CN109738571A - A kind of device and method dividing Valence change and measurement for gaseous mercury - Google Patents
A kind of device and method dividing Valence change and measurement for gaseous mercury Download PDFInfo
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- CN109738571A CN109738571A CN201910133370.5A CN201910133370A CN109738571A CN 109738571 A CN109738571 A CN 109738571A CN 201910133370 A CN201910133370 A CN 201910133370A CN 109738571 A CN109738571 A CN 109738571A
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- mercury
- absorption bottle
- peristaltic pump
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 148
- 238000005259 measurement Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000008859 change Effects 0.000 title claims abstract description 20
- 238000010521 absorption reaction Methods 0.000 claims abstract description 108
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 62
- 238000009833 condensation Methods 0.000 claims abstract description 19
- 230000005494 condensation Effects 0.000 claims abstract description 19
- 229910000474 mercury oxide Inorganic materials 0.000 claims abstract description 17
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims description 99
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 30
- 239000012670 alkaline solution Substances 0.000 claims description 17
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000012530 fluid Substances 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 abstract description 11
- 230000003647 oxidation Effects 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 abstract description 4
- 230000033116 oxidation-reduction process Effects 0.000 abstract description 3
- 238000011897 real-time detection Methods 0.000 abstract description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 36
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 7
- 239000003546 flue gas Substances 0.000 description 7
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 239000001119 stannous chloride Substances 0.000 description 4
- 235000011150 stannous chloride Nutrition 0.000 description 4
- 238000000738 capillary electrophoresis-mass spectrometry Methods 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004710 electron pair approximation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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Abstract
The invention discloses a kind of device and methods for dividing Valence change and measurement for gaseous mercury, device includes dedusting filter cylinder, condensation chamber, electric-control board, triple valve, multiple peristaltic pumps and multiple solution storage bottles are equipped with first order absorption bottle, second level absorption bottle, three-level absorption bottle and level Four absorption bottle in condensation chamber, it is connected with air inlet pipeline on dedusting filter cylinder, is connected with outlet pipe at the top of level Four absorption bottle；Maintaining condensation room temperature by electronic condenser is 2~6 DEG C；It is provided with triple valve on air inlet pipeline air inlet is divided into two-way and enters in different absorption bottles；The device of the invention is dusted under test gas, removes water, except the integrated treatment of sour gas, oxidation state mercury is converted to nonvalent mercury by the oxidation-reduction method absorbed using chemical solution, cooperation mercury in-line analyzer can realize element mercury, mercury oxide, state total mercury real-time detection.
Description
Technical field
The present invention relates to heavy metal Hg field of measuring technique in gas, more particularly to a kind of gaseous mercury that is used for divide Valence change
With the device and method of measurement.
Background technique
Mercury is a kind of trace heavy metal element, has the characteristics such as hypertoxicity, high volatile, migration and bioaccumulation,
Human body can be entered by modes such as breathing, skin contact, diet, harm is generated to human health and ecological environment.The energy in China
Source structure is based on coal, therefore fire coal becomes maximum Mercury In The Air emission source, accounts for about a quarter of artificial total mercury emission.
Nowadays, the situation is tense for mercury pollution, and the Test and control of mercury contaminants becomes the research hotspot of current clean coal utilization.
Gaseous mercury mainly includes three kinds of forms: gaseous elementary mercury (Hg0), gaseous oxidation mercury (Hg2+) and particulate Hg (Hgp).
It is particularly important to the accurately measurement of different shape mercury content in flue gas since the ratio of three kinds of mercury is different.It distinguishes in flue gas
Mercury shape is the important prerequisite realizing the on-line monitoring of mercury and mercury control and mercury contaminants and effectively removing, and is moved to mercury is probed into
Transfer law, exploitation Mercury vacancy technology, protection environment and energy-saving and emission-reduction have a very important significance.
At present the detecting instrument of mercury contaminants can only detection elements mercury, cannot directly detect mercury oxide.Thus how will
Conversion of oxidized mercury in gas be element mercury become current research core content and mercury pollution prevention and treatment it is in the urgent need to address
One of crucial problem.
