CN2775653Y - Air mercury detector for atomic fluorescent spectrum instrument - Google Patents

Air mercury detector for atomic fluorescent spectrum instrument Download PDF

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Publication number
CN2775653Y
CN2775653Y CN 200520000098 CN200520000098U CN2775653Y CN 2775653 Y CN2775653 Y CN 2775653Y CN 200520000098 CN200520000098 CN 200520000098 CN 200520000098 U CN200520000098 U CN 200520000098U CN 2775653 Y CN2775653 Y CN 2775653Y
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CN
China
Prior art keywords
mercury
quartz ampoule
spun gold
catching
gas
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Expired - Lifetime
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CN 200520000098
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Chinese (zh)
Inventor
张锦茂
董芳
陈璐
李继超
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BEIJING RUILI ANALYTICAL INSTRUMENT CORP
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BEIJING RUILI ANALYTICAL INSTRUMENT CORP
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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The utility model relates to an air mercury detector for an atomic fluorescent spectrum instrument, which comprises a gold-wire mercury catching quartz pipe, an air electromagnetic valve, a mercury releasing device and a temperature-controlling power supply, wherein the gold-wire mercury catching quartz pipe is filled with high-purity gold wire materials; the mercury releasing device is connected with the temperature-controlling power supply which controls the temperature of the mercury releasing device; the air electromagnetic valve realizes automatic control for air through the program of a microcomputer. When matched with an atomic fluorescent spectrum instrument, the utility model can detect trace amount of mercury in various air phases. The gold-wire mercury catching quartz pipe can be repeatedly used for a long term; the mercury releasing device has the advantages of long service life and convenient operation. The utility model can also be used for other various atomic spectrum instruments (comprising an AAS and an AES).

