CN104749018B - A kind of laser ablation signal removes mercury device online - Google Patents

A kind of laser ablation signal removes mercury device online Download PDF

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Publication number
CN104749018B
CN104749018B CN201510179501.5A CN201510179501A CN104749018B CN 104749018 B CN104749018 B CN 104749018B CN 201510179501 A CN201510179501 A CN 201510179501A CN 104749018 B CN104749018 B CN 104749018B
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mercury
corrugated plating
millimeters
pipe
laser ablation
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CN104749018A (en
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史晓丽
高伟
陈红芳
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Analysis Of Spectrum Science And Technology Ltd Co On Wuhan
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Analysis Of Spectrum Science And Technology Ltd Co On Wuhan
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Abstract

Mercury device is removed online the invention provides a kind of laser ablation signal, at least mercury pipe is removed including columned stainless steel, remove the two ends respectively air inlet and gas outlet of mercury pipe, it is described to go in mercury pipe to catch mercury barrier flaps group at least provided with one group, described mercury barrier flaps group of catching is made up of corrugated plating stacked on top of one another, the corrugated plating is from top to bottom evenly distributed in mercury pipe, and corrugated plating is parallel with the axial line of mercury pipe is removed, and two sides of corrugated plating are fixed on the inwall of mercury pipe;It is described to go on the inwall of mercury pipe and the surface of corrugated plating to be provided with gold coating.The present apparatus not only can remove the background element mercury in work carrier gas, can also online remove the mercury in laser ablation signal, and go mercury effect remarkable, and mercury is removed from the sample aerosol of laser ablation completely almost.

