetrating holes, in described hole, place in turn diaphragm, optical filter and detector, described diaphragm is positioned at the input end of described receiving element, and described detector is positioned at the output terminal of described receiving element;
Described optical filter adopts the bandpass filter that centre wavelength is 500nm-800nm;
Described diaphragm is diameter of phi 1-12mm continuous variable adjustable diaphragm;
Described sample cell is labware or outdoor open liquid level, with detection system be contactless;
Transmitter unit comprises coaxial laser instrument, chopper and the spectroscope of placing in turn, and the excitation source of wherein said laser instrument adopts laser diode;
The centre wavelength of the laser that described excitation source is launched is 405nm or 355nm;
Described signal processing unit comprises lock-in amplifier and host computer, wherein the input end of this lock-in amplifier connects the output terminal of described receiving element, the output terminal of this lock-in amplifier connects the input end of host computer, and the reference signal input end of described lock-in amplifier connects the chopper of transmitter unit.
2. according to petroleum-type pollutant detection system claimed in claim 1, it is characterized in that: the detector of described receiving element is photomultiplier.
3. according to petroleum-type pollutant detection system claimed in claim 1, it is characterized in that: described reference unit comprises reference detector, described reference detector is photomultiplier.
4. according to petroleum-type pollutant detection system claimed in claim 1, it is characterized in that: described petroleum-type pollutant detection system is surveyed for crude oil, diesel oil, gasoline, lubricating oil or other HC fuel oil.
5. right to use requires a detection method for the petroleum-type pollutant detection system described in 1, it is characterized in that comprising:
The laser diode Emission Lasers of transmitter unit, is modulated to " interchange " signal through chopper, is output as transmitted light and reflected light through spectroscope; Transmitted light and energy of reflection light respectively account for half;
Transmitted light enters in the detector of reference unit, and detector light signal is converted in the host computer that electric signal is sent to signal processing unit;
Reflected light is irradiated to sample cell, and excited sample produces fluorescence signal, and receiving element gathers fluorescence signal, regulates the luminous flux of fluorescence signal via diaphragm, by the interference of background signal in optical filter filtering fluorescence signal, exports lock-in amplifier to through detector;
Lock-in amplifier inputs to host computer after fluorescence signal is further amplified;
The output signal of lock-in amplifier signal and reference unit is compared computing by host computer, the impact bringing to eliminate light source fluctuation;
The output signal of lock-in amplifier, the output signal of reference unit input in host computer, calculate the concentration of petroleum-type pollutant with this.
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