Description

The bicycle pump measurement mechanism that is used for atomic fluorescence spectrometer
Technical field
The utility model relates to a kind of bicycle pump measurement mechanism that is used for atomic fluorescence spectrometer, particularly a kind ofly is exclusively used in Trace Hg measurement mechanism in the gas that has steam generation-atomic fluorescence spectrometer.
Background technology
At present, steam generation-atomic fluorescence spectrometer generally all is used to measure water sample or solid-like is converted into liquid through digestion process, uses reductive agent KBH 4Or SnCl 2With inorganic mercury and organic mercury Restore All is atomic state mercury vapour (Hg 0), the Hg steam of generation imports atomizer with carrier gas and measures.Has very high sensitivity for analysis.
But, at home and abroad there is no the commercial apparatus that atomic fluorescence spectrometer is used for the bicycle pump determinator so far.
External Russia produces Zeeman atomic absorption mercury vapor analyzer, has adopted Zeeman modulation polarization spectroscopy, has eliminated the influence of non-resonance line and non-selection interference to analysis result, can measure mercury in the atmosphere; Domesticly once produced the mercury that atomic absorption type mercury vapor analyzer is used for measuring soil air (earth gas).Its shortcoming is that sensitivity for analysis is lower.
Summary of the invention
The purpose of this utility model provides a kind of atomic fluorescence spectrometer bicycle pump measurement mechanism that is used for, to improve sensitivity for analysis.
The purpose of this utility model is achieved in that and comprises spun gold mercury catching quartz ampoule, mercury releasing device and automatically controlled gas solenoid valve, the spun gold mercury catching quartz ampoule inserts in the interior high quartz boiler tube of mercury releasing device, one end of spun gold mercury catching quartz ampoule stretches out mercury releasing device and is connected with the atomizer of atomic fluorescence spectrometer, and the other end is connected with automatically controlled gas solenoid valve by flexible pipe.
Described spun gold mercury catching quartz ampoule comprises quartz ampoule, little quartz ampoule, spun gold cake and spun gold ball, placing several is twined the spun gold cake that is pressed into after the globulate by spun gold at interval in quartz ampoule, between each spun gold cake, respectively place a little quartz ampoule, spun gold ball identical, that twined by spun gold is housed in each little quartz ampoule; Each is by two gravelstone English pipe plug plugs in the outer end of the spun gold cake that is positioned at two ends.
The external diameter of described quartz ampoule is 6mm, and long is 200mm; The used spun gold purity of described spun gold cake and spun gold ball is 99.99%, diameter of section φ 0.05mm.
Described mercury releasing device comprises shell, quartz ampoule, heating wire and temperature regulating device, and two ends are that the quartz ampoule of reducing is installed in the enclosure, and the two ends of shell are stretched out at the two ends of quartz ampoule, and an end internal diameter of quartz ampoule is slightly larger than the external diameter of described spun gold mercury catching quartz ampoule; Outer peripheral face at quartz ampoule is provided with heating wire; The thermal head of temperature regulating device is installed and is located in the shell.
Inboard at described shell two ends respectively is provided with ceramic briquetting.
Described automatically controlled gas solenoid valve is connected the realization gas flow and controls automatically with microcomputer.
Described flexible pipe is made by silica gel.
Described in the utility model is the bicycle pump measurement mechanism that is used for atomic fluorescence spectrometer, the spun gold mercury catching quartz ampoule of this device, being filled with high-purity spun gold in quartz ampoule inside is the amalgamation agent, it at normal temperatures spun gold can form gold amalgam with mercury, under hot conditions, can discharge quantitatively again.Described automatically controlled gas solenoid valve, the carrier gas of using (Ar) when releasing mercury under setting hot conditions is opened gas solenoid valve control carrier gas flux and regularly mercury vapour is discharged.Described mercury releasing device shell is made by metal material, and inside is provided with special-purpose Quartz stove tube and is tied with special heating wire at outer wall, by temperature-controlled power control mercury releasing device correct release the mercury temperature.
Characteristics of the present utility model are to make the Trace Hg in atomic fluorescence spectrometer and the bicycle pump device coupling detected gas become possibility, have enrichment and separate this characteristic of gaseous mercury, have very high sensitivity for analysis.The spun gold mercury catching quartz ampoule can prolonged and repeatedly use, the long service life of mercury releasing device.The structure and the measuring process of device have been simplified.
