CN108375562A - A kind of mercury detector of high measurement accuracy - Google Patents
A kind of mercury detector of high measurement accuracy Download PDFInfo
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- CN108375562A CN108375562A CN201810209678.9A CN201810209678A CN108375562A CN 108375562 A CN108375562 A CN 108375562A CN 201810209678 A CN201810209678 A CN 201810209678A CN 108375562 A CN108375562 A CN 108375562A
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- light
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- gas sample
- mercury lamp
- flow cell
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
Abstract
The present invention relates to a kind of mercury detectors of high measurement accuracy, it includes ultraviolet source system, condenser lens in ultraviolet source system input path and gas sample flow cell are set, fluorescence detection device above gas sample flow cell and system, control circuit, ultraviolet source system includes mercury lamp height adjustment base, the pen type mercury lamp that mercury lamp lampshade on mercury lamp height adjustment base is set and is arranged in mercury lamp lampshade, it is characterised in that：It further includes a spuious absorption means, and spuious absorption means are arranged between condenser lens and gas sample flow cell；After the ultraviolet light line focus lens that ultraviolet source system is sent out are focused, spuious light absorption is carried out into spuious absorption means, it is irradiated later to entering the mercurous gas sample stream in gas sample flow cell, the fluorescence that mercury atom is inspired in gas sample flow cell is detected by fluorescence detection device, obtains mercury atom concentration in gas sample stream.The present invention can be widely applied in mercury class compound test.
Description
Technical field
The present invention relates to mercury class compound test equipment, especially with regard to a kind of mercury detector of high measurement accuracy, the inspection
It surveys instrument combination light intensity temperature feedback and absorbs light path to improve mercury accuracy of detection, to obtain smaller detection limit.
Background technology
Characteristic that mercury pollution is diffused with atmospheric air circulation by it causes high risks to ecological environment and human health,
It is a kind of global contaminant.In mercury cycle, mercury mainly exists in the form of element mercury, inorganic mercury, three kinds of organic mercury, wherein having
Methyl mercury in machine mercury is the maximum form of toxicity.Although the harm of methyl mercury is very big, methyl mercury belongs to ultra trace pollution
Object, so high sensitivity is not achieved in detectors many at present, so to accurately detect the methyl mercury chemical combination in environment
Object is generally required by that can be realized after enrichment.The ultra trace substance for how fast and accurately measuring environment, to detector
Sensitivity propose very high requirement.
There are many method for measuring methyl mercury at present.For separation angle, there are the sides such as gas-chromatography, liquid chromatogram separation
Method has the methods of ECD detectors, ICP-MS and AFS, wherein ECD detectors are for mercury class from the perspective of detector
Compound, specificity is not strong, and impurity interference is big, and the level of ultra trace is also not achieved in the detection limit of itself.So there is no wide
General use.ICP-MS high sensitivities, and also have response to other metallic elements, applicability is wider, but price is relatively high, especially
It is HPLC-ICP-MS combinations, expensive, is required laboratory technician high.AFS, that is, atomic fluorescence detector has atomic emissions
Sensitivity of spectrograph higher, by the interference of the spectral line and matrix advantage low compared with smaller, detection limit, for mercury it is this it is volatile,
The metallic compound that can be stabilized in the environment with atomic state need not make metallic element by flame method, graphite furnace method
Atomization, so for Volatile Elements such as mercury elements, using CVAFS (Cold Atomic Fluorescent Mercury spectrometer hair), to detect environment
The mercury and form mercury of middle ultra trace are the most suitable and easy to spread.
In the method for Atomic Fluorescence Spectrometry mercury, after the mercury atom in flow cell absorbs the characteristic radiation of mercury lamp light source, atom
Outer-shell electron transits to higher energy level, and then transition returns to ground state again, while launching ultraviolet light identical as former excitation wavelength.Swash
Luminous light intensity is directly proportional to mercury atom concentration, and the intensity by detecting exciting light can be obtained by corresponding mercury atom concentration.
