CN102967677A - PCBs (Polychlorinated Biphenyls) elution device for intensifying target object desorption and mass transfer based on physical assistance - Google Patents
PCBs (Polychlorinated Biphenyls) elution device for intensifying target object desorption and mass transfer based on physical assistance Download PDFInfo
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- CN102967677A CN102967677A CN201210440070XA CN201210440070A CN102967677A CN 102967677 A CN102967677 A CN 102967677A CN 201210440070X A CN201210440070X A CN 201210440070XA CN 201210440070 A CN201210440070 A CN 201210440070A CN 102967677 A CN102967677 A CN 102967677A
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Abstract
The invention relates to a PCBs (Polychlorinated Biphenyl) elution device for intensifying target object desorption and mass transfer based on physical assistance, belonging to the field of analysis and testing. The PCBs refers to polychlorinated biphenyls; and the invention aims at solving the problem that in the prior art, detection of a target object elution section in a sampling procedure of pollutant in environmental water by using gas chromatography-mass spectrometry is not satisfactory. On the basis of the structure of a customary elution device with a needle cylinder and a needle cylinder filter, an ultrasonic transmission component which is of a wristwatch shape is further sleeved on the needle cylinder, and moreover the wristwatch is sleeved near the bottom of the needle cylinder. When the elution device is used, the elution section is intensified through the following steps that: an ultrasonic wave in a high frequency band is exerted before the needle cylinder filter is communicated with a negative pressure source so as to forcedly promote the desorption and the mass transfer of the target object; and while the needle cylinder filter is communicated with the negative pressure source to suck and filter, the ultrasonic wave in the high frequency band continuously radiates so as to forcedly repress the reabsorption of the target object in the suction filtration process.
Description
Technical field
The present invention relates to the PCBs wash-out device of the assisted and strengthened object desorb of a kind of physics and mass transfer, belong to the analytical test field.
Background technology
Character group PCBs refers to polychlorinated biphenyl, and the implication that refers to of this character group PCBs is known for the professional in analysis and testing technology field.
About the origin of Trace Polychlorinated Biphenyls in the environment water and the general background of analyzing and testing thereof, can be referring to Chinese invention patent application case 201210099400.3.
In many detection methods of Trace Polychlorinated Biphenyls, comparatively speaking, comparatively accurate, reliable with the GC-MS method in for environment water.Described GC-MS analyzes, and refers to gas chromatography-mass spectrometry, the GC-MS character group its refer to and art-recognized meanings itself for the professional in analysis and testing technology field, be known.
As mentioned above, in environment water Trace Polychlorinated Biphenyls analyzing and testing, the GC-MS method is than the tool advantage, and this point is described in detail in above-mentioned Chinese invention patent application case 201210099400.3.
According to the detailed introduction of Chinese invention patent application case 201210099400.3, among the GC-MS analytical test program for Trace Polychlorinated Biphenyls in the water body, comprise important standby sample step, the namely step of adsorptive separation target substance from water body; Employing is adsorbed target substance through the good magnetic composite nano adsorbent of the hydrophilicity of modification from water body, and through magnetic separation, wash-out, evaporate, dry up, the step such as organic solvent constant volume, finish standby sample, be a more high efficiency sampling method.
Elution step wherein is the focus that this case is paid close attention to.
Analyze in the standby sample for water body Trace Polychlorinated Biphenyls GC-MS existing, its elution step, to be placed within the syringe through the magnetic composite nano adsorbent that from water body, has adsorbed target substance that magnetic separates, and the syringe filtrator in micron order aperture is installed at the syringe front end, with the described magnetic composite nano adsorbent of organic solvent drip washing, and in conjunction with the suction filtration means, reach the purpose of wash-out target substance.
In elution step, such as how the least possible wash-out organic solvent, reach one desirable as far as possible near 100% eluting rate, for saving analysis time, and, the reliability, the accuracy that improve analysis result are all significant, and about this point, any one professional who is engaged in the GC-MS analysis is clear.