Description

A kind of laser ablation signal removes mercury device online
Technical field
Mercury device is removed online the invention provides a kind of laser ablation signal, belongs to laser ablation inductively coupled plasma Light/mass spectral analysis field.
Background technology
Laser ablation inductively coupled plasma light/mass spectrum LA-ICP-MS technologies are the most successful and effective directly right Solid sample enters one of technology of row element or isotope analysis.In the middle of numerous elements or isotope analysis, lead element is same Position element analysis and Within Monominerals uranium lead determine the effect for year key being played in research fields such as environment, geology, material, archaeologies.At present, Restriction obtains high accuracy lead isotope204Pb testing results are essentially from mercury isotope204The interference of Hg.Therefore, the back of the body of mercury is reduced Scape is very urgent in mass spectral analysis.
In mass spectral analysis, the background of mercury is mostly derived from mercury impurities and mineral sample in instrument work carrier gas argon gas, helium Product itself such as sulfide, zircon contain mercury.Glass, sulfide mineral, feldspar and some important secondary ore deposits are analyzed in LA-ICP-MS When the uranium lead isotope of thing, such as zircon determines year, a very tiny common lead204Pb signal peaks can produce it is very big not Degree of certainty.Therefore, except the interference of mercury impurities in work carrier gas argon gas to be eliminated, helium, LA-ICP-MS laser ablations are removed and is produced The interference of mercury is also extremely important in year is determined in lead element isotope analysis and Within Monominerals uranium lead in raw sample aerosol.
For the interference of mercury impurities in work carrier gas argon gas, helium, can be subtracted by filtration carrier gas argon gas and helium Few mercury.At present, frequently with method have gold-plated quartz sand for adsorbent method, charcoal filtering method etc..Can only be by work with these methods The signal for making the mercury in carrier gas is reduced to about original 50%, what removal LA-ICP-MS laser ablations that can not be online were produced Mercury in sample aerosol.
Laser Japanese scholars Hirata etc. has mainly invented a kind of charcoal filter with materials such as activated carbons, uses this volume For 200 milliliters of charcoal filters with filtration carrier gas and can degrade the aerosol of sample, the signal of mercury is reduced to original 30%, but excessively larger charcoal filter volume is (for example:400 milliliters) cause to reduce the signal intensity of lead and uranium (about 40%), it is impossible to meet the accurate measure of low lead content mercury Background Samples high.
The content of the invention
Mercury device is removed online the invention provides a kind of laser ablation signal, solves the deficiency in background technology, this dress The background element mercury that not only can remove in work carrier gas is put, the mercury in laser ablation signal can also be online removed, and go mercury to imitate Fruit is remarkable, and mercury is removed from the sample aerosol of laser ablation completely almost.
Realize technical scheme that above-mentioned purpose of the present invention used for:
A kind of laser ablation signal removes mercury device online, at least removes mercury pipe including columned stainless steel, goes the two of mercury pipe End is respectively air inlet and gas outlet, and described to go in mercury pipe to catch mercury barrier flaps group at least provided with one group, described catches mercury resistance Partition group is made up of at least 7 corrugated platings stacked on top of one another, and the corrugated plating is from top to bottom evenly distributed in mercury pipe, ripple Card is parallel with the axial line of mercury pipe is removed, and two sides of corrugated plating are fixed on the inwall of mercury pipe;Described removes mercury pipe Inwall and corrugated plating surface on be provided with gold coating.
The thickness of described gold coating is 5~20 microns.Preferably, the thickness of described gold coating is 10 micro- Rice.
The thickness of described corrugated plating is 0.1~0.2 millimeter, and the length of corrugated plating is 20~40 millimeters, the ripple of corrugated plating A height of 3~5 millimeters, the distance of two adjacent crests is 6~8 millimeters in corrugated plating.Preferably, the thickness of described corrugated plating Be 0.15 millimeter, the length of corrugated plating is 30 millimeters, the wave height of corrugated plating is 4 millimeters, in corrugated plating two adjacent crests away from From being 7 millimeters.
The ripple inclination angle of described corrugated plating is 45 °.
The described length for removing mercury pipe is 300 millimeters, a diameter of 20 millimeters.It is described to go in mercury pipe at heart position wherein It is provided with one group and catches mercury barrier flaps group, described mercury barrier flaps group of catching is made up of seven corrugated platings, and the width of corrugated plating is by up to Under be followed successively by 9 millimeters, 14 millimeters, 18 millimeters, 20 millimeters, 18 millimeters, 14 millimeters, 9 millimeters.
The direction of ripple is with to remove the axial line of mercury pipe perpendicular on described corrugated plating.
Compared with prior art, the present invention has advantages below:Laser ablation signal of the invention removes mercury device not online The background element mercury in work carrier gas is only can remove, the mercury in laser ablation signal can also be online removed.By apparatus of the present invention With on LA-ICP-MS, the background signal value of the mercury in the carrier gas that works can be will be so small as to 0.5 millivolt by original 6 millivolts.It is heavier Want, can be by mercury in international sulfide standard specimen MASS-1202Hg signal intensities are reduced to 0.7 millivolt by 256 millivolts, and this is abundant Show, mercury is almost removed completely from the aerosol of laser ablation.The laser ablation signal go online mercury device it is remarkable remove mercury Effect, can be used to accurately determine lead content relatively low mercury content sample high206Pb/204Pb isotopic ratios.The mercury back of the body high is captured The high accuracy lead isotope of the low lead content sample of scape determines problem.
Brief description of the drawings
Fig. 1 goes the overall structure diagram of mercury device for the laser ablation signal for providing of the invention online;
Fig. 2 is the A-A of Fig. 1 to sectional view;
Fig. 3 is removal efficiency of mercury figure of the invention;
In figure:1- removes mercury pipe, 2- air inlets, 3- gas outlets, 4- corrugated platings.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment does detailed specific description to the present invention, but protection scope of the present invention It is not limited to following examples.
Laser ablation signal provided by the present invention goes the structure of mercury device as depicted in figs. 1 and 2 online, including cylindric Stainless steel remove mercury pipe 1, the described length for removing mercury pipe 1 is 300 millimeters, a diameter of 20 millimeters.The two ends of mercury pipe are gone to be respectively Air inlet 2 and gas outlet 3, it is described go in mercury pipe 1 to be provided with one group catch mercury barrier flaps group, described catches mercury barrier flaps group by extremely Few 7 corrugated platings 4 stacked on top of one another are constituted, and the corrugated plating 4 is from top to bottom evenly distributed in mercury pipe, corrugated plating with go The axial line of mercury pipe is parallel, and two sides of corrugated plating are fixed on the inwall of mercury pipe;Ripple on described corrugated plating Direction is with to remove the axial line of mercury pipe perpendicular.
Mercury barrier flaps group of catching described in the present embodiment is made up of seven corrugated platings, and the width of corrugated plating is from top to bottom successively It is 9 millimeters, 14 millimeters, 18 millimeters, 20 millimeters, 18 millimeters, 14 millimeters, 9 millimeters.The thickness of described corrugated plating is 0.15 milli Rice, the length of corrugated plating is 30 millimeters, and the wave height of corrugated plating is 4 millimeters, and the distance of two adjacent crests is 7 millis in corrugated plating Rice.The ripple inclination angle of described corrugated plating is 45 °.
It is described to go to be provided with gold coating on the inwall of mercury pipe and the surface of corrugated plating, described gold coating Thickness is 10 microns.
In the device busy that the present invention is provided, the mercury atom entrance in the aerosol that carrier gas or laser ablation are produced is gone After mercury pipe, repeatedly collided with the ultrapure gold coating of corrugated plating waved surface and pipe internal surface and react and generate amalgam and fixed Enrichment capture is removed in mercury pipe is removed so as to the mercury in work carrier gas and sample aerosol be captured.
The present invention is passed through the position before argon gas and is passed through in being arranged on laser ablation inductively coupled plasma-mass spectrometry instrument Position after argon gas.The position before being passed through argon gas is placed on, work carrier gas helium can be removed and the mercury in aerosol is degraded;Put The position after being passed through argon gas is put, can remove remove simultaneously helium, argon gas and degrade the mercury in aerosol.
Fig. 3 (a, b) be by the present invention be arranged on be passed through the position before argon gas when, using forward and backward LA-ICP-MS of the invention with When 8 hertz of frequency degrades international sulfide standard specimen MASS-1202Hg、204Pb and208Pb elemental signals intensity contrasts, can from Fig. 3 To find out, the mercury in the carrier gas that worked after the present apparatus is used202The background signal intensities value of Hg is reduced to 0.5 milli by original 6 millivolts Volt;Mercury in MASS-1202The signal strength values of Hg will be so small as to 0.7 millivolt by original 256 millivolts, reduce 366 times202Hg believes Number.This result shows that mercury is almost removed completely from sample aerosol.

