CN101482497B - On-line electrochemical separation and enrichment tungsten wire electrothermal atomic absorption detection device - Google Patents
On-line electrochemical separation and enrichment tungsten wire electrothermal atomic absorption detection device Download PDFInfo
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- CN101482497B CN101482497B CN2009100777936A CN200910077793A CN101482497B CN 101482497 B CN101482497 B CN 101482497B CN 2009100777936 A CN2009100777936 A CN 2009100777936A CN 200910077793 A CN200910077793 A CN 200910077793A CN 101482497 B CN101482497 B CN 101482497B
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000000926 separation method Methods 0.000 title claims abstract description 33
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 13
- 238000001514 detection method Methods 0.000 title claims abstract description 10
- 238000004070 electrodeposition Methods 0.000 claims abstract description 38
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000004401 flow injection analysis Methods 0.000 claims abstract description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 51
- 239000010937 tungsten Substances 0.000 claims description 51
- 238000011049 filling Methods 0.000 claims description 10
- 230000001174 ascending effect Effects 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 238000005485 electric heating Methods 0.000 claims description 6
- 230000003028 elevating effect Effects 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000000889 atomisation Methods 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract 3
- 238000002347 injection Methods 0.000 abstract 2
- 239000007924 injection Substances 0.000 abstract 2
- 239000000523 sample Substances 0.000 description 15
- 239000007789 gas Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000002572 peristaltic effect Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000004380 ashing Methods 0.000 description 2
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
本发明公开了一种在线电化学分离富集钨丝电热原子吸收检测装置，包括：电沉积分离富集单元，钨丝原子化器、空心阴极灯，微型CCD光谱仪，钨丝加热电源，电沉积电源，流动注射系统，步进电机，计算机。所述电沉积单元垂直放置在原子化器腔体内，位于钨丝正下方，其上端有内外两层凹槽，内层凹槽贴有两片铂电极，中心有样品注入孔，两侧有铂电极导线引出孔；外层凹槽有排液孔。棒的下端和连接套相连，连接套上的样品注入管、排液管分别和流动注射系统的进液管、排液管相连，铂电极导线和电沉积电源正极相连；钨丝和原子化加热电源相连，再与电沉积电源的负极相连；连接套由步进电机带动，作上下运动。本装置抗干扰能力强，自动化程度高。
The invention discloses an on-line electrochemical separation and enrichment tungsten wire electrothermal atomic absorption detection device, comprising: an electrodeposition separation and enrichment unit, a tungsten wire atomizer, a hollow cathode lamp, a miniature CCD spectrometer, a tungsten wire heating power supply, and an electrodeposition Power supply, flow injection system, stepper motor, computer. The electrodeposition unit is vertically placed in the atomizer cavity, directly below the tungsten wire, with inner and outer grooves on its upper end, two platinum electrodes attached to the inner groove, a sample injection hole in the center, and platinum electrodes on both sides. Electrode wire lead-out hole; the outer groove has a drain hole. The lower end of the rod is connected to the connection sleeve, the sample injection tube and the liquid discharge pipe on the connection sleeve are respectively connected to the liquid inlet pipe and the liquid discharge pipe of the flow injection system, the platinum electrode wire is connected to the positive electrode of the electrodeposition power supply; the tungsten wire and the atomization heating The power supply is connected, and then connected with the negative electrode of the electrodeposition power supply; the connecting sleeve is driven by a stepping motor to move up and down. The device has strong anti-interference ability and high degree of automation.
Description
Technical field
The present invention relates to detection technique, relate in particular to a kind of online electro-chemistrical separation and concentration tungsten filament electric heating atomic absorption light spectrum detection device.
Background technology
(tungsten coil electrothermal atomic absorptionspectrometer TC-AAS) is a kind of Electrothermal Atomic Absorption spectral analysis technique that grows up the seventies in 20th century to tungsten filament Electrothermal Atomic Absorption spectrometer.
The process that present most of tungsten filament Electrothermal Atomic Absorption spectrum detection device is measured element is as follows: the solution of testing sample is passed through microsyringe, manually be injected into the tungsten filament surface; Program heats tungsten filament then, finishes evaporate to dryness, ashing, atomization, the purification analytic process of fluid sample successively; The whole analytical process is in argon hydrogen combination gas (common ratio: 10% hydrogen) carry out in the protection at the tungsten filament atomizer.
