CN207540976U - A kind of water quality total mercury detection device - Google Patents
A kind of water quality total mercury detection device Download PDFInfo
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- CN207540976U CN207540976U CN201721749255.3U CN201721749255U CN207540976U CN 207540976 U CN207540976 U CN 207540976U CN 201721749255 U CN201721749255 U CN 201721749255U CN 207540976 U CN207540976 U CN 207540976U
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Abstract
The utility model is related to a kind of water quality total mercury detection devices.A kind of water quality total mercury detection device, the device is using the pretreatment of ultraviolet digestion, the mercury reduction reaction of stannous chloride, then it is detected using the fluorescence detection of mercury lamp+photomultiplier, the flow path switching system of syringe pump+eight ways valve+triple valve is used on device, using the high-precision of syringe pump, the accurate quantification of various reagents is realized；Current-carrying liquid+argon gas isolation realizes syringe pump contact various reagents, the problem of reducing the material requirements of syringe pump, avoid syringe pump pollution.The utility model realizes full-automatic, accurate, the reliable trace detection to total mercury in water quality.
Description
Technical field
The utility model is related to a kind of water quality total mercury detection devices.
Background technology
Mercury is unique metal for being rendered as liquid at normal temperatures, and volatile, has diffusivity and larger fat-soluble.Mercury
Element is also a kind of accumulation property toxin in itself, for a long time with cumulative effect.The source of mercury is mainly with coal fire discharged wherein in air
Mercury element based on, wherein particulate form accounting 10%, gaseous mercury accounts for 90%.There are mainly three types of form, difference for mercury in natural water body
Hg for solubilised state0And Hg2+And more active Hg2 2+, particulate form mercury, organic mercury；Wherein organic Hg, may be from it is micro-
Hg Element generations under biology or natural environmental condition so that the pollution element toxicity enhances.
Pressurized sample digestion mercury context of detection in the water in laboratory field has had relatively broad application, compared to it
Its method, sensitivity higher, detection limit is lower, and disturbing factor is few, is very suitable for measuring the Trace Hg in water.This patent exists
On the basis of traditional manual Pressurized sample digestion, increase ultraviolet digestion, cooperation syringe pump realizes total in water quality as power end
The automatical analysis flow path of mercury can meet requirement of the country to I type water quality detections.
The measuring principle of water quality mercury on-line computing model is Pressurized sample digestion, and principle is as follows：Water sample to be detected
Process for producing mercuryvapour is learned, mercury vapour is ejected by atom nozzle under the drive of carrier gas, receives to send out wavelength by mercury lamp
Exciting light for 253.7nm irradiates, and ground state mercury atom can develop after receiving irradiation to upper state, is to give off altogether when returning to ground state
Shake fluorescence, and the fluorescence given off is focusing on photomultiplier after condenser, finally realizes opto-electronic conversion, photoelectricity after conversion
Stream carries out data processing using computer, calculates the concentration of water sample to be measured after amplification, A/D conversions.When the concentration of mercury
When relatively low, fluorescence intensity, in good linear relationship, the quantitative determination to Trace Hg is realized by standard liquid calibration with mercury concentration.
The Chemical Pretreatment of water sample to be measured is reduction.Reduction process uses main chlorine in excessive stannous chloride and water sample
Change mercury fully to be reacted, produce mercuryvapour, reactive chemistry equation is：
It not only can be outside spontaneous return ground state radiofluorescence, and can be touched with background particle for being excited rear mercury atom
Hitting makes energy be changed into all previous warm-up movement, generates the transition of unstressed configuration radiation in the process, and then makes the intensity of fluorescence big
Fluorescent quenching phenomenon occurs for big reduction.Due to being excited mercury atom with the probability of argon gas collision than nitrogen, oxygen, two in air
Carbonoxide etc. is much smaller, and caused fluorescent quenching is much smaller, therefore by the use of argon gas as carrier gas when with nitrogen during instrumental sensitivity
It is much higher.Air to be avoided to enter lasing region in measurement process simultaneously, while does shielding gas with argon gas and is caused therefrom with reducing
Fluorescence phenomenon, improve the stability of instrument.
