CN1320353C - On-line combination interface device for capillary electrophoresis and graphite furnace atomic absorption spectrometry - Google Patents
On-line combination interface device for capillary electrophoresis and graphite furnace atomic absorption spectrometry Download PDFInfo
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- CN1320353C CN1320353C CNB2004100727084A CN200410072708A CN1320353C CN 1320353 C CN1320353 C CN 1320353C CN B2004100727084 A CNB2004100727084 A CN B2004100727084A CN 200410072708 A CN200410072708 A CN 200410072708A CN 1320353 C CN1320353 C CN 1320353C
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Abstract
The present invention relates to an on-line combination interface device for the atomic absorption of capillary electrophoresis and graphite furnaces, which comprises an electrophoresis separating capillary pipe, a gas carrying pipe, a thermal spraying pipe and a graphite pipe, wherein one end of the capillary pipe is inserted into the thermal spraying pipe which penetrates through the gas carrying pipe, the periphery of the gas carrying pipe is simultaneously sheathed with a cooling sleeve, wherein the thermal spraying pipe, the gas carrying pipe and the cooling sleeve are metallic conductors and are connected with a cathode of a capillary electrophoresis apparatus. The present invention is mainly characterized in that a stable electric loop required by capillary electrophoresis separation is provided, the capillary electrophoresis separating species is led in the constant-temperature heating graphite pipe to be detected on line in the mode of continuous thermal spray under the condition of no external heating sources, a convenient and practical interface device which simultaneously meets the analysis requirement of two instruments is created, and the continuous on-line combination detection is realized. The interface device has the characteristics of simple structure, no need of external heating sources, no need of derivation reagents, low cost, friendly environment, etc. on the basis of reserving the advantages of the two analysis instruments.
Description
[technical field]: the present invention relates to a kind of interface arrangement of analytical chemistry instrument coupling, particularly the interface arrangement of Capillary Electrophoresis and GFAAS (graphite furnace atomic absorption spectrometry) on-line coupling.
[background technology]: the toxicity of element, bioavailability and animal migration depend on its existence form, and therefore the morphological analysis as the specific species of detection elements comes into one's own more.The morphological analysis process generally comprises chromatographic resolution and atom light (matter) spectrum detects.Because the complicacy of matrix and the trace of form of poluttants in environment and the biological sample, thereby the coupling of high efficient separation technology and high-sensitive element selectivity detection technique is the important channel that solves trace element morphological analysis in environment and the biological sample.The key of development coupling technique is an interfacing.
The coupling of various chromatographic techniques and atom light/mass spectrum detection is the most frequently used means of present trace toxic metals organic compound morphological analysis.The Capillary Electrophoresis that development in recent years is got up (CE) technology since have the resolution height, fast, reagent consumption is few and to advantages such as balance disturbance between the different plant species are less, be a kind of very attractive form isolation technics.CE and the coupling of element selective detector, not only selectivity is good and highly sensitive, and only needs the different shape of element-specific is separately got final product.At present, the research in this field almost all concentrates on the coupling technique of inductively coupled plasma atomic emission spectrum (ICP-AES) and inductivity coupled plasma mass spectrometry (ICP-MS) and CE.But these instruments cost an arm and a leg, operation cost high and the analyst is required height, thereby have limited popularizing and practical application of they.
GFAAS (graphite furnace atomic absorption spectrometry) (ETAAS) is one of at present the most frequently used trace element detection technique; have the following advantages; (1) sample size is few; (2) handle the big fluid sample of difficult atomizing viscosity in the flame easily; (3) directly measure the element (is protection gas and cleaning gas with oxygen-free inert gas) that resonance line is positioned at vacuum ultraviolet, (4) absolute sensitivity height, (5) control the chemical environment and the thermal environment of atomic vapour easily; (6) background is low, (7) handling safety.Independently ETAAS can only measure the total amount of element, so ETAAS just can be applied to morphological analysis when having only with other isolation technics couplings.Yet graphite-pipe is major obstacle place with ETAAS and chromatographic separation technology on-line coupling to " non-negotiable " of restricted (less than 50 microlitres) of sample capacity and graphite furnace.