Claims (9)

1. a kind of laser ablation signal removes mercury device online, it is characterised in that:Mercury pipe at least is removed including columned stainless steel, is gone The two ends of mercury pipe are respectively air inlet and gas outlet, described to go in mercury pipe to catch mercury barrier flaps group at least provided with one group, described Mercury barrier flaps group of catching be made up of at least 7 corrugated platings stacked on top of one another, the corrugated plating is from top to bottom evenly distributed in In mercury pipe, corrugated plating is parallel with the axial line of mercury pipe is removed, and two sides of corrugated plating are fixed on the inwall of mercury pipe;It is described Go on the inwall of mercury pipe and the surface of corrugated plating be provided with gold coating.
2. laser ablation signal according to claim 1 removes mercury device online, it is characterised in that:Described gold coating Thickness is 5~20 microns.
3. laser ablation signal according to claim 2 removes mercury device online, it is characterised in that:Described gold coating Thickness is 10 microns.
4. laser ablation signal according to claim 1 removes mercury device online, it is characterised in that:The thickness of described corrugated plating It is 0.1~0.2 millimeter to spend, and the length of corrugated plating is 20~40 millimeters, and the wave height of corrugated plating is 3~5 millimeters, adjacent in corrugated plating Two crests distance be 6~8 millimeters.
5. laser ablation signal according to claim 4 removes mercury device online, it is characterised in that:The thickness of described corrugated plating It is 0.15 millimeter to spend, and the length of corrugated plating is 30 millimeters, and the wave height of corrugated plating is 4 millimeters, two adjacent crests in corrugated plating Distance is 7 millimeters.
6. laser ablation signal according to claim 1 removes mercury device online, it is characterised in that:The ripple of described corrugated plating Line inclination angle is 45 °.
7. laser ablation signal according to claim 1 removes mercury device online, it is characterised in that:The described length for removing mercury pipe It is 300 millimeters to spend, a diameter of 20 millimeters.
8. laser ablation signal according to claim 7 removes mercury device online, it is characterised in that:It is described go in mercury pipe Its center position is provided with one group and catches mercury barrier flaps group, and described mercury barrier flaps group of catching is made up of seven corrugated platings, corrugated plating Width be from top to bottom followed successively by 9 millimeters, 14 millimeters, 18 millimeters, 20 millimeters, 18 millimeters, 14 millimeters, 9 millimeters.
9. laser ablation signal according to claim 1 removes mercury device online, it is characterised in that:Described corrugated plating upper ripple The direction of line is with to remove the axial line of mercury pipe perpendicular.
CN201510179501.5A 2015-04-15 2015-04-15 A kind of laser ablation signal removes mercury device online Active CN104749018B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105067415B (en) * 2015-08-11 2018-05-15 袁洪林 A kind of filter that can remove the mercury in high-purity gas or aerosol
CN107305168B (en) * 2016-04-22 2020-05-22 中国石油化工股份有限公司 Gaseous mercury catches mercury device
CN105954088B (en) * 2016-07-15 2019-02-05 中国工程物理研究院材料研究所 Laser ablation sample room

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992016284A1 (en) * 1991-03-18 1992-10-01 Stiftelsen Centrum För Dentalteknik Och Biomaterial I Huddinge Filter for the purification of gases
US5660795A (en) * 1994-02-25 1997-08-26 Tekran Inc. Cartridge for collection of a sample by adsorption onto a solid surface
CN201765146U (en) * 2010-06-24 2011-03-16 西北有色地质研究院 Mercury enrichment device of mercury detector
CN202676520U (en) * 2012-04-12 2013-01-16 中国科学院城市环境研究所 Device for collecting different species of mercury in atmosphere

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992016284A1 (en) * 1991-03-18 1992-10-01 Stiftelsen Centrum För Dentalteknik Och Biomaterial I Huddinge Filter for the purification of gases
US5660795A (en) * 1994-02-25 1997-08-26 Tekran Inc. Cartridge for collection of a sample by adsorption onto a solid surface
CN201765146U (en) * 2010-06-24 2011-03-16 西北有色地质研究院 Mercury enrichment device of mercury detector
CN202676520U (en) * 2012-04-12 2013-01-16 中国科学院城市环境研究所 Device for collecting different species of mercury in atmosphere

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