Invention content
In order to solve the technical issues of above-mentioned, the purpose of this utility model is to provide a kind of water quality total mercury detection device, should
Device realizes full-automatic, accurate, the reliable trace detection to total mercury in water quality.
In order to realize above-mentioned purpose, the utility model employs following technical solution：
A kind of water quality total mercury detection device, the device include multiple-way valve, digestion tube, reducing bottle and detection cell；Described is more
Port valve has：
One valve port is connected with the first feed pipe, and the first feed pipe is by setting the first solenoid valve to connect reducing agent material bottle respectively
With the reducing agent feed inlet of reducing bottle,
One valve port is connected with the second feed pipe, and the second feed pipe connects the water sample feed inlet of reducing bottle,
One valve port by the way that second solenoid valve is set to be connected with water sample feed pipe and standard liquid feed pipe,
One valve port is connected with nitric acid feed pipe,
One valve port by the digestion tube that sets the connection of third solenoid valve described,
One valve port is connected with waste liquid port,
One valve port is connected with syringe pump, and syringe pump is connected with current-carrying liquid feed pipe,
One valve port is connected with the first end of the first three-way pipe, and the second end of the first three-way pipe connects the detection cell, the
Three ends are connected with the first argon inlet pipe by flowmeter,
One valve port is connected with water pipe；
The discharge port of the reducing bottle is by setting the 4th solenoid valve to connect the detection cell；The reducing bottle
Air inlet by the way that the 5th solenoid valve is set to be connected with electronic flow control module, electronic flow control module connect the second argon gas into
Tracheae.
The utility model is related to valve port can be individual, also may be used if the substance of two valve ports will not generate to interfere with each other
To be that two valve ports share a valve port.
As a further improvement, first argon inlet pipe is connected with the second argon inlet pipe by the second three-way pipe
To argon gas source, pressure reducing valve and the 6th solenoid valve are provided between argon gas source and the second three-way pipe.
As a further improvement, the reducing bottle is additionally provided with waste liquid outlet, digestion tube top is additionally provided with the 7th electricity
Magnet valve.
As a further improvement, multiple-way valve is eight ways valve, the first feed pipe described in the first valve port connection of eight ways valve, the
Two valve ports connection, second feed pipe, the third valve port connection second solenoid valve；The 4th valve port connection nitre
Sour feed pipe, the 5th valve port connection third solenoid valve, the 6th valve port connection waste liquid outlet, the connection of the 7th valve port
The first end of the syringe pump and connection first three-way pipe, the 8th valve port connection water pipe.
As a further improvement, the side of digestion tube is provided with ultraviolet lamp, the side of detection cell is provided with mercury lamp, opposite side
It is provided with photomultiplier.
As a further improvement, the capacity of the second feed pipe is more than water sample sample size.
As a further improvement, the capacity of the first feed pipe is more than reducing agent extraction amount.
The utility model has the characteristics that following as a result of above-mentioned technical solution：
1st, the preprocess method of ultraviolet digestion passes through ultra violet lamp in the digestion tube of water sample to be measured and accelerates mercury in water quality
The unified resolution reaction of valence state, while 10% nitric acid is added in promote to clear up reaction speed in resolution is reacted；
2nd, the mercury reduction reaction of stannous chloride devises the mercury reducing bottle that can continuously analyze, and realizes that water sample to be measured is restoring
The reduction reaction of bottle, cooperation argon gas realize the discharge of waste liquid after detection, realize the continuous detection of mercury；
3rd, the fluorescence detection of mercury lamp+photomultiplier, mercury lamp sends out 253.7 wavelength lights, after the reduction of irradiating and detecting water sample
The mercury vapour of generation, photomultiplier detection are excited rear mercury atom and return to the fluorescence intensity that ground state generates, realize to mercury concentration
Detection；
4th, the flow path switching system of syringe pump+eight ways valve+triple valve using the high-precision of syringe pump, realizes various reagents
Accurate quantification；Current-carrying liquid+argon gas isolation realizes syringe pump contact various reagents, reduces the material requirements of syringe pump, keeps away
The problem of having exempted from syringe pump pollution；
5th, the carrier gas flux of electronic flow control module accurately controls.In the utility model device, in order to realize detection knot
Fruit consistency is good, carries out control that is accurate, stablizing to carrier gas flux by electronic flow control module.