Although the research of bibliographical information is used for the analytical test of all kinds of samples with tungsten filament Electrothermal Atomic Absorption spectrum at present, and obtained satisfied result of study.But the tungsten filament Electrothermal Atomic is received spectrometer in actual sample is analyzed at present, still exists a lot of deficiencies, and wherein topmost problem is: anti-matrix interference performance is relatively poor.This has seriously restricted its practical application, so the spectral analysis of present most of tungsten filament Electrothermal Atomic Absorption still rests on laboratory study.
Summary of the invention
For solving above-mentioned middle problem and the defective that exists, the invention provides a kind of online electro-chemistrical separation and concentration tungsten filament electric heating atomic absorption light spectrum detection device.
The present invention is achieved by the following technical solutions:
A kind of online electro-chemistrical separation and concentration tungsten filament electric heating atomic absorption light spectrum detection device involved in the present invention comprises:
Electro-deposition separation and concentration unit (1), tungsten filament atomizer cavity (2), hollow cathode lamp (3), miniature CCD spectrometer (4) tungsten filament atomizer heating power supply (5), electro-deposition power supply (6), the flow injection system, stepper motor lifting unit (8) and computing machine (9), it is characterized in that, described electro-deposition separation and concentration unit (1) is a cylindrical bar-shaped structure, and vertically be placed in the tungsten filament atomizer cavity (2), and be positioned at tungsten filament atomizer cavity (2) tungsten filament (19) under, the upper end of its electro-deposition separation and concentration unit (1) offers inside and outside two-layer groove with one heart, and the lower end of electro-deposition separation and concentration unit (1) links to each other with an adapter sleeve (16);
The two ends of described tungsten filament atomizer cavity (2) seal with quartz window (21), and two ends link to each other with miniature CCD spectrometer (4) with hollow cathode lamp (3) by a condenser lens (22) respectively;
The output terminal of described tungsten filament atomizer heating power supply (5) links to each other with the two poles of the earth of tungsten filament (19), and the utmost point in tungsten filament (19) the two poles of the earth also links to each other with the negative pole of electro-deposition power supply (6);
The output head anode of described electro-deposition power supply (6) links to each other with platinum electrode wire.
The inwall symmetry of wherein said internal layer groove (10) is posted two platinum electrodes (12), and offers sample filling orifice (13) at center, electro-deposition separation and concentration unit (1), respectively offers platinum electrode wire fairlead (14) in the both sides of filling orifice (13); Described outer groove (11) symmetry has two outages (15).
The adapter sleeve (16) that lower end, described electro-deposition separation and concentration unit (1) connects also is connected in ascending pipe (17), discharging tube (18) and platinum electrode wire fairlead (14), described ascending pipe (17) and described sample filling orifice (13) are connected, described discharging tube (18) and described outage (15) are connected, the lower end of described adapter sleeve (16) also connects an elevating lever, and this elevating lever moves up and down by the drive of stepper motor (8).
The beneficial effect of technical scheme provided by the invention is: utilize the heating material of tungsten filament as electrothermic atomizer, make attached to the sample on tungsten filament surface atomization at high temperature, carry out atomic absorption spectroscopy.Because tungsten filament electrothermal efficiency height, heating rate is fast, chemical inertness good, and do not need special cooling device.So compare with traditional Atomic Absorption Spectrometer, such apparatus structure is simple, volume is little.Because adopt online galvanochemistry separation and concentration technology, antijamming capability is strong, the automaticity height.
Description of drawings
Fig. 1 is an one-piece construction synoptic diagram of the present invention;
Fig. 2 is the A-A diagrammatic cross-section of atomizer among Fig. 1;
Fig. 3 is an electro-deposition separation and concentration unit sectional elevation synoptic diagram among Fig. 1;
Fig. 4, Fig. 5 are the cross sectional representation of electro-deposition separation and concentration unit.
Embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, embodiment of the present invention is described further in detail below in conjunction with accompanying drawing:
Present embodiment provides a kind of online electro-chemistrical separation and concentration tungsten filament electric heating atomic absorption light spectrum detection device.