Coal-fired flue-gas mercury shape concentration measuring method more mature at present mainly has 3 kinds: Ontario method (OHM) is inhaled
The attached offline sampling method of pipe (EPA Method 30B) and mercury on-line monitoring method (Hg-CEMS).The test method of OHM and 30B is opposite
It is cumbersome, therefore Hg-CEMS method has more prospect.The Hg-CEMS test macro of the prior art measures oxidation state mercury content
It needs by way of conversion equipment is reduced into the element mercury that can be measured.Therefore, the design is based on current mercury and detects skill
The research achievement of art is proposed, is designed, developing a kind of novel, easy, accurate, portable, inexpensive, practical coal-fired flue-gas
Middle mercury oxide high-precision conversion equipment cooperates the widely used mercury concentration in-line analyzer of existing maturation, it can be achieved that flue gas oxygen
Change mercury, element mercury, state total mercury concentration high-precision real-time detection.
Summary of the invention
In view of the above problems, it is an object of that present invention to provide a kind of oxidation-reduction methodes absorbed using chemical solution
Realize efficiently separating for oxidation state mercury and element mercury, at the same time, by mercury in-line analyzer, it can be achieved that element mercury, mercury oxide,
The device of the real-time detection of state total mercury.
In order to achieve the above object, The technical solution adopted by the invention is as follows: it is a kind of for gaseous mercury divide Valence change and
The device of measurement, the device include dedusting filter cylinder, condensation chamber, electric-control board, triple valve, multiple peristaltic pumps and multiple solution
Storage bottle is equipped with first order absorption bottle, second level absorption bottle, three-level absorption bottle and level Four absorption bottle in the condensation chamber, and described is molten
Liquid storage bottle includes KCl solution storage bottle, SnCl2Solution storage bottle, alkaline solution storage bottle and discharge solution storage bottle, connect on dedusting filter cylinder
There is air inlet pipeline, is connected with outlet pipe at the top of level Four absorption bottle.
The basic principle of apparatus of the present invention design is wet chemistry method, realizes gas using the oxidation-reduction method that chemical solution absorbs
State oxidation state mercury and element mercury efficiently separate；React SnCl in stannous chloride solution2+Hg2+→Hg0+Sn4++2Cl-, will
Mercury oxide is converted to the nonvalent mercury that can be measured, and state total mercury Hg can be obtained using mercury vapourmeter measurement output gasTConcentration；Chlorine
Change the KCl+Hg that reacts in potassium solution2+→HgCl2By Hg2+It absorbs, gas can be obtained using mercury vapourmeter measurement output gas
Middle oxidation mercury content Hg0；Finally utilize Hg2+=HgT-Hg0Oxidation mercury content Hg in flue gas can be obtained2+。
Air inlet pipeline is connected to the top of first order absorption bottle and second level absorption bottle by dedusting filter cylinder and triple valve, and one
The top of grade absorption bottle and second level absorption bottle is connected on three-level absorption bottle by pipeline and triple valve, the top of three-level absorption bottle
Pass through piping connection level Four absorption bottle.
The bottom of first order absorption bottle connects level-one peristaltic pump by disengaging liquid pipe, and the bottom of second level absorption bottle passes through liquid in-out
Pipe connects second level peristaltic pump, and the bottom of three-level absorption bottle connects three-level peristaltic pump, the bottom of level Four absorption bottle by disengaging liquid pipe
Level Four peristaltic pump is connected by outlet tube, level-one peristaltic pump is separately connected discharge solution storage bottle and KCl solution storage bottle by pipeline,
Second level peristaltic pump is separately connected discharge solution storage bottle and SnCl by pipeline2Solution storage bottle, three-level peristaltic pump are distinguished by pipeline
Solution storage bottle is discharged by piping connection in connection discharge solution storage bottle and alkaline solution storage bottle, level Four peristaltic pump.
Three-level absorption bottle of the present invention is made of two bottle body 3a and bottle body 3b in parallel, and the level Four absorbs
Bottle is made of two bottle body 4a and bottle body 4b in parallel；Peristaltic pump and alkaline solution storage are connected on bottle body 3a and bottle body 3b
Peristaltic pump and discharge solution storage bottle are connected on bottle, bottle body 4a and bottle body 4b.
The top of first order absorption bottle and second level absorption bottle on bottle body 3a, passes through pipe at the top of bottle body 3a by piping connection
Road connects bottle body 4a；The top of the first order absorption bottle and second level absorption bottle passes through piping connection on bottle body 3b, bottle body 3b
Top pass through piping connection bottle body 4b；Outlet pipe is respectively connected at the top of the bottle body 4a and bottle body 4b.
