CN108393047A - A kind of reaction kettle and mercury capture structure for Trace Hg analysis - Google Patents

A kind of reaction kettle and mercury capture structure for Trace Hg analysis Download PDF

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Publication number
CN108393047A
CN108393047A CN201711294424.3A CN201711294424A CN108393047A CN 108393047 A CN108393047 A CN 108393047A CN 201711294424 A CN201711294424 A CN 201711294424A CN 108393047 A CN108393047 A CN 108393047A
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CN
China
Prior art keywords
trace
inlet pipe
air inlet
analysis
reaction kettle
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Pending
Application number
CN201711294424.3A
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Chinese (zh)
Inventor
刁星
曹梦西
刘广良
梁勇
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Jianghan University
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Jianghan University
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Publication date
Application filed by Jianghan University filed Critical Jianghan University
Priority to CN201711294424.3A priority Critical patent/CN108393047A/en
Publication of CN108393047A publication Critical patent/CN108393047A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention belongs to mercury Analytical Methods of Trace fields, disclose a kind of reaction kettle and mercury capture structure for Trace Hg analysis;The reaction kettle includes:Autoclave body, kettle cover and air inlet pipe;The kettle cover is connected with autoclave body cooperation;Air admission hole is opened up on the kettle cover, the air inlet pipe is arranged in the autoclave body, and the first end of the air inlet pipe is connected to the air admission hole, and the second end of the air inlet pipe extends to the autoclave body lower part;Venthole and liquid injection port are opened up on the kettle cover;Wherein, the autoclave body, kettle cover and air inlet pipe use polytetrafluoroethylene (PTFE).The present invention provides a kind of remaining reaction kettle of reduction mercury.

