CN107991144A - A kind of coal pyrolysis gas Elemental Mercury sampling system - Google Patents
A kind of coal pyrolysis gas Elemental Mercury sampling system Download PDFInfo
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- CN107991144A CN107991144A CN201711236404.0A CN201711236404A CN107991144A CN 107991144 A CN107991144 A CN 107991144A CN 201711236404 A CN201711236404 A CN 201711236404A CN 107991144 A CN107991144 A CN 107991144A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
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Abstract
Mercury measurement sampling system in pyrolysis gas during being utilized the present invention relates to pyrolysis of coal.The present invention is surveyed in existing dry absorption on the basis of mercury method, designed, designed simultaneously establishes a set of sampling system, OHM methods are combined with Method 30B methods, sampling system includes the adsorbent of KCl solution and modified activated carbon, and the gaseous state bivalent mercury in flue gas and gaseous state nonvalent mercury are adsorbed respectively.The present invention is easy to operate, of low cost.Design sample system has the characteristics of mercury adsorption tube blank background value is low, and sampling volume is small, and the sampling time is short, sampling equipment packaging, transport facility, it is possible to achieve the analysis of gaseous state mercury shape in flue gas, has certain industrial value.
Description
Technical field
The invention belongs to gas Elemental Mercury detection technique field, and in particular to mercury is surveyed in pyrolysis gas during pyrolysis of coal utilizes
Measure sampling system, further to adsorption tube design to the adsorption treatment of mercury.
Background technology
One of main source to air discharge mercury is coal-fired, every year since mercury contaminants discharge caused by coal combustion accounts for people
Class activity discharges the major part of mercury.It is that effective coal-fired process that reduces is released to the rear gas detection improvement discharged after coal combustion
The measure of mercury quantity is put, this must just sample rear gas, detect mercury concentration therein.It is suitable according to different concentration selections
When control measures.
Mainly there are three kinds of forms in mercury in flue gas：Element mercury, bivalent mercury and particle states of matter mercury.Since mercury has zeroth order and two
The different shapes such as valency, its configuration can change because of the difference of the factor such as temperature or catalyst again, therefore to mercury contaminants
Detection is a difficult thing.Mainly there is Ontario flue gas wet sampling currently for the method for mercury in flue gas sampling
Method, adsorbent catch several distinct methods such as mercury method and mercury Continuous emission monitoring system, and wherein adsorbent catches mercury side
Method, is based particularly on the sorbent tube method of EPA Method30B standards（Hereinafter referred to as 30B methods）, because its is easy to operate, easy to taking
Band, the advantages that precision is high, both can be as reference method to the relatively accurate of the HgCEMS and HgSTMS installed in coal-burning boiler
Degree is detected examination ＆ verification, also can carry out conventional detection to the Hg of discharged from coal-fired boiler as standard method.
U.S.EPA Method30B are that the pairing with appropriate flow from flue or pipeline by being inserted into flue or pipeline is inhaled
Attached pipe extracts the flue gas of known volume, the calculating using the mercury being enriched on adsorption tube with sampling volume as discharge gas mercury concentration
Parameter.The mercury sampling system of 30B methods is referred at present, is all that adsorption tube is installed on feeler lever front end in accordance with 30B flows, is inserted into cigarette
In road or pipeline, and adsorption tube generally uses glass material, belongs to fragile article, is easily broken up in insertion flue or pipeline
And sampling is caused to fail；And sampling terminates to need replacing the adsorption tube of sampling feeler lever front end every time, is brought to spot sampling larger
Workload, reduce sampling efficiency.Meanwhile at the scene in complex environment, gas mercury sampling apparatus require it is easy to operate, into
This is low, small；The existence of mercury in flue gas under accurate response high temperature, high sulfur environment；Various valence states in accurate collection flue gas
Mercury；At the same time in order to ensure measurement accuracy and data validity, the collection of parallel double samples must be carried out during test every time, and complete
Scene recycling test.Existing sampling instrument generally existing sampling location is complicated, and it is inconvenient to carry, and sampling is of high cost, collection
Efficiency is low, and measurement accuracy is low, deviation is big, and environmental requirement is harsh, it is impossible to accurately reflects concentration under the various existences of mercury etc.