KOH or NaOH solution are equipped in alkaline solution storage bottle of the present invention；Pass through potassium hydroxide or sodium hydroxide
Solution bottle and condensing bulb can remove acid ingredient and water in gas, guarantee that mercury vapourmeter is done in the gas reduction for entering mercury vapourmeter
It disturbs, protects instrument.
First order absorption bottle of the present invention, second level absorption bottle and three-level absorption bottle are solution bottle, and the level Four is inhaled
Receipts bottle is condensing bulb；The top of solution bottle is equipped with air inlet and air outlet, and bottom is equipped with inlet and liquid outlet, inlet, outlet
Staggered on bottle body with liquid inlet and outlet, air inlet gos deep into solution bottle by pipeline, and liquid outlet gos deep into solution by pipeline
Bottle；The top of condensing bulb is equipped with inlet, outlet, and bottom is equipped with leakage fluid dram, and inlet, outlet and leakage fluid dram are arranged in one on bottle body
Straight line, leakage fluid dram are arranged between inlet, outlet, and air inlet gos deep into condensing bulb by pipeline；Air inlet pipe gos deep into phial, is lower than
Liquid level of solution, so that air inlet is sufficiently reacted with solution；Solution is entered in bottle by bottom liquid inlet mouth, after rising to drain open height
Discharge.Outlet tube is longer in vial, can prevent newly into discharged " short circuit " phenomenon of solution horse back, realize solution system
The dynamic equilibrium of system keeps solution fresh, improves Reduction with Stannous Chloride efficiency.Vial is in design between the outlet of bottom two
Exit angle is set, guarantees that managing interior no liquid when drain accumulates, and realizes waste liquid smooth discharge.
Electric-control board of the present invention is equipped with temperature controller and multiple control buttons, and the control button includes zeroth order
Mercury and total mercury automatically switch measurement button, zeroth order mercury measurement button, total mercury measurement button and stop measurement button；Electric-control board is logical
It crosses control route and is separately connected triple valve and peristaltic pump.
Peristaltic pump of the present invention is the dual-channel peristaltic pump with positive and negative rotating function；It is all the way feed pathway, all the way
For apocenosis passage, the use of conjugate solutions bottle can realize the disengaging balance of solution when opening, keep solution fresh；Instrument makes
Peristaltic pump reversion can be emptied into liquid in absorption bottle bottle by inlet tube after.
Divide the method for Valence change and measurement provided by the present invention for gaseous mercury, method is as follows:
1) control condensation room temperature is 2~6 DEG C, and the gas for being blended with mercury oxide and nonvalent mercury enters device by air inlet pipeline,
By the adjusting air inlet of triple valve, it is allowed to successively pass through first order absorption bottle, three-level absorption bottle, level Four absorption bottle, at this time level-one, three
Grade and level Four wriggling pump operation realize the update dynamic equilibrium of KCl and alkaline solution, and discharge gas is passed through in mercury vapourmeter and is carried out
Measurement, obtains the zeroth order mercury content in air inlet；
2) keeping condensation room temperature is 2~6 DEG C, and the gas for being blended with mercury oxide and nonvalent mercury enters device by air inlet pipeline,
It by the adjusting air inlet of electric T-shaped valve, is allowed to successively by second level absorption bottle, three-level absorption bottle and level Four absorption bottle, at this time two
Grade peristaltic pump, three-level peristaltic pump and level Four wriggling pump operation, realize SnCl2With the update dynamic equilibrium of alkaline solution, will be discharged
Gas is passed through in mercury vapourmeter and measures, and obtains the total mercury content in air inlet；
3) keeping condensation room temperature is 2~6 DEG C, and the gas for being blended with mercury oxide and nonvalent mercury enters device by air inlet pipeline,
Alternate run step 1) and step 2 at regular intervals are set by triple valve, level-one peristaltic pump and second level peristaltic pump, is passed through
Mercury vapourmeter measurement discharge gas, alternately measures total mercury and zeroth order mercury content in air inlet；
4) pass through Hg2+=HgT-Hg0It is calculated, obtains aoxidizing mercury content in air inlet；
5) after device use, the residual liquid in device is pooled in discharge solution storage bottle by peristaltic pump reversion, emptying dress
Interior solution is set, operation is terminated.
