CN1424579A - Online interface for capillary calaphorestic hydride generated atomic spectrofluorimetry - Google Patents
Online interface for capillary calaphorestic hydride generated atomic spectrofluorimetry Download PDFInfo
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- CN1424579A CN1424579A CN 03100702 CN03100702A CN1424579A CN 1424579 A CN1424579 A CN 1424579A CN 03100702 CN03100702 CN 03100702 CN 03100702 A CN03100702 A CN 03100702A CN 1424579 A CN1424579 A CN 1424579A
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Abstract
The co-using interface of the method of atom fluorescence spectrum and generation of the hybride in capillary electrophoresis relates to an apparatus thereof. This interface provides the key solutios that the capillary electrophoresis needs stable electric circuit, and that the method of atom fluorescence spectrum needs to convert analysed agent into hydride. The interface includes cross passage 1, T passage with small inner diameter 5, T passage with large inner diameter 7 and gas-liquid separator 6, cross passage 1 connected in turn to T passage with small inner diameter 5, T passage with large inner diameter 7 and gas-liquid separator 6. The interface has ingenious and novel design, having such features as small dead volume, short connecting piping and simple and practical operation.
Description
Technical field
The present invention relates to the interface arrangement of analytical chemistry instrument coupling, particularly the interface arrangement of Capillary Electrophoresis and atomic fluorescence spectrometry on-line coupling.
Technical background
Its existence form is depended in a kind of environmental organism behavior strictness of element, so more and more draw attention as the morphological analysis of measuring the specific species of element.The morphological analysis process generally comprises chromatographic resolution and atom light (matter) spectrum detects.Chromatographic separation technology commonly used comprises gas chromatography, liquid chromatography and Capillary Electrophoresis etc.Compare with liquid chromatography with gas chromatography, Capillary Electrophoresis has the advantage that resolution height, disengaging time are short, the sample reagent dosage is little.Detection means commonly used comprises atomic absorption spectrography (AAS), atomic emission spectrometry, atomic fluorescence spectrometry and inductivity coupled plasma mass spectrometry.Compare with atomic emission spectrometry with atomic absorption spectrography (AAS), atomic fluorescence spectrometry has highly sensitive, the advantage that antijamming capability is strong; Compare with inductivity coupled plasma mass spectrometry, to some element, when having similar sensitivity, atomic fluorescence spectrometry instrument price and operation cost are lower.But low, the poor anti jamming capability of sensitivity when the ultraviolet detection Capillary Electrophoresis is used for morphological analysis; And traditional atomic fluorescence spectrometry only can be measured the element total amount.Theoretically, Capillary Electrophoresis-atomic fluorescence spectrometry coupling can become the morphological analysis strong tool.But how to realize the electric loop that Capillary Electrophoresis is stable, atomic fluorescence spectrometry need be converted into hydride with analyte, has become the subject matter in Capillary Electrophoresis-atomic fluorescence spectrometry coupling technique.Therefore, Capillary Electrophoresis and atomic fluorescence spectrometry coupling are not arranged at present as yet.
Summary of the invention
At above-mentioned situation, the invention solves the stable electric loop of Capillary Electrophoresis in the coupling technique, atomic fluorescence spectrometry need be converted into analyte the problem of hydride, and Capillary Electrophoresis hydride generation atomic fluorescence spectrometry on-line coupling interface is provided.By the selection of connecting line, effectively overcome the influence that back-pressure produces capillary electrophoresis separation in the coupling technique.