Referring to Fig. 1, this device comprises: electro-deposition separation and concentration unit 1, tungsten filament atomizer cavity 2, hollow cathode lamp 3, miniature CCD spectrometer 4 tungsten filament atomizer heating power supplies 5, electro-deposition power supply 6, the flow injection system, stepper motor lifting unit 8 and computing machine 9, described electro-deposition separation and concentration unit 1 is a cylindrical bar-shaped structure, and vertically be placed in the tungsten filament atomizer cavity 2, and be positioned at tungsten filament atomizer cavity 2 tungsten filaments 19 under, the upper end of its electro-deposition separation and concentration unit 1 offers inside and outside two-layer groove with one heart, inwall at internal layer groove 10, symmetry is posted two platinum electrodes 12, and the heart has sample filling orifice 13 therein, respectively opens platinum electrode wire fairlead 14 in its both sides; 11 symmetries have two outages 15 (referring to Fig. 3) in the outer groove.Described electro-deposition separation and concentration unit adopts the polytetrafluoroethylmaterial material of acid and alkali-resistance to make formation one teflon rod, and the lower end of teflon rod links to each other with an adapter sleeve 16; Adapter sleeve is connected with ascending pipe 17, discharging tube 18 and platinum electrode wire fairlead 14; Wherein, described ascending pipe 17 and sample filling orifice 13 are connected; Described discharging tube 18 and outage 15 are connected; Described adapter sleeve lower end is connected with an elevating lever, and the drive of elevating lever by stepper motor 8 moves up and down.The output head anode of described electro-deposition power supply 6 links to each other with platinum electrode wire.
The output terminal of described tungsten filament 19 the two poles of the earth and tungsten filament atomization heating power supply 5 links to each other, wherein the arbitrary utmost point in tungsten filament 19 the two poles of the earth also link to each other with the negative pole of electro-deposition power supply 6 (referring to Fig. 2).Described flow injection system comprises that six transfer valves 7 and peristaltic pump 20 constitute, it is A inlet position, B inlet position, C inlet position, D inlet position, E inlet position and F inlet position that its six transfer valves include a plurality of inlets position, and wherein E inlet position is connected a sample hose 23 and a purge pipe 24 respectively with F inlet position.The top of described tungsten filament atomizer cavity 2 is provided with vent port 26, and the both sides of the below of tungsten filament atomizer cavity 2 are provided with air admission hole 25, and protection gas is introduced by this air admission hole 25, and is discharged by described vent port 26.
Fig. 4, Fig. 5 is the cross-sectional structure of electro-deposition separation and concentration unit, the structure of this electro-deposition separation and concentration unit is a cylindrical bar-shaped structure, because adopting the teflon of acid and alkali-resistance is material, so form a poly-tetrafluoro rod, there is a sample filling orifice 13 centre that should gather the tetrafluoro rod, two of sample filling orifice 13 is surveyed and is respectively arranged with platinum electrode wire fairlead 14, the outer end of platinum electrode wire fairlead 14 is respectively equipped with an internal layer groove and an outer groove, post two platinum electrodes 12 in the inwall symmetry of internal layer groove, symmetry has two outages 15 in outer groove.
Present embodiment its step when measuring is as follows:
Do in the preparation: open protection gas cylinder valve, tensimeter is transferred to the formulation dividing potential drop.Open analytical instrument and computer power supply, operation instrument specific program is provided with the hollow cathode lamp current, and the protection gas that feeds certain flow rate enters atomizer.
Sample galvanochemistry separation and concentration: the stepping electrode unit rises, and poly-tetrafluoro rod upper end groove is contacted with tungsten filament.Start the peristaltic pump of flow injection system, six transfer valves place inlet F, suck sample solution by sample hose, with the rinse pipe system; After rinse finishes, start the electro-deposition power supply, carry out the electro-deposition separation and concentration of setting-up time; After electro-deposition is finished, keeping electro-deposition power supply potential state, six transfer valves place inlet E, suck distilled water by purge pipe,, stop peristaltic pump then to clean the substrate medium on tungsten filament surface, the stepper motor unit descends, and poly-tetrafluoro rod upper end groove is separated with tungsten filament.