The concentration of the solution of KCl in KCl solution storage bottle of the invention are as follows: 1~3N equivalent concentration；The SnCl2Solution storage
SnCl in bottle2Solution concentration are as follows: 0.3~1N equivalent concentration；The concentration of the alkaline solution storage bottle neutral and alkali solution are as follows: 1~
3N equivalent concentration.
The present invention has the advantages that apparatus of the present invention absorb different valence state mercury in reduction method measurement flue gas using chemical solution
The mercury oxide of content/element mercury efficient conversion realizes the real-time update of chemical solution by dual-channel peristaltic pump, realizes dynamic
State balance, improves transfer efficiency.
Apparatus of the present invention are realized by process control electric T-shaped valve and peristaltic pump and automatically control switching, and maloperation is reduced,
Convenience flexible in application；The air inlet pipeline of device is equipped with dedusting filter cylinder, can be dusted, remove water under test gas, except sour gas
Integrated treatment, can be applied to coal-burning power plant, industrial exhaust gas, in laboratory mercury shape concentration real-time monitoring, have certain
Market popularization value.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention；
Fig. 2 a-2c is first order absorption bottle of the invention, the sectional structure chart of second level absorption bottle and three-level absorption bottle；
Fig. 3 a-3b is the sectional structure chart of level Four absorption bottle of the invention；
Fig. 4 is structural schematic diagram of the device of the invention in embodiment 2 and embodiment 7.
Wherein, 1 air inlet pipeline, 2 dedusting filter cylinders, 3-1,3-2,3-3 triple valve, 4,4a, 4b outlet pipe, 5 condensation chambers,
5-1 first order absorption bottle, 5-2 second level absorption bottle, 5-3 three-level absorption bottle, 5-3a bottle body 3a, 5-3b bottle body 3b, 5-4 level Four
Absorption bottle, 5-4a bottle body 4a, 5-4b bottle body 4b, 6 electric-control boards, 6-1 temperature controller, 6-2 nonvalent mercury and total mercury automatically switch to survey
Measure button, 6-3 zeroth order mercury measurement button, the total mercury measurement button of 6-4,6-5 stopping measurement button, 7-1 level-one peristaltic pump, 7-2 bis-
Grade peristaltic pump, 7-3,7-3a, 7-3b three-level peristaltic pump, 7-4 level Four peristaltic pump, 8-1 KCl solution storage bottle, 8-2 SnCl2Solution
Solution storage bottle, the gas outlet of 10-1 solution bottle, the air inlet of 10-2 solution bottle is discharged in storage bottle, 8-3 alkaline solution storage bottle, 8-4
Mouthful, the inlet of 10-3 solution bottle, the liquid outlet of 10-4 solution bottle, the gas outlet of 11-1 condensing bulb, 11-2 condensing bulb
Air inlet, the leakage fluid dram of 11-3 condensing bulb.
Specific embodiment
The present invention is described in further detail with specific embodiment for explanation with reference to the accompanying drawing.
Embodiment 1: a kind of device dividing Valence change and measurement for gaseous mercury as shown in Figure 1, the device packet
Include dedusting filter cylinder 2, condensation chamber 5, electric-control board 6, triple valve 3-1,3-2,3-3, multiple peristaltic pump 7-1,7-2,7-3,7-4 and more
A solution storage bottle 8-1,8-2,8-3,8-4 are equipped with first order absorption bottle 5-1, second level absorption bottle 5-2, three-level in the condensation chamber
Absorption bottle 5-3 and level Four absorption bottle 5-4, the solution storage bottle include KCl solution storage bottle 8-1, SnCl2Solution storage bottle 8-2, alkali
Property solution storage bottle 8-3 and discharge solution storage bottle 8-4, be connected with air inlet pipeline 1, the top of level Four absorption bottle 5-4 on dedusting filter cylinder 2
It is connected with outlet pipe 4.
Air inlet pipeline 1 is connected to first order absorption bottle 5-1 and second level absorption bottle by dedusting filter cylinder 2 and triple valve 3-1
The top of the top of 5-2, first order absorption bottle 5-1 and second level absorption bottle 5-2 are connected to three-level by pipeline and triple valve 3-2 and absorb
On bottle 5-3, the top of three-level absorption bottle 5-3 passes through piping connection level Four absorption bottle 5-4.
