CN203216852U - Atomic vapor sampling device based on electrodeposition and electric heating - Google Patents
Atomic vapor sampling device based on electrodeposition and electric heating Download PDFInfo
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- CN203216852U CN203216852U CN 201320102578 CN201320102578U CN203216852U CN 203216852 U CN203216852 U CN 203216852U CN 201320102578 CN201320102578 CN 201320102578 CN 201320102578 U CN201320102578 U CN 201320102578U CN 203216852 U CN203216852 U CN 203216852U
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Abstract
The utility model discloses an atomic vapor sampling device based on electrodeposition and electric heating. The atomic vapor sampling device comprises an insulated evaporation cavity with a sampling hole and a gas discharge hole, wherein the evaporation cavity is internally provided with an electric heating wire; the two ends of the electric heating wire penetrates through the walls of the evaporation cavity so as to be respectively connected with a lead; the two opposite walls of the evaporation cavity are respectively provided with an electrode. During electrolysis, the two electrodes are connected with a direct-current power supply through leads and the two ends of the electric heating wire are connected with the negative pole of the direct-current power supply through leads; during electric heating, the two ends of the electric wire are respectively connected with the positive pole and the negative pole of an electric heating power supply through a lead. After a liquid to be detected is electrolytically enriched, a waste liquid is discharged and an electrolysis cavity is dried, so that desolvation of the liquid to be detected is realized, a desolventizer is omitted, a small size is achieved and instrument miniaturization is realized; a powerful technological base is provided for miniaturization and portability of an atomic spectroscopy instrument.
Description
Technical field
The utility model relates to electro-deposition-Electrothermal Atomic steam sampling device, belongs to the instrument analysis technology field.
Background technology
It is " bottleneck " that the sensitivity of restriction atomic spectroscopy improves that sample is introduced technology always, is the most active and most important research field in the atomic spectrometry determination development.Mainly comprise pneumatic nebulization method, ultrasonic atomizatio method, hot atomization, outstanding slurry atomization, high-pressure atomization method and electron spray method etc. now.The pneumatic nebulization method mainly has than obvious defects at aspects such as nebulization efficiency, anti-high salt ability and memory effects; The ultrasonic atomizatio cost is higher, and matrix effect is bigger, and molten backup system must be arranged, and is unfavorable for instrument miniaturization; The heat atomizing has higher nebulization efficiency, but matrix effect is serious, has must possess to assist to remove dissolving device, is unfavorable for instrument miniaturization; Outstanding slurry atomization requires particle to wash and evenly; High-pressure atomization requires to provide high pressure, and at present during low discharge effect bad, be unfavorable for instrument miniaturization.
Electro-deposition refers to that simple metal ion or complexation of metal ions form the process of metal or alloy coating at material surface by the galvanochemistry approach.These processes are carried out under certain electrolyte and operating conditions, and the complexity of metal electrodeposition and sedimental form are relevant with the character of plated metal, also depend on factors such as electrolytical composition, pH value, temperature, current density.Set an appropriate sedimentation potential according to element to be measured, can realize separating with element less than this sedimentation potential, namely less than the element of this sedimentation potential still in liquid, and arrived electrode surface greater than the element deposition of this sedimentation potential.
Electric heating evaporation is big electric current by resistance heating, and when temperature acquires a certain degree, the on-gaseous material gasification of being heated around the conductor is if temperature continues to raise and will make the material on every side excited atomization of being heated.Different gasification substances, atomization temperature difference possess certain separating power.
At present, the report that electro-deposition-electric heating is used for ultimate analysis atomic vapour sample introduction is not also arranged.It is having broad application prospects aspect atomic spectrum sample introduction, particularly the miniaturization of analytical instrument and aspect linearize.
Summary of the invention
The utility model purpose:For solving the problems of the technologies described above, the purpose of this utility model provides electro-deposition-Electrothermal Atomic steam sampling device, and the sample that electro-deposition-electroheat technology is applied to atomic spectroscopy is introduced.
Technical scheme:For reaching above-mentioned technique effect, the utility model adopts following technical scheme:
A kind of based on electro-deposition Electrothermal Atomic steam sampling device, comprise the insulation evaporation cavity, evaporation cavity is provided with injection port 3 and exhausr port 4, described evaporation cavity inside is provided with heating wire 6, described heating wire 6 two ends are passed the chamber wall and are connected with lead 2 respectively, are respectively equipped with an electrode 1 on relative two the chamber walls of described evaporation cavity; When electrolysis: described two electrodes 1 are connected with direct supply by lead, and described heating wire 6 two ends are connected with dc power cathode by lead 2; When heating: described heating wire 6 two ends are connected with the electric heating power positive cathode respectively by lead 2.