The sample Electrothermal Atomic Absorption is measured: after finishing step sample galvanochemistry separation and concentration, start tungsten filament atomizer heating power supply tungsten filament is carried out the program heating, finish drying, ashing, cooling, atomization and five typical steps of cleaning successively, when opening heating power supply, start the miniature CCD spectrometer, gather spectral signal in real time, handle test result automatically by corresponding software at last.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (1)
1. online electro-chemistrical separation and concentration tungsten filament electric heating atom absorption detection apparatus, comprise: electro-deposition separation and concentration unit (1), tungsten filament atomizer cavity (2), hollow cathode lamp (3), miniature CCD spectrometer (4), tungsten filament atomizer heating power supply (5), electro-deposition power supply (6), the flow injection system, stepper motor lifting unit (8) and computing machine (9), it is characterized in that, described electro-deposition separation and concentration unit (1) is a cylindrical bar-shaped structure, and vertically be placed in the tungsten filament atomizer cavity (2), and be positioned at tungsten filament atomizer cavity (2) tungsten filament (19) under, the upper end of its electro-deposition separation and concentration unit (1) offers inside and outside two-layer groove with one heart, and the lower end of electro-deposition separation and concentration unit (1) links to each other with an adapter sleeve (16);
The two ends of described tungsten filament atomizer cavity (2) seal with quartz window (21), and two ends link to each other with miniature CCD spectrometer (4) with hollow cathode lamp (3) by a condenser lens (22) respectively;
The output terminal of described tungsten filament atomizer heating power supply (5) links to each other with the two poles of the earth of tungsten filament (19), and the utmost point in tungsten filament (19) the two poles of the earth also links to each other with the negative pole of electro-deposition power supply (6);
The inwall symmetry of described internal layer groove (10) is posted two platinum electrodes (12), and offers sample filling orifice (13) at center, electro-deposition separation and concentration unit (1), respectively offers platinum electrode wire fairlead (14) in the both sides of filling orifice (13); Described outer groove (11) symmetry has two outages (15);
The output head anode of described electro-deposition power supply (6) links to each other with platinum electrode wire;
The adapter sleeve (16) that lower end, described electro-deposition separation and concentration unit (1) connects also is connected in ascending pipe (17), discharging tube (18) and platinum electrode wire fairlead (14), described ascending pipe (17) and described sample filling orifice (13) are connected, described discharging tube (18) and described outage (15) are connected, the lower end of described adapter sleeve (16) also connects an elevating lever, and this elevating lever moves up and down by the drive of stepper motor (8).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100777936A CN101482497B (en) | 2009-02-19 | 2009-02-19 | On-line electrochemical separation and enrichment tungsten wire electrothermal atomic absorption detection device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100777936A CN101482497B (en) | 2009-02-19 | 2009-02-19 | On-line electrochemical separation and enrichment tungsten wire electrothermal atomic absorption detection device |
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| Publication Number | Publication Date |
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| CN101482497A CN101482497A (en) | 2009-07-15 |
| CN101482497B true CN101482497B (en) | 2010-10-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102519781A (en) * | 2011-11-21 | 2012-06-27 | 南京金塔高速分析仪器有限公司 | Automatic sample dissolving device |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5343033B2 (en) * | 2010-04-12 | 2013-11-13 | 株式会社日立ハイテクノロジーズ | Elemental analysis apparatus and method |
| 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 |
| CN103207172B (en) * | 2013-03-06 | 2016-06-01 | 河海大学 | A kind of miniature atomic/ionization detection device and method thereof |
| CN106353262B (en) * | 2015-07-15 | 2019-04-12 | 北京普析通用仪器有限责任公司 | Atomic absorption measurement method and measuring device |
| CN111257257A (en) * | 2020-03-27 | 2020-06-09 | 四川大学 | Analysis device and method for simultaneous measurement of tungsten filament electrothermal atomic absorption/emission spectroscopy |
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2009
- 2009-02-19 CN CN2009100777936A patent/CN101482497B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102519781A (en) * | 2011-11-21 | 2012-06-27 | 南京金塔高速分析仪器有限公司 | Automatic sample dissolving device |
| CN102519781B (en) * | 2011-11-21 | 2014-07-30 | 南京金塔高速分析仪器有限公司 | Automatic sample dissolving device |
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