The bottom of first order absorption bottle 5-1 connects level-one peristaltic pump 7-1, the bottom of second level absorption bottle 5-2 by disengaging liquid pipe
Second level peristaltic pump 7-2 is connected by disengaging liquid pipe, the bottom of three-level absorption bottle 5-3 connects three-level peristaltic pump 7- by disengaging liquid pipe
The bottom of 3, level Four absorption bottle 5-4 connect level Four peristaltic pump 7-4 by outlet tube, and level-one peristaltic pump 7-1 is connected respectively by pipeline
The solution storage bottle 8-4 and KCl solution storage bottle 8-1, second level peristaltic pump 7-2 out that run in is separately connected by pipeline is discharged solution storage bottle 8-
4 and SnCl2Solution storage bottle 8-2, three-level peristaltic pump 8-3 are separately connected discharge solution storage bottle 8-4 by pipeline and alkaline solution stores up
Solution storage bottle 8-4 is discharged by piping connection in bottle 8-3, level Four peristaltic pump 8-4.
Embodiment 2: as shown in figure 4, three-level absorption bottle 5-3 is made of two bottle body 5-3a and bottle body 5-3b in parallel,
The level Four absorption bottle 5-4 is made of two bottle body 5-4a and bottle body 5-4b in parallel；On bottle body 5-3a and bottle body 5-3b
It is connected on three-level peristaltic pump 7-3a, 7-3b and alkaline solution storage bottle 8-3, bottle body 5-4a and bottle body 5-4b and is connected with level Four wriggling
Pump 7-4 and discharge solution storage bottle 8-4.
The top of first order absorption bottle 5-1 and second level absorption bottle 5-2 pass through piping connection on bottle body 5-3a, bottle body 5-3a's
Top passes through piping connection bottle body 5-4a；Pass through piping connection at the top of the first order absorption bottle 5-1 and second level absorption bottle 5-2
On bottle body 5-3b, the top of bottle body 5-3b passes through piping connection bottle body 5-4b；The top of the bottle body 5-4a and bottle body 5-4b
Portion is respectively connected with outlet pipe 4a, 4b.
Embodiment 3: as shown in figs. 1 and 4, KOH or NaOH solution are equipped in alkaline solution storage bottle 8-3；Pass through potassium hydroxide
Or sodium hydroxide solution bottle and condensing bulb can remove acid ingredient and water in gas, guarantee that the gas for entering mercury vapourmeter is reduced
Instrument is protected in interference to mercury vapourmeter.
Embodiment 4: as shown in Fig. 1,2,3 and 4, first order absorption bottle 5-1, second level absorption bottle 5-2 and three-level absorption bottle 5-3 is equal
For solution bottle, the level Four absorption bottle 5-4 is condensing bulb；The top of solution bottle 5-1,5-2,5-3 be equipped with air inlet 10-2 and
Gas outlet 10-1, bottom are equipped with inlet 10-3 and liquid outlet 10-4, inlet, outlet 10-1 and 10-2 and liquid inlet and outlet 10-3
Staggered on bottle body with 10-4, air inlet 10-2 gos deep into solution bottle 5-1,5-2,5-3 by pipeline, and liquid outlet 10-4 passes through
Pipeline gos deep into solution bottle 5-1,5-2,5-3；The top of condensing bulb 5-4 is equipped with inlet, outlet 11-1 and 11-2, and bottom is equipped with drain
Mouthful 11-3, inlet, outlet 11-1,11-2 and leakage fluid dram 11-3 arrange in alignment on bottle body, and leakage fluid dram 11-3 setting exists
Between inlet, outlet 11-1 and 11-2, air inlet 11-2 gos deep into condensing bulb 5-4 by pipeline.
Embodiment 5: as shown in Fig. 1,4, electric-control board 6 is equipped with temperature controller 6-1 and multiple control buttons, the control
Button includes that nonvalent mercury automatically switches measurement button 6-2, zeroth order mercury measurement button 6-3, total mercury measurement button 6-4 with total mercury and stops
Only measure button 6-5；Electric-control board 6 by control route be separately connected triple valve 3-1,3-2,3-3 and peristaltic pump 7-1,7-2,
7-3,7-3a,7-3b,7-4.Peristaltic pump 7-1,7-2,7-3,7-3a, 7-3b, 7-4 are that the binary channels with positive and negative rotating function is compacted
Dynamic pump.