Technical scheme of the present invention is that it comprises four-way 1, fine inner diameter threeway 5, large diameter threeway 7 and gas-liquid separator 6; Its connected mode is: four-way 1 is connected with fine inner diameter threeway 5, large diameter threeway 7, gas-liquid separator 6 successively.Wherein, four-way 1 is a right cylinder, high 5 millimeters, diameter d is 25 millimeters, in the middle, have by center and orthogonal two passes 12 along diametric(al), its diameter is 0.5 millimeter, center teflon bolt 13 with holes respectively is housed on passage 12 outer ends, and bolt 13 inner faces of two symmetries are apart from d
1It is 6 millimeters.Bolt 13 is distinguished the connecting pipe and the decorating liquid transfer tube 3 of fixed capillary 2, platinum electrode 8, fine inner diameter threeway 5 successively, the position of bolt 13 fixed capillary 2 wherein will make the endpiece A of kapillary 2 pass the central point O of passage 12 and is the 1-2.5 millimeter apart from the distance of four-way 1 central point O.Gas-liquid separator 6 body height H are 20 millimeters, and diameter of phi is 15 millimeters, in the middle and lower part of gas-liquid separator 6, are 15 millimeters places apart from gas-liquid separator main body neck length h promptly, a level is housed, has the upwards glass tube 14 of groove, and its internal diameter is 3 millimeters; Gas-liquid separator 6 lower body part outlet 9 is a L type conduit, and its diameter is 5 millimeters; Gas-liquid separator 6 main body tops export 10 diameters and also are 5 millimeters.Need to prove that the connecting line of interface is selected the different inner diameters threeway for use, i.e. fine inner diameter threeway 5 internal diameters are that 1 millimeter, large diameter threeway 7 internal diameters are 2.5 millimeters, and with connecting hoop 15 and connecting pipe each parts are coupled together.
The invention has the beneficial effects as follows: be skillfully constructed, modern design.This interface has the advantages that dead volume is little, connecting pipe is short out.Do as a wholely, the present invention had both realized the condition in the required stable electrical of capillary electrophoresis separation loop, reached atomic fluorescence spectrometry again and analyte need be converted into hydride to sample preparation, the requirement of these two key issues.The fine inner diameter threeway can effectively reduce the diffusion that kapillary flows out thing, the large diameter threeway eliminated that the hydride generating process produces a large amount of gas and the back-pressure that causes to the influence of capillary electrophoresis separation.Utilize this design, realized of the requirements of two kinds of instruments, for Capillary Electrophoresis and atomic fluorescence spectrometry coupling provide a simple and practical interface arrangement analyzing.Wherein, the fixed position of kapillary 2, the peak shape that can obtain; Four-way 1 is from physically having solved the timely transmission of kapillary outflow thing; Decorating liquid not only is convenient to the transmission that kapillary flows out thing, keeps electrophoresis electricity loop, but also as the medium that the subsequent hydrogenation thing takes place, the coupling of Capillary Electrophoresis and atomic fluorescence spectrometry is come true from theory.In addition, its inlet of gas-liquid separator generally is positioned at the top of main body, and gas transmits downwards, and the inlet of the gas-liquid separator 6 among the present invention is in the middle and lower part of main body, and its horizontal conduit level is installed, and groove upwards is convenient to the gas transmission.Another characteristics of gas-liquid separator 6 are that intrinsic volume is little, and these characteristics can reduce the diffusion that gas-liquid separator causes.In a word, the present invention had both kept the advantage that resolution height, disengaging time are short, the sample reagent dosage is little of Capillary Electrophoresis, had possessed again that atomic fluorescence spectrometry is highly sensitive, antijamming capability strong, advantages such as low instrument price and low operation cost; Shortcomings such as sensitivity is lower when simultaneously, having overcome traditional atomic fluorescence spectrophotometer and only be fit to measure the total amount of element and ultraviolet detection Capillary Electrophoresis and be used for morphological analysis, antijamming capability is relatively poor.Coupling technique provided by the invention can obtain the information abundanter than single instrument, from putting into practice the coupling that has realized Capillary Electrophoresis-atomic fluorescence spectrometry, for morphological analysis provides a kind of strong tool.Measure when can realize different arsenic compound, and only use atomic fluorescence spectrometry to analyze respectively.This interface is applicable to the morphological analysis of steam generation element (as arsenic, mercury, selenium etc.).
