CN1299793C - Cyclic condensation solid-phase extraction apparatus - Google Patents
Cyclic condensation solid-phase extraction apparatus Download PDFInfo
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- CN1299793C CN1299793C CNB2005100279557A CN200510027955A CN1299793C CN 1299793 C CN1299793 C CN 1299793C CN B2005100279557 A CNB2005100279557 A CN B2005100279557A CN 200510027955 A CN200510027955 A CN 200510027955A CN 1299793 C CN1299793 C CN 1299793C
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Abstract
The present invention relates to a cyclic condensation solid-phase microextraction device which not only comprises a sampler, a solid-phase microextraction bottle and a bunsen beaker, but also particularly comprises a cyclic condenser, wherein the cyclic condenser is a hollow circular cone with a cover; a cooling water inlet pipe, a sampler protective pipe and a cooling water outlet pipe are vertically arranged on the end plane of the condenser; one end of the sampler protective pipe is exposed out of the end plane of the condenser and is sealed, and the other end penetrates through the top end of the circular cone. Cooling water cools the external wall of the cyclic condenser; therefore, liquid to be measured which is heated and volatilized to gas phases is condensed on the external wall of the cyclic condenser, and liquid drips are formed and flow downwards along the external wall. The liquid drips are converged on solid-phase microextraction fibers on the outlet of the sampler protective pipe, and a stable condensation cyclic loop is formed. When the microextraction fibers sufficiently contact the volatilized condensed liquid of the liquid to be measured, and partition equilibrium is achieved, the microextraction fibers are taken out for chromatographic analyses. The extraction fibers of the present invention don't directly contact the liquid to be measured; consequently, the possibility of pollution is reduced, the adsorption capacity is improved, and the detection limit of objects to be measured is reduced.
Description
Technical field
The present invention relates to a kind of cyclic condensation solid-phase extraction apparatus, utilize this device can improve the SPME effect, the detectability of expanding unit and the scope of application.Belong to environmental analysis and analytical chemistry field.
Background technology
Chromatographic technique is one of main means of Analysis of environmental samples.Because the environmental sample complexity, changeable and concentration is lower, so just can carry out various Instrumental Analysis after must passing through pre-treatment.That traditional pre-treating method generally has is with an organic solvent more, the processing time is long and the many shortcomings of operating procedure, and in The whole analytical process the sample collection with handle the larger proportion (greater than 2/3) that accounts for consuming time.So research degree of accuracy height, simple and sample-pretreating method solvent free is a focus in field, contemporary analytical chemistry forward position fast.Since nineteen nineties, various novel sample-pretreating methods successively emerge, as methods such as supercritical fluid extraction, SPE, Subcritical Water Extraction, EXTRACTION BY SUPPORTED LIQUID MEMBRANES, SPMEs.Wherein SPME (SPME) technology is used more, its advantage is: 1. the extracting fiber head has good extraction or adsorptivity to volatilization and half volatile-type sample, is particularly suitable for the assay determination of volatilizable or half volatile component in gas phase, liquid phase, the solid phase sample; 2. finish from general of the process that is extracted into analysis and need tens minutes, in addition faster; 3. the extractor volume is little, can directly extract fast from atmosphere and water sample, takes back the laboratory easily and directly analyzes; 4. to the extraction of test substance, enrichment, desorb have been avoided the inconvenience of the steps such as sampling, enrichment, preservation and elimination interference in traditional sample pretreatment process in one.Because of not needing organic solvent, so be the sample pre-treatments technology of " green ".
At present, the extraction mode of SPME mainly contains two kinds, the one, immerse extraction, being about to fiber directly immerses in the sample solution, fiber contacts with sample solution and carries out solid-liquid distribution extraction, the taking-up fiber carries out chromatography after waiting to reach partition equilibrium, and the method is applicable to analyzes the big or bigger class material of molecular weight of the solubility of determinand in liquid phase; The 2nd, headspace extraction method, this method are to carry out headspace extraction on the determinand liquid level, thereby can avoid being disturbed by matrix impurity, thereby reduce fiber contamination, are applicable to the component that detects volatility and half volatile.
