CN101143270A - A sleeve type high temperature and high pressure resistant extraction cell and kit for solvent extraction - Google Patents
A sleeve type high temperature and high pressure resistant extraction cell and kit for solvent extraction Download PDFInfo
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- CN101143270A CN101143270A CNA2006100477656A CN200610047765A CN101143270A CN 101143270 A CN101143270 A CN 101143270A CN A2006100477656 A CNA2006100477656 A CN A2006100477656A CN 200610047765 A CN200610047765 A CN 200610047765A CN 101143270 A CN101143270 A CN 101143270A
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- 238000000638 solvent extraction Methods 0.000 title claims abstract description 13
- 238000007789 sealing Methods 0.000 claims abstract description 107
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Abstract
The invention relates to a sample extraction device which is a sleeve typed high temperature and high pressure resistance extraction tank used for solvent extraction. The invention contains an extraction tank pressure cap, a sealing ring pressure cap, a sample tank, a sample tank fixed sleeve, a sealing ring, a porous filter and so on. The sample tank is in a pot structure. One end of the cavity of the sample tank is a close typed conical structure. The sample tank fixed sleeve is sheathed outside of the sample tank. The two ends of the sample tank fixed sleeve are separately connected with extraction tank pressure cap in screw-threaded connection. The sealing ring pressure cap is arranged between the two ends of the sample tank fixed sleeve and the extraction tank pressure cap. The sealing ring is arranged inside the sealing ring pressure cap. The porous filter is arranged on the sealing ring. A convex sealing knife edge is arranged on the two end faces of the sample tank. Correspondingly, a convex pressure cap sealing knife edge is arranged on the pressure cap. The sealing ring is arranged between the sealing knife edge and the pressure cap sealing knife edge. The invention is convenient to be used and has low manufacture cost and use-cost.
Description
Technical field
The present invention relates to the sample extraction device, a kind ofly specifically be used for solvent-extracted high pressure resistant high temperature abstraction pool, be applicable under the pressurized conditions of heating the organic matter in solid or the semi-solid sample is extracted, be used for next step analysis.Abstraction pool structure of the present invention also is fit to miniaturization, can be made into the small-sized abstraction pool of 100 micro updatings, realizes and the chromatograph on-line coupling.
Background technology
The sample analysis process comprises several steps such as sampling, sample preparation and processing, assay determination, data processing, the time of finding sample treatment institute palpus by statistics accounts for 61% of The whole analytical process, and the time of assay determination has only accounted for 6%, and the sample preparation time is 10 times of assay determination unexpectedly.So efficiently, the research of the pre-treating method of sample preparation fast and automation has become one of main direction of modern analysis chemical research.The employed sample pre-treatments technology in laboratory has traditional Soxhlet to extract at present, liquid-liquid extraction, and microwave abstracting, novel extraction technology such as supercritical fluid extraction and accelerated solvent extraction are also ripe gradually.
In analytical chemistry, the target components in solid and the semi-solid sample is extracted, then extract is filtered.The dead volume and the dead angle area of abstraction pool are as much as possible little, to reduce the residual of sample.
Pressurized liquid extraction is to utilize under uniform temperature and pressure, and extremely strong dissolving that solvent had and penetrating power come the target components in solid and the semisolid is extracted.It is fast that this method has speed, and the solvent use amount is few, characteristics such as good reproducibility.The notion of pressurized liquid extraction proposed in nineteen ninety-five, was also referred to as accelerated solvent extraction, pressure fluid extraction or the solvent extraction that strengthens.Dai An company (Dionex) develops it and this technology commercialization, the registration mark of its product is ASE.Dai An company to employed abstraction pool application in the own instrument United States Patent (USP) (U.S.Pat.No.5647976).The accelerated solvent extraction pool volume of Dai An company is at 1mL-100mL, process nitrogen blows and is concentrated into 0.05 to 2mL, get 1 microlitre or 20 microlitres then and give gas-chromatography or the analysis of liquid chromatogram sample introduction, the sample utilization rate is greatly about 0.2%~4%, the solvent for use amount is at 2mL-150mL, be unfavorable for micro-example is extracted analysis, can not be applied in the gas-chromatography on-line analysis.
