CN109187716A - A kind of sulfur dioxide on-line monitoring method and system - Google Patents
A kind of sulfur dioxide on-line monitoring method and system Download PDFInfo
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- CN109187716A CN109187716A CN201811066607.4A CN201811066607A CN109187716A CN 109187716 A CN109187716 A CN 109187716A CN 201811066607 A CN201811066607 A CN 201811066607A CN 109187716 A CN109187716 A CN 109187716A
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- sulfur dioxide
- gas
- citrate solution
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- line monitoring
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
Abstract
The invention discloses a kind of sulfur dioxide on-line monitoring methods, comprising the following steps: (1) sampling to test sample gas；(2) it will be entered in citrate solution to test sample conductance by carrier gas, and obtain the citrate solution containing sulfur dioxide；(3) after the gas evolution insoluble in citrate solution, the citrate solution containing sulfur dioxide is performed under heating conditions parsing, obtains sulfur dioxide gas；(4) under conditions of 150 DEG C or more, sulfur dioxide gas obtained by above-mentioned parsing and distilled water is mixed according to the ratio of volume ratio 1:2-3, obtain mixed gas；(5) mixed gas is ionized using ultraviolet source, and carries out ionic migration spectrum detection.The present invention also provides a kind of systems for implementing this method.The present invention is controlled by above-mentioned multipolarity, greatly improves the accuracy of sulfur dioxide detection, and the sulfur dioxide suitable for low concentration accurately measures.
Description
Technical field
The present invention relates to pollutant monitoring technical field, in particular to a kind of sulfur dioxide on-line monitoring method and system.
Background technique
SO2It is most important a kind of sulfurous pollutants in air, atmosphere and ecological environment is very significant considering that.Such as
As chemical fumes, acid rain, greenhouse effects and ozone layer go to pot etc. it is closely bound up with it.SO2To the eye of people, nose, throat, lung
Equal organs have strong impulse, can cause mucositis, smell and dysgeusia, the chronic diseases such as lassitude.With dirt
Contaminate source emission standard receives tight and flue gas desulfurization in the universal of China increasingly, and the sulfur dioxide concentration of fixed-contamination source emission is got over
Next smaller, the sulfur dioxide concentration in even some places reaches the level of tens ppm.Therefore, how to this type
SO2Gas concentration, which carries out sensitivity monitoring, seems most important.
In the prior art, for SO2Detection, Environmental Protection in China standard mainly defines following several detection methods: one, first
Aldehyde absorbs Pararosaniline spectrophotometry；Two, tetrachloro mercury salt absorbs Pararosaniline spectrophotometry；Three, ultraviolet fluorescence method.
However in the case that sulfur dioxide concentration along with fixed-contamination source emission is smaller and smaller, the detection quality of above-mentioned detection method
It is unsatisfactory.
At the same time, the sulfur dioxide of low concentration is detected and generally uses ion mobility spectrometry in the prior art
Technology.Ion mobility spectrometry has high sensitivity as a kind of gas phase analysis method, and fast response time is cheap, uses
The advantages that facilitating is very suitable for the on-line analysis of gaseous sample.Under appropriate operating conditions, which can detecte
Into wherein medium with the amount of the micromicrogram order of magnitude or with gas existing for the concentration of one of trillion parts deal grades or evaporative substance.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of sulfur dioxide on-line monitoring methods, and two suitable for low concentration
In sulfur oxide on-line monitoring.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows:
A kind of sulfur dioxide on-line monitoring method, comprising the following steps:
(1) sampling to test sample gas；
(2) it will be entered in citrate solution to test sample conductance by carrier gas, it is molten to obtain the citrate containing sulfur dioxide
Liquid；
(3) after the gas evolution insoluble in citrate solution, the citrate solution containing sulfur dioxide is being added
It is parsed under heat condition, obtains sulfur dioxide gas；
(4) under conditions of 150 DEG C or more, by sulfur dioxide gas obtained by above-mentioned parsing and distilled water according to volume ratio 1:
The ratio of 2-3 is mixed, and mixed gas is obtained；
(5) mixed gas is ionized using ultraviolet source, and carries out ionic migration spectrum detection.
Preferably, in order to guarantee that the sulfur dioxide to contain in test sample gas is sufficiently absorbed, in the step (2)
The pH value of citrate solution is 1-3, concentration 0.5-1.5mol/L.
Preferably, the citrate solution containing sulfur dioxide gas is either micro- by water-bath in the step (3)
Wave carries out heating and is parsed.
Preferably, the ultraviolet source is vacuum UV lamp, xenon lamp either ultraviolet laser.
Preferably, the carrier gas is that atmosphere gained after a kind of in active carbon or molecular sieve or two kinds of filterings is clean
Air.