Described cavity also is provided with air admission hole, forms gas distribution system with injection port, and described air admission hole is a plurality of, forms even gas distribution system.Described heating wire material is tungsten, molybdenum, platinum or tantalum, and described electrode material is gold-plated or platinum plating; Described insulation evaporation cavity is made of heat proof material, and the insulation heat proof material is simple glass, pyroceram, quartz or ceramic.
Use in the utility model process, when adopting the potentiostatic method electrolysis, direct supply voltage is-10V ~+10V; When adopting the galvanostatic method electrolysis, the direct supply electric current is 0.2A ~ 5A; The electric heating supply voltage is 220V among the step b, and electric current is 50HZ.Described carrier gas is at least a and hydrogen 0 ~ 10% combination gas in helium, argon gas, neon and the nitrogen.The complete electrolytic deposition of described determinand is: voltage jump, electric current are close to 0 or to set electrolysis time be 5 ~ 50 minutes.
The utility model is applied to the sample introduction of plasma generator with electrolysis and electroheat technology combination.Wherein electric heating comprises electric heating evaporation and electric atomizing.Wherein electrolysis and electroheat technology combination are present, and heating wire as electrolysis electrode, plays electric action in electrolytic process, play heating functioin in the electric heating process.These parts generate heat under the effect of power supply, realize drying in the chamber and determinand is vaporized, atomization.
Beneficial effect:
The utility model with liquid electrolysis enrichment to be measured after effluent discharge, the oven dry electrolyte chamber, it is molten to realize that liquid to be measured goes, save dissolving device, volume is little, has realized the miniaturization of instrument, for the miniaturization of atomic spectroscopy instrument, portablely provide strong technical foundation;
2. the utlity model has the concentration and separation effect, in electrolytic process, realize initial gross separation and the enrichment of determinand by adopting appropriate voltage, in the electric heating process, by appropriate air inlet and heating mode, further realize separation and the enrichment of determinand.At the determinand volatilization temperature near excitation temperature, the carrier gas intake velocity is 0 or near 0, forms to fill the air effect, increases the testing concentration that enters next stage, increase first stage ionization efficient, can effectively improve sensitivity, reduce the matrix interference and reduce memory effect.The condensation rate of determinand is very high, has further improved sensitivity.Through one-level atomization, can effectively reduce the next stage condition of work, improve next stage atomization/Ionization Efficiency.
Description of drawings
Fig. 1 is the structural representation of electro-deposition-Electrothermal Atomic steam sampling device.
Fig. 2 is base plate vertical view among Fig. 1.
Wherein: 1. electrode, 2. lead, 3. injection port, 4. exhausr port, 5. base plate, 6. heating wire, 7,8. insulated cavity wall.
Embodiment
Below in conjunction with drawings and Examples the utility model is elaborated:
A kind of electro-deposition Electrothermal Atomic of the utility model steam sampling device as shown in Figure 1, comprise by insulated cavity wall 7,8 and the evaporation cavity formed of base plate 5, evaporation cavity is provided with injection port 3 and exhausr port 4, described evaporation cavity inside is provided with heating wire 6, described heating wire 6 two ends are passed the chamber wall and are connected with lead 2 respectively, are respectively equipped with an electrode 1 on relative two the chamber walls of described evaporation cavity; When electrolysis: described two electrodes 1 are connected with direct supply by lead, and described heating wire 6 two ends are connected with dc power cathode by lead 2; When heating: described heating wire 6 two ends are connected with the electric heating power positive cathode respectively by lead 2.
Embodiment 1: as shown in Figure 1, evaporation cavity by pyroceram 7,8 and pyroceram base plate 5 form injection port 3 and exhausr port 4, form gas handling system, gold,platinized electrolysis electrode 1 is at the plate two ends, and tungsten filament heating wire 6 two ends are passed base plate 5 and connected lead 2, and the opposite is exhausr port 4.By injection port fluid injection, discharge opeing, be the feedback current power supply but air admission hole feeds the carrier gas heating with power supply, can realize the precision control of temperature.
With standard solution Cr(Cr
3+) enter from injection port 3 after, the combination gas of argon gas 95% and hydrogen 5% is entered by injection port 3 with 15ml/min, electrolysis is down stirred in carrier gas, adopt potentiostatic electrodeposition, sedimentation potential is-1.3V, this moment, two electrodes 1 connect dc power anode by lead, heating wire 6 two ends connect dc power cathode by lead 2, setting electrolysis time is 30 minutes, waste liquid is discharged by injection port 3, and heating wire 6 two ends connect 220V alternating-current power supply ground wire and live wire respectively by lead 2 afterwards, and heating wire 6 is heated to 100 ± 10 ℃, carrier gas simultaneously feeds with the speed of 100ml/min, dry back heating wire 6 heats up, and carrier gas feeds with 10ml/min speed, stops for 30 seconds to 1750 ℃, carrier gas speed is zero, heating wire 6 is rapidly heated to 2800 ℃ then, afterwards with the logical carrier gas of 50ml/min, treats that the signal stabilization of next stage stops heating afterwards, continuation is cooled to 50 ℃ of target temperatures with the logical carrier gas of 3000ml/min until heating wire.
