CN102221540A - Method and device for analyzing trace gaseous elemental mercury - Google Patents
Method and device for analyzing trace gaseous elemental mercury Download PDFInfo
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- CN102221540A CN102221540A CN2010101493722A CN201010149372A CN102221540A CN 102221540 A CN102221540 A CN 102221540A CN 2010101493722 A CN2010101493722 A CN 2010101493722A CN 201010149372 A CN201010149372 A CN 201010149372A CN 102221540 A CN102221540 A CN 102221540A
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 18
- 229910052753 mercury Inorganic materials 0.000 claims abstract description 30
- 238000000197 pyrolysis Methods 0.000 claims abstract description 30
- 238000004458 analytical method Methods 0.000 claims abstract description 17
- 239000012159 carrier gas Substances 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 3
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004454 trace mineral analysis Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims 1
- 238000004445 quantitative analysis Methods 0.000 claims 1
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 238000003795 desorption Methods 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000012113 quantitative test Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 229910000497 Amalgam Inorganic materials 0.000 description 2
- 235000008645 Chenopodium bonus henricus Nutrition 0.000 description 2
- 244000138502 Chenopodium bonus henricus Species 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002530 cold vapour atomic fluorescence spectroscopy Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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Abstract
一种用于分析痕量气态单质汞的方法和装置，属于大气环境监测技术领域。该方法采用程控器控制分析全过程，将采集了大气气态单质汞(GEM)样品的捕汞管置于热解释放器后快速升温，释放的Hg0蒸气经除去携带的酸性组份后，进入二次富集/热解释放器，并被其中的捕汞管二次吸附。之后，二次富集/热解释放器快速升温，二次热解脱附的Hg0蒸气被载气吹入冷原子荧光检测器进行定量检测。本发明装置系统简单，运行可靠，捕汞管所采集的大气气态单质汞(GEM)样品，经过二次富集与热解释后进行分析，可有效地降低仪器的检测限，满足大气GEM痕量分析的要求。
A method and device for analyzing trace gaseous elemental mercury, belonging to the technical field of atmospheric environment monitoring. The method adopts a program controller to control the whole process of analysis. The mercury trapping tube that collects the atmospheric gaseous elemental mercury (GEM) sample is placed in the pyrolysis releaser and then the temperature is raised rapidly. The released Hg 0 vapor is removed into the Secondary enrichment/pyrolysis releaser, and is secondarily adsorbed by the mercury trapping tube in it. Afterwards, the temperature of the secondary enrichment/pyrolysis releaser was raised rapidly, and the Hg 0 vapor desorbed by the secondary thermal desorption was blown into the cold atomic fluorescence detector by the carrier gas for quantitative detection. The device system of the present invention is simple and reliable in operation. The atmospheric gaseous elemental mercury (GEM) sample collected by the mercury trap can be analyzed after secondary enrichment and thermal interpretation, which can effectively reduce the detection limit of the instrument and meet the requirements of the atmospheric GEM trace. analysis requirements.
Description
Technical field
The invention belongs to the atmosphere environment supervision technical field, is a kind of trace form mercury in the atmosphere to be made up the method and apparatus of sampling.
Background technology
Mercury (Hg) is a kind of highly toxic, interior nonessential heavy metal element of biosome, also is unique heavy metal contaminants that mainly is present in atmosphere with gaseous form.Atmospheric environment is the important place that the mercury migration transforms, and the mercury in the atmospheric environment mainly is divided into according to the physical chemistry form: gaseous elemental mercury (Hg
0, Gaseous ElementalMercury, GEM), active gaseous mercury (Hg
2+, Reactive Gaseous Mercury, RGM) and three kinds of particle mercuries (pHg, Particle Mercury is adsorbed in the Atmospheric particulates).Wherein, GEM accounts for about 90% of atmosphere total mercury, and global GEM concentration background value is about 1.5～2.0ng/m
3Because have higher volatility and very low water-soluble, GEM very easily becomes global contaminant by the diffusion mobility of growing distance in general circulation, the mean residence time in atmosphere is about 0.5～2a.
Since the industrial revolution, the mercury release strength of artificial source constantly increases.Research thinks, wherein the burst size of GEM is about 1480t approximately to airborne release 2100t mercury every year for global artificial source.About 500～700 tons/year of China's artificial source atmosphere mercury emission, the more main cause of mercury emissions are China, and the disposal of pollutants Governance Ability is comparatively backward to the demand of the energy is big.Coal-fired and non-ferrous metal metallurgy is the artificial mercury emissions source of two maximums, and average annual discharge capacity accounts for 80% of total release.Under quick urbanization of China and industrialized background, consumption sustainable growths such as fire coal, the atmosphere mercury emission also will constantly rise.