Description of drawings
Fig. 1 is a Capillary Electrophoresis hydride generation atomic fluorescence spectrometry on-line coupling interface synoptic diagram;
Fig. 2 is the four-way right cylinder proportional sizes among the present invention;
Fig. 3 is the gas-liquid separator proportional sizes among the present invention;
Embodiment (in conjunction with the accompanying drawings technical characterictic of the present invention being described in detail):
Embodiment 1:
As shown in Figure 1, 2, the present invention mainly comprises: four-way 1, fine inner diameter threeway 5, large diameter threeway 7 and gas-liquid separator 6 and connecting pipe; Its connected mode is: four-way 1 is connected with fine inner diameter threeway 5, large diameter threeway 7, gas-liquid separator 6 successively.Wherein, four-way 1 is a right cylinder, and is high 5 millimeters, and diameter d is 25 millimeters, in the middle, has by center and orthogonal two passes 12 along diametric(al), and its diameter is 0.5 millimeter.Center teflon bolt 13 with holes respectively is housed on passage 12 outer ends, and bolt 13 inner faces of two symmetries are apart from d
1It is 6 millimeters.Bolt 13 is distinguished the connecting pipe and the decorating liquid transfer tube 3 of fixed capillary 2, platinum electrode 8, fine inner diameter threeway 5 successively.Need to prove that exporting relative port with kapillary 2 in the four-way 1 is the outlet of four-way 1, is connected with fine inner diameter threeway 5.The arm of fine inner diameter threeway 5 is used to connect solution of potassium borohydride transfer tube 4.On four-way 1 two other relative port, the transfer tube 3 of platinum electrode 8 and decorating liquid is installed respectively.The position of bolt 13 fixed capillary 2 wherein will make the endpiece A of kapillary 2 pass the central point O of passage 12 and is the 1-2.5 millimeter apart from the distance of four-way 1 central point O.As shown in Figure 3, gas-liquid separator 6 body height H are 20 millimeters, and diameter phi is 15 millimeters, middle and lower part at distance gas-liquid separator 6, be 15 millimeters places promptly, a level be housed, have the upwards glass tube 14 of groove that its internal diameter is 3 millimeters apart from gas-liquid separator main body neck length h; Gas-liquid separator 6 lower body part outlet 9 is a L type conduit, and its diameter is 5 millimeters; Gas-liquid separator 6 main body tops export 10 diameters and also are 5 millimeters.Also need to prove, the connecting line of interface is selected the different inner diameters threeway for use, be that fine inner diameter threeway 5 internal diameters are that 1 millimeter, large diameter threeway 7 internal diameters are 2.5 millimeters, and each parts is coupled together with connecting hoop 15 and connecting pipe, be four-way 1 and fine inner diameter threeway 5, the inlet 14 of fine inner diameter threeway 5 and large diameter threeway 7 and large diameter threeway 7 and gas-liquid separator 6 all is connected hoop 15 by polyethylene elastomer and connects.Two pumps 16 be installed in respectively the decorating liquid transfer tube 3 that is connected with four-way 1 with solution of potassium borohydride transfer tube 4 that fine inner diameter threeway 5 is connected on, be used to pump into decorating liquid and solution of potassium borohydride.Large diameter threeway 7-arm is connected the argon gas steel cylinder provides argon gas to transfer tube 11, and argon gas is as the carrier gas of gas transmission.The outlet 10 of gas-liquid separator 6 is connected with the atomizer of atomic fluorescence spectrophotometer.The outlet 9 of gas-liquid separator 6 connects sewer pipe.During use, applying high voltage between the inlet end B of kapillary 2 and platinum electrode as shown in Figure 18, by the endpiece A of kapillary 2, decorating liquid transfer tube 3 and platinum electrode 8 form stablize the electric loop of electrophoresis.Analyte is after kapillary 2 electrophoretic separation, transmission in time under the carrying of decorating liquid (dilute hydrochloric acid solution), the acidity of the analyte of decorating liquid adjusting simultaneously is used for hydride and takes place, and analyte and the online reaction of potassium borohydride with appropriate acidity form corresponding hydride.Carry secretly down at argon gas, gas-liquid mixture enters gas-liquid separator 6, the atomizer that enters into atomic fluorescence spectrophotometer that gas part wherein is unobstructed, and the fluorescence signal of acquisition analyte, waste liquid is from sewer pipe 9 drainage gas-liquid separators 6.Can obtain the content of identity element different plant species like this.Utilize this interface to reach the requirement of capillary electrophoresis separation and atomic fluorescence spectrometry detection simultaneously.
Claims (4)
1. Capillary Electrophoresis hydride generation atomic fluorescence spectrometry on-line coupling interface, it is characterized in that: it comprises four-way (1), fine inner diameter threeway (5), large diameter threeway (7) and gas-liquid separator (6); Its connected mode is: four-way (1) is connected with fine inner diameter threeway (5), large diameter threeway (7) and gas-liquid separator (6) successively.