Description

A kind of reaction kettle and mercury capture structure for Trace Hg analysis
Technical field
The present invention relates to mercury Analytical Methods of Trace field, more particularly to a kind of reaction kettle and mercury for Trace Hg analysis is caught Structure set.
Background technology
Mercury compound is generally oxidized to divalent by the trace mercury compound in determination of the environment medium by digestion procedure at present Mercury ion, recycle reducing agent dimercurion is reduced into gaseous mercury in a kettle, using gold sand trap tube by with gas State mercury generates gold amalgam and traps gaseous mercury and fix, and finally utilizes atomic fluorescence or Atomic absorption instrument to measure gold amalgam and adsorbs The mercury concentration that pipe thermal desorption gets off.
Existing reaction bulb generally uses simple glass bottle or quartzy bottle, but outstanding in the new method for exploring measurement mercury sample Incomplete due to clearing up when it is the method for the mercury compound that exploitation measures synthesis, reduction dosage is not enough or the reaction time does not conform to The factors such as suitable, can cause mercury compound to be remained in reaction bulb, cause blank value higher experiment, measured value is unstable, finally Influence the accuracy of experimental result.Moreover, in remaining mercury compound in handling reaction bulb, it will also result in reaction bulb one Determine the damage of degree.
Invention content
The present invention provides a kind of reaction kettle and mercury capture structure for Trace Hg analysis, solves trace point in the prior art The technical issues of mercury remains in analysis.
In order to solve the above technical problems, the present invention provides a kind of reaction kettles for Trace Hg analysis, including:Autoclave body, Kettle cover and air inlet pipe;
The kettle cover is connected with autoclave body cooperation;
Open up air admission hole on the kettle cover, the air inlet pipe is arranged in the autoclave body, the first end of the air inlet pipe with The air admission hole connection, the second end of the air inlet pipe extend to the autoclave body lower part;
Venthole and liquid injection port are opened up on the kettle cover;
Wherein, the autoclave body, kettle cover and air inlet pipe use polytetrafluoroethylene (PTFE).
Further, the reaction kettle further includes:Suction nozzle;
The suction nozzle is connected to the air inlet pipe second end;
Through-hole array is opened up on the suction nozzle.
Further, the inlet suction port for connecting inert gas source is set on the air admission hole.
Further, the first end of the air inlet pipe is connected with the air admission hole screw thread, and is sealed by the first gasket;
The second end of the air inlet pipe is connected with the suction nozzle screw thread, and is sealed by the second gasket.
Further, the escape pipe for connecting mercury capture structure is set on the venthole.
Further, matching liquid injection port plug is set in the liquid injection port.
Further, observation window is opened up on the kettle cover, and closed by light transmission quartz glass.
Further, the light transmission quartz glass is pressed on by fixed block on the kettle cover;
Between the light transmission quartz glass and the kettle cover be arranged third gasket, the light transmission quartz glass with it is described solid Determine that the 4th gasket is arranged between block.
The autoclave body, kettle cover and air inlet pipe use polytetrafluoroethylene (PTFE).
A kind of Trace Hg analysis mercury capture structure, including:Purity nitrogen air source, gold sand trap tube and the reaction kettle;
Wherein, the purity nitrogen air source connects the air admission hole, and the gold sand trap tube connects the venthole.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
The reaction kettle for Trace Hg analysis provided in the embodiment of the present application, by the way that air inlet pipe and company are arranged in autoclave body Lead on kettle cover, path is blown to form air inlet;Under the cooperation in external pure nitrogen gas source, autoclave body bottom is purged so that gaseous state Mercury can be quickly discharged by venthole;Experiment acid-base value can preferably be reduced to anti-using the polytetrafluoroethylene material of acid-fast alkali-proof The influence of autoclave body is answered, and reduces the absorption residual of mercury, the rate of recovery of mercury reaches 95% or more.Meanwhile sealing structure is good, fluid injection It is convenient, it effectively reduces mercury in operating process and volatilizees, reduce influence of the mercury to health in experimentation.Pass through observation window, energy Timely observing response carries out.
Description of the drawings
Fig. 1 is the structural schematic diagram for the reaction kettle analyzed provided by the present invention for Trace Hg;
Fig. 2 is kettle cover provided by the invention and air inlet pipe fit structure schematic diagram;
Fig. 3 is kettle cover structural schematic diagram provided by the invention;
Fig. 4 is kettle cover inside structure schematic diagram provided by the invention;
Fig. 5 is suction nozzle structural schematic diagram provided by the invention.
Specific implementation mode
The embodiment of the present application solves existing skill by providing a kind of reaction kettle and mercury capture structure for Trace Hg analysis The technical issues of mercury remains in trace analysis in art.
In order to better understand the above technical scheme, in conjunction with appended figures and specific embodiments to upper It states technical solution to be described in detail, it should be understood that the specific features in the embodiment of the present invention and embodiment are to the application skill The detailed description of art scheme, rather than to the restriction of technical scheme, in the absence of conflict, the embodiment of the present application And the technical characteristic in embodiment can be combined with each other.
Referring to Fig. 1 and Fig. 2, a kind of reaction kettle for Trace Hg analysis, including:Autoclave body 1, kettle cover 2 and air inlet pipe 3.
The kettle cover 2 is connected with the cooperation of the autoclave body 1;Realization is stably connected with.
Referring to Fig. 3 and Fig. 4, air admission hole 8 is opened up on the kettle cover 2, the air inlet pipe 3 is arranged in the autoclave body 1, described The first end of air inlet pipe 3 is connected to the air admission hole 9, and the second end of the air inlet pipe 3 extends to 1 lower part of the autoclave body;To It forms purging path to purge gaseous mercury under the action of external pure nitrogen gas source, 10 row of venthole is opened up from the kettle cover 2 Go out.
Liquid injection port 8 is opened up on the kettle cover 2, is injected for reactant.Matched plug 7 is set simultaneously.It is general and The material of speech, plug selects silica gel.
Referring to Fig. 2 and Fig. 5, the reaction kettle further includes:Suction nozzle 4;The suction nozzle 4 and 3 second end of the air inlet pipe Connection;Through-hole array 15 is opened up on the suction nozzle 4.Hereby, it is achieved that the full angle water conservancy diversion of air-flow so that 1 bottom of autoclave body obtains Comprehensive purging reduces mercury residual.
In general, the inlet suction port 14 for connecting inert gas source is set on the air admission hole 9.
The first end of the air inlet pipe 3 is connected with 9 screw thread of the air admission hole, and is sealed by the first gasket;It is described into The second end of tracheae 3 is connected with 4 screw thread of the suction nozzle, and is sealed by the second gasket, lift structure reliability.
Tube spigot 11 is set on the kettle cover 2 and is connected to the venthole 10, the escape pipe for connecting mercury capture structure 13。
Observation window 12 is opened up on the kettle cover 2, and is closed by light transmission quartz glass 5.Convenient for observing 1 inside feelings of autoclave body Condition.
The light transmission quartz glass 5 is pressed on by fixed block 6 on the kettle cover 2;Lift-off seal stability.
In general, third gasket can also be set between the light transmission quartz glass 5 and the kettle cover 2, it is described 4th gasket can also be set between light quartz glass 5 and the fixed block 6.
Further, the autoclave body 1, kettle cover 2 and air inlet pipe 3 use polytetrafluoroethylene (PTFE).Mercury absorption can be effectively reduced, and And only use diluted acid soaking and washing.Cleaning process is simple and convenient.
The present embodiment also provides a kind of capture structure based on reaction kettle.
A kind of Trace Hg analysis mercury capture structure, including:Purity nitrogen air source, gold sand trap tube and the reaction kettle;
Wherein, the purity nitrogen air source connects the air admission hole, and the gold sand trap tube connects the venthole.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
The reaction kettle for Trace Hg analysis provided in the embodiment of the present application, by the way that air inlet pipe and company are arranged in autoclave body Lead on kettle cover, path is blown to form air inlet;Under the cooperation in external pure nitrogen gas source, autoclave body bottom is purged so that gaseous state Mercury can be quickly discharged by venthole;Experiment acid-base value can preferably be reduced to anti-using the polytetrafluoroethylene material of acid-fast alkali-proof The influence of autoclave body is answered, and reduces the absorption residual of mercury, the rate of recovery of mercury reaches 95% or more.Meanwhile sealing structure is good, fluid injection It is convenient, it effectively reduces mercury in operating process and volatilizees, reduce influence of the mercury to health in experimentation.Pass through observation window, energy Timely observing response carries out.
It should be noted last that the above specific implementation mode is merely illustrative of the technical solution of the present invention and unrestricted, Although being described the invention in detail with reference to example, it will be understood by those of ordinary skill in the art that, it can be to the present invention Technical solution be modified or replaced equivalently, without departing from the spirit of the technical scheme of the invention and range, should all cover In the scope of the claims of the present invention.