Description of the drawings
Fig. 1 is the structure diagram of the utility model.
Specific embodiment
Specific embodiment of the present utility model is made a detailed explanation below in conjunction with the accompanying drawings.
A kind of water quality total mercury detection device as shown in Figure 1, the device include eight ways valve 7, digestion tube 11,15 and of reducing bottle
Detection cell 5；The eight ways valve 7 has：First valve port is connected with the first feed pipe, and the first feed pipe is by setting the first electromagnetism
Valve 14 connects the reducing agent feed inlet of reducing agent material bottle and reducing bottle 15 respectively, and the capacity of the first feed pipe is extracted more than reducing agent
Amount, the second valve port are connected with the second feed pipe, and the second feed pipe connects the water sample feed inlet of reducing bottle 15, the appearance of the second feed pipe
Amount is more than water sample sample size, and third valve port is by setting second solenoid valve 13 to be connected with water sample feed pipe and standard liquid feed pipe, and the
Four valve ports are connected with nitric acid feed pipe, and the 5th valve port is by setting third solenoid valve 12 to connect the digestion tube 11, the 6th valve
Mouth is connected with waste liquid port, and the 7th valve port is connected with syringe pump 10, and syringe pump 10 is connected with current-carrying liquid feed pipe, and the 7th valve port
The first end of the first three-way pipe is also associated with, the detection cell 5 described in the second end connection of the first three-way pipe, third end passes through flow
Meter 2 is connected with the first argon inlet pipe, and the 8th valve port is connected with water pipe；The discharge port of the reducing bottle 15 passes through setting the
Four solenoid valves 16 connect the detection cell 5；The reducing bottle 15 is additionally provided with waste liquid outlet.The reducing bottle 15 into
For gas port by the way that the 5th solenoid valve 3 is set to be connected with electronic flow control module 1, electronic flow control module 1 connects the second argon gas
Air inlet pipe.First argon inlet pipe and the second argon inlet pipe is connected to argon gas source, argon gas source by the second three-way pipe
17 and the 6th solenoid valve 18 of pressure reducing valve is provided between the second three-way pipe.The side of digestion tube 11 is provided with ultraviolet lamp 8, described
11 top of digestion tube be additionally provided with the 7th solenoid valve 9.The side of detection cell 5 is provided with mercury lamp 4, and opposite side is provided with photoelectricity times
Increase pipe 6.
The detection method of the device, this method include the following steps：
1）The cleaning of digestion tube 11 and reducing bottle 15：
Syringe pump 10 extracts 10% nitric acid and ejected wash water by 7 common end of eight ways valve, injects in digestion tube 11 and cleans, then will
Washing lotion, which is drawn back, is injected into cleaned and reduced bottle 15 in reducing bottle 15, and reducing bottle 15 empties later；
2）Water sample sample introduction is cleared up：
Ultraviolet lamp is opened, eight ways valve 7 extracts water sample, is injected into digestion tube 11, and continues to inject into digestion tube 11 few
It measures 10% nitric acid and promotes resolution, the water sample to be measured in ultra violet lamp digestion tube 11 is fully to clear up water sample to be measured, mercury in water at this time
Become dimercurion；
3）Water sample preparation enters reducing bottle 15：
Eight ways valve 7 extracts the water sample cleared up in digestion tube 11, injects the second feed pipe；Designing the second feed pipe will
More than water sample sample size, so the water sample after clearing up at this time has been rested in the second feed pipe；
4）Current-carrying liquid is replaced：
After water sample preparation sample introduction, syringe pump 10 extracts current-carrying liquid by current-carrying liquid end, is arranged by 7 waste liquid port of eight ways valve
Liquid plays the purpose for replacing current-carrying liquid between eight ways valve 7 and syringe pump 10；
5）Reducing agent sample introduction：
By eight ways valve 7, syringe pump 10 extracts a small amount of reducing agent, the amount of reducing agent extraction at this time be no more than the first feed pipe it
Between distance, that is, ensure reducing agent will not extract into eight ways valve common end；After syringe pump 10 extracts argon gas by eight ways valve 7,
Switch 7 mouthfuls of positions of eight ways valve, pushed to reducing agent in reducing bottle 15 with argon gas；
6）Detection：
After reducing agent sample introduction, 1 stability of flow of electronic flow control module is kept, argon gas is by the second argon inlet pipe, electricity
Enter in detection cell 5 after sub- flow-control module 1, the 5th solenoid valve 3, reducing bottle 15, the 4th solenoid valve 16 and carry out fluoroscopic examination；
The blank fluorescence signal of reducing agent is scanned at this time；Baseline value is recorded after stabilization；
7）Sample detection：
After Baseline detection, eight ways valve 7 extracts enough argon gas, by step 3）In be deposited in the second feed pipe water sample push-in
In reducing bottle 15；And be sent into water sample, fluoroscopic examination is carried out in detection cell 5, the signal data of mercury in water sample is swept immediately
It retouches；Data peaks is taken to preserve and record as fluorescent signal data；
8）Emptying cleaning：
Liquid in reducing bottle 15 can be emptied, and repeat step 1 by closing the 4th solenoid valve 16）It is clear after progress sample introduction
It washes.