The present invention also provides a kind of system for implementing this method, sampling probe, the first container including successively piping connection,
Second container, ionic migration spectrometer accommodate citrate solution in the first container；It further include to heat the first container
Heating device and ultraviolet source that mixed gas in second container is ionized；Carrier gas is connected on the sampling probe
Pipeline；Distillation water lines are connected on the second container.
The beneficial effects of the present invention are:
(1) present invention, will be to the interference in test sample gas by that will be dissolved in citrate solution to test sample gas by carrier gas
After the gas discharge not soluble in water such as atmospheric CO, nitric oxide, then by heating to the citric acid containing sulfur dioxide
Salting liquid carries out parsing to isolated more pure sulfur dioxide gas, finally by isolated sulfur dioxide gas
It uses distilled water as carrier to be ionized, and then carries out ionic migration spectrum detection.It is controlled by above-mentioned multipolarity, is greatly mentioned
The high accuracy of sulfur dioxide detection, the sulfur dioxide suitable for low concentration accurately measure.
(2) present invention in citrate solution can recycle carry out using, be conducive to save reagent consumption.
(3) pure air obtained by using atmosphere after a kind of in active carbon or molecular sieve or two kinds of filterings, which is used as, to be carried
Gas has and obtains quickly, advantage low in cost.
(4) system structure in the present invention is simple, easy to operate, may be implemented to carry out Gao Ling to the sulfur dioxide of low concentration
Quick detection, sensitivity can achieve ppt grades.
Detailed description of the invention
Fig. 1 is the structure diagram of sulfur dioxide on-line monitor system in the present invention.
In figure, 1- sampling probe, 2- the first container, 3- second container, 4- ionic migration spectrometer, 5- gas-carrier pipeline, 6- steaming
Distilled water pipeline.
Specific embodiment
Below with reference to embodiment and attached drawing, specific embodiments of the present invention will be further explained.It needs to illustrate herein
It is the explanation of these embodiments to be used to help to understand the present invention, but and do not constitute a limitation of the invention.Under in addition,
Technical characteristic involved in each embodiment of the present invention described in face as long as they do not conflict with each other can phase
Mutually combination.
As shown in Figure 1, a kind of sulfur dioxide on-line monitor system, the sampler 1, first including successively piping connection holds
Device 2, second container 3, ionic migration spectrometer 4 accommodate citrate solution in the first container 2；It further include to heat
The heating device (not shown) of the first container 2 and the ultraviolet source that mixed gas in second container 3 is ionized (figure
In be not shown)；Gas-carrier pipeline 5 is connected on the sampler 1；Distillation water lines 6 are connected on the second container 3.
Embodiment 1
A kind of sulfur dioxide on-line monitoring method, comprising the following steps:
(1) test sample gas is treated by sampling probe 1 to be sampled；
(2) being passed through carrier gas by gas-carrier pipeline 5 will enter in the first container 2 equipped with citrate solution to test sample conductance,
Wherein: carrier gas is atmosphere gained pure air after active carbon and molecular sieve filtration, and the pH of citrate solution is 1, concentration
For 0.5mol/L, the citrate solution containing sulfur dioxide is obtained；
(3) it after the gas evolution insoluble in citrate solution, is specifically set in the first container 2 there are three through-hole,
One for being connected to sampling probe 1, one is used to be connected to second container 3, and there are one for releasing before citrate solution parsing
It puts insoluble gas to use, release later then blocks the through-hole；By magnetic agitation water-bath heater to equipped with citrate solution
2 one side heating water bath of the first container, carry out magnetic agitation on one side, the citrate solution containing sulfur dioxide solved
Analysis, obtains more pure sulfur dioxide gas, wherein the temperature of heating water bath is 90 °, and the time of heating is 30min；
(4) under conditions of 150 DEG C, by gas obtained by above-mentioned parsing and distilled water according to the ratio of volume ratio 1:2 the
It is mixed in two containers 3, obtains mixed gas；
(5) mixed gas is ionized using vacuum UV lamp, and carries out ion mobility spectrometry using ionic migration spectrometer 4
Detection.
Embodiment 2
A kind of sulfur dioxide on-line monitoring method, comprising the following steps:
(1) test sample gas is treated by sampling probe 1 to be sampled；
(2) being passed through carrier gas by gas-carrier pipeline 5 will enter in the first container 2 equipped with citrate solution to test sample conductance,
Wherein: carrier gas is atmosphere gained pure air after active carbon filters, and the pH of citrate solution is 1.5, concentration is
1.5mol/L obtains the citrate solution containing sulfur dioxide；
(3) after the gas evolution insoluble in citrate solution, the first of citrate solution will be equipped with using microwave
Container 2 carries out heating parsing, to more pure sulfur dioxide gas, wherein the frequency of microwave is 2450MHz, microwave heating
Time be 10min；
(4) under conditions of 180 DEG C, by gas obtained by above-mentioned parsing and distilled water according to the ratio of volume ratio 1:3 the
It is mixed in two containers 3, obtains mixed gas；
(5) mixed gas is ionized using xenon lamp, and carries out ionic migration spectrum detection using ionic migration spectrometer 4.
