CN106198494A - A kind of inductive coupling plasma emission spectrograph - Google Patents
A kind of inductive coupling plasma emission spectrograph Download PDFInfo
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- CN106198494A CN106198494A CN201610509616.0A CN201610509616A CN106198494A CN 106198494 A CN106198494 A CN 106198494A CN 201610509616 A CN201610509616 A CN 201610509616A CN 106198494 A CN106198494 A CN 106198494A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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Abstract
The invention provides a kind of inductive coupling plasma emission spectrograph, belong to plasma spectrometer technical field.nullThe lower end of bracing frame is fixing with insulator foot to be connected，Cylinder is fixed on the insulator foot of bracing frame side，The upper end of bracing frame is fixed with water cooled electrode，The lower end of quarter bend is fixing with upper water cooled electrode to be connected，The middle part of upper graphite cone is embedded in water cooled electrode，The top of upper graphite cone is located in quarter bend，Lower water cooled electrode is fixed on the upper end of the piston of cylinder，Lower graphite cone is fixed in lower water cooled electrode，Graphite-pipe is arranged between lower graphite cone and upper graphite cone，Central canal is arranged in quarter bend，The lower end of central canal is connected with upper graphite cone，It is provided with quarter bend sealing ring between upper graphite cone and quarter bend，It is provided with basepipe seal circle between central canal and upper graphite cone，The top of quarter bend is provided with loading coil，The middle part of described quarter bend is provided with cooling gas and high-tension ignition entrance and shielding gas entrance，The top of quarter bend is provided with quarter bend lateral openings and quarter bend axially open.
Description
Technical field
The present invention relates to a kind of inductive coupling plasma emission spectrograph, belong to plasma spectrometer technical field.
Background technology
Existing inductance coupling plasma emissioning spectral analysis mainly uses solution continuous sample introduction mode, works as measuring samples
During middle trace element, owing to being limited by instrument detection limit, it is impossible to implement to measure.It addition, it is to utilize nebulizer to be introduced by solution,
Become in the flame that aerosol enters inductively coupled plasma, and be allowed to atomization, excite characteristic spectral line.But, it is subject to
The nebulizer requirement to liquid viscosity, the sample every time measured is required for doing clears up process, and it is numerous that early stage prepares fluid sample process
Miscellaneous, impact analysis person works's efficiency.In modern analysis work, sample size and the abundant species of detection are various, especially with people
Live closely bound up foodstuff sample mostly presented in solid, dirty solution, by the survey of present sampling system requirement
Solid sample must be prepared as fluid sample by method for testing, this just generally require carry out dissolving, clear up, evaporate, constant volume etc. is
Row complex process, takes time and effort.
Also someone utilizes the method for spark ablation or laser ablation solid to realize solid sampling, and its principle is put for utilizing spark
Solid sample ablation is become aerosol to be incorporated in square flame by the energy that electricity or laser produce.Although the method can also realize solid
Sample introduction, but can be with substantial amounts of flue dust during ablation solid sample, and the stability of interference square flame, background influence is relatively big, shadow
Ring accuracy and the credibility of measurement result.
Summary of the invention
The invention aims to solve the problem that above-mentioned prior art exists, i.e. can accompany during ablation solid sample
With substantial amounts of flue dust, the stability of interference square flame, background influence is relatively big, affects accuracy and the credibility of measurement result.And then
A kind of inductive coupling plasma emission spectrograph is provided.
