CN108845024A - A kind of matrix stable introducing device - Google Patents

A kind of matrix stable introducing device Download PDF

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Publication number
CN108845024A
CN108845024A CN201810332380.7A CN201810332380A CN108845024A CN 108845024 A CN108845024 A CN 108845024A CN 201810332380 A CN201810332380 A CN 201810332380A CN 108845024 A CN108845024 A CN 108845024A
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China
Prior art keywords
vaporization chamber
connector
heating mantles
matrix
waste liquid
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CN201810332380.7A
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Chinese (zh)
Inventor
胡兆初
陈力飞
罗涛
张文
李明
刘勇胜
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China University of Geosciences
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China University of Geosciences
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Priority to CN201810332380.7A priority Critical patent/CN108845024A/en
Publication of CN108845024A publication Critical patent/CN108845024A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating 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
    • G01N27/64Investigating 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 using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Toxicology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses a kind of matrix stable introducing devices, including vaporization chamber, upper heating mantles, lower heating mantles, pump line, peristaltic pump, reagent bottle;The side of vaporization chamber, which is equipped with, introduces connector, and one end connection reagent bottle of pump line, other end connection introduce connector, and the middle part of pump line winds peristaltic pump;Peristaltic pump drives pump line that the matrix reagent in the reagent bottle is introduced into the vaporization chamber;Two sides at the top of vaporization chamber are respectively equipped with carrier gas inlet suction port and steam air outlet adapter, access carrier gas into vaporization chamber by carrier gas inlet suction port, export steam by steam air outlet adapter;The side of vaporization chamber bottom end is equipped with waste liquid connector, and waste liquid is discharged by waste liquid connector;Upper heating mantles, lower heating mantles are respectively assembled in the top and lower part of vaporization chamber, are used for heating evaporation room.The present invention can be controlled freely to stablize and introduce active matrix steam and be avoided that pollution, be remarkably improved Plasma Mass Spectrometry analysis sensitivity, reduced the matrix effect in plasma.