Capillary Electrophoresis and ETAAS coupling can be become the morphological analysis strong tool.But the key that realizes this coupling technique is the appropriate design of interface.Key technical problem comprises in the Interface design of Capillary Electrophoresis-GFAAS (graphite furnace atomic absorption spectrometry) coupling, should realize the electric loop that capillary electrophoresis separation is stable; Need not to realize the high-level efficiency atomizing under the situation of external heat source; Conductive liquid imports graphite-pipe with sample effectively, and flow velocity is as far as possible little, to adapt to the restriction of graphite-pipe to sample capacity; Install micro cooler additional, prevent that thermal spray pipe head end from replenishing the air-resistance phenomenon that the liquid vaporization produces because of the overheated negative electrode that causes; To atomizer particularly graphite-pipe improve, to adapt to the demand of Continuous Heat spraying sample introduction.
[summary of the invention]: purpose of the present invention is exactly the above-mentioned key issue that solves effectively in Capillary Electrophoresis and the GFAAS (graphite furnace atomic absorption spectrometry) coupling technique, development Capillary Electrophoresis and GFAAS (graphite furnace atomic absorption spectrometry) coupling new technology are set up the new technical platform of easy quick, economic and reliable for Elemental Speciation Analysis.
Capillary Electrophoresis of the present invention and sampling Graphite Furnace Atomic Absorption on-line coupling interface arrangement, mainly comprise the electrophoretic separation kapillary, the carrier gas pipe, thermal spray pipe and graphite-pipe, the electrophoretic separation other end capillaceous of being drawn by sample cell inserts in the thermal spray pipe that has the decorating liquid inlet on it, whole thermal spray pipe has from it in the carrier gas pipe of carrier gas inlet and passes, the thermal spray mouth of thermal spray pipe front end is in the hollow plumbago cap that the hollow plumbago awl inserts with the graphite-pipe sample holes closely contacts, be set with a cooling jacket which is provided with cooling water inlet and coolant outlet simultaneously in carrier gas pipe periphery, thermal spray pipe wherein, carrier gas pipe and cooling jacket are metallic conductor and are connected with the negative electrode of capillary electrophoresis apparatus.The thermal spray mouth of thermal spray pipe head end vertically inserts in the graphite cap.The former sample holes internal diameter of graphite-pipe is screwed into a hollow plumbago cap after drawing together Kong Kaida.At the two ends of graphite-pipe, open two small de-air hole respectively with the equidistant place of sample holes.
Advantage of the present invention and effect: 1, the present invention is novel, design is created, structure is simple and direct; Need not external heat source, need not derivative reagent, no dead volume, direct injected, atomizing fully, online in real time detect.2, core technology of the present invention has provided the needed stable electrical of capillary electrophoresis separation loop, and under the condition of no external heat source, the capillary electrophoresis separation species with online detection in the graphite-pipe of Continuous Heat Sprayable importing heated at constant temperature, have been created easy, the practical interface arrangement that a kind of analysis of satisfying two kinds of instruments simultaneously requires.3, the stainless steel hot injection spray pipe is connected with the negative electrode of capillary electrophoresis apparatus, an electrophoretic separation end capillaceous inserts in the sample cell, the terminal insertion in the thermal spray pipe, the thermal spray pipe is with the carrier gas pipe outward, the carrier gas pipe is outward a recirculated water cooling cover, be fixed with one section hollow plumbago awl under the cooling jacket, fix a hollow plumbago cap on the sample holes of graphite-pipe, the thermal spray mouth of thermal spray pipe head end is vertical to be inserted in the graphite cap that is fixed on the graphite-pipe sample holes.4, the thermal spray mouth of stainless steel hot injection spray pipe head end probes in the graphite cap that is fixed on the sample holes.Decorating liquid in the stainless steel hot fog nozzle is carrying the isolated species of Capillary Electrophoresis negative electrode and is at high temperature vaporizing, and imports absorption cell continuously, steadily, evenly in the mode of thermal spray, is detected in real time continuously in graphite-pipe through the atomizing steam of high temperature.5, the former sample holes of graphite-pipe both sides are left two small de-air hole equidistantly, and the steam of continuous importing graphite-pipe is evenly discharged from vent port.6, regulate by gas meter,, enter negative electrode conduction liquid pool, promote the gap that the negative electrode conductive liquid flows through thermal spray pipe and separation capillary with the micro updating constant flow rate from the argon gas that graphite furnace power supply carrier gas air intake opening branches out.7, regulate by other one road gas meter, the argon gas of flow through carrier gas pipe and spraying tube lane enters graphite-pipe from the gap between thermal spray mouth and graphite cap, is beneficial to atomization steam evenly diffusion in graphite-pipe.8, stainless steel carrier gas pipe is equipped with cooling jacket outward, recirculated cooling water comes from the graphite furnace main cooling water circulation system, cooling jacket is by slideway lift adjustment height, can reduce thermal spray jet pipe head end temperature, prevent that thermal spray pipe head end from replenishing the air-resistance phenomenon that the liquid vaporization produces because of the overheated negative electrode that causes, and promote that the terminal effluent of Capillary Electrophoresis is carried outside and thermal spray reposefully.9, in view of the unique design of this interface, the species that capillary electrophoresis separation goes out directly import by the thermal spray mode in the graphite-pipe of continuous constant temperature heating, and the hold-up time prolongs on light path, and detection sensitivity is effectively improved.In a word, the present invention has realized that the uninterrupted on-line coupling of Capillary Electrophoresis and graphite furnace atomic absorption spectrophotometer detects, on the basis that has kept two kinds of analytical instrument advantages, have more simple in structurely, need not external heat source, need not derivative reagent, expense is cheap, characteristics such as environmental friendliness.