In the prior art, comprise that GC-MS analyzes the standby sample program of multiple instrumental analysis of standby sample program, the absorb-elute step of its target substance, usually, all be to adopt simple, traditional syringe to add the apparatus structure of filtrator, and realize wash-out in the mode that the simple drip washing of organic solvent adds suction filtration; Because there is special affinity interaction power in the evaluating objects material usually and between the selected adsorbent, this is the basis that selected adsorbent has good trapping ability, yet, also just because the special affinity interaction power that exists between selected adsorbent and the evaluating objects material is difficult to reach a desirable eluting rate so that the simple drip washing of common organic solvents adds the mode of suction filtration; In other words, selected adsorbent its early stage is to the trapping ability of target substance, with the wash-out difficulty of evaluating objects material in the later stage elution step be the desorb difficulty, both are contradiction each other; Generally speaking, be to improve the eluting rate of evaluating objects material, must take sacrifice adsorbent early stage to the trapping ability of evaluating objects material as prerequisite, vice versa; More particularly, the Capture by Sorbents During ability is weak, comparatively speaking, and just easy wash-out, otherwise, if the Capture by Sorbents During ability is strong, just be not easy to reach desirable eluting rate.
As mentioned above, there is special affinity interaction power in the evaluating objects material usually and between the selected adsorbent, as the specialty chemical worker, this be extremely hold intelligible, as an example, can and evaluating objects material polychlorinated biphenyl between form special π-π combination power, and has again special high-ratio surface, and carry out easily that magnetic separates, certainly the magnetic Nano activated charcoal that first-selected is through hydrophilic modifying, this is the first-selected adsorbent that can reach optimum capture rate, but, just because of the magnetic Nano activated charcoal to polychlorinated biphenyl π-π combination power is strong, specific surface is large especially, it is not strong to capture Z-TEK, so, the problem that causes is exactly that its eluting rate lowers greatly, usual wash-out means become fully unreliable at this, to such an extent as to can't consider to use among the actual analysis Test Application described magnetic Nano activated charcoal to be used as trapping agent or to say adsorbent fully.Just because of this, adopt described magnetic Nano activated charcoal through hydrophilic modifying to be used as the standby sample trapping agent of GC-MS and so on instrumental analysis or say adsorbent, in the prior art basic nobody mention, more report without pertinent literature.
Above-mentioned Chinese invention patent application case 201210099400.3, obviously be that the carbon nano-tube of magnetic coupling captures the polychlorinated biphenyl in the water body not as the trapping agent through the magnetic active carbon of hydrophilic modifying with a kind of trapping ability, the scheme of this application case is real to be a kind of power of capture and eluting rate two-phase balance unavoidable newly measures afterwards.
As seen, if rest on the existing elution technique level always, so, the situation that adsorbent selection face receives greatly to limit to will continue.
In brief, in the so specific field of water body Trace Polychlorinated Biphenyls analytical test work, the wash-out means in the existing standby sample program usually can not be satisfactory; Therefore, how improving the object elution technique in the standby sample program of water body Trace Polychlorinated Biphenyls analytical test, is a problem that merits attention.
Summary of the invention
Technical matters to be solved by this invention is, for the unsafty present situation of elution technique in its standby sample program of water body Trace Polychlorinated Biphenyls analytical test work, researches and develops a kind of new washing device of addressing this problem of helping.