Pressurized liquid extraction (PLE) can realize that microminiaturization is (referring to disclosed patent application the accelerated solvent extraction device and method of capillary gas chromatography on-line coupling " a kind of with ", application number 200510047011.6), thereby the mode that might utilize large volume sample injection realizes online sample treatment and gas chromatographic detection, perhaps, realize the high-sensitivity analysis of some the low content organic components in the environment or in the biological sample is detected with the liquid chromatogram coupling.
Summary of the invention
The object of the present invention is to provide a kind of solvent-extracted sleeve type high-temperature and high-pressure resistant abstraction pool and external member of being used for, it can realize under the HTHP solvent extraction to trace organic substance in the sample (solid or semisolid), sample cell memory effect in the abstraction pool is little, the long service life of gasket seal, so use cost is low.It is safer that tube-in-tube structure makes the high pressure-temperature of abstraction pool use, and when accident took place, the high pressure-temperature organic solvent can at first enter the sleeve district and release is flowed out along the screw thread between pressure cap and the sleeve then.And do not have this safeguard function in the existing abstraction pool patent design.Design of the present invention also is particularly suitable for small abstraction pool, the abstraction pool of this miniaturization can be used on the device with the chromatograph on-line coupling, can with extract all or the overwhelming majority change in the chromatographic system, the sample utilization rate is high, can reduce the consumption of extractant greatly, environmentally friendly, be applicable to the micro-example occasion, in the sample for chemical analysis pre-treatment as micro-solid, semi-solid sample in atmosphere fine particle (aerosol), criminal investigation and the forensic medical examination.
For achieving the above object, the present invention adopts technical scheme to be:
A kind ofly be used for solvent-extracted sleeve type high-temperature and high-pressure resistant abstraction pool, comprise the abstraction pool pressure cap, the sealing ring pressure cap, sample cell, sample cell fixed muffle, and sealing ring, assemblies such as porous filtering sheet,
Sample cell is a tubular structure, and an end of its internal cavities is a closing in type frustum structure, its outer sample cell fixed muffle that is arranged with; The two ends inwall of sample cell fixed muffle has screw thread, can cooperate with the screw thread A on the abstraction pool pressure cap; Sample cell separates with the sleeve of fixed sample pond and pressure cap; One cover abstraction pool assembly can have a plurality of sample cells, the convenient use;
Sample cell fixed muffle two ends are threaded with the abstraction pool pressure cap respectively, are provided with the sealing ring pressure cap between sample cell fixed muffle two ends and abstraction pool pressure cap, are provided with sealing ring in the sealing ring pressure cap, and sealing ring is provided with the porous filtering sheet;
Two end faces of sample cell are provided with the sealing edge of a knife of projection, are convenient to load sample and additive; The corresponding pressure cap sealing edge of a knife of the projection that is provided with in pressure cap, sealing ring places between the sealing edge of a knife and the pressure cap sealing edge of a knife.Sealing between sample cell pressure cap and the sample cell compresses and realizes by laying respectively at the raised seals edge of a knife on the pressure cap and the raised seals edge of a knife on the sample cell end face and the sealing ring between them;
The sealing ring pressure cap is threaded with the abstraction pool pressure cap, and the porous filtering sheet of abstraction pool pressure cap inboard is a stainless steel material, forms the solvent allocation space between filter and the abstraction pool pressure cap, and it is the solvent guide hole that the abstraction pool pressure cap of middle upper end is provided with a guide hole;
The sealing ring pressure cap is used for fixing sealing ring, sealing ring is compressed and sealing porous filter disc and peripheral slit, avoids extractant from peripheral slit flow mistake.Abstraction pool pressure cap bottom outer wall has screw thread B, the rotation of sealing ring pressure cap is fixed on the sample cell pressure cap, screw thread on the sealing ring pressure cap cooperates with screw thread B on the sample cell pressure cap, thereby sealing ring and porous filtering sheet is spacing fixing, and helps forming with sample cell the enclosure space of given volume; The lateral wall of abstraction pool pressure cap has screw thread A, can be threaded with the sample cell fixed muffle, thereby formation adapts to the sealing system of the abstraction pool of different volumes.
