CN205301259U - Be applied to mercury isotopc analysis's pyrolysis injection formula mercury vapour sampling device - Google Patents

Be applied to mercury isotopc analysis's pyrolysis injection formula mercury vapour sampling device Download PDF

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Publication number
CN205301259U
CN205301259U CN201620043689.0U CN201620043689U CN205301259U CN 205301259 U CN205301259 U CN 205301259U CN 201620043689 U CN201620043689 U CN 201620043689U CN 205301259 U CN205301259 U CN 205301259U
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China
Prior art keywords
mercurous
column
check valve
syringe pump
activated
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Expired - Fee Related
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CN201620043689.0U
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Chinese (zh)
Inventor
孙鲁闽
叶鑫怡
郝文博
蔡扶琛
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Xiamen University Tan Kah Kee College
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Xiamen University Tan Kah Kee College
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Priority to CN201620043689.0U priority Critical patent/CN205301259U/en
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Abstract

The utility model relates to a be applied to mercury isotopc analysis's pyrolysis injection formula mercury vapour sampling device, including having the simple substance mercury thermal desorption system of mercurous principal column or mercurous active carbon post, the feed end management way of mercurous principal column or mercurous active carbon post is connected with the argon gas source, and the discharge end of mercurous principal column or mercurous active carbon post is connected with the syringe pump through first check valve, be connected with the multiple collector plasma mass spectrograph through the second pipeline on the syringe pump, be provided with the second check valve by syringe pump flow direction multiple collector plasma mass spectrograph on the second pipeline. The device is compact structure not only, need not to use liquid reagent in addition, the effective risk that exposes of lowering apparatus acid when reducing reagent consumption.