Problem.
The content of the invention
Solid absorbent sampling analysis method is employed in the present invention, since it does not have Process of Chemical Cleaning, also not to liquid
The absorption process of body, therefore it is fairly simple to operate, cost is relatively low.The method can not only realize gaseous state mercury shape in flue gas
Analysis, and it is low with mercury adsorption tube blank background value, and sampling volume is small, the shorter sampling time, easy to operate, of low cost
The advantages that, the packed and transported of sampling equipment is also more convenient.Since the concentration of Hg in coal pyrolysis gas will be higher by 10-30 times, pyrolysis
There is H in gas2The reducibility gas such as S exist, these are unfavorable for absorption of the adsorbent to Hg, and the boiling point of mercury is very low, in pyrolysis gas
The middle overwhelming majority all exists in a gaseous form, particle mercury proportion very little, and the influence to atmospheric environment is also relatively limited.This
Invention is directed to pyrolysis gas sampling environment, has inquired into the characterization of adsorption of adsorbent, has included the adsorption efficiency and adsorption time of adsorbent
Relation between adsorption temp, the method for sampling of proposition is practical, works well.
The present invention is on the basis of mercury method is surveyed in existing dry absorption, and designed, designed simultaneously establishes a set of sampling system, by OHM
Method is combined with Method 30B methods, and sampling system includes KCl solution (1mol/L) and adsorbent, respectively in flue gas
Gaseous state bivalent mercury and gaseous state nonvalent mercury are adsorbed.The adsorption tube of the present invention has a good performance, and its making material
Mercury background value is low, and secondly the adsorbent of filling is particularly adsorption efficiency and adsorption capacity to the good adsorption performance of mercury.Pyrolysis gas
Being passed through through silica wool filtering ensures the stability of sampling system in the absorption bottle equipped with Klorvess Liquid, and selective
Absorb bivalent mercury.And gaseous state nonvalent mercury then enters absorption bottle and is fitted with the adsorption tube absorption of adsorbent.Three sections of adsorption tube point.For
Ensure the measuring accuracy and adsorption efficiency of adsorption tube, the filling length and loading for having larger adsorbent.The method operates
Simplicity, again can be with the mercury shape in detection gas on the basis of measurement accuracy is ensured.After to be sampled, adsorption tube is taken out simultaneously
Mercury content in laboratory is using EPA747 methods measure silica wool with activated carbon in adsorption tube.
Technical scheme is as follows：
The present invention is that one kind is used for coal pyrolysis gas Elemental Mercury sampling system, which includes sampling gun, adsorption tube, absorption
Agent, solution absorption cell；Sampling gun is connected with adsorption tube, and absorption tube inlet is equipped with silica wool, and adsorbent is located inside adsorption tube, molten
Liquid absorption cell is located at the adsorption tube port of export；Adsorption tube is quartz ampoule material；Adsorption tube is reducer pipe, and sampling gun is connected with adsorption tube
Inlet diameter tapers into, and internal diameter fades to 4mm by 10mm；Adsorption tube points three sections, first segment are adsorption section, internal diameter for 10mm ~
6mm；Second segment is to penetrate section, internal diameter 6mm；3rd section is pre-add bid section, and internal diameter is 6mm ~ 4mm；Adsorbent is activated carbon, is adopted
It is modified with halogen compounds, modifier preferred HCl, KI, NaBr, CaBr2、CuCl2、I2One or several kinds；Solution absorbs
Pond is equipped with the KCl solution that concentration is 1mol/L.
Adsorption tube of the present invention is arranged in parallel two, and first is mark-on adsorption tube, and second is common adsorption tube；Wherein plus
Mark adsorption tube is to fill activated carbon in adsorption section to add the mercury of known quantity to be used to carry out mark-on experiment, and common adsorption tube is filling nothing
Mercury activated carbon is used for the measure for carrying out mercury quantity；True mercury quantity is known with mark-on adsorption tube, reduces what common adsorption tube surveyed mercury quantity
Error.
The preferred cocoanut active charcoal of adsorbent of the present invention, method of modifying are：Corrresponding quality halide is weighed, activated carbon is impregnated
In halide solution, when concussion 24 is small under rotating speed is 150 revs/min of shaking table, then dried in 80 DEG C of constant temperature oven.