Sealing ring is high temperature high voltage resistant and the macromolecular material that certain morphotropism is arranged, and the cross section is a stepped ramp type, and is adaptive with the sealing ring pressure cap, and is spacing fixing by sealing ring pressure cap institute;
Inside, described abstraction pool pressure cap upper end is provided with guide-localization platform awl groove, guide-localization platform awl groove lower end is provided with zero circle draw-in groove, device has that there is stainless steel porous filtering sheet the inboard, formation solvent allocation space between filter and the sample cell pressure cap under the sealing zero circle abstraction pool pressure cap in it.
Under the sealing ring pressure cap on the relative aperture bore little, can tangle sealing ring, the inwall of sealing ring pressure cap has screw thread, is connected with abstraction pool pressure cap lower end outer wall thread, thus can be with sealing ring and porous filtering sheet location.
Described sample cell fixed muffle adopts stainless steel material, and enough mechanical strengths and suitable heat conductivility are arranged; Sample cell adopts the good stainless steel material of inertia to make, and the inner surface polishing changes the total measurement (volume) that sample cell length or internal diameter can change sample cell.
Describedly be used for solvent-extracted sleeve type high-temperature and high-pressure resistant abstraction pool external member, be used for that sample cell is loaded sample and the Seal Kit of usefulness is preserved in sealing, comprise that cover bucket, bucket bottom spacer, seal cover and the sample of sample cell loaded rod:
Cover bucket bottom is conical, and bucket outer, top is provided with screw thread, has screwed togather seal cover on it, makes with metal or macromolecular material;
The bucket of installation bottom spacer is arranged at cover bucket bottom, and the center is provided with a protruding round platform above the bucket bottom spacer, is cone below, and the angle of cone is identical with the angle of bucket end circular cone, and round platform is corresponding with the circular hole of sample cell bottom, is used for sealing.The bucket bottom spacer is made with macromolecular material.
The round platform that a projection is arranged in the seal cover, round platform external diameter are used for compressing sealing with sample cell more than or equal to the sample cell external diameter.Last inboard screw thread is adaptive with the external screw thread on the cover bucket;
It is a cylindrical bar that sample is loaded rod, and internal diameter is made with metal or macromolecular material less than the sample cell diameter, is used for the sample of compacting filling.
The present invention compares with commercial means with existing patent design and has the following advantages:
1) telescopic abstraction pool provides safer design, when abstraction pool was out of shape because of overvoltage and breaks, inner organic solvent can not come out in direct injection, but is subjected to stopping of outer sleeve, flow out in screw slit between pressure cap and sleeve, unloads simultaneously and be depressed into normal pressure;
2) lined sample cell design simplification the processing of sample cell, guarantee the processing of sample cell best bright finish easily, be easy to the processing of sample cell surface inertness, the sample cell materials reduce, can select the inertia better material for use, the cleaning of pond body and preservation in the process easy to use are easy to load sample and temporary and use thereafter.Sample cell is designed to single closing in structure, is convenient to load sample.
3) lined sample cell design can change the volume of sample cell easily by changing pond body length and internal diameter, meets the different needs; The outer fixed muffle of abstraction pool is born the location of assembly, the heat conduction of sample cell heating, the effect of fixing and protect sample cell of sample cell pressure cap, and it does not contact with sample or extractant.Sample cell is placed in the fixed muffle, and there is the sealing edge of a knife at the two ends, pond, compresses sealing with sealing ring on the sample cell pressure cap.