It is an object of the invention to be achieved through the following technical solutions:
A kind of inductive coupling plasma emission spectrograph, including: radio-frequency signal generator, solid-liquid sampling system, beam splitting system,
Detecting system and computer system, described radio-frequency signal generator and solid-liquid sampling system are connected with each other, solid-liquid sampling system and light splitting
System is connected with each other, and beam splitting system and detecting system are connected with each other, computer system respectively with radio-frequency signal generator, solid-liquid sample introduction system
System, beam splitting system are connected with detecting system；Described solid-liquid sampling system includes: insulator foot, bracing frame, cylinder, lower water-cooled
Electrode, lower graphite cone, graphite-pipe, upper graphite cone, upper water cooled electrode, quarter bend sealing ring, basepipe seal circle, central canal, quarter bend
And loading coil, the lower end of support frame as described above is fixing with insulator foot to be connected, and cylinder is fixed on the insulator foot of bracing frame side
On, the upper end of bracing frame is fixed with water cooled electrode, and the lower end of quarter bend is fixing with upper water cooled electrode to be connected, the middle part of upper graphite cone
Being embedded in water cooled electrode, the top of upper graphite cone is located in quarter bend, and lower water cooled electrode is fixed on the upper end of the piston of cylinder, under
Graphite cone is fixed in lower water cooled electrode, and graphite-pipe is arranged between lower graphite cone and upper graphite cone, and central canal is arranged on quarter bend
In, the lower end of central canal is connected with upper graphite cone, is provided with quarter bend sealing ring, central canal and upper stone between upper graphite cone and quarter bend
Being provided with basepipe seal circle between ink cone, the top of quarter bend is provided with loading coil, and the middle part of described quarter bend is provided with cooling gas and height
Pressure point fire entrance and shielding gas entrance, the top of quarter bend is provided with quarter bend lateral openings and quarter bend axially open.
The inductive coupling plasma emission spectrograph of the present invention, has broken the constraint of traditional input mode, it is achieved solid,
Micro-amounts of liquids sampling technique, utilize graphite furnace power supply to equipped with sample graphite-pipe heat realize sample be dried, ashing, atom
Changing, sample matrices and element sepatation to be measured, ambient interferences is little.Sample is elements vaporization to be measured effusion after being heated, and is directed to inductance
In the square flame of coupled plasma optical emission spectrogrph, element to be measured is heated atomization in square flame again, and inspires corresponding unit
The spectral line of emission of element, by carrying out qualitative and quantitative measurement to element to be measured to the analysis of spectral line.When trace in measuring samples
During element, owing to sample can be enriched with at drying stage repeatedly, at atomized stage, atom is concentrated release, is considerably increased square
Atomic concentration in flame, it is possible to realize the measurement of trace element in sample.
Accompanying drawing explanation
Fig. 1 is the annexation schematic diagram of inductive coupling plasma emission spectrograph of the present invention.
Fig. 2 is the original state schematic diagram of solid-liquid sampling system.Graphite-pipe 15 can take out or change.
Fig. 3 is the original operating state schematic diagram of solid-liquid sampling system.
Fig. 4 is the original operating state sectional view of solid-liquid sampling system.
Fig. 5 is the sectional view of the graphite-pipe 15 being placed with testing sample.
Fig. 6 is Electromagnetic Heating schematic diagram.
Fig. 7 is that tungsten filament heats schematic diagram.
Reference in figure, 1 is radio-frequency signal generator, and 2 is solid-liquid sampling system, and 3 is beam splitting system, and 4 is detecting system,
5 is computer system, and 10 is insulator foot, and 11 is bracing frame, and 12 is cylinder, and 12-1 is piston, and 13 is lower water cooled electrode, and 14 are
Lower graphite is bored, and 15 is graphite-pipe, and 15-1 is tangential hole, and 16 is upper graphite cone, and 17 is upper water cooled electrode, and 18 is quarter bend sealing ring,
Seal of tube circle centered by 19, manages centered by 20, and 21 is quarter bend, and 21-1 is cooling gas and high-tension ignition entrance, and 21-2 is shielding gas
Entrance, 21-3 is quarter bend lateral openings, and 21-4 is quarter bend axially open, and 22 is loading coil, and 23 connect for upper water cooled electrode cold water
Mouthful, 24 is air inlet, and 25 is lower water cooled electrode cold water interface, and 26 is cylinder air inlet/outlet one, and 27 is cylinder air inlet/outlet two, 28
For testing sample, I is vertical relations mouth, and II is axial observation mouth, and 201 is coil, and 202 is power supply, 203 protection sets.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail: the present embodiment with technical solution of the present invention is being
Implement under premise, give detailed embodiment, but protection scope of the present invention is not limited to following embodiment.