Embodiment 6: it as shown in Figure 1, being verifying apparatus of the present invention to oxidation state mercury Valence change effect, controls air inlet and always flows
Amount is 1.5L/min, and mercuryvapour generator exports Hg0Concentration is 35 μ g/m3, Hg2+Concentration is 15 μ g/m3, using Russian Lumex
The RA-915M mercury analyzer that company produces measurable nonvalent mercury concentration is measured mercury concentration in output gas, including as follows
Step:
1) solution is prepared:
KOH solution (1N): 112gKOH is dissolved with deionized water and is diluted to 2000ml.
KCl solution (1N): 149gKCl is dissolved with deionized water and is diluted to 2000ml.
Reduction with Stannous Chloride agent (SnCl2·2H2O, 100g/L): 200g stannous chloride is dissolved in 15% sulfuric acid solution,
And 2000ml is diluted to 15% sulfuric acid solution.
2) air inlet pipe and an air outlet pipe is cleaned with 10% nitric acid, the mercury for preventing pipeline from adsorbing has an impact to experimental result.
3) zeroth order mercury content is measured:
Adjusting temperature controller control condensation room temperature is 2-6 DEG C, presses zeroth order mercury measurement button, is mixed with mercury oxide and zeroth order at this time
The gas of mercury enters device by air inlet, and electric T-shaped valve regulating gas enters lower road, successively passes through absorption bottle 5-1,5-3,5-
4, peristaltic pump 7-1,7-3,7-4 is run at this time, maintains the update dynamic equilibrium of KCl, KOH solution, and output gas enters RA-915M
Zeroth order mercury content is measured in mercury vapourmeter, 10min average value is 34.6 μ g/m3, measurement real time data is 34.8 μ g/ after 2h
m3。
4) total mercury content is measured:
Adjusting temperature controller control condensation room temperature is 2-6 DEG C, when pressing total mercury measurement button, is mixed with mercury oxide and zeroth order at this time
The gas of mercury enters device by air inlet, and electric three passes valve regulation makes gas enter upper road, successively by absorption bottle 5-2,5-3,
5-4, peristaltic pump 7-2,7-3,7-4 is run at this time, maintains SnCl2, KOH solution update dynamic equilibrium, output gas enters RA-
Total mercury content is measured in 915M mercury vapourmeter, 10min average value is 49.2 μ g/m3, measurement real time data is 49.4 μ after 2h
g/m3.Output gas, which enters to measure in mercury vapourmeter, can be obtained total mercury content.
5) oxidation state mercury content is measured:
Utilize HgT=Hg2++Hg0, the concentration of the total mercury measured and nonvalent mercury is subtracted each other, it is flat to obtain oxidation state mercury concentration 10min
Mean value is 14.6 μ g/m3, measurement real time data is 14.6 μ g/m after 2h3。
6) nonvalent mercury and total mercury automatically switch to measure:
Adjusting temperature controller control condensation room temperature is 2-6 DEG C, presses nonvalent mercury and total mercury automatically switches measurement button, mix at this time
There is the gas of mercury oxide and nonvalent mercury to enter device by air inlet, electric T-shaped valve and peristaltic pump 7-1 and 7-2 are arranged to every 5
Minute alternate run process 1) and process 2), output gas is measured by mercury vapourmeter, 0-5min nonvalent mercury mean concentration is 34.8 μ
g/m3, 6-10min total mercury mean concentration is 49.4 μ g/m3, 10min mercury oxide mean concentration is 14.6 μ g/m before being calculated3。
Data are analyzed when choosing measurement close to 2h, and 110-115min nonvalent mercury mean concentration is 34.9 μ g/m3, 116-120min is total
Mercury mean concentration is 49.6 μ g/m3, it is 14.7 μ g/m that 10min internal oxidition mercury mean concentration at this time, which is calculated,3。
7) described device use finishes stop using after, press stopping measurement button invert peristaltic pump, all feed liquors
Pipe is pooled in the beaker of a dress waste liquid, is emptied solution in bottle, is realized discharging of waste liquid.