The stability of incident uv directly affects detection precision to the end, and the collimation of incident uv directly influences detection
Limit.Current ultraviolet source most on the market is all the TUV ultraviolet lamps (cast ultraviolet lamp) of not feedback mechanism, volume
Greatly, light-emitting surface is uneven, and light source stability is poor or the ultraviolet lamp of front-end control, can only be controlled by controlling mercury lamp electric current
The intensity of ultraviolet light, but the intensity of ultraviolet light not only with it is current related, it is also related with temperature).The intensity of light source be temperature and
Input power it is coefficient as a result, and incident light has diffusing for other directions certainly, there is presently no simultaneously to this
A little disturbing factors carry out the measure of direct regulation and control.
Invention content
In view of the above-mentioned problems, the object of the present invention is to provide a kind of combination light intensity temperature feedbacks and absorption light path to improve
The accuracy of detection of mercury, to obtain the mercury detector of the high measurement accuracy of smaller detection limit.
To achieve the above object, the present invention takes following technical scheme：A kind of mercury detector of high measurement accuracy comprising
The condenser lens in the ultraviolet source system input path and gas sample flow cell is arranged in ultraviolet source system, setting
Fluorescence detection device and system, control circuit above the gas sample flow cell, the ultraviolet source system includes mercury
Lamp height adjustment base is arranged the mercury lamp lampshade on the mercury lamp height adjustment base and is arranged in the mercury lamp lampshade
Pen type mercury lamp, it is characterised in that：It further includes a spuious absorption means, and the spuious absorption means setting is described poly-
Between focus lens and gas sample flow cell；The ultraviolet light that the ultraviolet source system is sent out is focused through the condenser lens
Afterwards, spuious light absorption is carried out into the spuious absorption means, later to entering the mercurous gas sample in the gas sample flow cell
Stream is irradiated, and the fluorescence that mercury atom is inspired in the gas sample flow cell is detected by the fluorescence detection device, obtains gas
Mercury atom concentration in sample stream.
The spuious absorption means include upper light path and lower light path；The upper light path and lower light path are vertically oppositely arranged on
Between the condenser lens and gas sample flow cell, and the inner wall of the upper light path is arranged at intervals with top reflection light absorption layer, institute
It states and is provided on lower light path inner wall and the one-to-one lower part reflection light absorption layer in top reflection light absorption layer position；It is described
It is reserved with key light paths among top reflection light absorption layer and the lower part reflection light absorption layer so that the upper light path and institute
It states and constitutes a tooth-like belt between lower light path.
In the spuious absorption means, the length of the upper light path and lower light path is 45mm, the upper and lower part reflected light
Each seven of absorbed layer, the spacing between reflection light absorption layer is 7.5mm, each reflection light absorption layer thickness 1.5mm, height two-by-two
28mm。
The mercury detector further includes a stabilized intensity device, and the stabilized intensity device includes light splitting feedback module and temperature
Spend feedback module；The light splitting feedback module is arranged inside the spuious absorption means, for the ultraviolet source
The ultraviolet light that system is sent out, which is reflected and forms electro-optical feedback signal, is sent to the system, control circuit, by the system control
Circuit processed controls light stability；The mercury lamp lampshade in the ultraviolet source system is arranged in the temperature feedback module
On, for being heated to the mercury lamp lampshade, and the temperature signal for acquiring the mercury lamp lampshade in real time is sent to the system
Control circuit controls light-source temperature by the system, control circuit.
The stabilized intensity device includes spectroscope, optical filter, electro-optical feedback module and EOM holders；The EOM branch is set up
It sets in the spuious absorption means interior forward end, the optical filter setting is in the EOM pedestal upper ends, for through described poly-
Ultraviolet light after focus lens focus filters, and filters out the ultraviolet light other than 254mm wavelength；The spectroscope and the EOM branch
Frame is oppositely arranged, and for reflecting the ultraviolet light after optical filtering, 2% ultraviolet light is reflected into the electro-optical feedback module,
Remaining ultraviolet light enters subsequent optical path；The electro-optical feedback module is arranged on the EOM holders, is used for the spectroscope
The light of reflection is converted to electric signal and is sent to the system, control circuit；The system, control circuit is given birth to according to the electric signal
The light stability of the ultraviolet source system is controlled at negative-feedback signal.