As shown in Fig. 1～Fig. 7, a kind of inductive coupling plasma emission spectrograph involved by the present embodiment, including: penetrate
Frequency generator 1, solid-liquid sampling system 2, beam splitting system 3, detecting system 4 and computer system 5, described radio-frequency signal generator 1 is with solid
Liquid sampling system 2 is connected with each other, and solid-liquid sampling system 2 and beam splitting system 3 are connected with each other, and beam splitting system 3 and detecting system 4 are mutual
Connecting, computer system 5 is connected with radio-frequency signal generator 1, solid-liquid sampling system 2, beam splitting system 3 and detecting system 4 respectively；Institute
State solid-liquid sampling system 2 to include: insulator foot 10, bracing frame 11, cylinder 12, lower water cooled electrode 13, lower graphite cone 14, graphite-pipe
15, upper graphite cone 16, upper water cooled electrode 17, quarter bend sealing ring 18, basepipe seal circle 19, central canal 20, quarter bend 21 and load
Coil 22, the lower end of support frame as described above 11 is fixing with insulator foot 10 to be connected, and cylinder 12 is fixed on the insulation of bracing frame 11 side
On base 10, the upper end of bracing frame 11 is fixed with water cooled electrode 17, and the lower end of quarter bend 21 is fixing with upper water cooled electrode 17 to be connected,
The middle part of upper graphite cone 16 is embedded in water cooled electrode 17, and the top of upper graphite cone 16 is located in quarter bend 21, lower water cooled electrode 13
Being fixed on the upper end of the piston 12-1 of cylinder 12, lower graphite cone 14 is fixed in lower water cooled electrode 13, and graphite-pipe 15 is arranged on down
Between graphite cone 14 and upper graphite cone 16, central canal 20 is arranged in quarter bend 21, and 16 phases are bored with upper graphite in the lower end of central canal 20
Connection, is provided with quarter bend sealing ring 18, is provided with center between central canal 20 and upper graphite cone 16 between upper graphite cone 16 and quarter bend 21
Seal of tube circle 19, the top of quarter bend 21 is provided with loading coil 22, and the middle part of described quarter bend 21 is provided with cooling gas and high-tension ignition enters
Mouth 21-1 and shielding gas entrance 21-2, the top of quarter bend 21 is provided with quarter bend lateral openings 21-3 and quarter bend axially open 21-4.
Described radio-frequency signal generator 1 uses the auto-excitation type high frequency generator of 27.12MHz or 40.68MHz.
The conical surface vicinity, top of described graphite-pipe 15 is provided with three tangential hole 15-1, and the gas entered from there can be at stone
Ink pipe 15 is centrally formed gas swirling flow, can be loaded in square flame by the atom of the element to be measured being evaporated in testing sample 28,
Also can realize by other structure, such as gas is from the internal entrance of graphite-pipe 15, and gas can be argon or nitrogen.
As shown in Figure 2 to 4, cylinder 12 and bracing frame 11 are fixed on insulating base 10, can drive after cylinder 12 ventilation
Lower water cooled electrode 13 moves up or down together with lower graphite cone 14.Upper water cooled electrode 17 is arranged on bracing frame 11, upper stone
The external cylindrical surface of ink cone 16 and the centre bore secure fit of upper water cooled electrode 17, central canal 20 is inserted into the endoporus of graphite cone 16
In, quarter bend 21 is inserted in the outside cylinder of graphite cone 16.In order to ensure to seal, bore between 16 at described quarter bend 21 and upper graphite
The quarter bend sealing ring 18 of two zero shapes is installed, it is ensured that from the cooling gas of cooling gas and high-tension ignition entrance 21-1 entrance the most upwards
Flowing；The basepipe seal circle 19 installing zero shape between 16 is bored, it is ensured that from shielding gas entrance at central canal 20 and upper graphite
The shielding gas that 21-2 enters only flows up.The loading coil 22 of radio-frequency signal generator 1 is concentric with quarter bend 21, and loading coil 22
Between central canal 20 and quarter bend 21 top end face.After work in every condition meets, the top exit site at quarter bend 21 can shape
Become square flame, from quarter bend lateral openings 21-3 (radial survey mouth I) and quarter bend axially open 21-4 (the axial observation mouth of quarter bend 21
II) light the launched system 3 that is split receives, and complex light is converted into monochromatic light, transfers to detecting system 4 to carry out photoelectricity and turn
Change, then be controlled processing with data by computer system 5.