Above-mentioned measured data of experiment is analyzed, nonvalent mercury, mercury oxide, total mercury content average detected error are respectively less than
1%, error is smaller, is acceptable error.And since the solution in absorption bottle is in real-time update, measurement is remained to for a long time
Keep measurement accuracy.
Embodiment 7: as shown in figure 4, another embodiment of the present invention, including the absorption bottle 5-3a of two sets of KOH
It is sequentially communicated with 5-3b, liquor charging peristaltic pump 7-3a and 7-3b, condensing bulb 5-4a and 5-4b and outlet tube road 4a and 4b, remaining part
Pipe-line system.
In this embodiment, gas inlet is directly divided into two-way by triple valve: entering KCl absorption bottle 5-1, KOH all the way and inhales
It receives in bottle 5-3a, condensing bulb 5-4a, measurement gas outlet 4a output gas obtains nonvalent mercury concentration in air inlet；
Another way enters SnCl2In absorption bottle 5-2, KOH absorption bottle 5-3b, condensing bulb 5-4b, gas is exported in measurement gas outlet 4b
Body obtains state total mercury concentration in air inlet.
Cooperate the use simultaneously of two mercury vapourmeters can be in real time according to HgT=Hg2++Hg0Obtain oxidation state mercury concentration.
It should be noted that above-mentioned is only presently preferred embodiments of the present invention, protection model not for the purpose of limiting the invention
It encloses, any combination or equivalents made on the basis of the above embodiments all belong to the scope of protection of the present invention.
Claims (10)
1. a kind of device for dividing Valence change and measurement for gaseous mercury, which is characterized in that the device includes dedusting filter cylinder,
Condensation chamber, electric-control board, triple valve, multiple peristaltic pumps and multiple solution storage bottles, be equipped in the condensation chamber first order absorption bottle,
Second level absorption bottle, three-level absorption bottle and level Four absorption bottle, the solution storage bottle include KCl solution storage bottle, SnCl2Solution storage
Bottle, alkaline solution storage bottle and discharge solution storage bottle, are connected with air inlet pipeline on dedusting filter cylinder, are connected at the top of level Four absorption bottle
Outlet pipe；
Air inlet pipeline is connected to the top of first order absorption bottle and second level absorption bottle by dedusting filter cylinder and triple valve, and level-one is inhaled
The top for receiving bottle and second level absorption bottle is connected on three-level absorption bottle by pipeline and triple valve, is passed through at the top of three-level absorption bottle
Piping connection level Four absorption bottle；
The bottom of first order absorption bottle connects level-one peristaltic pump by disengaging liquid pipe, and the bottom of second level absorption bottle is connected by disengaging liquid pipe
Second level peristaltic pump is connect, the bottom of three-level absorption bottle connects three-level peristaltic pump by disengaging liquid pipe, and the bottom of level Four absorption bottle passes through
Outlet tube connects level Four peristaltic pump, and level-one peristaltic pump is separately connected discharge solution storage bottle and KCl solution storage bottle, second level by pipeline
Peristaltic pump is separately connected discharge solution storage bottle and SnCl by pipeline2Solution storage bottle, three-level peristaltic pump are separately connected by pipeline
Solution storage bottle and alkaline solution storage bottle is discharged, solution storage bottle is discharged by piping connection in level Four peristaltic pump.
2. the device according to claim 1 for dividing Valence change and measurement for gaseous mercury, which is characterized in that described three
Grade absorption bottle be made of two bottle body 3a and bottle body 3b in parallel, the level Four absorption bottle by two bottle body 4a in parallel with
Bottle body 4b is formed.
3. the device according to claim 2 for dividing Valence change and measurement for gaseous mercury, which is characterized in that the bottle
It is connected with peristaltic pump and alkaline solution storage bottle on body 3a and bottle body 3b, is connected with peristaltic pump on bottle body 4a and bottle body 4b and is discharged molten
Liquid storage bottle.
4. the device according to claim 2 for dividing Valence change and measurement for gaseous mercury, which is characterized in that described one
Through piping connection on bottle body 3a, the top of bottle body 3a passes through piping connection bottle body at the top of grade absorption bottle and second level absorption bottle
4a；The top of the first order absorption bottle and second level absorption bottle on bottle body 3b, is passed through by piping connection at the top of bottle body 3b
Piping connection bottle body 4b；Outlet pipe is respectively connected at the top of the bottle body 4a and bottle body 4b.