Further specify structure of the present utility model below in conjunction with accompanying drawing:
Description of drawings
Fig. 1 is a general structure synoptic diagram of the present utility model;
Fig. 2 is the structural representation of spun gold mercury catching quartz ampoule of the present utility model;
The structural representation of Fig. 3 mercury releasing device of the present utility model;
Fig. 4 is the right view of Fig. 3.
Embodiment
Referring to Fig. 1, the utility model comprises spun gold mercury catching quartz ampoule 1, mercury releasing device 2 and automatically controlled gas solenoid valve 4, in the high quartz boiler tube 21 that spun gold mercury catching quartz ampoule 1 inserts in the mercury releasing device 2, one end of spun gold mercury catching quartz ampoule 1 stretches out an end of mercury releasing device 2, and is connected with an end of automatically controlled gas solenoid valve 4 by silicone tube 3.Described automatically controlled gas solenoid valve 4 is connected the realization gas flow and controls automatically with microcomputer.
Referring to Fig. 2, described spun gold mercury catching quartz ampoule 1 comprises quartz ampoule 11, little quartz ampoule 12, spun gold cake 13 and spun gold ball 14, in quartz ampoule 11, place the spun gold cake 13 that is pressed into after several twine globulate by spun gold at interval, between each spun gold cake, respectively place a little quartz ampoule 12.Spun gold ball 14 identical, that twined by spun gold is housed in each little quartz ampoule 12.Each is stopped up by two little quartz ampoules 12 in the outer end of the spun gold cake 13 that is positioned at two ends.The external diameter of described quartz ampoule 11 is 6mm, and long is 200mm; Described spun gold cake 13 and spun gold ball 14 used spun gold purity are 99.99%, diameter of section φ 0.05mm.
Referring to Fig. 3 and Fig. 4, described mercury releasing device 2 comprises quartz ampoule 21, shell 22, heating wire (23), temperature regulating device 24 and ceramic briquetting 25.Shell 22 is made by the tubular metal material, and the two ends of quartz ampoule 21 are respectively air intake opening 211 and gas outlet 212, and two ends are reducing.The internal diameter of air intake opening 211 is slightly larger than the external diameter of described spun gold mercury catching quartz ampoule 1, is used for inserting spun gold mercury catching quartz ampoule 1.Quartz ampoule 21 is installed in the shell 22, and the two ends of shell 22 are stretched out at the two ends of quartz ampoule 21, respectively is provided with ceramic briquetting 25 in the inboard at shell 22 two ends, is used for fixing quartz ampoule 21.Outer peripheral face at quartz ampoule 21 is tied with special heating wire 23; The thermal head of temperature regulating device 24 (employing thermopair) 26 is installed and is located in the shell 22, realizes the temperature control to high quartz pipe 21.
Introduce the course of work of the present utility model below, be divided into two steps:
Step 1 is the operation of mercury in the captured gas.One end of spun gold mercury catching quartz ampoule 1 is connected in the air intake opening of air sampler, regulates the flow velocity and the sampling time of sampling thief as required.Treat to take off mercury-traping tube 1 after sampling finishes, the mercury in the atmosphere by spun gold cake 13 and 14 enrichments of spun gold ball, forms gold amalgam in spun gold mercury catching quartz ampoule 11 at this moment.
Step 2 is the operation that spun gold mercury catching quartz ampoule 1 is released mercury.The gas outlet 212 of the high quartz pipe 21 during this device duty in the mercury releasing device 2 links to each other with atomizer in the atomic fluorescence spectrometer (AFS).Opening attemperating unit 24 makes mercury releasing device 2 keep 700 ℃ of steady state (SS)s.The end that to collect the spun gold mercury catching quartz ampoule 1 of mercury in the gas in operating process is connected with gas solenoid valve 4 with silicone tube 3.Spun gold mercury catching quartz ampoule 1 is directly inserted in mercury releasing device 2 interior 700 ℃ of high quartz pipes 21 then.By microcomputor program control, behind the heating 1min, electromagnetic gas solenoid valve 4 is opened immediately, and Ar gas enters spun gold mercury catching quartz ampoule 1 through gas solenoid valve 4, mercury vapour in the amalgam is all discharged in the atomizer that enters atomic fluorescence spectrometer (AFS) detect.
The sensitivity for analysis that facts have proved AFS DETERMINATION mercury is than high several times of atomic absorption method, has special advantages, therefore steam generation-atomic fluorescence spectrometer is in conjunction with bicycle pump measurement mechanism of the present utility model, lower detection limit can be obtained, the measurement of bicycle pump in atmospheric environment, soil air (gas in the earth), rock gas, industrial gasses, bulb workshop and the laboratory environment etc. can be measured.

