CN114544744A - Rapid mercury measurement method - Google Patents
Rapid mercury measurement method Download PDFInfo
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- CN114544744A CN114544744A CN202210138511.4A CN202210138511A CN114544744A CN 114544744 A CN114544744 A CN 114544744A CN 202210138511 A CN202210138511 A CN 202210138511A CN 114544744 A CN114544744 A CN 114544744A
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- mercury
- gas
- flue gas
- detection unit
- enriched
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 69
- 238000000691 measurement method Methods 0.000 title claims abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 24
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003546 flue gas Substances 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 18
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001871 ion mobility spectroscopy Methods 0.000 claims abstract description 14
- 229910052737 gold Inorganic materials 0.000 claims abstract description 13
- 239000010931 gold Substances 0.000 claims abstract description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000497 Amalgam Inorganic materials 0.000 claims abstract description 11
- 239000002019 doping agent Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 13
- 239000012159 carrier gas Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- MHAOVLQYUNAHGO-UHFFFAOYSA-N gold mercury Chemical compound [Au].[Hg] MHAOVLQYUNAHGO-UHFFFAOYSA-N 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 10
- 238000000926 separation method Methods 0.000 abstract description 4
- 150000001298 alcohols Chemical class 0.000 abstract description 2
- 150000001299 aldehydes Chemical class 0.000 abstract description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract description 2
- 150000001412 amines Chemical class 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 150000002576 ketones Chemical class 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 239000012855 volatile organic compound Substances 0.000 abstract description 2
- 238000005070 sampling Methods 0.000 description 11
- 239000000523 sample Substances 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 3
- 238000002482 cold vapour atomic absorption spectrometry Methods 0.000 description 2
- 238000002530 cold vapour atomic fluorescence spectroscopy Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 238000004164 analytical calibration Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019688 fish Nutrition 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000004094 preconcentration Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 235000014102 seafood Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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Classifications
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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
- G01N27/622—Ion mobility spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a rapid measurement method of mercury, which is based on an ion mobility spectrometry detection unit, introduces gas enriched with mercury for detection, adds chloroform as a dopant, can realize rapid measurement of mercury, avoids the problem of data hysteresis, and provides scientific basis for monitoring and controlling mercury pollution; and since many volatile organic compounds, such as alcohols, amines, aldehydes, ketones, and alkanes do not ionize in the CD-IMS negative mode, these compounds do not interfere with the detection of Hg. The invention realizes the effective separation of the complex matrix and the element to be analyzed in the flue gas by means of the gold amalgam and realizes the direct detection of low-concentration mercury in the flue gas.
Description
Technical Field
The invention belongs to the field of environment, and particularly relates to a rapid mercury measurement method.
Background
Atomic Absorption Spectroscopy (AAS) and cold vapor atomic absorption spectroscopy (CV-AAS) are the primary techniques used to detect and measure mercury in environmental samples. Cold vapor atomic fluorescence spectroscopy (CV-AFS) is also widely used to analyze mercury content in different samples, such as water, food, fish and seafood, soil and ash. However, these techniques require multiple pre-concentration and sample preparation methods to achieve the determination of trace amounts of mercury in complex samples. Inductively coupled plasma mass spectrometry (ICP-MS) has been increasingly used for the detection and measurement of mercury as a rapid method. But there is a certain positive and negative deviation in the quantitative analysis of Hg by ICP-MS and a memory effect is shown.
The off-line mercury measuring method can only obtain an average value for a period of time, the pollution condition of mercury cannot be observed in time, the time consumption of sampling and analyzing is long, and the quick measurement of the mercury in the flue gas is very necessary.
Disclosure of Invention
The invention aims to overcome the defects and provide a rapid mercury measuring method, which can solve the delay problem of mercury sampling and testing and furthest shorten the sampling and testing time.
In order to achieve the above object, a method for rapid measurement of mercury includes the steps of:
s1, collecting mercury in the flue gas by using gold, wherein the mercury and the gold form gold amalgam to realize that the mercury content in the flue gas is not lower than 0.01 mu g/m3Separation and enrichment of concentrated mercury;
s2, heating the gold amalgam to 850-1000 ℃, and releasing the enriched mercury;
and S3, conveying the gas enriched with mercury into an ion mobility spectrometry detection unit through carrier gas, adding chloroform as a dopant, adjusting the ion mobility spectrometry detection unit to be in a CD-IMS negative mode, and detecting mercury in the flue gas to obtain a mercury detection result.