5. the device according to claim 1 for dividing Valence change and measurement for gaseous mercury, which is characterized in that the alkali
Property solution storage bottle in be equipped with KOH or NaOH solution.
6. the device according to claim 1 for dividing Valence change and measurement for gaseous mercury, which is characterized in that described one
Grade absorption bottle, second level absorption bottle and three-level absorption bottle are solution bottle, and the level Four absorption bottle is condensing bulb；
The top of solution bottle is equipped with air inlet and air outlet, and bottom is equipped with inlet and liquid outlet, inlet, outlet and liquid inlet and outlet
Mouth is staggered on bottle body, and air inlet gos deep into solution bottle by pipeline, and liquid outlet gos deep into solution bottle by pipeline；
The top of condensing bulb is equipped with inlet, outlet, and bottom is equipped with leakage fluid dram, and inlet, outlet and leakage fluid dram are arranged on bottle body
Straight line, leakage fluid dram are arranged between inlet, outlet, and air inlet gos deep into condensing bulb by pipeline.
7. the device according to claim 1 for dividing Valence change and measurement for gaseous mercury, which is characterized in that the electricity
Control panel and be equipped with temperature controller and multiple control buttons, the control button include nonvalent mercury and total mercury automatically switch measurement by
Button, zeroth order mercury measurement button, total mercury measurement button and stopping measurement button；Electric-control board is separately connected threeway by controlling route
Valve and peristaltic pump.
8. the device according to claim 1 for dividing Valence change and measurement for gaseous mercury, which is characterized in that described is compacted
Dynamic pump is the dual-channel peristaltic pump with positive and negative rotating function.
9. a kind of the apparatus according to claim 1 divides the method for Valence change and measurement for gaseous mercury, which is characterized in that
The method is as follows:
1) control condensation room temperature is 2~6 DEG C, and the gas for being blended with mercury oxide and nonvalent mercury enters device by air inlet pipeline,
By the adjusting air inlet of triple valve, it is allowed to successively pass through first order absorption bottle, three-level absorption bottle, level Four absorption bottle, at this time level-one, three
Grade and level Four wriggling pump operation realize the update dynamic equilibrium of KCl and alkaline solution, and discharge gas is passed through in mercury vapourmeter and is carried out
Measurement, obtains the zeroth order mercury content in air inlet；
2) keeping condensation room temperature is 2~6 DEG C, and the gas for being blended with mercury oxide and nonvalent mercury enters device by air inlet pipeline,
It by the adjusting air inlet of electric T-shaped valve, is allowed to successively by second level absorption bottle, three-level absorption bottle and level Four absorption bottle, at this time two
Grade peristaltic pump, three-level peristaltic pump and level Four wriggling pump operation, realize SnCl2With the update dynamic equilibrium of alkaline solution, will be discharged
Gas is passed through in mercury vapourmeter and measures, and obtains the total mercury content in air inlet；
3) keeping condensation room temperature is 2~6 DEG C, and the gas for being blended with mercury oxide and nonvalent mercury enters device by air inlet pipeline,
Alternate run step 1) and step 2 at regular intervals are set by triple valve, level-one peristaltic pump and second level peristaltic pump, is passed through
Mercury vapourmeter measurement discharge gas, alternately measures total mercury and zeroth order mercury content in air inlet；
4) pass through Hg2+=HgT-Hg0It is calculated, obtains aoxidizing mercury content in air inlet；
5) after device use, the residual liquid in device is pooled in discharge solution storage bottle by peristaltic pump reversion, emptying dress
Interior solution is set, operation is terminated.
10. the method according to claim 9 for dividing Valence change and measurement for gaseous mercury, which is characterized in that described
The concentration of the solution of KCl in KCl solution storage bottle are as follows: 1~3N；The SnCl2SnCl in solution storage bottle2Solution concentration are as follows: 0.3
~1N；The concentration of the alkaline solution storage bottle neutral and alkali solution are as follows: 1~3N.
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Cited By (1)
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| CN112924246A (en) * | 2021-01-29 | 2021-06-08 | 南京理工大学 | System and method for simultaneously capturing and sampling mercury with different valence states and provided with scaling spray pipe |
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