The method of sampling of GEM mainly contains wet absorption method and gold amalgam method in the atmosphere.Wet absorption is with the absorption liquid that contains strong oxidizer, as H
2O
2, KMnO
4-H
2SO
4, K
2Cr
2O
7-HNO
3(all form gaseous mercuries all are oxidized to Hg Deng the gaseous mercury that absorbs in the atmosphere
2+), utilize SnCl then
2Be reduced to Hg
0Steam adopts Cold Atomic Fluorescent Mercury method (CVAFS) or cold-vapour atomic absorption method (CVAAS) to measure at last.Owing to be subjected to the influence of reagent blank, the wet absorption method is subjected to great restriction on using.
Using at present wider is to utilize noble metal (golden mercury-traping tube) such as gold to carry out the sample preenrichment, pyrolysis afterwards, the Hg of release with the principle that mercury forms amalgam at normal temperatures
0Steam enters detecting device analyses such as CVAFS.This method has been eliminated the reagent blank problem in the chemical analysis, have blank low, golden mercury-traping tube and advantage such as can reuse, but still exist analyze consuming time, reappearance is relatively poor, and analysis result is subjected to problems such as the sampling process acidic gas in air influences.Therefore set up that the GEM reliable analytical method is very necessary in the atmosphere.
Summary of the invention
It is strong to the object of the present invention is to provide a kind of simple to operate, favorable reproducibility, anti-error to disturb, and realizes Atmospheric Trace gaseous elemental mercury (GEM) detection by quantitative fast, accurately, and satisfies the analysis requirement of the low detectability of atmosphere GEM.
Technical scheme of the present invention is that the big bicycle pump sample that mercury-traping tube (being generally gold-plated filler) is gathered is carried out pyrolysis release and secondary enrichment, carries out the secondary pyrolysis afterwards and discharges, at last by Cold Atomic Fluorescent Mercury detecting device quantitative test mercury content.
Analytical equipment is made up of parts such as sample pyrolysis release, clarifier, secondary enrichment/pyrolysis release, miniature cooling fan and program controllers.Select for use the nickel chromium triangle material as the sample heater strip, mini-fan is set cools off fast in order to mercury-traping tube, installing CaO powder clarifier is so that remove sour gas.
The structure of apparatus of the present invention is shown in Figure of description.The cavity of sample pyrolysis release (1) is circular quartz glass tube, and the outside twines scratches the nickel chromium triangle heater strip, to realize placing being rapidly heated of mercury-traping tube in the cavity, mini-fan is set simultaneously to realize that mercury-traping tube cools off fast; Clarifier is filled out the CaO powder in (2); The similar of secondary enrichment/pyrolysis release (3) and sample pyrolysis release (1), but mercury-traping tube wherein is the secondary enrichment that is used for mercury; Atomic fluorescence detecting device (4) is used for the quantitative test of mercury vapour; The duty of each parts of program controller (5) tunable control analysis device.
Operating process of the present invention is: the program control analysis operating condition that Atmospheric Trace mercury is set is rapidly heated the Hg of release after the mercury-traping tube of having gathered sample places the pyrolysis release
0Steam enters secondary enrichment/pyrolysis release after removing the acidic components that carries, by mercury-traping tube second adsorption wherein.Afterwards, the mini-fan of pyrolysis release starts, and with quick cooling sample mercury-traping tube, meanwhile, secondary enrichment/pyrolysis release is rapidly heated, the Hg of secondary pyrolysis desorption
0Steam is blown into the Cold Atomic Fluorescent Mercury detecting device by carrier gas and carries out quantitative test.
Characteristics of the present invention are mainly as follows:
(1) the atmosphere GEM sample gathered of mercury-traping tube is released through secondary enrichment and pyrolysis, has reduced the detectability of instrument effectively, satisfies the requirement of atmosphere GEM trace analysis.
(2) Hg that a pyrolysis is discharged
0Steam flow purifies, and reducing sour gas may be to the influence of detecting device generation.
(3) adopt program control technology, analytic process is simple, quick, realizes robotization.