Described solid-liquid sampling system 2 is for utilizing graphite furnace technology heating graphite-pipe 15 and testing sample 28.Solid-liquid sample introduction system
System 2 is not limited solely to graphite furnace heating technique, and it can also use electromagnetic heating technique, as shown in Figure 6 utilize alternating source
202 pairs of coils 201 are powered, and produce alternating electromagnetic field so that graphite-pipe 15 is heated, it is achieved testing sample 28 atomization；It is also
Conductive material can be used to pass to electric current directly heat, protection is overlapped the tungsten filament etc. in 203 by the power supply 202 that utilizes as shown in Figure 7
The coil 201 that material makes is powered so that on coil 201, testing sample 28 is heated, it is achieved testing sample 28 atomization.
The working method of solid-liquid sampling system 2 is as follows:
As shown in 3 and Fig. 4, after cylinder air inlet/outlet 2 27 ventilation, the piston 12-1 stress in cylinder 12 moves up, with
Lower water cooled electrode 13 and lower graphite cone 14 that piston 12-1 tightens together move up therewith, until the upper end cone of graphite-pipe 15
Till the inner conical surface good contact of 16 is bored with upper graphite in face.After lower water cooled electrode 13 and upper water cooled electrode 17 energising, pass through respectively
Lower graphite cone 14 and upper graphite cone 16 conduction, graphite-pipe 15 is heated, the testing sample 28 in graphite-pipe 15 be heated through
Be dried, ashing, after atomization, metallic element therein evaporation effusion, the carrier gas swirling flow disturbance entered by air inlet 24, by center
Pipe 20 is brought in the square flame of quarter bend 21.
Owing to utilizing graphite furnace mode to produce high temperature (up to 3000 DEG C), so must prevent during heating sample
Protect.Cold water enters in lower water cooled electrode 13, from upper water-cooled from lower water cooled electrode cold water interface 25 (two, one-in-and-one-out) respectively
Electrode cold water interface 23 (two, one-in-and-one-out) enters into and carries out cooling protection in water cooled electrode 17, is passed through from air inlet 24
Indifferent gas enters in the cavity of graphite cone 16 and lower graphite cone 14 formation, and a part of gas is from upper graphite cone 16 and lower graphite
Gap effusion between cone 14, prevents graphite cone 16 and the oxidized corrosion of inner surface of lower graphite cone 14；Another part gas from
It is internal that three tangential hole 15-1 (shown in Fig. 5) at graphite-pipe 15 top enter into graphite-pipe 15, enters within graphite-pipe 15
Gas forms swirling flow, is taken out of by the element to be measured of effusion from the testing sample 28 of solid.
Otherwise, after cylinder air inlet/outlet 1 ventilation, the piston 12-1 stress in cylinder 12 moves down, with piston 12-1
The lower water cooled electrode 13 of fastening and lower graphite cone 14 move down therewith, make graphite-pipe 15 separate with upper graphite cone 16.So stone
Ink pipe 15 can take out, or the replaceable graphite-pipe 15 being placed with new testing sample 28 carries out test next time, the most repeatedly
Work.
Obtaining due to solid powder sample and goods are relatively easy to, the plasma hence with solid-liquid sampling system 2 is sent out
Penetrate spectrogrph and can be effectively improved work efficiency, be a kind of can rapid batch analyze instrument.