Description

A kind of matrix stable introducing device
Technical field
The present invention relates to chemical analysis technology field more particularly to a kind of matrix stable introducing devices.
Background technique
Laser ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) directly can carry out main, micro member to sample to be tested The rapid and accurate determination of element and isotopic ratio, it is possible to provide the micro-zone in situ information of sample.Due to its high spatial resolution, low sample Many advantages, such as product consume, sample analysis time is short.Therefore, which has had within short decades quickly since appearance Development, has been widely used in the fields such as geology, biology, environment, archaeology, metallurgy.
The matrix effect of different sample rooms in LA-ICP-MS instrumental sensitivity and analytic process is to influence laser quantitatively to divide The key factor of analysis.Studies have shown that active matrix (water or organic reagent), which is introduced to plasma mass, can greatly improve Its analysis ability has remarkable result for increasing instrumental sensitivity and reducing the matrix effect in analytic process.It is shelled in laser During losing Plasma Mass Spectrometry analysis, water is introduced how stably and controllablely or organic reagent matrix is current a great problem.Mesh Before, conventional be atomized matrix reagent using atomiser system is introduced, but this method is introduced into reagent while also will be miscellaneous in reagent Matter introduces mass spectrograph, and active matrix introduction volume can not be controlled preferably.Matrix reagent can also be placed in laser ablation pond with Naturally the mode volatilized introduces mass spectrograph, and still, the method stability of the introducing matrix reagent is poor, can not practical application.
Therefore, how to realize matrix reagent (water or organic reagent) stablize introduce and avoid due to reagent purity not enough and Caused by pollution be always problem anxious to be resolved.Up to the present, it yet there are no dedicated equipment to solve this problem.
Summary of the invention
To solve the deficiencies in the prior art, it the present invention provides a kind of matrix stable introducing device, can freely control steady Surely it introduces active matrix (water, organic reagent etc.) steam and can be avoided the device of pollution, be remarkably improved plasma constitution Spectrum analysis sensitivity reduces the matrix effect in plasma, to improve the analysis ability of laser ablation plasma mass.
To achieve the above object, present invention employs a kind of technical solutions:A kind of matrix stable introducing device, described matrix Stablizing introducing device includes vaporization chamber, upper heating mantles, lower heating mantles, pump line, peristaltic pump, reagent bottle;The side of the vaporization chamber Equipped with connector is introduced, one end of the pump line connects the reagent bottle, the other end connects the introducing connector;The pump line winding The peristaltic pump, the peristaltic pump drive the pump line that the matrix reagent in the reagent bottle is introduced into the vaporization chamber;Institute It states the two sides at the top of vaporization chamber and is respectively equipped with carrier gas inlet suction port and steam air outlet adapter, accessed by the carrier gas inlet suction port Carrier gas exports steam into the vaporization chamber, through the steam air outlet adapter;The side of the vaporization chamber bottom end is equipped with waste liquid Waste liquid is discharged by the waste liquid connector in connector;The upper heating mantles, lower heating mantles are respectively assembled in the top of the vaporization chamber And lower part, for heating the vaporization chamber.
Further, the vaporization chamber has a vaporization chamber cavity, the both ends of the vaporization chamber be two semicircular spherical shells, Centre is cylindrical shell.
Further, the interior bottom of the vaporization chamber cavity is equipped with drainage trough, one end of the drainage trough and the introducing Connector connection, the other end are connect with the waste liquid connector.
Further, the pump line, introduce connector, drainage trough, waste liquid connector quantity be two, each pump line connects An introducing connector is connect, one end of each drainage trough is all connected with an introducing connector, the other end is all connected with a waste liquid connector, and two are drawn Chute is parallel to each other.
Further, for the introducing connector towards the waste liquid connector horizontal tilt, inclined angular range is 10-15 °.
Further, the making material of the vaporization chamber is quartz.
Further, the upper heating mantles, lower heating mantles making material be the aluminium alloy of anodic oxidation.
Further, the upper heating mantles, lower heating mantles inside be equipped with heating rod, for by the upper heating mantles And/or the internal temperature control of lower heating mantles is at 0-100 DEG C.
Further, the upper heating mantles are equipped with the first nipple orifice, the second nipple orifice, the carrier gas inlet suction port and steaming Vapour air outlet adapter is respectively corresponded across first nipple orifice, the second nipple orifice;The lower heating mantles are equipped with third nipple orifice, The waste liquid connector passes through the third nipple orifice.
The embodiment of the present invention provide technical solution bring beneficial effect be:(1) present invention greatly improves matrix The stability that reagent (such as water, organic reagent etc.) introduces;(2) present invention is processed into using high purity quartz, high temperature resistant corrosion resistant Erosion, evaporation introduce reagent, avoid the pollution of reagent bring itself;(3) wriggling pump speed, flow rate of carrier gas and heating temperature are adjustable, Convenient for controlling steam introduction volume.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of matrix stable introducing device of the invention;
Fig. 2 is the structural schematic diagram of vaporization chamber of the invention;
Fig. 3 is the test data figure present invention introduces pure water.
In figure:1- vaporization chamber, the upper heating mantles of 2-, 3- pump line, 4- peristaltic pump, 5- reagent bottle, 6- vaporization chamber cavity, 7- carrier gas Inlet suction port, 8- evaporate air outlet adapter, and 9- introduces connector, 10- drainage trough, 11- waste liquid connector, heating mantles under 12-, 13- first Nipple orifice, the second nipple orifice of 14-, 15- third nipple orifice.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention Formula is further described.
As illustrated in fig. 1 and 2, the present invention provides a kind of matrix stable introducing device, described matrix stablizes introducing device packet Include vaporization chamber 1, upper heating mantles 2, lower heating mantles 12, pump line 3, peristaltic pump 4, reagent bottle 5.
The vaporization chamber 1 has vaporization chamber cavity 6, it is preferred that the both ends of the vaporization chamber 4 are two semicircular balls Shell, centre are cylindrical shell.The vaporization chamber 1 is integrally formed, it is preferred that the making material of the vaporization chamber 1 is quartz.Institute The two sides for stating 1 top of vaporization chamber are respectively equipped with carrier gas inlet suction port 7 and steam air outlet adapter 8, pass through the carrier gas inlet suction port 7 Carrier gas is accessed into the vaporization chamber cavity 6, steam is exported by the steam air outlet adapter 8, such as introduce plasma constitution In spectrum.It is equipped in side one end of the vaporization chamber 1 and introduces connector 9, the introducing connector 9 is described for introducing matrix reagent It introduces connector 9 and is arc-shaped the drainage trough 10 for being connected to bottom in the vaporization chamber cavity 6, for example, the length of the drainage trough 10 Degree may range from 70-80mm, and the drainage trough 10 is designed as up-side down triangle, can make matrix reagent held stationary when flowing through Uniformly, allow the evaporation of matrix reagent more stable.One end of the drainage trough 10 connect with the introducing connector 9, the other end and useless Liquid connector 11 connects, and waste liquid is discharged by the waste liquid connector 11, and the waste liquid connector 11 is set to 1 bottom end of vaporization chamber Side.