The embodiment of the utility model has the characteristics that following：
1. water circuit system, using syringe pump as power source, syringe pump both ends can extract and drain, by one end to injection
Pump provides current-carrying liquid, and the other end connects eight ways valve as common end, extracts water sample sample introduction into digestion tube, which exists
In syringe pump is simultaneously as proportioning device and power source, without adding extra proportioning device.Water sample can be reduced to the full extent
The risk being contaminated in complex pipeline, and facilitate the cleaning on flow road.
2. having several big advantages by the method for current-carrying liquid sample introduction, first, current-carrying liquid carrier fluid completely cuts off relative to conventional air
It is more accurate on quantitative.Secondly, acid current-carrying liquid ensure that common end always full of being soaked in the pipeline of eight ways valve common end
The cleaning of pipeline is replaced the operation of a current-carrying liquid by each flow, further functions as the effect of cleaning channels, and play
Exclude the effect of common end bubble.
3. reducing agent sample introduction sets advantage.Since reducing agent contacts the special nature reacted with water sample standard liquid, so needing
It to avoid making reducing agent that cross contamination occur with water sample before detection as far as possible.Syringe pump-current-carrying liquid-eight ways valve system can be with
The easier physical isolation realized between reducing agent and water sample.By adding a triple valve, increase an area that can be quantified
Between 2-eight ways valve of solenoid valve mouth 1 utilize the part pipeline, realize it is quantitative extraction reducing agent be deposited in quantitative section and do not enter
Eight ways valve common end and sample introduction.The program it is possible to prevente effectively from reducing agent eight ways valve common end and water sample mutual pollution,
Ensure the cleaning of pipeline system.
4. argon gas pushes sample introduction advantage.The another key advantages of syringe pump-current-carrying liquid-eight ways valve system are restored pushing
During agent and water sample standard liquid sample introduction, have two large problems on measuring accuracy have very big influence, air interference problem and
Quantitative sample injection problem.If using common air push water sample sample introduction, a small amount of air is inevitably brought into, and air meeting
Generating very big quenching effect to fluorescence influences.Experimental data is influenced very big.And use liquid estimated amount sample introduction, i.e., first by water
Sample is full of pipeline, then is quantitatively pushed with carrier fluid.This method is it is possible to prevente effectively from the quenching of air influences, but inevitably go out
The problems such as existing port hangs liquid, to quantitatively impacting, and the program can cause sample introduction flow sufficiently complex, time lengthening, examination
The problems such as agent consumption increases.
And in existing syringe pump-current-carrying liquid-eight ways valve system, 7 mouthfuls of an argon gas mouth position eight ways valve can be added, it should
Argon gas mouth, which can have in the protection gas of gas circuit system, to be directly led out, the parameter requirements such as no air pressure, by syringe pump first by quantitative examination
Agent is pushed into pre- sample feeding pipe, then draws argon gas and reagent is pushed to enter reducing bottle.First, although gas pushes, power source is note
Pump is penetrated, reagent can completely be pushed into reducing bottle, be not in that air-flow shakiness leads to tube wall by sample introduction velocity-stabilization undisturbed
The problems such as hanging liquid；Secondly argon gas is protection gas, can be extracted in excessive argon gas push-in reducing bottle without worrying interference quenching etc.