The temperature feedback module includes temperature feedback module housing, two heating power pipes and electric thermo-couple temperature sensing
Device, the two heating power pipes are separately positioned on temperature feedback module housing lower part, for being carried out to the mercury lamp lampshade
Heating；The thermocouple temperature sensor is arranged between the two heating power pipes, for detecting the mercury lamp lampshade in real time
Temperature, and the temperature signal of acquisition is sent to the system, control circuit, the system, control circuit is according to the temperature
Signal generates the two heating power pipe of negative-feedback signal pair and controls, and ensures the temperature of the ultraviolet source system pre-
If in temperature range.
The mercury detector further includes a reflective mirror, and the speculum is arranged below the gas sample flow cell, and being used for will
The be excited downward 254nm atomic fluorescences of generation of mercury atom are directly reflected into outside in the gas sample flow cell.
The reflective mirror forms 45° angle with the input path.
The invention adopts the above technical scheme, which has the following advantages：1, the present invention is due in stabilized intensity device
It is provided with electro-optical feedback module and temperature feedback module, the intensity and temperature of mercury lamp can be controlled, effectively increase note
The stability for entering gas sample flow cell inner light source, improves accuracy of detection.2, the present invention is due to being provided with upper light path and lower light path, and two
Person constitutes a tooth-like belt, has effectively filtered out the stray light for beating that reflection and diffusing reflection are formed on inner wall so that enters gas sample and circulates
The collimation of pond inner light source is more preferable, effectively reduces detection limit.3, the present invention is reflective due to being provided with below gas sample flow cell
The downward light that mercury atom in gas sample flow cell is sent out can be all reflected into outside by mirror, and the light for reducing other directions is anti-
It is emitted back towards to influence the testing result of photomultiplier, further improves accuracy of detection.The configuration of the present invention is simple, it is easy to operate,
It can be widely applied in methyl mercury detection.
Description of the drawings
Fig. 1 is the decomposition diagram of structure of the invention；
Fig. 2 is the overall schematic of structure of the invention；
Fig. 3 (a) is that the present invention interferes spuious absorption means front view；
Fig. 3 (b) is that the present invention interferes spuious absorption means stereogram；
Fig. 4 is electro-optical feedback of the present invention and temperature feedback modular structure schematic diagram；
Fig. 5 is temperature feedback modular structure schematic diagram of the present invention.
Specific implementation mode
The present invention is described in detail below with reference to the accompanying drawings and embodiments.
As shown in Figure 1 and Figure 2, the mercury detector of a kind of high measurement accuracy provided by the invention, including be arranged on holder 1
Ultraviolet source system 2, be successively set in 2 input path of ultraviolet source system condenser lens 3, spuious light absorption dress
4 and gas sample flow cell 5 are set, fluorescence detection device 6 and the system, control circuit being arranged above gas sample flow cell 5.Ultraviolet light
The ultraviolet light that light-source system 2 is sent out is after the condenser lens 3 of input path inlet is focused, into spuious absorption means
4 carry out spuious light absorption, are irradiated later to entering the mercurous gas sample stream in gas sample flow cell 5, and mercury is former in gas sample flow cell 5
The fluorescence that son is inspired is detected by fluorescence detection device 6, obtains mercury atom concentration in gas sample stream.