Description of drawings
Figure of description Atmospheric Trace form mercury harvester synoptic diagram
Embodiment
Embodiment 1:
Gather atmosphere GEM sample under the fine weather condition, place described analytical equipment.It is 20～100mL/min that carrier gas (high-purity Ar) flow is set, and sample pyrolysis release is managed interior Hg at 300～700 ℃ of following heated sample mercury-traping tube 10～60s
0Steam is through purifying by the secondary enrichment, at 300～700 ℃ of heating secondary enrichment down/pyrolysis release 0～60s, the Hg that the secondary pyrolysis discharges
0Steam enters the fluorescence detector analysis, and the atmosphere GEM concentration of acquisition is 3.6ng/m
3, the relative deviation of continuous online mercury vapor analyzer monitoring concentration mean value is 3.5% with the same period.
Embodiment 2:
Under the thick weather condition, gather atmosphere GEM sample, place described analytical equipment.It is 20～100mL/min that carrier gas (high-purity Ar) flow is set, and sample pyrolysis release is managed interior Hg at 300～700 ℃ of following heated sample mercury-traping tube 10～60s
0Steam is through purifying by the secondary enrichment, at 300～700 ℃ of heating secondary enrichment down/pyrolysis release 0～60s, the Hg that the secondary pyrolysis discharges
0Steam enters the fluorescence detector analysis, and the atmosphere GEM concentration of acquisition is 5.3ng/m
3, the relative deviation of continuous online mercury vapor analyzer monitoring concentration mean value is 2.9% with the same period.
Claims (5)
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| CN2010101493722A CN102221540A (en) | 2010-04-15 | 2010-04-15 | Method and device for analyzing trace gaseous elemental mercury |
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|---|---|---|---|
| CN2010101493722A CN102221540A (en) | 2010-04-15 | 2010-04-15 | Method and device for analyzing trace gaseous elemental mercury |
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| Publication Number | Publication Date |
|---|---|
| CN102221540A true CN102221540A (en) | 2011-10-19 |
Family
ID=44778150
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103604892A (en) * | 2013-11-28 | 2014-02-26 | 北京雪迪龙科技股份有限公司 | Mercury monitoring apparatus and mercury monitoring method |
| CN103616269A (en) * | 2013-11-28 | 2014-03-05 | 北京雪迪龙科技股份有限公司 | Mercury monitoring method |
| CN103852370A (en) * | 2014-03-04 | 2014-06-11 | 天津市环境保护科学研究院 | Mobile low-temperature adsorption concentration-thermal desorption device and application method thereof |
| CN105044000A (en) * | 2015-06-29 | 2015-11-11 | 天津师范大学 | Dispersion-free gas phase photometer |
| CN106442606A (en) * | 2016-09-28 | 2017-02-22 | 华中科技大学 | A method and device for identifying mercury species |
| CN107389387A (en) * | 2017-06-26 | 2017-11-24 | 杭州超距科技有限公司 | Portable trace mercury analyzer |
| CN107462557A (en) * | 2017-07-31 | 2017-12-12 | 贵州民族大学 | A kind of power plant's Mercury In The Air detection method |
| CN107880970A (en) * | 2017-11-14 | 2018-04-06 | 华北电力大学（保定） | A kind of microwave radiation formula low-temperature pyrolysis of coal demercuration system and application method |
| CN109061063A (en) * | 2018-08-10 | 2018-12-21 | 中国石油天然气股份有限公司 | Tower column structure for evaluating performance of natural gas mercury removing agent |
| CN109142017A (en) * | 2018-09-12 | 2019-01-04 | 河南理工大学 | Separation, collecting device and the method for mercury in a kind of crude oil |
| CN109613181A (en) * | 2018-11-28 | 2019-04-12 | 中国计量科学研究院 | A standard generation system for trace gaseous mercury |
| CN109883803A (en) * | 2017-12-06 | 2019-06-14 | 中国科学院大连化学物理研究所 | A device and method for secondary enrichment analysis |
| CN110462368A (en) * | 2017-03-31 | 2019-11-15 | 拉皮斯坎系统股份有限公司 | The heating of quick desorption device and cooling for trace detection |
| CN110864946A (en) * | 2019-11-13 | 2020-03-06 | 清华大学 | A device and method for measuring mercury content in flue gas |
| CN111398328A (en) * | 2020-04-30 | 2020-07-10 | 江苏天瑞仪器股份有限公司 | On-line monitoring method and monitoring device for concentration of various target elements in flue gas |