And when the enriched mercury is released, heating the gold amalgam for 0.1-1 minute.
And (3) conveying the gas enriched with mercury into the ion mobility spectrometry detection unit through carrier gas, wherein the flow rate of the carrier gas is 0.1-2L/min.
The peak value at the drift time of 7.55ms when the ion mobility spectrometry detection unit is in the negative mode is HgCl-，HgCl-Peak relative to Cl-The peak relative drift time was 1.52.
The temperature of the drift gas is 160-180 ℃, and the flow rate of the drift gas is 50-1000 mL/min.
Compared with the prior art, the method has the advantages that the detection is carried out by introducing the gas enriched with mercury on the basis of the ion mobility spectrometry detection unit and adding chloroform as a dopant, so that the rapid measurement of mercury can be realized, the problem of data hysteresis is avoided, and a scientific basis is provided for monitoring and controlling mercury pollution; and since many volatile organic compounds, such as alcohols, amines, aldehydes, ketones, and alkanes do not ionize in the CD-IMS negative mode, these compounds do not interfere with the detection of Hg. The method realizes effective separation of the complex matrix and the element to be analyzed in the flue gas by means of the gold amalgam, and realizes direct detection of low-concentration mercury in the flue gas.
Drawings
FIG. 1 is a system diagram of the present invention;
the system comprises a flue gas sampling probe 1, a back flushing system 2, a preprocessing system 3, an oxygen sensor 4, a mercury measuring system 5, a calibration system 6 and a data acquisition and transmission system 7.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
A method for rapid measurement of mercury, comprising the steps of:
s1, collecting mercury in the flue gas by using gold, wherein the mercury and the gold form gold amalgam to realize that the mercury content in the flue gas is not lower than 0.01 mu g/m3Separation and enrichment of concentrated mercury;
s2, heating the gold amalgam to 850-1000 ℃, and heating for 0.1-1 minute to release the enriched mercury;
s3, conveying the gas enriched with mercury into an ion mobility spectrometry detection unit through carrier gas, wherein the carrier gas flow is 0.1-2L/min, adding chloroform as a dopant, and adjusting the ion mobility spectrometry detection unit to be in a CD-IMS negative mode to flue gasMercury in the sample was detected, and the peak value at a drift time of 7.55ms was HgCl-，HgCl-Peak relative to Cl-The peak relative drift time was 1.52. The temperature of the drift gas is 160-180 ℃, the flow rate of the drift gas is 50-1000mL/min, and the detection result of mercury is obtained.
Referring to fig. 1, an on-line mercury measuring system is characterized by comprising a flue gas sampling probe 1, wherein the flue gas sampling probe 1 is inserted into a flue, the flue gas sampling probe 1 is connected with a pretreatment system 3, the pretreatment system 3 is connected with a mercury measuring system 5, an oxygen sensor 4 is arranged on a connecting pipeline of the pretreatment system 3 and the mercury measuring system 5, the oxygen sensor 4 is used for detecting the oxygen concentration in flue gas, the mercury measuring system 5 is connected with a data acquisition and transmission system 7, and a back-blowing system 2 is arranged on the flue gas sampling probe 1, so that the problem of blockage of the probe is solved; the blow-back system 2 may also be used as an interface for a meter calibration module. The mercury measuring system 5 and the flue gas sampling probe 1 are both connected with a calibration system 6, and the calibration system 6 is used for providing mercury standard gas. The mercury standard gas can be introduced into the flue gas sampling probe 1, the whole sampling test system is subjected to work such as gas tightness test, instrument calibration and the like, and the accuracy of the measurement data of the analysis system is ensured. The calibration system 6 may also send mercury standard gas to the mercury measurement system 5 for direct use in the calibration of the mercury analyzer.
The pretreatment system 3 is used for removing dust and water in the flue gas; the mercury measuring system 5 is used for heating the gold amalgam to 850-1000 ℃ and releasing the enriched mercury; and (3) conveying the gas enriched with mercury into an ion mobility spectrometry detection unit through carrier gas, adding chloroform as a doping agent, and adjusting the ion mobility spectrometry detection unit to a CD-IMS negative mode to detect mercury in the flue gas to obtain a mercury detection result. The data acquisition and transmission system 7 is used to collect data from the mercury measurement system 5. The data acquisition and transmission system 7 is used for acquiring and transmitting data of the mercury measurement system 5, and can transmit the data to a computer or a mobile phone in real time by adopting a communication bus or wireless transmission.