Ultraviolet source system 2 includes mercury lamp height adjustment base 21, pen type mercury lamp 22 and mercury lamp lampshade 23.Wherein,
The setting of mercury lamp height adjustment base 21 is arranged in 1 upper surface side of holder, mercury lamp lampshade 23 above mercury lamp adjustment base 21, and
It is connected with mercury lamp height adjustment base 21 by adjusting screw, pen type mercury lamp 22 is arranged in mercury lamp lampshade 23, the purple of transmitting
Outer light enters input path through the window on mercury lamp lampshade 23.By adjusting the i.e. adjustable mercury lamp lampshade 23 of each adjusting screw and mercury
Gap between lamp height adjustment base 21, and then realize that the height of pen type mercury lamp 22 is adjusted.
Condenser lens 3 is arranged by the high low trestle of lens 7 in the input path of ultraviolet source system 2, and and mercury lamp
Window on lampshade 23 maintains an equal level, and to ensure that the ultraviolet light sent out to ultraviolet source system 2 is focused, obtains relatively parallel
Ultraviolet light.
As shown in Fig. 3 (a), Fig. 3 (b), spuious absorption means 4 include upper light path 41 and lower light path 42.41 He of upper light path
Lower light path 42 is vertically oppositely arranged between focus lens unit 3 and gas sample flow cell 5, and the inner wall interval setting of upper light path 41
Have top reflection light absorption layer, be provided on 42 inner wall of lower light path it is anti-with the one-to-one lower part in top reflection light absorption layer position
Light absorbing layer is penetrated, and key light paths are reserved among top reflection light absorption layer and lower part reflection light absorption layer so that glazing
A tooth-like belt is constituted between road 41 and lower light path 42.
Fluorescence detection device 6 includes photomultiplier transit pipe holder 61, photomultiplier 62 and photomultiplier shading cover 63.Light
Electricity multiplication pipe holder 61 is arranged above gas sample flow cell 5, and photomultiplier 62 is plugged in inside photomultiplier transit pipe holder 61, light
Electric multiplier tube shading cover 63 is arranged on photomultiplier transit pipe holder 61, is used for shading.
As a preferred embodiment, as shown in figure 4, the mercury detector further includes a stabilized intensity device 8 comprising
Electro-optical feedback module 81 and temperature feedback module 82.The spuious absorption means 4 in input path are arranged in electro-optical feedback module 81
Inside, the ultraviolet light for being sent out to ultraviolet source system 2, which is reflected and forms electro-optical feedback signal, is sent to system control
Circuit processed controls light stability by system, control circuit；Temperature feedback module 82 is arranged in ultraviolet source system 2
Mercury lamp lampshade 23 on, be sent to for being heated to mercury lamp lampshade 23, and according to 23 temperature signal of mercury lamp lampshade of acquisition
System, control circuit controls light-source temperature by system, control circuit.
Specifically, electro-optical feedback module 81 includes spectroscope 811, optical filter 812, electro-optical feedback module 813 and EOM holders
814；The setting of EOM holders 814 is used in 4 interior forward end of spuious absorption means, the setting of optical filter 812 in 814 upper end of EOM holders
Ultraviolet light after being focused to line focus lens 4 filters, and filters out the ultraviolet light other than 254mm wavelength；Spectroscope 811 with
EOM holders 814 are oppositely arranged, and for reflecting the ultraviolet light after optical filtering, it is anti-that 2% or so ultraviolet light is reflected into photoelectricity
Module 813 is presented, remaining ultraviolet light enters subsequent optical path；Electro-optical feedback module 813 is arranged on EOM holders 814, for that will divide
The light that light microscopic 811 reflects is converted to electric signal and is sent to system, control circuit；System, control circuit generates negative according to electric signal
Feedback signal controls the light stability of ultraviolet source system 2.
As shown in figure 5, temperature feedback module 82 includes two heating power pipes 821 and a thermocouple temperature sensor 822, two
Heating power pipe 821 is separately positioned on temperature feedback module housing lower part, for being heated to mercury lamp lampshade 23；Thermocouple temperature
It spends sensor 822 to be arranged between two heating power pipes 821, for detecting 23 temperature of mercury lamp lampshade in real time, and by the temperature of acquisition
Degree signal is sent to system, control circuit, and negative-feedback signal is generated to heating power according to the temperature signal by system, control circuit
Pipe is controlled, and ensures ultraviolet source system 2 in preset temperature range.