Problem so that data precision greatly improves.
Claims (7)
1. a kind of water quality total mercury detection device, which is characterized in that the device includes multiple-way valve（7）, digestion tube（11）, reducing bottle
（15）And detection cell（5）；The multiple-way valve（7）Have：
One valve port is connected with the first feed pipe, and the first feed pipe is by setting the first solenoid valve（14）Reducing agent material bottle is connected respectively
And reducing bottle（15）Reducing agent feed inlet,
One valve port is connected with the second feed pipe, the second feed pipe connection reducing bottle（15）Water sample feed inlet,
One valve port is by setting second solenoid valve（13）Water sample feed pipe and standard liquid feed pipe are connected with,
One valve port is connected with nitric acid feed pipe,
One valve port is by setting third solenoid valve（12）The connection digestion tube（11）,
One valve port is connected with waste liquid port,
One valve port is connected with syringe pump（10）, syringe pump（10）Current-carrying liquid feed pipe is connected with,
One valve port is connected with the first end of the first three-way pipe, the detection cell described in the second end connection of the first three-way pipe（5）, third
End passes through flowmeter（2）The first argon inlet pipe is connected with,
One valve port is connected with water pipe；
The reducing bottle（15）Discharge port pass through set the 4th solenoid valve（16）The connection detection cell（5）；Described
Reducing bottle（15）Air inlet pass through set the 5th solenoid valve（3）It is connected with electronic flow control module（1）, electronic flow control
Module（1）Connect the second argon inlet pipe.
A kind of 2. water quality total mercury detection device according to claim 1, which is characterized in that first argon inlet pipe
Argon gas source is connected to by the second three-way pipe with the second argon inlet pipe, pressure reducing valve is provided between argon gas source and the second three-way pipe
（17）With the 6th solenoid valve（18）.
A kind of 3. water quality total mercury detection device according to claim 1, which is characterized in that the reducing bottle（15）Also set
It is equipped with waste liquid outlet, digestion tube（11）Top is additionally provided with the 7th solenoid valve（9）.
A kind of 4. water quality total mercury detection device according to claim 1, which is characterized in that multiple-way valve（7）For eight ways valve, eight
The first feed pipe described in the first valve port connection of port valve, the second valve port connection second feed pipe, the connection of third valve port
The second solenoid valve（13）；The 4th valve port connection nitric acid feed pipe, the 5th valve port connection third electromagnetism
Valve（12）, the 6th valve port connection waste liquid outlet, the 7th valve port connection syringe pump（10）And connect described the
The first end of one three-way pipe, the 8th valve port connection water pipe.
A kind of 5. water quality total mercury detection device according to claim 1, which is characterized in that digestion tube（11）Side setting
There is ultraviolet lamp（8）, detection cell（5）Side be provided with mercury lamp（4）, opposite side is provided with photomultiplier（6）.
6. a kind of water quality total mercury detection device according to claim 1, which is characterized in that the capacity of the second feed pipe is more than
Water sample sample size.
7. a kind of water quality total mercury detection device according to claim 1, which is characterized in that the capacity of the first feed pipe is more than
Reducing agent extraction amount.
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| CN201721749255.3U CN207540976U (en) | 2017-12-14 | 2017-12-14 | A kind of water quality total mercury detection device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109253994A (en) * | 2018-10-31 | 2019-01-22 | 中国石油天然气股份有限公司 | A kind of oil-gas-source mercury isotope detection method and device |
-
2017
- 2017-12-14 CN CN201721749255.3U patent/CN207540976U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109253994A (en) * | 2018-10-31 | 2019-01-22 | 中国石油天然气股份有限公司 | A kind of oil-gas-source mercury isotope detection method and device |
| CN109253994B (en) * | 2018-10-31 | 2021-05-28 | 中国石油天然气股份有限公司 | Oil and gas source mercury isotope detection method and device |
| US11119085B2 (en) | 2018-10-31 | 2021-09-14 | Petrochina Company Limited | Methods and devices for detecting mercury isotopes in oil-gas sources |
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