In general, the scope of application of headspace extraction method is wider, and especially sample is complicated and all the more so when having big molecule to disturb.If at this moment adopt to immerse extraction, interfering material is adsorbed on the extracting fiber easily, influence its absorption property and cause unstability of base line or produce impurity peaks in chromatography, and the life-span that can pollute chromatographic column, fiber also can reduce etc. greatly.The headspace extraction rule has been avoided above-mentioned adverse consequences, but when test substance has higher boiling point, component to be measured dividing potential drop in gas phase is little, and concentration is low, and the head space method reaches adsorption equilibrium required time length, sensitivity material lower, half-and-half volatile macromolecule is all the more so.Therefore, higher and when having big molecule chaff interference to exist, above-mentioned two kinds of methods and resultses all can not be satisfactory when determinand boiling point in the sample.In order to improve the deficiency of above two kinds of methods, be necessary to invent a kind of new circulating condensing extraction equipment and new extracting process.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of cyclic condensation solid-phase extraction apparatus is provided, simple in structure, easy to use, can improve the sensitivity of detection, reduce the detectability of determinand.
In order to realize this purpose, except injector, SPME bottle, beaker, also designed cycle condenser especially in the solid-phase micro-extracting device provided by the invention.Cycle condenser is a hollow cone that lid is arranged, and wherein cone shaft section drift angle 2 θ values are 20 °≤2 θ≤60 °.The condenser end face is circular; closely link together with the cone bottom surface; form closed system; the radius of condenser end face is greater than conical bottom radius surface 1-2mm; the injector protection tube, the cooling water outlet pipe that on the condenser end face, vertically be provided with cooling water inlet pipe, supply injector to insert; the injector protection tube crosses cycle condenser, and an end is showed out and sealed by sealing gasket from condenser end, and the other end passes from cone tip.
Cycle condenser is put into the SPME bottle, make the bottleneck EDGE CONTACT of the edge and the SPME bottle of cycle condenser end face, tighten the bottle cap of SPME bottle and realize fixing seal, place stirrer in the liquid to be measured of SPME bottle bottom, the SPME bottle is fixed by iron stand, and place the water-bath beaker, and beaker places on the constant temperature blender with magnetic force, and beaker bottom is placed with stirrer.
When utilizing device of the present invention to carry out cyclic condensation solid-phase extraction, the liquid heating to be measured with in the SPME bottle evaporate in the gas phase of SPME bottle liquid to be measured.Simultaneously in whole process; the cooling water that feeds is with the outer wall cooling of cycle condenser; make and be heated the outer wall condensation of the liquid to be measured that evaporate in the gas phase at cycle condenser; forming droplet flows down along outer wall; on the solid-phase micro-extraction fibre of injector protection tube outlet, converge, form stable condensing circuit.When solid-phase micro-extraction fibre inserts along the injector protection tube of cycle condenser, and fiber exposed the injector protection tube fully contact with liquid volatilization condensate liquid to be measured, reach partition equilibrium after, chromatography is carried out in taking-up.
The present invention integrates the advantage of extraction of head space formula and immersion extraction, given full play to vaporization at high temperature, the materialization rule of cryogenic condensation absorption can reduce the detectability of determinand, improve the sensitivity that detects, widened the range of application of solid phase micro-extraction technique in analyzing and testing.Extracting fiber in the device does not need directly to contact with liquid to be measured, thereby has reduced the contaminated possibility of fiber,
Description of drawings
Fig. 1 is the structural representation of extraction equipment of the present invention.
Among Fig. 1,1 is the injector protection tube, and 2 is cycle condenser; 3 is the condenser end face, and 4 is cooling water inlet pipe, and 5 is sealing gasket; 6 is cooling water outlet pipe, and 7 is injector, and 8 is iron stand; 9 are the SPME bottle, and 10 is beaker, and 11 is solid-phase micro-extraction fibre; 12 is heat medium, and 13 is liquid to be measured, and 14 is the stirrer in the extraction flask; 15 is the stirrer in the beaker, and 16 is constant temperature blender with magnetic force.
Fig. 2 is the cross-sectional view of cycle condenser among the present invention.
Among Fig. 2,1 is the injector protection tube, and 2 is cycle condenser, and 3 is the condenser end face, and 4 is cooling water inlet pipe, and 5 is sealing gasket, and 6 is cooling water outlet pipe.
The specific embodiment
Below in conjunction with drawings and Examples technical scheme of the present invention is further described.