As a preferred embodiment, mercury detector further includes a speculum 9, and the speculum 9 setting is circulated in gas sample
5 lower section of pond, 45° angle, the downward 254nm for generation that mercury atom in gas sample flow cell 5 is excited are formed with input path
Atomic fluorescence is directly reflected into outside.
It as a preferred embodiment, interferes in spuious absorption means 4, the length of upper light path 41 and lower light path 42 is
45mm, upper and lower part reflection light absorption layer have seven, spacing 7.5mm, thickness 1.5mm altogether, height 28mm.
The operation principle of the present invention is that：Start mercury detector, gas sample flow cell 5 is connected to gas sample to be detected.Ultraviolet light
Enter input path after the ultraviolet light line focus lens focus that pen type mercury lamp 22 is sent out in light-source system 2, spectroscope 811 is to focusing
Ultraviolet light afterwards is reflected, and 95% or more ultraviolet light is directly transmitted into subsequent optical path, and the light of residue 4% or so is by anti-
It is irradiated on light sensor 813 after penetrating and is converted into electric signal, handled by system, control circuit and adjust the pen type mercury lamp 22 that comes in and goes out
Electric current, and then by output intensity stablize 1 ‰.Meanwhile the heating work(in system, control circuit control temperature feedback module 82
Rate pipe 821 heats mercury lamp lampshade 23, and the temperature of the mercury lamp lampshade 23 acquired in real time according to thermocouple temperature sensor 222
Degree variation adjusts heating power pipe 821, and then by the control of the temperature change of mercury lamp lampshade 23 in ± 0.5 DEG C.
After the ultraviolet light of the transmission of spectroscope 3 enters and interferes spuious absorption means 4, through upper light path 41 and lower 42 structure of light path
At tooth-like belt, all beat is sponged in the light on inner wall by the gradually reflection in structure, makes this part of light will not
It is irradiated in gas sample flow cell 5.
The 254nm atomic fluorescences that mercury atom in gas sample flow cell 5 is inspired can be sent out to all directions, and reflective
Downward atomic fluorescence can be directly reflected into outside by mirror 9, and the photomultiplier 62 of top is pointed into without going past reflection.
The intensity for the 254nm atomic fluorescences that photomultiplier devices 6 are inspired mercury atom in gas sample flow cell 5 carries out
Detection, and then obtain corresponding mercury atom concentration.
The various embodiments described above are merely to illustrate the present invention, wherein the structure of each component, connection type and manufacture craft etc. are all
It can be varied from, every equivalents carried out based on the technical solution of the present invention and improvement should not exclude
Except protection scope of the present invention.
Claims (8)
1. a kind of mercury detector of high measurement accuracy comprising ultraviolet source system is arranged in the ultraviolet source system
Condenser lens in input path and gas sample flow cell are arranged the fluorescence detection device above the gas sample flow cell and are
System control circuit, the ultraviolet source system includes mercury lamp height adjustment base, is arranged in the mercury lamp height adjustment base
On mercury lamp lampshade and the pen type mercury lamp that is arranged in the mercury lamp lampshade, it is characterised in that：It further includes that a stray light is inhaled
Receiving apparatus, the spuious absorption means are arranged between the condenser lens and gas sample flow cell；The ultraviolet source system
The ultraviolet light sent out unite after the condenser lens is focused, spuious light absorption is carried out into the spuious absorption means,
It is irradiated later to entering the mercurous gas sample stream in the gas sample flow cell, mercury atom is inspired in the gas sample flow cell
Fluorescence detected by the fluorescence detection device, obtain mercury atom concentration in gas sample stream.