The above, the only present invention preferably detailed description of the invention, these detailed description of the invention are all based on the present invention
Different implementations under general idea, and protection scope of the present invention is not limited thereto, any are familiar with the art
Technical staff in the technical scope that the invention discloses, the change that can readily occur in or replacement, all should contain the present invention's
Within protection domain.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (4)
1. an inductive coupling plasma emission spectrograph, including: radio-frequency signal generator (1), solid-liquid sampling system (2), light splitting
System (3), detecting system (4) and computer system (5), described radio-frequency signal generator (1) interconnects mutually with solid-liquid sampling system (2)
Connecing, solid-liquid sampling system (2) and beam splitting system (3) are connected with each other, and beam splitting system (3) and detecting system (4) are connected with each other, and calculate
Machine system (5) is connected with radio-frequency signal generator (1), solid-liquid sampling system (2), beam splitting system (3) and detecting system (4) respectively；
It is characterized in that, described solid-liquid sampling system (2) including: insulator foot (10), bracing frame (11), cylinder (12), lower water-cooled electricity
Pole (13), lower graphite cone (14), graphite-pipe (15), upper graphite cone (16), upper water cooled electrode (17), quarter bend sealing ring (18), in
Heart seal of tube circle (19), central canal (20), quarter bend (21) and loading coil (22), the lower end of support frame as described above (11) and the insulation end
Seat (10) is fixing to be connected, and cylinder (12) is fixed on the insulator foot (10) of bracing frame (11) side, the upper end of bracing frame (11)
Being fixed with water cooled electrode (17), the lower end of quarter bend (21) is fixing with upper water cooled electrode (17) to be connected, in upper graphite cone (16)
Portion is embedded in water cooled electrode (17), and the top of upper graphite cone (16) is located in quarter bend (21), and lower water cooled electrode (13) is fixed on
The upper end of the piston (12-1) of cylinder (12), lower graphite cone (14) is fixed in lower water cooled electrode (13), and graphite-pipe (15) is arranged
Between lower graphite cone (14) and upper graphite cone (16), central canal (20) is arranged in quarter bend (21), the lower end of central canal (20)
Be connected with upper graphite cone (16), between upper graphite cone 16 and quarter bend (21), be provided with quarter bend sealing ring (18), central canal (20) and
Being provided with basepipe seal circle (19) between upper graphite cone (16), the top of quarter bend (21) is provided with loading coil (22), described quarter bend
(21) middle part is provided with cooling gas and high-tension ignition entrance (21-1) and shielding gas entrance (21-2), and the top of quarter bend (21) is provided with
Quarter bend lateral openings (21-3) and quarter bend axially open (21-4).
Inductive coupling plasma emission spectrograph the most according to claim 1, it is characterised in that described radio-frequency signal generator
(1) the auto-excitation type high frequency generator of 27.12MHz or 40.68MHz is used.
Inductive coupling plasma emission spectrograph the most according to claim 1, it is characterised in that described graphite-pipe (15)
Conical surface vicinity, top be provided with three tangential holes (15-1).
Inductive coupling plasma emission spectrograph the most according to claim 1, it is characterised in that described quarter bend (21) with
Between upper graphite cone (16), two zero shapes quarter bend sealing ring (18) are installed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610509616.0A CN106198494A (en) | 2016-06-30 | 2016-06-30 | A kind of inductive coupling plasma emission spectrograph |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610509616.0A CN106198494A (en) | 2016-06-30 | 2016-06-30 | A kind of inductive coupling plasma emission spectrograph |
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| CN106198494A true CN106198494A (en) | 2016-12-07 |
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| CN201610509616.0A Pending CN106198494A (en) | 2016-06-30 | 2016-06-30 | A kind of inductive coupling plasma emission spectrograph |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107591310A (en) * | 2017-09-30 | 2018-01-16 | 北京普析通用仪器有限责任公司 | A kind of graphite furnace Electrothermal vaporization feeding device ion gun and its plasma mass spectrograph |
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| CN107591310A (en) * | 2017-09-30 | 2018-01-16 | 北京普析通用仪器有限责任公司 | A kind of graphite furnace Electrothermal vaporization feeding device ion gun and its plasma mass spectrograph |
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Application publication date: 20161207 |