Extraction equipment structure of the present invention mainly comprises cycle condenser 2, injector 7 as shown in Figure 1, SPME bottle 9, beaker 10.Cycle condenser 2 is the hollow cones that lid is arranged, and condenser end face 3 closely links together with the cone bottom surface, forms closed system.The radius of condenser end face 3 is greater than conical bottom radius surface 1-2mm.On condenser end face 3, vertically be provided with cooling water inlet pipe 4, the injector protection tube 1 that links to each other with injector 7, cooling water outlet pipe 6.Injector protection tube 1 crosses cycle condenser 2, one ends and exposes and by silicone rubber seal pad 5 sealing, the other end passes from cone tip from condenser end face 3.The largest outer diameter of cycle condenser 2 equates with SPME bottle internal diameter.Cycle condenser 2 is put into SPME bottle 9, makes the bottleneck EDGE CONTACT of the edge and the SPME bottle 9 of cycle condenser end face 3, tightens the bottle cap of SPME bottle 9 and realizes fixing seal.Place stirrer 14 in the liquid to be measured of SPME bottle 9 bottoms, SPME bottle 9 is fixing by iron stand 8, and places water-bath beaker 10, beaker 10 to place on the constant temperature blender with magnetic force 16, and beaker 10 bottoms are placed with stirrer 15.
Fig. 2 is the cross-sectional view of cycle condenser among the present invention.
As shown in Figure 2, the specially designed cycle condenser 2 of the present invention is the hollow cones that lid is arranged, and cone shaft section drift angle is 2 θ, and value is 20 °≤2 θ≤60 °.On condenser end face 3, vertically be provided with cooling water inlet pipe 4, the injector protection tube 1 that links to each other with injector 7, cooling water outlet pipe 6; wherein injector protection tube 1 crosses cycle condenser 2; one end exposes and by sealing gasket 5 sealing, the other end passes from cone tip from condenser end face 3.
When carrying out cyclic condensation solid-phase extraction, SPME bottle 9 usefulness iron stands 8 are fixing, make it to be in the correct position in the water-bath device, make below the water-bath liquid level of liquid level in beaker 10 of liquid to be measured in the SPME bottle 9, be placed with stirrer 15 in the beaker 10, be positioned on the constant temperature blender with magnetic force 16.Open constant temperature blender with magnetic force 16, set suitable temperature,,, liquid 13 to be measured is evaporate in the gas phase of SPME bottle 9 13 heating of the liquid to be measured in the SPME bottle 9 by the heat medium 12 in the heating beaker 10.Simultaneously; cooling water enters from cooling water inlet pipe 4; derive from cooling water outlet pipe 6; in whole process, the cooling water of feeding is the cooling of the outer wall of cycle condenser 2, makes to be heated the outer wall condensation at cycle condenser 2 of the liquid to be measured 13 that evaporate in the gas phase; form droplet; flow down along outer wall, on the solid-phase micro-extraction fibre 11 of injector protection tube 1 outlet, converge, form stable condensing circuit.After solid-phase micro-extraction fibre 11 fully contacts with liquid volatilization condensate liquid to be measured, reaches partition equilibrium, take out and carry out chromatography.
Embodiment:
Utilize cyclic condensation solid-phase extraction apparatus of the present invention (2 θ=20 °, Cu matter, 0 ℃ of cooling water temperature), to being dissolved in acetone soln and extracting with the ultrapure water-reducible third body BHC, and the use gas-chromatography is analyzed.Under 80 ℃ of water bath with thermostatic control conditions, extraction 15min just can reach balance.With Tianjin, island GC-14B gas chromatograph join the ECD detector, the N2000 chromatographic work station is analyzed, testing conditions: column temperature: 170 ℃, injector temperature: 210 ℃, detector temperature: 230 ℃, carrier gas: N
2, nitrogen pressure is controlled at 100kpa, not split sampling.Experiment detects and is limited to 10ng/L, and the range of linearity is 0.2 μ g/l-120.0 μ g/l, repeatability 9.58%, and the rate of recovery is 96.0%.
Under the similar detection condition, compare with headspace extraction method and the result that immerses extraction, as shown in the table:
| Analytical method | The range of linearity (μ g/l) | Coefficient correlation (r 2) | Detectability (LOD) (ng/l) | Reappearance (RSD%) |
| Condensation abstraction | 0.2-120.0 | 0.998 | 10 | 9.58 |
| Immerse extraction | 5.0-180.0 | 0.996 | 60 | 4.52 |
| Headspace extraction | 1.0-150.0 | 0.997 | 100 | 5.63 |
As seen, the extraction that adopts circulating condensing extraction equipment of the present invention to carry out is better than other method aspect detectability, and the range of linearity and reappearance are also satisfied.