The present invention is by the described technical matters of following solution; this scheme provides the PCBs wash-out device of the assisted and strengthened object desorb of a kind of physics and mass transfer; this PCBs refers to polychlorinated biphenyl; this application of installation detects its standby sample program in PCBs gas-matter coupling; the structure of this device comprises syringe; and; syringe filter; a port of this syringe filter and the injection port of this syringe are socketed mutually; emphasis is; the structure of this device also comprises ultrasonic transducer; and; the ultrasonic transducer containment vessel; this ultrasonic transducer containment vessel is a box or drum; described ultrasonic transducer is the inside that is installed in this ultrasonic transducer containment vessel; the both sides of this ultrasonic transducer containment vessel respectively are equiped with a ring; the installing mode of this ring on the ultrasonic transducer containment vessel is fixedly installing mode or hinged installing mode; and; elastic cord; this elastic cord is to have flexible ribbon; the two ends of this elastic cord are connected with two described rings respectively; the part of the remainder of this elastic cord holds and is fitted on the syringe outer wall surface; it pulls strength and causes this ultrasonic transducer containment vessel to be close on the outer wall surface of syringe to hold the described elastic cord that is fitted on the syringe outer wall surface; this is close to the bottom of the contiguous syringe of its locations of structures of ultrasonic transducer containment vessel on the syringe outer wall surface; and the ultrasonic transducer containment vessel that elastic cord links together is to be easy to the independent assortment structural relation that mutually breaks away from together with the structural relation between its content itself and the syringe; its radiable ultrasonic frequency scope of this ultrasonic transducer is between 100KHz and 12MHz; and; higher-order of oscillation electric signal transmission cable, an end of this higher-order of oscillation electric signal transmission cable see through the ultrasonic transducer containment vessel and are connected with described ultrasonic transducer.
Described its art-recognized meanings of ultrasonic transducer one word is known for the ultrasound wave professional and technical personnel; Be suitable for the ultrasonic transducer of this case yes hypomegetic ultrasonic transducer, the hypomegetic ultrasonic transducer of various forms all has commercially available, also can customize to ultrasound wave specialized factory.
Described ultrasonic transducer containment vessel is for the protection of ultrasonic transducer, makes it avoid exposing in hostile environment; This its material of ultrasonic transducer containment vessel can be any selected material, and its material of described containment vessel is metal, pottery, glass, plastics for example, etc., its material can be selected as required.
Described its art-recognized meanings of higher-order of oscillation electric signal transmission cable one word is known for the ultrasound wave professional and technical personnel; Higher-order of oscillation electric signal transmission cable market is on sale, also can customize to ultrasound wave specialized factory.
The ultrasound wave of described frequency range between 100KHz and 12MHz is the ultrasound wave of the weak high-frequency band of ultrasonic cavitation effect, has many different from the ultrasound wave of the strong low-frequency band of ultrasonic cavitation effect; Its difference is known for the professional and technical personnel of art of ultrasound, is not repeated herein.
The structure of this device of this case can comprise higher-order of oscillation electric signal generator certainly, and the other end of described higher-order of oscillation electric signal transmission cable can be connected with this higher-order of oscillation electric signal generator.Various higher-order of oscillation electric signal generator all has commercially available; Also can customize to ultrasound wave specialized factory.
Its radiable ultrasonic frequency of this ultrasonic transducer, further preferred scope is between 300KHz and 12MHz.
This syringe filter, the aperture of the filter bores of its filter membrane can be the arbitrarily selected apertures between from 0.01 micron to several microns, and still, the preferable range in its filter membrane aperture of this syringe filter is between 0.05 micron and 1.00 microns.Described syringe filter with and interior filter membrane market on sale, also can customize to specialized factory.
Described syringe, its pattern is analogous to usual medical syringe; Its material of described syringe can be plastics, glass, metal, pottery, etc.; Its preferred material of this syringe is quartz glass material or stainless steel.
The structure of this device of this case can also comprise some annexes, described annex for example: the fixed mount that is used for fixing described syringe; Described annex is again for example: the filtrate receiver that is used for receiving filtrate that is connected with syringe filter; Described annex is also for example: with the negative pressure source equipment of described filtrate receiver and syringe filter UNICOM, this negative pressure source refers to any equipment that can make vacuum condition, and described negative pressure source specifically refers to the equipment of vacuum pump and so on; Known with regard to itself art-recognized meanings of vacuum pump one word in the vacuum technique field only; Etc..