Claims (5)
1. A rapid mercury measurement method is characterized by comprising the following steps:
s1, collecting mercury in flue gas by using goldMercury and gold form gold amalgam to realize that the content of mercury in flue gas is not less than 0.01 mu g/m3Separating and enriching mercury with concentration;
s2, heating the gold amalgam to 850-1000 ℃, and releasing the enriched mercury;
and S3, conveying the gas enriched with mercury into an ion mobility spectrometry detection unit through carrier gas, adding chloroform as a dopant, adjusting the ion mobility spectrometry detection unit to be in a CD-IMS negative mode, and detecting mercury in the flue gas to obtain the concentration of mercury.
2. The method of claim 1, wherein the gold amalgam is heated for 0.1-1 min when the enriched mercury is released.
3. The method for rapidly measuring mercury according to claim 1, wherein the mercury-enriched gas is fed into the ion mobility spectrometry detection unit through a carrier gas, and the carrier gas flow is 0.1-2L/min.
4. The method of claim 1, wherein the peak value at drift time of 7.55ms in the negative mode of the ion mobility spectrometry detection unit is HgCl-，HgCl-Peak relative to Cl-The peak relative drift time was 1.52.
5. The method of claim 1, wherein the drift gas temperature is 160-180 ℃ and the drift gas flow rate is 50-1000 mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210138511.4A CN114544744A (en) | 2022-02-15 | 2022-02-15 | Rapid mercury measurement method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210138511.4A CN114544744A (en) | 2022-02-15 | 2022-02-15 | Rapid mercury measurement method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114544744A true CN114544744A (en) | 2022-05-27 |
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ID=81675878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210138511.4A Pending CN114544744A (en) | 2022-02-15 | 2022-02-15 | Rapid mercury measurement method |
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| Country | Link |
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| CN (1) | CN114544744A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101667518A (en) * | 2008-09-05 | 2010-03-10 | 中国科学院大连化学物理研究所 | Photoemission ionization source and application thereof in mass spectrometry or ion mobility spectrometry |
| CN101713762A (en) * | 2008-10-07 | 2010-05-26 | 中国科学院大连化学物理研究所 | Method for identifying and detecting halogenated hydrocarbons |
| CN103512945A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院大连化学物理研究所 | Application of chlorinated hydrocarbon compound in detection of explosives through using ion mobility spectrometry |
| CN103811265A (en) * | 2012-11-09 | 2014-05-21 | 中国科学院大连化学物理研究所 | Doping agent auxiliary ionization source and application thereof in ion mobility spectrometry |
| CN103868979A (en) * | 2012-12-12 | 2014-06-18 | 中国科学院大连化学物理研究所 | Method for detecting sulfide with reducing property |
| CN110864946A (en) * | 2019-11-13 | 2020-03-06 | 清华大学 | Device and method for measuring mercury content in flue gas |
-
2022
- 2022-02-15 CN CN202210138511.4A patent/CN114544744A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101667518A (en) * | 2008-09-05 | 2010-03-10 | 中国科学院大连化学物理研究所 | Photoemission ionization source and application thereof in mass spectrometry or ion mobility spectrometry |
| CN101713762A (en) * | 2008-10-07 | 2010-05-26 | 中国科学院大连化学物理研究所 | Method for identifying and detecting halogenated hydrocarbons |
| CN103512945A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院大连化学物理研究所 | Application of chlorinated hydrocarbon compound in detection of explosives through using ion mobility spectrometry |
| CN103811265A (en) * | 2012-11-09 | 2014-05-21 | 中国科学院大连化学物理研究所 | Doping agent auxiliary ionization source and application thereof in ion mobility spectrometry |
| CN103868979A (en) * | 2012-12-12 | 2014-06-18 | 中国科学院大连化学物理研究所 | Method for detecting sulfide with reducing property |
| CN110864946A (en) * | 2019-11-13 | 2020-03-06 | 清华大学 | Device and method for measuring mercury content in flue gas |
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