[description of drawings]:
Fig. 1, Capillary Electrophoresis and GFAAS (graphite furnace atomic absorption spectrometry) on-line coupling interface arrangement simplified schematic diagram;
Fig. 2, Capillary Electrophoresis of the present invention and GFAAS (graphite furnace atomic absorption spectrometry) on-line coupling interface section simplified schematic diagram.
[embodiment]:
As shown in Figure 1, 2, on-line coupling interface arrangement A of the present invention mainly comprises graphite-pipe 1, graphite-pipe exhausr port 3, hollow plumbago cap 4, hollow plumbago awl 5, stainless steel cooling jacket 6, cooling water inlet 7, coolant outlet 8, stainless steel carrier gas pipe 9, carrier gas inlet 10, stainless steel hot injection spray pipe 11, decorating liquid inlet 12, electrophoretic separation kapillary 13 and the sample cell 14 that has sample holes 2 on it.
One end of electrophoretic separation kapillary 13 inserts in the sample cell 14, the other end inserts in the thermal spray pipe 11, the thermal spray pipe is with carrier gas pipe 9 outward, the carrier gas pipe is outward a recirculated water cooling cover 6, be fixed with one section hollow plumbago awl 5 under the cooling jacket, fix a hollow plumbago cap 4 on the sample holes of graphite-pipe, the thermal spray mouth of thermal spray pipe 11 head ends vertically inserts in the graphite cap 4.The modified liquid inlet 12 of decorating liquid is pressed into stainless steel hot injection spray pipe 11, and argon gas enters carrier gas pipe 9 by carrier gas inlet 10.7 enter cooling jacket 6 from the chilled water of major cycle water system joint from the cooling water inlet, flow back to main cooling system from coolant outlet 8.Thermal spray pipe, carrier gas pipe and cooling jacket are metallic conductor (this example is selected stainless steel for use) and are connected with the negative electrode of capillary electrophoresis apparatus, formed the stable electrical loop of electrophoretic separation.
The electric conductivity decorating liquid imports in the stainless steel hot injection spray pipe from the gap between electrophoretic separation kapillary outer wall and the stainless steel hot injection spray pipe inwall by gas pressure.Insert the decorating liquid in the stainless steel fog nozzle in the hollow plumbago cap 4, carrying the isolated species to be measured of Capillary Electrophoresis negative electrode, vaporization at high temperature, mode with thermal spray imports graphite-pipe continuously, steadily, evenly, realized direct, complete sample introduction, detected in the graphite-pipe of lasting heated at constant temperature through the atomizing steam of high temperature, the absorption signal of acquisition analyte.So promptly can obtain the content of certain element different plant species simultaneously.This interface has reached the requirement of capillary electrophoresis separation and the detection of GFAAS (graphite furnace atomic absorption spectrometry) B (see figure 1) simultaneously.