Claims (9)

1. a kind of reaction kettle for Trace Hg analysis, which is characterized in that including:Autoclave body, kettle cover and air inlet pipe;
The kettle cover is connected with autoclave body cooperation;
Open up air admission hole on the kettle cover, the air inlet pipe is arranged in the autoclave body, the first end of the air inlet pipe with it is described Air admission hole is connected to, and the second end of the air inlet pipe extends to the autoclave body lower part;
Venthole and liquid injection port are opened up on the kettle cover;
Wherein, the autoclave body, kettle cover and air inlet pipe use polytetrafluoroethylene material.
2. the reaction kettle for Trace Hg analysis as described in claim 1, which is characterized in that the reaction kettle further includes:Into Gas nozzle;
The suction nozzle is connected to the air inlet pipe second end;
Through-hole array is opened up on the suction nozzle.
3. the reaction kettle for Trace Hg analysis as claimed in claim 2, it is characterised in that:Setting is used on the air admission hole Connect the inlet suction port of inert gas source.
4. the reaction kettle for Trace Hg analysis as claimed in claim 2, it is characterised in that:The first end of the air inlet pipe with The air admission hole screw thread is connected, and is sealed by the first gasket;
The second end of the air inlet pipe is connected with the suction nozzle screw thread, and is sealed by the second gasket.
5. the reaction kettle for Trace Hg analysis as described in claim 1, it is characterised in that:Setting is used on the venthole Connect the escape pipe of mercury capture structure.
6. the reaction kettle for Trace Hg analysis as described in claim 1, it is characterised in that:It is arranged therewith in the liquid injection port Matched liquid injection port plug.
7. as claim 1~6 any one of them is used for the reaction kettle of Trace Hg analysis, which is characterized in that on the kettle cover Observation window is opened up, and is closed by light transmission quartz glass.
8. the reaction kettle for Trace Hg analysis as claimed in claim 7, it is characterised in that:The light transmission quartz glass passes through Fixed block is pressed on the kettle cover;
Third gasket, the light transmission quartz glass and the fixed block are set between the light transmission quartz glass and the kettle cover Between be arranged the 4th gasket.
9. a kind of Trace Hg analysis mercury capture structure, which is characterized in that including:Purity nitrogen air source, gold sand trap tube and such as power Profit requires the reaction kettle described in 7;
Wherein, the purity nitrogen air source connects the air admission hole, and the gold sand trap tube connects the venthole.
CN201711294424.3A 2017-12-08 2017-12-08 A kind of reaction kettle and mercury capture structure for Trace Hg analysis Pending CN108393047A (en)

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CN201711294424.3A CN108393047A (en) 2017-12-08 2017-12-08 A kind of reaction kettle and mercury capture structure for Trace Hg analysis

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Application Number Priority Date Filing Date Title
CN201711294424.3A CN108393047A (en) 2017-12-08 2017-12-08 A kind of reaction kettle and mercury capture structure for Trace Hg analysis

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110538614A (en) * 2019-01-08 2019-12-06 天津大学 Generating device and generating method for stably generating active gaseous mercury in laboratory

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000131212A (en) * 1998-10-22 2000-05-12 Mitsubishi Chemicals Corp Surface tension measuring device
CN201000434Y (en) * 2007-01-12 2008-01-02 北京瑞利分析仪器公司 Ultra trace mercury measuring apparatus in water sample for atomic fluorescence optical spectrometer
CN103242872A (en) * 2012-02-07 2013-08-14 北京低碳清洁能源研究所 Carbon material pyrolysis device
CN203291834U (en) * 2013-06-24 2013-11-20 朱何俊 Fluidized bed reactor for powder catalyst activating

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000131212A (en) * 1998-10-22 2000-05-12 Mitsubishi Chemicals Corp Surface tension measuring device
CN201000434Y (en) * 2007-01-12 2008-01-02 北京瑞利分析仪器公司 Ultra trace mercury measuring apparatus in water sample for atomic fluorescence optical spectrometer
CN103242872A (en) * 2012-02-07 2013-08-14 北京低碳清洁能源研究所 Carbon material pyrolysis device
CN203291834U (en) * 2013-06-24 2013-11-20 朱何俊 Fluidized bed reactor for powder catalyst activating

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110538614A (en) * 2019-01-08 2019-12-06 天津大学 Generating device and generating method for stably generating active gaseous mercury in laboratory

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