4) exclusive sealing ring pressure cap designs, and sealing ring, filter and sample cell pressure cap are incorporated into together, without any need for instrument, just can easily install and fix above-mentioned parts.After each disassembly, cleaning, can guarantee that with the sealing ring pressure cap installation site of sealing ring is repeated accurately, so can prolong sealing ring service life;
5) abstraction pool of tube-in-tube structure can be made the small-sized abstraction pool that volume is 100 microlitres.Small-sized abstraction pool can improve the sample utilization rate, and solvent load is little, is particularly useful for the abstraction pool in do pressurization heating solvent extraction-chromatogram on-line coupling device.Can be widely used in criminal investigation, atmosphere fine particle sample sizes such as (aerosols) tens milligrams in addition zero point several milligrams of micro-examples preliminary treatment (the quick extraction and the analyzing and testing of trace organic substance in micro-solid, the semi-solid sample).
The abstraction pool of stock size can be used for the extraction of samples such as food, soil, environment, macromolecular material and geological prospecting rock core.The abstraction pool of tube-in-tube structure both can have been made the accelerated solvent extraction pond of stock size, can also make miniature abstraction pool.
6) design of lined sample cell and sample cell are preserved Seal Kit, made things convenient for and packed sample into and preserve the sample cell that installs sample, can a plurality of sample cells of one-time pad, extract and change other 1 sample cell and sealing filtration members after 1 sample is finished immediately, then extract following 1 sample, greatly improve operating efficiency, reduced operating cost.
Telescopic abstraction pool of the present invention is easy to use, and cost of manufacture is low, and use cost is also low.
Description of drawings
Fig. 1 is abstraction pool global design figure of the present invention;
Fig. 2 is an abstraction pool decomposition texture design drawing of the present invention;
Wherein: 100-abstraction pool pressure cap; 101-abstraction pool pressure cap screw thread A; 102-abstraction pool pressure cap sealing edge of a knife; 103-O encloses draw-in groove; 104-solvent allocation space; 105-abstraction pool pressure cap screw thread B; 106-guide-localization platform awl groove; 200-sealing ring pressure cap; 201-sealing ring; 202-solvent guide hole; 203-sealing O circle; 204-porous filtering sheet; 205-sealing ring pressure cap screw thread; 300-abstraction pool; 301-abstraction pool closing in guide hole; 302-abstraction pool sealing edge of a knife; 400-abstraction pool fixed muffle; 401-abstraction pool fixed muffle screw thread;
The Seal Kit of Fig. 3 for being used with sample cell among the present invention;
Wherein: 500-Seal Kit; 501-sample cell cover bucket; 502-cover bucket screw thread; 503-bucket end circular cone; 510-bucket bottom spacer; 511-pad projection round platform; 520-seal cover; 521-seal cover projection round platform; 522-seal cover screw thread; 530-sample is loaded rod
Fig. 4 is the design drawing with small-sized abstraction pool of the present invention and gas-chromatography coupling;
Wherein: 1-solvent bottle; 2-pump; 3-extraction cells; 4-pressure sensor; 5-quantity tube; 6-ten-way valve; 7-flow stabilizing valve; 8-six-way valve; 9-column sample injection device; 10-pre-column; 11-crimp head; 12-analytical column; 13-hydrogen flame ionization detector; 14-chromatogram stove case.
Fig. 5 is the chromatogram with normal paraffin content in small-sized abstraction pool of the present invention and the online detection Atmospheric particulates of gas chromatography combined usefulness.
Fig. 6 separates the chromatogram that detects with liquid chromatogram afterwards for the polycyclic aromatic hydrocarbon in the grit of abstraction pool extraction of the present invention seashore.