Claims (3)
1, a kind of Capillary Electrophoresis and GFAAS (graphite furnace atomic absorption spectrometry) on-line coupling interface arrangement, comprise the electrophoretic separation kapillary, the carrier gas pipe, thermal spray pipe and graphite-pipe, it is characterized in that the electrophoretic separation of being drawn by the sample cell other end capillaceous inserts in the thermal spray pipe that has the decorating liquid inlet on it, whole thermal spray pipe has from it in the carrier gas pipe of carrier gas inlet and passes, the thermal spray mouth of thermal spray pipe front end is in the hollow plumbago cap that the hollow plumbago awl vertically inserts with the graphite-pipe sample holes closely contacts, be set with a cooling jacket which is provided with cooling water inlet and coolant outlet simultaneously in carrier gas pipe periphery, thermal spray pipe wherein, carrier gas pipe and cooling jacket are metallic conductor and are connected with the negative electrode of capillary electrophoresis apparatus.
2, Capillary Electrophoresis according to claim 1 and GFAAS (graphite furnace atomic absorption spectrometry) on-line coupling interface arrangement is characterized in that thermal spray pipe, carrier gas pipe and cooling jacket are stainless steel and make.
3, Capillary Electrophoresis according to claim 1 and 2 and GFAAS (graphite furnace atomic absorption spectrometry) on-line coupling interface arrangement, it is characterized in that being screwed into a hollow plumbago cap after the former sample holes internal diameter of graphite-pipe is drawn together the hole, and, have two vent ports respectively with the equidistant place of sample holes at the two ends of graphite-pipe.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100727084A CN1320353C (en) | 2004-11-12 | 2004-11-12 | On-line combination interface device for capillary electrophoresis and graphite furnace atomic absorption spectrometry |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100727084A CN1320353C (en) | 2004-11-12 | 2004-11-12 | On-line combination interface device for capillary electrophoresis and graphite furnace atomic absorption spectrometry |
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| Publication Number | Publication Date |
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| CN1605858A CN1605858A (en) | 2005-04-13 |
| CN1320353C true CN1320353C (en) | 2007-06-06 |
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| CNB2004100727084A Expired - Fee Related CN1320353C (en) | 2004-11-12 | 2004-11-12 | On-line combination interface device for capillary electrophoresis and graphite furnace atomic absorption spectrometry |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101793864A (en) * | 2010-03-26 | 2010-08-04 | 南开大学 | Micro-fluidic chip-based capillary electrophoresis and graphite furnace atomic absorption online coupling interface device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5856671A (en) * | 1995-05-19 | 1999-01-05 | Cornell Research Foundation, Inc. | Capillary electrophoresis-mass spectrometry interface |
| US6511850B1 (en) * | 1999-07-13 | 2003-01-28 | The Texas A&M University System | Pneumatic nebulizing interface to convert an analyte-containing fluid stream into an aerosol, method for using same and instruments including same |
| CA2483493A1 (en) * | 2001-11-08 | 2003-05-22 | Medinnova Sf | Capillary electrophoresis mass spectometry interface |
| CN2599579Y (en) * | 2003-01-21 | 2004-01-14 | 南开大学 | Capillary tube electrophoresis hydride generating atomic fluorescence spectrum on line joint use interface |
-
2004
- 2004-11-12 CN CNB2004100727084A patent/CN1320353C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5856671A (en) * | 1995-05-19 | 1999-01-05 | Cornell Research Foundation, Inc. | Capillary electrophoresis-mass spectrometry interface |
| US6511850B1 (en) * | 1999-07-13 | 2003-01-28 | The Texas A&M University System | Pneumatic nebulizing interface to convert an analyte-containing fluid stream into an aerosol, method for using same and instruments including same |
| CA2483493A1 (en) * | 2001-11-08 | 2003-05-22 | Medinnova Sf | Capillary electrophoresis mass spectometry interface |
| CN2599579Y (en) * | 2003-01-21 | 2004-01-14 | 南开大学 | Capillary tube electrophoresis hydride generating atomic fluorescence spectrum on line joint use interface |
Non-Patent Citations (3)
| Title |
|---|
| 毛细管电泳和电感耦合等离子体质谱接口技术进展 叶美英 等，光谱学与光谱分析，第23卷第1期 2003 * |
| 毛细管电泳-电感耦合等离子质谱联用的接口技术 康建珍 等，分析化学，第32卷第2期 2004 * |
| 毛细管电泳-电感耦合等离子质谱联用的接口技术 康建珍 等，分析化学，第32卷第2期 2004;毛细管电泳和电感耦合等离子体质谱接口技术进展 叶美英 等，光谱学与光谱分析，第23卷第1期 2003 * |
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Granted publication date: 20070606 Termination date: 20131112 |