The upper heating mantles 2, lower heating mantles 12 can be respectively assembled in the top and lower part of the vaporization chamber 1, to right The vaporization chamber 1 is heated, such as heating temperature may be configured as 0-100 DEG C.Preferably, the upper heating mantles 2, lower heating mantles 12 material is the aluminium alloy of anodic oxidation.The upper heating mantles 2 are equipped with the first nipple orifice 13, the second nipple orifice 14, institute First nipple orifice 13, the second nipple orifice 14 can be each passed through by stating carrier gas inlet suction port 7 and steam air outlet adapter 8.Under described Heating mantles 12 are equipped with third nipple orifice 15, and the waste liquid connector 11 may pass through the third nipple orifice 15, it is preferred that described the The quantity of three nipple orifices 15 is one, and two waste liquid connectors 11 can be each passed through the third nipple orifice 15.The upper heating mantles 2, the inside of lower heating mantles 12 is equipped with heating rod (such as two heating rods, because being not shown in inside, Fig. 1), is used for institute The internal temperature control of heating mantles 2 and/or lower heating mantles 12 is stated at 0-100 DEG C.
One end of the pump line 3 connects the reagent bottle 5, the other end connects the introducing connector 9, in the pump line 3 Portion winds the peristaltic pump 4, and the peristaltic pump 4 drives the pump line 3 that the matrix reagent in the reagent bottle 5 is introduced the steaming It sends out in room 1, the revolving speed of the peristaltic pump 4 is adjustable, speed is pumped into control matrix reagent, for example, the revolving speed of the peristaltic pump 4 Range:0.1-0.5RPS rotation is per second.
The pump line 3, the quantity for introducing connector 9, drainage trough 10 and waste liquid connector 11 can be one or more, and quantity It is all the same, it is preferred that the pump line 3, the quantity for introducing connector 9, drainage trough 10 and waste liquid connector 11 are two, each pump line 3 are all connected with an introducing connector 9, and one end of each drainage trough 10 is all connected with an introducing connector 9, the other end is all connected with a waste liquid connector 11, and two drainage troughs 10 are parallel to each other.
The workflow of matrix stable introducing device of the invention is:Firstly, device prepares:It is filled in the reagent bottle 5 Enter matrix reagent (such as water, organic reagent etc.), one end of the pump line 3 is put into the reagent bottle 5, can be touched Matrix reagent in the reagent bottle 5;The other end of the pump line 3 is connect with the introducing connector 9, the pump line 3 is twined Around the peristaltic pump 4;The upper heating mantles 2, lower heating mantles 12 are assembled respectively in top, the lower part of the vaporization chamber 1, by institute It states carrier gas inlet suction port 7 and accesses carrier gas port, the steam air outlet adapter 8 accesses plasma mass;By drawing for the vaporization chamber 1 Enter connector 9 towards 11 slant setting of waste liquid connector, such as 15 ° of inclination;Secondly, starting to introduce:Carrier gas port is opened, and sets carrier gas Flow accesses carrier gas by the carrier gas inlet suction port 7;The peristaltic pump 4 is opened, and sets wriggling pump speed, by described Reagent in the reagent bottle 5 is pumped into the vaporization chamber cavity 6 by peristaltic pump 4;Heater switch is opened, and sets heating temperature Degree, heats the vaporization chamber by the upper heating mantles 2, lower heating mantles 12, to accelerate the evaporation of reagent, extra examination Agent will be flowed out from the waste liquid connector 11, introducing plasma mass that can be stable by water vapour.During introducing, carrier gas stream The parameters such as amount, wriggling pump speed, heating temperature can be adjusted according to the actual situation.
In order to keep matrix stable introducing device operability of the invention stronger, main ginseng involved in the present invention is given Number recommended value, it should be pointed out that when carrying out practical operation, above-mentioned parameter can be modified, and should be included in the present invention Protection scope in.
The internal diameter of the pump line 3 is 0.762mm;
The total length of the vaporization chamber 1 is 104mm, and wherein the internal diameter of spherical shell and cylindrical shell is 30mm;
The carrier gas inlet suction port 7, evaporation air outlet adapter 8, introduce connector 9, waste liquid connector 11 internal diameter be 3mm;
The length of the drainage trough 10 is 73mm, and the distance of two parallel drainage troughs 10 is 7mm, and the drainage trough 10 is The up-side down triangle of special designing, joint length 15mm, internal diameter 3mm, outer diameter and the pump line 3 or with waste liquid connector 11 Connecting tube be sealed into it is suitable;
When placing the vaporization chamber 1, the introducing connector 9 is toward 11 slant setting of waste liquid connector, tilt angle 10-15°。
For convenience of the present invention is understood, the test data figure of introducing pure water as shown in Figure 3, ordinate is signal strength (Signal intensity/106Cps), abscissa is testing time (Time/min), is using laser ablation plasma constitution In the test of spectrometer, stablizes introducing device using collective of the invention and introduce pure water (H2When O), monitoring17O+Signal is when long It is interior to be always maintained at steadily.Wherein wriggling pump speed is 0.1RPS, and using argon gas as carrier gas, flow velocity is 0.2L min-1.
The embodiment of the present invention provide technical solution bring beneficial effect be:(1) present invention greatly improves matrix The stability that reagent (such as water, organic reagent etc.) introduces;(2) present invention is processed into using high purity quartz, high temperature resistant corrosion resistant Erosion, evaporation introduce reagent, avoid the pollution of reagent bring itself;(3) wriggling pump speed, flow rate of carrier gas and heating temperature are adjustable, Convenient for controlling steam introduction volume.
It is worth noting that:In the description of the present invention, the meaning of " plurality " is two or more, unless otherwise bright It is really specific to limit.In the present invention unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " Gu It is fixed " etc. terms shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected, can To be mechanical connection, for the ordinary skill in the art, above-mentioned term can be understood in this hair as the case may be Concrete meaning in bright.
Herein, the nouns of locality such as related front, rear, top, and bottom are to be located in figure with components in attached drawing and zero Part mutual position defines, only for the purpose of expressing the technical solution clearly and conveniently.It should be appreciated that the noun of locality Use should not limit the claimed range of the application.
In the absence of conflict, the feature in embodiment and embodiment herein-above set forth can be combined with each other.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (9)