Wherein the Cr sample solution is by [product IDs number] 107346[production code member] the GSBG62017-90[Chinese] chromium Cr, standard value: 1000ppm, matrix: 10%HCl (crome metal, trivalent) dilution obtain.
This apparatus structure is simple, and is easy for installation, do not going to have realized under the situation of dissolving device well going molten effect, obviously enrichment determinand, effectively reduced chaff interference, be very beneficial for the miniaturization of sampling device.
Embodiment 2: as shown in Figure 1, evaporation cavity is made up of quartz 7,8 and pyroceram base plate 5, and injection port 3 and exhausr port 4 are formed gas handling system, and gold,platinized electrolysis electrode 1 is at the plate two ends, and tungsten filament heating wire 6 two ends are passed base plate 5 and connected leads 2, and the opposite is exhausr port 4.
With standard solution Cd
2+After entering from injection port 3, enter stirring under electrolysis with 20ml/min by injection port 3 at 96% helium and 4% hydrogen mixed gas carrier gas, adopt galvanostatic deposition, electric current is 2A, this moment, electrolysis electrode 1 connect dc power anode by lead, heating wire 6 connects dc power cathode by lead 2, after finishing enrichment to determinand, this moment, sedimentation potential transitted to lower current potential suddenly at-1.0V, and waste liquid is discharged by injection port 3, and heating wire 6 connects 220V alternating-current power supply ground wire and live wire respectively by lead afterwards, PID controls temperature, be heated to 100 ± 10 ℃, carrier gas simultaneously feeds with the speed of 150ml/min, and dry back heating wire 10 heats up, carrier gas feeds with 20ml/min speed, stopped for 40 seconds to 280 ℃, carrier gas speed is zero, is rapidly heated then to 800 ℃, with the logical carrier gas of 80ml/min, the signal stabilization for the treatment of the next stage stops heating afterwards, continues the logical carrier gas with 1500ml/min, is cooled to 30 ℃ of target temperatures until heating wire.
Cd wherein
2+Sample solution is by [product IDs number] 98072[production code member] the GSB04-1721-2004[Chinese] cadmium standard solution [product specification] 50mL/ bottle standard value: 1000 μ g/ml dilution obtains.
Claims (3)
1. one kind based on electro-deposition Electrothermal Atomic steam sampling device, it is characterized in that: comprise the insulation evaporation cavity, evaporation cavity is provided with injection port (3) and exhausr port (4), described evaporation cavity inside is provided with heating wire (6), described heating wire (6) two ends are passed the chamber wall and are connected with lead (2) respectively, are respectively equipped with an electrode (1) on relative two the chamber walls of described evaporation cavity; During electrolysis: described two electrodes (1) are connected with direct supply by lead, and described heating wire (10) two ends are connected with dc power cathode by lead (2); During heating: described heating wire (10) two ends are connected with the electric heating power positive cathode respectively by lead (2).
2. device according to claim 1: it is characterized in that: described evaporation cavity also is provided with air admission hole, forms gas distribution system with injection port, and described air admission hole is a plurality of, forms even gas distribution system.
3. device according to claim 1: it is characterized in that: described heating wire (10) material is tungsten, molybdenum, platinum or tantalum, and described electrode material is gold-plated or platinum plating; Described insulation evaporation cavity is made of heat proof material, and the insulation heat proof material is simple glass, pyroceram, quartz or ceramic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320102578 CN203216852U (en) | 2013-03-06 | 2013-03-06 | Atomic vapor sampling device based on electrodeposition and electric heating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320102578 CN203216852U (en) | 2013-03-06 | 2013-03-06 | Atomic vapor sampling device based on electrodeposition and electric heating |
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| CN203216852U true CN203216852U (en) | 2013-09-25 |
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| CN 201320102578 Expired - Fee Related CN203216852U (en) | 2013-03-06 | 2013-03-06 | Atomic vapor sampling device based on electrodeposition and electric heating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149197A (en) * | 2013-03-06 | 2013-06-12 | 河海大学 | Atomic vapor sampling method and device based on electro-deposition and electro-heat |
| CN107328886A (en) * | 2016-04-28 | 2017-11-07 | 中国石油化工股份有限公司 | The sampling device of on-line chromatographic analysis system and the method that sample is handled using it |
-
2013
- 2013-03-06 CN CN 201320102578 patent/CN203216852U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149197A (en) * | 2013-03-06 | 2013-06-12 | 河海大学 | Atomic vapor sampling method and device based on electro-deposition and electro-heat |
| CN107328886A (en) * | 2016-04-28 | 2017-11-07 | 中国石油化工股份有限公司 | The sampling device of on-line chromatographic analysis system and the method that sample is handled using it |
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| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130925 Termination date: 20150306 |
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| EXPY | Termination of patent right or utility model |