| CN112649457A (en) * | 2021-01-15 | 2021-04-13 | 钢研纳克检测技术股份有限公司 | X-ray fluorescence rapid analysis method for trace heavy metal mercury in solid sample |
| CN113884649A (en) * | 2021-11-05 | 2022-01-04 | 中国科学院地球化学研究所 | Automatic analysis device for analyzing gaseous total mercury |
| CN114235761A (en) * | 2021-11-24 | 2022-03-25 | 清华大学 | Fractional Atmospheric Mercury Monitoring Equipment and Monitoring Methods |
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| CN103604892A (en) * | 2013-11-28 | 2014-02-26 | 北京雪迪龙科技股份有限公司 | Mercury monitoring apparatus and mercury monitoring method |
| CN103616269A (en) * | 2013-11-28 | 2014-03-05 | 北京雪迪龙科技股份有限公司 | Mercury monitoring method |
| CN103604892B (en) * | 2013-11-28 | 2015-09-23 | 北京雪迪龙科技股份有限公司 | A kind of mercury monitoring device and mercury monitoring method |
| CN103852370A (en) * | 2014-03-04 | 2014-06-11 | 天津市环境保护科学研究院 | Mobile low-temperature adsorption concentration-thermal desorption device and application method thereof |
| CN105044000A (en) * | 2015-06-29 | 2015-11-11 | 天津师范大学 | Dispersion-free gas phase photometer |
| CN106442606A (en) * | 2016-09-28 | 2017-02-22 | 华中科技大学 | A method and device for identifying mercury species |
| CN106442606B (en) * | 2016-09-28 | 2019-01-15 | 华中科技大学 | A kind of method and apparatus identifying mercury shape |
| CN110462368A (en) * | 2017-03-31 | 2019-11-15 | 拉皮斯坎系统股份有限公司 | The heating of quick desorption device and cooling for trace detection |
| CN107389387A (en) * | 2017-06-26 | 2017-11-24 | 杭州超距科技有限公司 | Portable trace mercury analyzer |
| CN107462557A (en) * | 2017-07-31 | 2017-12-12 | 贵州民族大学 | A kind of power plant's Mercury In The Air detection method |
| CN107880970A (en) * | 2017-11-14 | 2018-04-06 | 华北电力大学（保定） | A kind of microwave radiation formula low-temperature pyrolysis of coal demercuration system and application method |
| CN107880970B (en) * | 2017-11-14 | 2023-10-31 | 华北电力大学（保定） | Microwave radiation type coal low-temperature pyrolysis mercury removal system and use method thereof |
| CN109883803A (en) * | 2017-12-06 | 2019-06-14 | 中国科学院大连化学物理研究所 | A device and method for secondary enrichment analysis |
| CN109061063A (en) * | 2018-08-10 | 2018-12-21 | 中国石油天然气股份有限公司 | Tower column structure for evaluating performance of natural gas mercury removing agent |
| CN109061063B (en) * | 2018-08-10 | 2021-01-01 | 中国石油天然气股份有限公司 | Tower column structure for evaluating performance of natural gas mercury removing agent |
| CN109142017A (en) * | 2018-09-12 | 2019-01-04 | 河南理工大学 | Separation, collecting device and the method for mercury in a kind of crude oil |
| CN109142017B (en) * | 2018-09-12 | 2023-09-12 | 河南理工大学 | Equipment and method for separating and collecting mercury in crude oil |
| CN109613181A (en) * | 2018-11-28 | 2019-04-12 | 中国计量科学研究院 | A standard generation system for trace gaseous mercury |
| CN109613181B (en) * | 2018-11-28 | 2022-03-22 | 中国计量科学研究院 | A standard generation system for trace gaseous mercury |
| CN110864946A (en) * | 2019-11-13 | 2020-03-06 | 清华大学 | A device and method for measuring mercury content in flue gas |
| CN111398328A (en) * | 2020-04-30 | 2020-07-10 | 江苏天瑞仪器股份有限公司 | On-line monitoring method and monitoring device for concentration of various target elements in flue gas |
| CN112649457A (en) * | 2021-01-15 | 2021-04-13 | 钢研纳克检测技术股份有限公司 | X-ray fluorescence rapid analysis method for trace heavy metal mercury in solid sample |
| CN113884649A (en) * | 2021-11-05 | 2022-01-04 | 中国科学院地球化学研究所 | Automatic analysis device for analyzing gaseous total mercury |
| CN114235761A (en) * | 2021-11-24 | 2022-03-25 | 清华大学 | Fractional Atmospheric Mercury Monitoring Equipment and Monitoring Methods |
| CN114235761B (en) * | 2021-11-24 | 2023-01-24 | 清华大学 | Different forms of atmospheric mercury monitoring equipment and monitoring methods |
| WO2023093203A1 (en) * | 2021-11-24 | 2023-06-01 | 清华大学 | Monitoring device and monitoring method for atmospheric mercury in different states |
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Application publication date: 20111019 |