Description

It is applied to the pyrolysis injection mercuryvapour sampling device that mercury isotope is analyzed
Technical field
This utility model relates to a kind of pyrolysis injection mercuryvapour sampling device being applied to mercury isotope analysis.
Background technology
The sampling device of cold atom mercuryvapour gas-liquid separation is to measure sampling device during hydrargyrum stable isotope as multiple-collector plasma source mass spectrometry instrument (MC-ICP/MS), and it is generally made up of gas-liquid separation unit, gas piping, liquid line and hydrodynamic pump. During work, mercurous sample solution and reductant solution fully react after threeway converges in mixed pipe line, and dimercurion is reduced into Elemental Mercury; Mixed liquor is separated entrance gas phase feeding MC-ICP/MS from liquid phase with high-purity carrier gas after entering gas-liquid separation unit and is detected.
The sampling device of existing cold atom mercuryvapour gas-liquid separation generally adopt straight tube gas-liquid separator with peristaltic pump as gas-liquid separation unit and hydrodynamic pump (see figure 1). After being flowed into by gas-liquid separator top-side after the blended pipeline mixing of stock solution, Elemental Mercury therein, by leading to from the high-purity argon gas of gas-liquid separator bottom sides from liquid phase purging entrance gas phase, is entered MC-ICP/MS by blowout directly over separator top and detects; Waste liquid then bottom discharge immediately below gas-liquid separator. Job requirement according to MC-ICP/MS, the operating parameter of this sampling device needs matched. The step that device specifically performs has rinse, sample introduction, cleans, varies four steps, and operation switching is and is performed manually by so that each sample completes sample introduction and measures 860s consuming time, wherein the detection time of 600s.
Adopt this kind of sampling device to there is also following defect: the first, this sampling device requires that sample preparation form is solution simultaneously. For the hydrargyrum sample utilizing principal column or activated-charcoal column absorption method to gather, it is impossible to direct analysis measures, and need the hydrargyrum Thermal desorption being adsorbed on principal column or activated carbon to be gaseous mercury, and these hydrargyrum are absorbed in solution again. The second, in the process measuring sample, it is necessary to gas-liquid separator is carried out and rinse by elapsed time and reagent.Removing the consumption of self of reagent, the acidity that reagent is higher is likely to and accurate MC-ICP/MS can be caused corrosion.
Summary of the invention
The purpose of this utility model is in that providing a kind of is applied to the pyrolysis injection mercuryvapour sampling device that mercury isotope is analyzed, this device not only compact conformation, and without using liquid reagent, reduce reagent consume while can effectively lowering apparatus acid exposure risk.
The technical solution of the utility model is in that: a kind of pyrolysis injection mercuryvapour sampling device being applied to mercury isotope analysis, including the Elemental Mercury thermal desorption system with mercurous principal column or mercurous activated-charcoal column, the feed end of described mercurous principal column or mercurous activated-charcoal column is connected with argon gas source by the road, the discharge end of mercurous principal column or mercurous activated-charcoal column is connected with syringe pump through the first check valve, described syringe pump is connected with multiple-collector plasma source mass spectrometry instrument through the second pipeline, described second pipeline is provided with the second check valve being flowed to multiple-collector plasma source mass spectrometry instrument by syringe pump.
Further, described Elemental Mercury thermal desorption system also includes the heating resistor for mercurous principal column or the heating of mercurous activated-charcoal column and the cooling fan lowered the temperature for mercurous principal column or mercurous activated-charcoal column.
Further, pipeline between described argon gas source and mercurous principal column or mercurous activated-charcoal column is silica gel sleeve pipe, and described mercurous principal column or mercurous activated-charcoal column are connected through the second silica gel sleeve pipe with the first check valve being flowed to syringe pump by mercurous principal column or mercurous activated-charcoal column.
Further, it is connected through Teflon casing joint respectively between described second silica gel sleeve pipe and the first check valve and between the first check valve and syringe pump.
Further, described syringe pump is 20mL precise injection pump, and syringe pump is connected with the second check valve through Teflon casing joint, is connected through PFA pipe between described second check valve with multiple-collector plasma source mass spectrometry instrument matter.
Further, it is connected through Teflon casing joint between described second check valve and PFA pipe.
Compared with prior art, the invention have the advantages that
One, this device not only compact conformation, and achieve sample feeding without preparing into solution form, this makes many steps can prepared without increasing solution by the Elemental Mercury sample of principal column/activated-charcoal column absorptive collection be made directly analysis mensuration. Aneroid sample form also makes sampling system without using the liquid reagent such as reducing agent, cleanout fluid simultaneously, thus enormously simplify the consumption of the structure of experimental provision (without using peristaltic pump and gas-liquid separator) and reagent. The degree of accuracy simultaneously utilizing precise injection pump achieve enter MC-ICP/MS throughput keep constant, reduce reagent consume while can effectively lowering apparatus acid exposure risk;
Two, make the operating process of device have higher automatization with monolithic processor controlled design, saved manually-operated loaded down with trivial details, improve the accuracy of operation, when analyzing continuously, there is obvious advantage.
Accompanying drawing explanation
Fig. 1 is the structural representation of the sampling device of existing cold atom mercuryvapour gas-liquid separation;
Fig. 2 is structural representation of the present utility model;
Fig. 3 is job step timetable of the present utility model;
In figure: the mercurous principal column of 10-or mercurous activated-charcoal column 11-heating resistor 12-cool down fan 20-argon gas source 30-the first check valve 40-syringe pump 50-the second check valve 60-multiple-collector plasma source mass spectrometry instrument 70-silica gel sleeve pipe 80-the second silica gel sleeve pipe 90-PFA pipe 110-pipeline sample or 3% nitric acid washing liquid 120-Reduction with Stannous Chloride agent 130-sample introduction peristaltic pump 140-gas-liquid separator 150-waste liquid peristaltic pump 160-waste liquid barrel.
Detailed description of the invention
For features described above of the present utility model and advantage can be become apparent, special embodiment below, and coordinate accompanying drawing, it is described in detail below, but this utility model is not limited to this.
Referring to figs. 2 and 3.
A kind of pyrolysis injection mercuryvapour sampling device being applied to mercury isotope analysis, including the Elemental Mercury thermal desorption system with mercurous principal column or mercurous activated-charcoal column 10, the feed end of described mercurous principal column or mercurous activated-charcoal column is connected with argon gas source 20 by the road, the discharge end of mercurous principal column or mercurous activated-charcoal column is connected with syringe pump 40 through the first check valve 30, described syringe pump is connected with multiple-collector plasma source mass spectrometry instrument 60 through the second pipeline, described second pipeline is provided with the second check valve 50 being flowed to multiple-collector plasma source mass spectrometry instrument by syringe pump.
In the present embodiment, described Elemental Mercury thermal desorption system also includes the heating resistor 11 for mercurous principal column or the heating of mercurous activated-charcoal column and the cooling fan 12 lowered the temperature for mercurous principal column or mercurous activated-charcoal column.
In the present embodiment, pipeline between described argon gas source and mercurous principal column or mercurous activated-charcoal column is silica gel sleeve pipe 70, and described mercurous principal column or mercurous activated-charcoal column are connected through the second silica gel sleeve pipe 80 with the first check valve being flowed to syringe pump by mercurous principal column or mercurous activated-charcoal column.
In the present embodiment, it is connected through Teflon casing joint respectively between described second silica gel sleeve pipe and the first check valve and between the first check valve and syringe pump.
In the present embodiment, described syringe pump is 20mL precise injection pump and by Single-chip Controlling, syringe pump is connected with the second check valve through Teflon casing joint, and between described second check valve with multiple-collector plasma source mass spectrometry instrument matter, the PFA pipe 90 through 0.75mm internal diameter is connected.
In the present embodiment, it is connected through Teflon casing joint between described second check valve and PFA pipe.
In the present embodiment, each sample completes sample introduction and measures 700s consuming time, and wherein the detection time of 660s, 40s varies the time. During device work, syringe pump is the unique power resources of system, and the load mercury quantity of single mercurous principal column/mercurous activated-charcoal column is 6 to 10ng.
Operation principle: during work, the mercurous principal column of heating resistor electrified regulation/mercurous activated-charcoal column discharges adsorbing hydrargyrum thereon with the form of Elemental Mercury; Now syringe pump work, by mercurous argon suction pump chamber. When Thermal desorption process terminates, cooling fan work gives mercurous principal column/mercurous activated-charcoal column cooling; Now syringe pump is reversely operated, is slowly pushed among MC-ICP/MS containing mercuryvapour with constant flow rate to be measured by mix homogeneously in injecting cavity.
The foregoing is only preferred embodiment of the present utility model, all equalizations done according to this utility model claim change and modify, and all should belong to covering scope of the present utility model.