Claims (2)
1. cyclic condensation solid-phase extraction apparatus; comprise injector (7); SPME bottle (9); beaker (10); it is characterized in that also comprising cycle condenser (2); cycle condenser (2) is a hollow cone that lid is arranged; condenser end face (3) closely links together with the cone bottom surface; form closed system; the radius of condenser end face (3) is greater than conical bottom radius surface 1-2mm; on condenser end face (3), vertically be provided with cooling water inlet pipe (4); injector protection tube (1) for injector (7) insertion; cooling water outlet pipe (6); injector protection tube (1) crosses cycle condenser (2); one end exposes and is sealed by sealing gasket (5) from condenser end face (3); the other end passes from cone tip; cycle condenser (2) is put into SPME bottle (9); make the bottleneck EDGE CONTACT of the edge and the SPME bottle (9) of cycle condenser end face (3); tighten the bottle cap of SPME bottle (9) and realize fixing seal; place stirrer (14) in the liquid to be measured of SPME bottle (9) bottom; beaker (10) is fixed and placed to SPME bottle (9) by iron stand (8); beaker (10) places on the constant temperature blender with magnetic force (16), and beaker (10) bottom is placed with stirrer (15).
2, according to the cyclic condensation solid-phase extraction apparatus of claim 1, the material that it is characterized in that described cycle condenser (2) is a metal, and wherein cone shaft section drift angle 2 θ values are 20 °≤2 θ≤60 °.
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| CNB2005100279557A CN1299793C (en) | 2005-07-21 | 2005-07-21 | Cyclic condensation solid-phase extraction apparatus |
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| CNB2005100279557A CN1299793C (en) | 2005-07-21 | 2005-07-21 | Cyclic condensation solid-phase extraction apparatus |
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| CN1299793C true CN1299793C (en) | 2007-02-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140033835A1 (en) * | 2012-07-31 | 2014-02-06 | Jan Hendrikse | Solid phase micro extraction (spme) vacuum inlet |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100469412C (en) * | 2007-03-02 | 2009-03-18 | 华中师范大学 | Ultrasonic auxiliary headspace liquid-phase microextraction method |
| CN102100976B (en) * | 2009-12-18 | 2013-01-30 | 中国科学院大连化学物理研究所 | Headspace liquid phase micro-extraction device adopting volatile solvent |
| CN101813584B (en) * | 2010-04-23 | 2012-07-25 | 延边大学 | Gas flow type dynamic liquid phase micro-extraction method |
| CN102455330B (en) * | 2010-10-27 | 2013-07-03 | 中国科学院大连化学物理研究所 | Head-space liquid-phase microextraction device based on semiconductor refrigeration technology |
| CN105911197B (en) * | 2016-05-25 | 2018-06-29 | 延边大学 | Automatic sample thermal desorption and liquid phase microemulsion preconcentrate device |
| CN107478497A (en) * | 2017-09-21 | 2017-12-15 | 国家地质实验测试中心 | SPME low temperature auxiliary equipment and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1039288A2 (en) * | 1999-03-26 | 2000-09-27 | Gerstel Systemtechnik GmbH & Co. KG | Method for solid phase micro-extraction, analysis and collector therefor |
| US6405608B1 (en) * | 2000-01-25 | 2002-06-18 | Sandia Corporation | Method and apparatus for optimized sampling of volatilizable target substances |
| CN2700880Y (en) * | 2004-06-09 | 2005-05-18 | 上海交通大学 | Solid-phase micro extraction apparatus |
| CN1628889A (en) * | 2003-12-18 | 2005-06-22 | 中国科学院大连化学物理研究所 | On-line solid phase micro-extraction method in capillary column and apparatus therefor |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1039288A2 (en) * | 1999-03-26 | 2000-09-27 | Gerstel Systemtechnik GmbH & Co. KG | Method for solid phase micro-extraction, analysis and collector therefor |
| US6405608B1 (en) * | 2000-01-25 | 2002-06-18 | Sandia Corporation | Method and apparatus for optimized sampling of volatilizable target substances |
| CN1628889A (en) * | 2003-12-18 | 2005-06-22 | 中国科学院大连化学物理研究所 | On-line solid phase micro-extraction method in capillary column and apparatus therefor |
| CN2700880Y (en) * | 2004-06-09 | 2005-05-18 | 上海交通大学 | Solid-phase micro extraction apparatus |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140033835A1 (en) * | 2012-07-31 | 2014-02-06 | Jan Hendrikse | Solid phase micro extraction (spme) vacuum inlet |
| US9134208B2 (en) * | 2012-07-31 | 2015-09-15 | Smiths Detection Montreal Inc. | Solid phase micro extraction (SPME) vacuum inlet |
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