Adsorption tube of the present invention sets the internal and external threads or frosted interface that cooperate with sampling gun docking location.
Coal pyrolysis gas Elemental Mercury sampling system of the invention is easy to operate, cost is low, small；Solution absorbed pyrolysis of coal
Gas Elemental Mercury sampling system can react the concentration under high temperature, high sulfur environment in flue gas under gaseous mercury existence；Activated carbon is made
Gaseous mercury in low concentration dust atmosphere and flue gas can be reacted for adsorbent.Solution temperature is controlled 0 through ice bath in solution absorption cell
Below DEG C, the interference of reducing substances in flue gas can be excluded, the mercury of various valence states in flue gas can be accurately gathered, improve to flue gas
The collecting efficiency of middle mercury.Sampling system is set by double gas circuit structures carries out series connection sampling two-way Parallel Sampling, ensure that measurement
As a result the validity of accuracy, precision and data.
Brief description of the drawings
Fig. 1 is adsorption tube schematic diagram；Fig. 2 is coal pyrolysis gas Elemental Mercury sampling system schematic diagram, and label meaning is distinguished in Fig. 2
For；1：Sampling gun；2：Adsorption tube；3：Solution absorption cell；4：Flow divider；5：Ice bath absorbing liquid.
Embodiment
Coal pyrolysis gas Elemental Mercury sampling system includes sampling gun, adsorption tube, adsorbent, solution absorption cell；Sampling gun is with inhaling
Attached pipe is connected, and adsorption tube sets the internal and external threads or frosted interface that cooperate with sampling gun docking location.Adsorb tube inlet dress
There is silica wool, adsorbent is located inside adsorption tube, and solution absorption cell is located at the adsorption tube port of export；Adsorption tube is quartz ampoule material,
Adsorption tube is reducer pipe, and sampling gun is connected inlet diameter with adsorption tube and tapers into, and internal diameter fades to 4mm by 10mm.
As shown in Figure 1, adsorption tube points three sections, first segment are adsorption section, internal diameter 8mm；Second segment is to penetrate section, internal diameter
For 6mm；3rd section is pre-add bid section, internal diameter 6mm；The adsorbent is activated carbon, is modified using halogen compounds.
Solution absorption cell is equipped with the KCl solution that concentration is 1mol/L, and solution temperature is controlled 5 through ice bath in solution absorption cell
Below DEG C.
Adsorption tube is arranged in parallel two, and first is mark-on adsorption tube, and second is common adsorption tube；Wherein mark-on adsorbs
Pipe is to fill activated carbon in adsorption section to add the mercury of known quantity to be used to carry out mark-on experiment, and the common adsorption tube is filling mercury-free
Activated carbon is used for the test for carrying out total mercury.
Adsorbent is modified using halogen compounds, and adsorbent selects cocoanut active charcoal, activated carbon（It is conventional+modified）Ginseng
Number is as shown in table 2.The modifier used has HCl, KI, NaBr, CaBr2、CuCl2、I2, method of modifying is：Weigh corrresponding quality
Halide, 10% is dissolved in by 20g activated carbons and halide（200 milliliters）In solution, in shaking table（150 revs/min）Place 24 it is small when
Afterwards, dried in 80 DEG C of constant temperature oven.Table 1 is parameter after modified cocoanut active charcoal, and C1 is conventional cocoanut active charcoal, and C2 is to change
Property cocoanut active charcoal.