Claims (6)

1. one kind is applied to the pyrolysis injection mercuryvapour sampling device that mercury isotope is analyzed, it is characterized in that, including the Elemental Mercury thermal desorption system with mercurous principal column or mercurous activated-charcoal column, the feed end of described mercurous principal column or mercurous activated-charcoal column is connected with argon gas source by the road, the discharge end of mercurous principal column or mercurous activated-charcoal column is connected with syringe pump through the first check valve, described syringe pump is connected with multiple-collector plasma source mass spectrometry instrument through the second pipeline, described second pipeline is provided with the second check valve being flowed to multiple-collector plasma source mass spectrometry instrument by syringe pump.
2. the pyrolysis injection mercuryvapour sampling device being applied to mercury isotope analysis according to claim 1, it is characterized in that, described Elemental Mercury thermal desorption system also includes the heating resistor for mercurous principal column or the heating of mercurous activated-charcoal column and the cooling fan lowered the temperature for mercurous principal column or mercurous activated-charcoal column.
3. the pyrolysis injection mercuryvapour sampling device being applied to mercury isotope analysis according to claim 1 and 2, it is characterized in that, pipeline between described argon gas source and mercurous principal column or mercurous activated-charcoal column is silica gel sleeve pipe, and described mercurous principal column or mercurous activated-charcoal column are connected through the second silica gel sleeve pipe with the first check valve being flowed to syringe pump by mercurous principal column or mercurous activated-charcoal column.
4. the pyrolysis injection mercuryvapour sampling device being applied to mercury isotope analysis according to claim 3, it is characterized in that, be connected through Teflon casing joint respectively between described second silica gel sleeve pipe and the first check valve and between the first check valve and syringe pump.
5. the pyrolysis injection mercuryvapour sampling device being applied to mercury isotope analysis according to claim 1 and 2, it is characterized in that, described syringe pump is 20mL precise injection pump, syringe pump is connected with the second check valve through Teflon casing joint, is connected through PFA pipe between described second check valve with multiple-collector plasma source mass spectrometry instrument matter.
6. the pyrolysis injection mercuryvapour sampling device being applied to mercury isotope analysis according to claim 5, it is characterised in that be connected through Teflon casing joint between described second check valve and PFA pipe.
CN201620043689.0U 2016-01-18 2016-01-18 Be applied to mercury isotopc analysis's pyrolysis injection formula mercury vapour sampling device Expired - Fee Related CN205301259U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108801721A (en) * 2017-04-27 2018-11-13 中国科学院寒区旱区环境与工程研究所 Stable carbon isotope apparatus for pre-analysis treatment in the carbonate dissolved in a kind of water body

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108801721A (en) * 2017-04-27 2018-11-13 中国科学院寒区旱区环境与工程研究所 Stable carbon isotope apparatus for pre-analysis treatment in the carbonate dissolved in a kind of water body

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