The specific embodiment:
Referring to Fig. 1, Fig. 2 and shown in Figure 3, a kind ofly can under HTHP, carry out solvent-extracted abstraction pool to the organic matter in solid or the semi-solid sample, mainly by abstraction pool pressure cap 100, sealing ring pressure cap 200, sample cell 300, sample cell fixed muffle 400, be used for sample cell and load sample and sealing and preserve five parts such as Seal Kit 500 of usefulness and form.
1) the abstraction pool pressure cap is made with stainless steel material, and there is the sealing edge of a knife 102 lower end, can seal with sealing ring 201 crimping;
There is guide-localization platform awl groove 106 abstraction pool pressure cap upper end, when being used for solvent conducting joint insertion sample cell pressure cap realization hydrostatic seal externally, finds the location automatically accurately.There is ' zero ' circle draw-in groove 103 guide table awl groove lower end, and when the coupling hydrostatic seal, ' zero ' circle 203 compressive deformations expand, and interior edge compresses with joint and forms sealing, and the right-angle side of outer and groove is along forming sealing.Concentric with the axle center of pond body;
Abstraction pool pressure cap outer wall has abstraction pool pressure cap screw thread A101, can with 401 combinations of sample cell fixed muffle screw thread, in the process that rotation tightens, the sample cell and the sealing ring of inside can be compressed, realize sealing;
Abstraction pool pressure cap lower end outer wall has sample cell pressure cap screw thread B105; can with 205 combinations of sealing ring pressure cap screw thread; sealing edge of a knife tightening seal with sealing ring and abstraction pool pressure cap; also that filter 204 is fixing simultaneously; make abstraction pool pressure cap, porous filtering sheet, sealing ring form an integral body thus; operate being more prone in the assembling of follow-up abstraction pool, also with sealing ring, the strict location of filter, assembling back better tightness has effectively been protected the sealing edge of a knife again simultaneously.
2) the sealing ring pressure cap is a stainless steel material, and inwall has seal cover pressure cap screw thread, as mentioned above can with sample cell pressure cap screw thread B combination, play location and protective effect;
The bottom internal diameter of sealing ring pressure cap is received little, holds the sealing ring of step cutting pattern shape, plays location and fixing seal ring.
3) sample cell adopts the good stainless steel material of inertia to make, and the inwall polishing can be born operating pressure 20Mpa, 200 ℃ of temperature, and its cavity internal diameter is 5-25mm, length is 6-120mm.
The bossed sealing edge of a knife 302 of the end face of pond body forms the crimping sealing with sealing ring; Intracoelomic cavity one end in pond can prevent losing of solid or semi-solid sample for the design 301 of closing up.
4) the sample cell fixed muffle also is a stainless steel material, and enough mechanical strengths and suitable heat conductivility are arranged, and in the process of accelerated solvent extraction, heat can be passed to inner abstraction pool, simultaneously sample cell is shielded, and guarantees that experimental implementation is safer;
Sample cell fixed muffle inwall port has screw thread, as front 1) as described in, be used for and the combination of sealing ring pressure cap, the fixed extractor pond, and form confined space.
5) be used for the Seal Kit that sample cell is loaded sample and sealing preservation usefulness, comprise that cover bucket 501, bucket bottom spacer 510, seal cover 520 and the sample of sample cell loaded rod 530 etc.501 and 530 usefulness metals or macromolecular material are made, and 510 usefulness macromolecular materials are made, and 520 usefulness macromolecular materials or composite are made;
Cover bucket bottom is a taper shape 503, is convenient to install bucket bottom spacer 510; There is screw thread 502 bucket outer, top, is used for fixing seal cover 520;
There is a protruding round platform 511 at the center above the bucket bottom spacer, and is corresponding with the circular hole of sample cell bottom, is used for sealing;
Below the bucket bottom spacer is cone, and the angle of cone is identical with the angle of bucket end circular cone 502;
The round platform 521 that a projection is arranged in the seal cover, round platform external diameter are used for compressing sealing with sample cell more than or equal to the sample cell external diameter;
6) the employed gasket seal of sample cell is PEEK or composite, its heatproof T 〉=200 ℃, and the withstand voltage 25Mpa that is not less than can use repeatedly, and organic solvent-resistant is difficult for aging; Abstraction pool is installed filter, and the thickness of filter is more bigger than the degree of depth of groove, can form a circle slit between its edge and the seal cover; Just in time being pressed on this slit of gasket seal design, the little distortion behind the back cushion sheet pressurized is with this gap sealing.Make the solvent can only can not be by the slit at edge by filter disc;
Above-mentioned design hand-tight make-up abstraction pool pressure cap just can satisfy the withstand voltage requirement of sealing.The high workload pressure of this device pond body is 20Mpa, 200 ℃ of maximum operating temperatures.