2. a kind of mercury detector of high measurement accuracy as described in claim 1, it is characterised in that：The spuious absorption means
Including upper light path and lower light path；The upper light path and lower light path be vertically oppositely arranged on the condenser lens and gas sample flow cell it
Between, and the inner wall of the upper light path be arranged at intervals with top reflection light absorption layer, be provided on the lower light path inner wall with it is described
The one-to-one lower part reflection light absorption layer in top reflection light absorption layer position；The top reflection light absorption layer and the lower part
Key light paths are reserved among reflection light absorption layer so that a flute profile is constituted between the upper light path and the lower light path
Band.
3. a kind of mercury detector of high measurement accuracy as claimed in claim 2, it is characterised in that：The spuious absorption means
In, the length of the upper light path and lower light path is 45mm, each seven of the upper and lower part reflection light absorption layer, the two-by-two reflection
Spacing between light absorbing layer is 7.5mm, each reflection light absorption layer thickness 1.5mm, height 28mm.
4. a kind of mercury detector of high measurement accuracy as described in claim 1, it is characterised in that：The mercury detector further includes
One stabilized intensity device, the stabilized intensity device include light splitting feedback module and temperature feedback module；
The light splitting feedback module is arranged inside the spuious absorption means, the purple for being sent out to ultraviolet source system
Outer light, which is reflected and forms electro-optical feedback signal, is sent to the system, control circuit, by the system, control circuit to light intensity
Stability is controlled；The temperature feedback module is arranged on the mercury lamp lampshade of the ultraviolet source system, for institute
It states mercury lamp lampshade to be heated, and the temperature signal for acquiring the mercury lamp lampshade in real time is sent to the system, control circuit, by
The system, control circuit controls light-source temperature.
5. a kind of mercury detector of high measurement accuracy as claimed in claim 4, it is characterised in that：The stabilized intensity device packet
Include spectroscope, optical filter, electro-optical feedback module and EOM holders；The EOM holders are arranged inside the spuious absorption means
Front end, the optical filter are arranged in the EOM pedestal upper ends, for being filtered to the ultraviolet light after the line focus lens focus
Light filters out the ultraviolet light other than 254mm wavelength；The spectroscope is oppositely arranged with the EOM holders, for the purple after optical filtering
Outer light is reflected, and 2% ultraviolet light is reflected into the electro-optical feedback module, remaining ultraviolet light enters subsequent optical path；Institute
It states electro-optical feedback module to be arranged on the EOM holders, the light for reflecting the spectroscope is converted to electric signal and sends
To the system, control circuit；The system, control circuit generates negative-feedback signal to the ultraviolet light light according to the electric signal
The light stability of source system is controlled.
6. a kind of mercury detector of high measurement accuracy as claimed in claim 4, it is characterised in that：The temperature feedback module packet
Temperature feedback module housing, two heating power pipes and a thermocouple temperature sensor are included, the two heating power pipes are respectively set
In temperature feedback module housing lower part, for being heated to the mercury lamp lampshade；The thermocouple temperature sensor is set
It sets between the two heating power pipes, the temperature for detecting the mercury lamp lampshade in real time, and the temperature signal of acquisition is sent out
It is sent to the system, control circuit, the system, control circuit is generated according to the temperature signal to be added described in negative-feedback signal pair two
Thermal power pipe is controlled, and ensures the temperature of the ultraviolet source system in preset temperature range.
7. a kind of mercury detector of high measurement accuracy as described in claim 1, it is characterised in that：The mercury detector further includes
One reflective mirror, the speculum is arranged below the gas sample flow cell, for being swashed mercury atom in the gas sample flow cell
The downward 254nm atomic fluorescences that hair generates directly are reflected into outside.
8. a kind of mercury detector of high measurement accuracy as claimed in claim 7, it is characterised in that：The reflective mirror with it is described enter
It penetrates light path and forms 45° angle.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115931808A (en) * | 2023-02-09 | 2023-04-07 | 北京鹏宇昌亚环保科技有限公司 | Totally-enclosed light path device of mercury detector |
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