1. a kind of matrix stable introducing device, it is characterised in that:It includes vaporization chamber, upper heating that described matrix, which stablizes introducing device, Cover, lower heating mantles, pump line, peristaltic pump, reagent bottle;The side of the vaporization chamber, which is equipped with, introduces connector, and one end of the pump line connects Connect the reagent bottle, the other end connects the introducing connector;The pump line winds the peristaltic pump, described in the peristaltic pump drives Matrix reagent in the reagent bottle is introduced into the vaporization chamber by pump line;Two sides at the top of the vaporization chamber are respectively equipped with carrier gas Inlet suction port and steam air outlet adapter access carrier gas into the vaporization chamber by the carrier gas inlet suction port, pass through the steaming Vapour air outlet adapter exports steam;The side of the vaporization chamber bottom end is equipped with waste liquid connector, and waste liquid is discharged by the waste liquid connector; The upper heating mantles, lower heating mantles are respectively assembled in the top and lower part of the vaporization chamber, for heating the vaporization chamber.
2. matrix stable introducing device according to claim 1, it is characterised in that:The vaporization chamber is with evaporation chamber Body, the both ends of the vaporization chamber are two semicircular spherical shells, centre is cylindrical shell.
3. matrix stable introducing device according to claim 2, it is characterised in that:The interior bottom of the vaporization chamber cavity is set There is drainage trough, one end of the drainage trough is connect with the introducing connector, the other end is connect with the waste liquid connector.
4. matrix stable introducing device according to claim 3, it is characterised in that:The pump line introduces connector, drainage Slot, waste liquid connector quantity be two, each pump line is all connected with an introducing connector, and one end of each drainage trough is all connected with one and draws Enter connector, the other end is all connected with a waste liquid connector, and two drainage troughs are parallel to each other.
5. matrix stable introducing device according to claim 1, it is characterised in that:The introducing connector connects towards the waste liquid Head horizontal tilt, inclined angular range are 10-15 °.
6. matrix stable introducing device according to claim 1, it is characterised in that:The making material of the vaporization chamber is stone English.
7. matrix stable introducing device according to claim 1, it is characterised in that:The upper heating mantles, lower heating mantles Making material is the aluminium alloy of anodic oxidation.
8. matrix stable introducing device according to claim 1, it is characterised in that:The upper heating mantles, lower heating mantles Inside is equipped with heating rod, for by the internal temperature control of the upper heating mantles and/or lower heating mantles at 0-100 DEG C.
9. matrix stable introducing device according to claim 1, it is characterised in that:The upper heating mantles are equipped with first and connect Head bore, the second nipple orifice, the carrier gas inlet suction port and steam air outlet adapter are respectively corresponded across first nipple orifice, second Nipple orifice;The lower heating mantles are equipped with third nipple orifice, and the waste liquid connector passes through the third nipple orifice.
CN201810332380.7A 2018-04-13 2018-04-13 A kind of matrix stable introducing device Pending CN108845024A (en)

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Publication number Priority date Publication date Assignee Title
CN117153660A (en) * 2023-11-01 2023-12-01 中国地质大学(武汉) Automatic sampling solution laser ablation pond

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117153660A (en) * 2023-11-01 2023-12-01 中国地质大学(武汉) Automatic sampling solution laser ablation pond
CN117153660B (en) * 2023-11-01 2024-01-12 中国地质大学(武汉) Automatic sampling solution laser ablation pond

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