2. according to the described Capillary Electrophoresis hydride generation atomic fluorescence spectrometry of claim 1 on-line coupling interface, it is characterized in that: four-way (1) is a right cylinder, high 5 millimeters, diameter (d) is 25 millimeters, in the middle, have by center and orthogonal two passes (12) along diametric(al), its diameter is 0.5 millimeter, center teflon bolt (13) with holes respectively is housed on passage (12) outer end, and the bolt of two symmetries (13), its inner face distance (d1) is 6 millimeters, bolt (13) is distinguished fixed capillary (2) successively, platinum electrode (8), the connecting pipe of fine inner diameter threeway (5) and decorating liquid transfer tube (3), the position of bolt (13) fixed capillary (2) wherein will make the endpiece A of kapillary (2) pass the central point (O) of passage (12), and the distance apart from four-way (1) central point (O) is the 1-2.5 millimeter.
3. according to the described Capillary Electrophoresis hydride generation atomic fluorescence spectrometry of claim 1 on-line coupling interface, it is characterized in that: gas-liquid separator (6) body height (H) is 20 millimeters, diameter of phi is 15 millimeters, middle and lower part in gas-liquid separator (6), be 15 millimeters places promptly apart from gas-liquid separator main body neck length (h), one level is housed, has the upwards glass tube (14) of groove, its internal diameter is 3 millimeters; Gas-liquid separator (6) lower body part outlet (9) is (L) type conduit, and its diameter is 5 millimeters; Gas-liquid separator (6) main body top outlet (10) diameter also is 5 millimeters.
4. according to the described Capillary Electrophoresis hydride generation atomic fluorescence spectrometry of claim 1 on-line coupling interface, it is characterized in that: connecting line is selected the different inner diameters threeway for use, be that fine inner diameter threeway (5) internal diameter is that 1 millimeter, large diameter threeway (7) internal diameter are 2.5 millimeters, and each parts coupled together with connecting hoop (15) and connecting pipe.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031007023A CN1195223C (en) | 2003-01-21 | 2003-01-21 | Online interface for capillary calaphorestic hydride generated atomic spectrofluorimetry |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB031007023A CN1195223C (en) | 2003-01-21 | 2003-01-21 | Online interface for capillary calaphorestic hydride generated atomic spectrofluorimetry |
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| CN1424579A true CN1424579A (en) | 2003-06-18 |
| CN1195223C CN1195223C (en) | 2005-03-30 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101995439A (en) * | 2009-08-12 | 2011-03-30 | 中国科学院生态环境研究中心 | Efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms |
| CN104048918A (en) * | 2014-06-04 | 2014-09-17 | 徐静 | Total contact fluorescence detection pool for capillary electrophoresis |
| CN105301087A (en) * | 2014-05-30 | 2016-02-03 | 中国科学院生态环境研究中心 | Method for separating and detecting nano-silver |
| CN107894511A (en) * | 2017-10-27 | 2018-04-10 | 河北莱博瑞特电子科技有限公司 | A kind of Elemental Speciation Analysis instrument |
| CN109142253A (en) * | 2018-10-19 | 2019-01-04 | 中国科学院大连化学物理研究所 | Liquid phase reactor chemical kinetic systems and electrochemistry spectrum synchronous measuring apparatus and method |
-
2003
- 2003-01-21 CN CNB031007023A patent/CN1195223C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101995439A (en) * | 2009-08-12 | 2011-03-30 | 中国科学院生态环境研究中心 | Efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms |
| CN105301087A (en) * | 2014-05-30 | 2016-02-03 | 中国科学院生态环境研究中心 | Method for separating and detecting nano-silver |
| CN104048918A (en) * | 2014-06-04 | 2014-09-17 | 徐静 | Total contact fluorescence detection pool for capillary electrophoresis |
| CN107894511A (en) * | 2017-10-27 | 2018-04-10 | 河北莱博瑞特电子科技有限公司 | A kind of Elemental Speciation Analysis instrument |
| CN107894511B (en) * | 2017-10-27 | 2023-09-15 | 河北莱博瑞特电子科技有限公司 | Elemental morphology analyzer |
| CN109142253A (en) * | 2018-10-19 | 2019-01-04 | 中国科学院大连化学物理研究所 | Liquid phase reactor chemical kinetic systems and electrochemistry spectrum synchronous measuring apparatus and method |
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| Publication number | Publication date |
|---|---|
| CN1195223C (en) | 2005-03-30 |
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