Claims (7)

1, a kind of gas mercury measurement device that is used for atomic fluorescence spectrometer, it is characterized in that: comprise spun gold mercury catching quartz ampoule (1), mercury releasing device (2) and automatically controlled gas solenoid valve (4), spun gold mercury catching quartz ampoule (1) inserts in the interior high quartz boiler tube (21) of mercury releasing device (2), one end of spun gold mercury catching quartz ampoule (1) stretches out an end of mercury releasing device (2), and is connected with an end on automatically controlled gas trap island (4) by flexible pipe (3).
2, the gas mercury measurement device that is used for atomic fluorescence spectrometer according to claim 1, it is characterized in that: described spun gold mercury catching quartz ampoule (1) comprises quartz ampoule (11), little quartz ampoule (12), spun gold cake (13) and spun gold ball (14), in quartz ampoule (11), place the spun gold cake (13) that is pressed into after several twine globulate by spun gold at interval, between each spun gold cake, respectively place a little quartz ampoule (12), spun gold ball (14) identical, that twined by spun gold is housed in each little quartz ampoule (12); Each is stopped up by two little quartz ampoules (12) in the outer end of the spun gold cake (13) that is positioned at two ends.
3, the gas mercury measurement device that is used for atomic fluorescence spectrometer according to claim 2, it is characterized in that: the external diameter of described quartz ampoule (11) is 6mm, long is 200mm; Described spun gold cake (13) and the used spun gold purity of spun gold ball (14) are 99.99%, diameter of section φ 0.05mm.
4, the gas mercury measurement device that is used for atomic fluorescence spectrometer according to claim 1, it is characterized in that: described mercury releasing device (2) comprises shell (22), heating wire (23), temperature regulating device (24) and described quartz ampoule (21), two ends are that the quartz ampoule (21) of reducing is installed in the shell (22), the two ends of shell (22) are stretched out at the two ends of quartz ampoule (21), and an end internal diameter of quartz ampoule (21) is slightly larger than the external diameter of described spun gold mercury catching quartz ampoule (1); Outer peripheral face at quartz ampoule (21) is provided with heating wire (23); The thermal head (26) of temperature regulating device (24) is installed and is located in the shell (22).
5, the gas mercury measurement device that is used for atomic fluorescence spectrometer according to claim 4, it is characterized in that: the inboard at described shell (22) two ends respectively is provided with ceramic briquetting (25).
6, the gas mercury measurement device that is used for atomic fluorescence spectrometer according to claim 1 is characterized in that: described automatically controlled gas solenoid valve (4) can be connected the realization gas flow with microcomputer and control automatically.
7, the gas mercury measurement device that is used for atomic fluorescence spectrometer according to claim 1, it is characterized in that: described flexible pipe (3) is made by silica gel.
CN 200520000098 2005-01-06 2005-01-06 Air mercury detector for atomic fluorescent spectrum instrument Expired - Lifetime CN2775653Y (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102374978A (en) * 2010-08-06 2012-03-14 上海光谱仪器有限公司 Atomic fluorescence analyzing device
CN102500204A (en) * 2011-11-10 2012-06-20 北京吉天仪器有限公司 Foam mercury trap material and application thereof
CN104280268A (en) * 2014-09-17 2015-01-14 力合科技(湖南)股份有限公司 Trapping device and trapping system
WO2017024815A1 (en) * 2015-08-11 2017-02-16 袁洪林 Filter capable of removing mercury in high purity gas or aerosol
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
CN109596546A (en) * 2018-12-15 2019-04-09 力合科技(湖南)股份有限公司 Mercury filters eliminating machine by washing, mercury analyzer and analysis method
CN110864946A (en) * 2019-11-13 2020-03-06 清华大学 Device and method for measuring mercury content in flue gas

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102374978A (en) * 2010-08-06 2012-03-14 上海光谱仪器有限公司 Atomic fluorescence analyzing device
CN102500204A (en) * 2011-11-10 2012-06-20 北京吉天仪器有限公司 Foam mercury trap material and application thereof
CN102500204B (en) * 2011-11-10 2014-09-24 北京吉天仪器有限公司 Foam mercury trap material and application thereof
CN104280268A (en) * 2014-09-17 2015-01-14 力合科技(湖南)股份有限公司 Trapping device and trapping system
WO2017024815A1 (en) * 2015-08-11 2017-02-16 袁洪林 Filter capable of removing mercury in high purity gas or aerosol
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
CN109596546A (en) * 2018-12-15 2019-04-09 力合科技(湖南)股份有限公司 Mercury filters eliminating machine by washing, mercury analyzer and analysis method
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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Expiration termination date: 20150106

Granted publication date: 20060426