Table 1 selects activated carbon parameter
| Numbering | C1 | C2 |
| Particle diameter (mesh) | 16-30 (0.6-0.9 mm) | 8-16 |
| Moisture content (%) | ≤5 | ≤4 |
| Ash (%) | ≤5 | ≤4 |
| Bulk density (g/mL) | 0.32 | 0.25 |
Claims (5)
- A kind of 1. coal pyrolysis gas Elemental Mercury sampling system, it is characterised in that：The sampling system includes sampling gun, adsorption tube, suction Attached dose, solution absorption cell；Sampling gun is connected with adsorption tube, and absorption tube inlet is equipped with silica wool, and adsorbent is located inside adsorption tube, Solution absorption cell is located at the adsorption tube port of export；The adsorption tube is quartz ampoule material；The adsorption tube is reducer pipe, sampling gun with Adsorption tube connection inlet diameter tapers into, and internal diameter fades to 4mm by 10mm；Three sections of the adsorption tube point, first segment are absorption Section, internal diameter is 10mm ~ 6mm；Second segment is to penetrate section, internal diameter 6mm；3rd section is pre-add bid section, and internal diameter is 6mm ~ 4mm；Institute It is activated carbon to state adsorbent, is modified using halogen compounds, and modifier is HCl, KI, NaBr, CaBr2、CuCl2、I2One Kind is several；The solution absorption cell is equipped with the KCl solution that concentration is 1mol/L.
- 2. a kind of coal pyrolysis gas Elemental Mercury sampling system according to claim 1, it is characterised in that the adsorption tube is parallel Two are set, first is mark-on adsorption tube, and second is common adsorption tube；It is characterized in that the mark-on adsorption tube is to inhale Activated carbon is filled in attached section adds the mercury of known quantity to be used to carry out mark-on experiment, and the common adsorption tube is that filling mercury-free activated carbon is used In the measure for carrying out mercury quantity.
- 3. a kind of coal pyrolysis gas Elemental Mercury sampling system according to claim 1, it is characterised in that the adsorbent is coconut palm Shell activated carbon, through being immersed in halide solution, after rotating speed is when concussion 24 is small under 150 revs/min of shaking table, in 80 DEG C of constant temperature Gained is dried in baking oven.
- 4. a kind of coal pyrolysis gas Elemental Mercury sampling system according to claim 1, it is characterised in that the adsorption tube is with adopting Sample rifle docking location sets the internal and external threads or frosted interface to cooperate.
- A kind of 5. coal pyrolysis gas Elemental Mercury sampling system according to claim 1, it is characterised in that the solution absorption cell Middle solution temperature is controlled below 5 DEG C through ice bath.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013375A (en) * | 2019-12-30 | 2020-04-17 | 暨南大学 | CO2Absorption trap and method for improving detection peak shape of atmospheric volatile organic compound by using same |
| CN111426526A (en) * | 2020-04-16 | 2020-07-17 | 南京理工大学 | Device and method for simultaneously sampling multiple-valence mercury in coal-fired flue gas |
| CN112414790A (en) * | 2020-09-29 | 2021-02-26 | 清华大学 | Industry trace gaseous pollutant adsorbs and desorbs integration sampling pipe |
| CN112414791A (en) * | 2020-09-29 | 2021-02-26 | 清华大学 | Device and method for collecting trace sulfur trioxide in industrial gas |
| CN115112587A (en) * | 2022-07-22 | 2022-09-27 | 北京清新环境技术股份有限公司 | Method for detecting mercury content in industrial flue gas and dry adsorption sampling device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013375A (en) * | 2019-12-30 | 2020-04-17 | 暨南大学 | CO2Absorption trap and method for improving detection peak shape of atmospheric volatile organic compound by using same |
| CN111426526A (en) * | 2020-04-16 | 2020-07-17 | 南京理工大学 | Device and method for simultaneously sampling multiple-valence mercury in coal-fired flue gas |
| CN112414790A (en) * | 2020-09-29 | 2021-02-26 | 清华大学 | Industry trace gaseous pollutant adsorbs and desorbs integration sampling pipe |
| CN112414791A (en) * | 2020-09-29 | 2021-02-26 | 清华大学 | Device and method for collecting trace sulfur trioxide in industrial gas |
| CN112414790B (en) * | 2020-09-29 | 2021-08-24 | 清华大学 | Industry trace gaseous pollutant adsorbs and desorbs integration sampling pipe |
| CN112414791B (en) * | 2020-09-29 | 2022-03-18 | 清华大学 | Device and method for collecting trace sulfur trioxide in industrial gas |
| CN115112587A (en) * | 2022-07-22 | 2022-09-27 | 北京清新环境技术股份有限公司 | Method for detecting mercury content in industrial flue gas and dry adsorption sampling device |
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Application publication date: 20180504 |