Referring to Fig. 1, Fig. 2 and shown in Figure 3, a kind of telescopic miniature abstraction pool that can carry out online detection with the gas-chromatography coupling, pond body adopt design and the material identical with embodiment 1, sample cell is of a size of internal diameter 2-5mm, length 3-10mm, high workload pressure is 20Mpa, 200 ℃ of maximum operating temperatures.
Application examples 1 and the gas chromatography combined content that can suck n-alkane on the solid particulate matter in the atmosphere that detects with on-line coupling
Adopt flow chart shown in Figure 4.Sample cell volume 200 microlitres, the PM10 sample strip of gathering in the air standard sampler is put into sample cell, with n-hexane/cyclohexane (1: 1) is solvent, abstraction pool is forced into 12Mpa, extracted 8 minutes down at 100 ℃, cooling back with the large volume sample injection technology with in the online pre-column that is transferred in the capillary gas chromatography system of extract, post compartment analysis by analysis, the oxygen ionized detector detection of hydrogen fire.Fig. 5 is the chromatogram that can suck normal paraffin content on the solid particulate matter in the online detection atmosphere of pressurized liquid extraction-gas chromatography combined usefulness.
Environmental contaminants in the application examples 2 extraction soil
Pedotheque was sieved, air-dry, get 10 grams, use abstraction pool of the present invention, abstraction pool volume 10mL, extractant adopts n-hexane/acetone (1: 1), 100 ℃ of extraction temperature, pressure is 10Mpa, extracts 10 minutes.To extract liquid nitrogen and blow and be concentrated into 2mL, use capillary gas chromatography-GC-MS and liquid-phase chromatographic analysis organic pollution respectively.
Polycyclic aromatic hydrocarbon in the application examples 3 extraction beaches
Adopt the device in the example 1, the sample cell volume is 5mL.Grit 5 grams that the seashore is got place abstraction pool, and remaining space fills up with quartz sand.Extractant adopts n-hexane, 100 ℃ of extraction temperature, and pressure is 10MPa, extracts 10 minutes.The extraction solution that obtains blown with nitrogen be concentrated into 0.5mL, liquid chromatogram sample introduction 0.2 microlitre adopts UV-Vis to detect, and detects wavelength 254nm, measures the polycyclic aromatic hydrocarbon in the extract, and chromatogram is seen Fig. 7.
Claims (8)
Priority Applications (1)
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CNB2006100477656A CN100525875C (en) | 2006-09-15 | 2006-09-15 | Sleeve type high-temperature and high-pressure resistant extracting pool and external member used for solvent extraction |
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CNB2006100477656A CN100525875C (en) | 2006-09-15 | 2006-09-15 | Sleeve type high-temperature and high-pressure resistant extracting pool and external member used for solvent extraction |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102607929A (en) * | 2012-03-05 | 2012-07-25 | 中国科学院地质与地球物理研究所 | Pneumatic type sample loader |
CN103267728A (en) * | 2012-02-16 | 2013-08-28 | 恩德莱斯和豪瑟尔分析仪表公司 | Inline optical sensor with modular flowcell |
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