Embodiment 3
A kind of sulfur dioxide on-line monitoring method, comprising the following steps:
(1) test sample gas is treated by sampling probe 1 to be sampled；
(2) being passed through carrier gas by gas-carrier pipeline 5 will enter in the first container 2 equipped with citrate solution to test sample conductance,
Wherein: carrier gas is atmosphere gained pure air after molecular sieve filtration, and the pH of citrate solution is 3, concentration 1mol/L,
Obtain the citrate solution containing sulfur dioxide；
(3) after the gas evolution insoluble in citrate solution, the first of citrate solution will be equipped with using microwave
Container 2 carries out heating parsing, and the frequency of microwave is 2425MHz, to more pure sulfur dioxide gas；Wherein, the frequency of microwave
Rate is 2450MHz, and the time of microwave heating is 15min；
(4) under conditions of 200 DEG C, gas obtained by above-mentioned parsing and distilled water are existed according to the ratio of volume ratio 1:2.5
It is mixed in second container 3, obtains mixed gas；
(5) mixed gas is ionized using ultraviolet laser, and carries out ion mobility spectrometry using ionic migration spectrometer 4
Detection.
The embodiments of the present invention are described in detail in conjunction with the embodiments above, but the present invention is not limited to described realities
Apply mode.For a person skilled in the art, in the case where not departing from the principle of the invention and spirit, to these embodiment party
Formula carries out a variety of change, modification, replacement and modification, still falls in protection scope of the present invention.
Claims (6)
1. a kind of sulfur dioxide on-line monitoring method, it is characterised in that: the following steps are included:
(1) sampling to test sample gas；
(2) it will be entered in citrate solution to test sample conductance by carrier gas, and obtain the citrate solution containing sulfur dioxide；
(3) after the gas evolution insoluble in citrate solution, by the citrate solution containing sulfur dioxide in fire-bar
It is parsed under part, obtains sulfur dioxide gas；
(4) under conditions of 150 DEG C or more, by sulfur dioxide gas obtained by above-mentioned parsing and distilled water according to volume ratio 1:2-3
Ratio mixed, obtain mixed gas；
(5) mixed gas is ionized using ultraviolet source, and carries out ionic migration spectrum detection.
2. a kind of sulfur dioxide on-line monitoring method according to claim 1, it is characterised in that: lemon in the step (2)
The pH value of lemon acid salt solution is 1-3, concentration 0.5-1.5mol/L.
3. a kind of sulfur dioxide on-line monitoring method according to claim 1, it is characterised in that: contain in the step (3)
There is the citrate solution of sulfur dioxide gas to carry out heating by water-bath either microwave to be parsed.
4. a kind of sulfur dioxide on-line monitoring method according to claim 1, it is characterised in that: the ultraviolet source is true
Empty ultraviolet lamp, xenon lamp either ultraviolet laser.
5. a kind of sulfur dioxide on-line monitoring method according to claim 1, it is characterised in that: the carrier gas is atmosphere warp
Cross one of active carbon or molecular sieve either two kinds filtering after gained pure air.
6. a kind of system to realize any one of claim 1-5 the method, it is characterised in that: connect including successively pipeline
Sampling probe (1), the first container (2), second container (3), the ionic migration spectrometer (4) connect, the first container (2) is middle to be accommodated
There is citrate solution；It further include heating device to heat the first container (2) and to mixed gas in second container (3)
The ultraviolet source ionized；Gas-carrier pipeline (5) are connected on the sampling probe (1)；It is connected on the second container (3)
It distills water lines (6).
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| CN201811066607.4A CN109187716A (en) | 2018-09-12 | 2018-09-12 | A kind of sulfur dioxide on-line monitoring method and system |
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| CN201811066607.4A CN109187716A (en) | 2018-09-12 | 2018-09-12 | A kind of sulfur dioxide on-line monitoring method and system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110552643A (en) * | 2019-10-10 | 2019-12-10 | 中国地质科学院勘探技术研究所 | Fidelity sampling device applied to shale gas and method for thermally analyzing shale gas |
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| CN1660761A (en) * | 2004-12-24 | 2005-08-31 | 西安建筑科技大学 | Method for deprivig sulfur dioxide in solution of citrate |
| CN1796354A (en) * | 2004-12-27 | 2006-07-05 | 西安建筑科技大学 | Method for eliminating sulfur dioxide in citrate solution enhanced by ultrasonic |
| CN1736551A (en) * | 2005-07-01 | 2006-02-22 | 西安建筑科技大学 | Method and equipment for removing sulfur dioxide from waste gas |
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| CN110552643A (en) * | 2019-10-10 | 2019-12-10 | 中国地质科学院勘探技术研究所 | Fidelity sampling device applied to shale gas and method for thermally analyzing shale gas |
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