Advantage of the present invention is, be that syringe adds on the basis of syringe filter with apparatus structure at usual standby sample, the ultrasonic transducer containment vessel that includes ultrasonic transducer that further is set with elastic cord and combines with this elastic cord in the syringe outer wall surface, the strength that pulls of elastic cord causes this ultrasonic transducer containment vessel to be close on the syringe outer wall surface, the bottom of the contiguous syringe in the position that it is close to, so, when application this case device carries out the wash-out operation, can first the adsorbent that has captured target substance be moved in the syringe, and in the syringe filling of adsorbent region or spray wash-out organic solvent, simultaneously, open higher-order of oscillation electric signal generator, form of energy conversion via described ultrasonic transducer, and the sound wave that sees through ultrasonic transducer containment vessel and needle cylinder wall transmits, the adsorbent region sustained radiation ultrasonic cavitation effect ultrasound wave of weak high-frequency band in the syringe, and during this period, connect off and on negative pressure source, off and on suction filtration; Among its application of this case device, it is the reinforcement of reaching the wash-out link by following mechanism: the ultrasound wave that before connecting negative pressure source, applies high frequency band, brute force is facilitated desorb, the mass transfer of object, and during connection negative pressure source suction filtration, the ultrasound wave of high-frequency band still continues acting on simultaneously, and brute force checks the again absorption of target substance in the suction filtration process; Can so repeat to operate several times according to the needs of actual conditions, to reach desirable wash-out target.
On the other hand; and the ultrasonic transducer containment vessel that elastic cord links together is to be easy to the independent assortment structural relation that mutually breaks away from together with the structural relation between its content itself and the syringe; based on this, its structure of this case device is a flexibly structure that dismounting is convenient to both.
The application of this case device can be so that be similar to the trapping agent that its such inside of magnetic active carbon has the huge brute force of the specific surface in large and small duct of flood tide, and its target substance that captures no longer is difficult to wash-out; Based on the application of this case device, magnetic active carbon cheap and easy to get application in the standby sample program of instrumental analysis just becomes a kind of actual option that allows.
Description of drawings
Fig. 1 is the brief synoptic diagram of this case apparatus structure.
Among the figure; the 1st, syringe; the 2nd, elastic cord; the 3rd, the ultrasonic transducer containment vessel, 4,6 is respectively two rings that locations of structures is different, the 5th, ultrasonic transducer; the 7th, syringe filter; the 8th, higher-order of oscillation electric signal transmission cable is not drawn described other annex among the figure, has carried out amplifying in the legend and to the part of apparatus structure and has showed.
Embodiment
In this case embodiment that Fig. 1 shows; the structure of this device comprises syringe 1; and; syringe filter 7; port of this syringe filter 7 and the injection port of this syringe 1 are socketed mutually; emphasis is; the structure of this device also comprises ultrasonic transducer 5; and; ultrasonic transducer containment vessel 3; this ultrasonic transducer containment vessel 3 is a box or drum; described ultrasonic transducer 5 is the inside that is installed in this ultrasonic transducer containment vessel 3; the both sides of this ultrasonic transducer containment vessel 3 respectively are equiped with a ring; always have two rings; respectively ring 4 and ring 6; this ring 4; 6 installing modes on ultrasonic transducer containment vessel 3 are fixedly installing mode or hinged installing mode; what show in the legend is described fixedly installing mode; described hinged installing mode is not showed with legend; described hinged installing mode namely is with ring 4; 6 change the hinged movable or juncture that swings with the junction surface of ultrasonic transducer containment vessel 3 into by fixing Immobile juncture; a hinged word its art-recognized meanings for the personnel of mechanical major is known; and; elastic cord 2; this elastic cord 2 is to have flexible ribbon; the two ends of this elastic cord 2 respectively with two described rings 4; 6 connect; the part of the remainder of this elastic cord 2 holds and is fitted on syringe 1 outer wall surface; it pulls strength and causes this ultrasonic transducer containment vessel 3 to be close on the outer wall surface of syringe 1 to hold the described elastic cord 2 that is fitted on syringe 1 outer wall surface; this is close to the bottom of the contiguous syringe 1 of ultrasonic transducer containment vessel 3 its locations of structures on syringe 1 outer wall surface; and the ultrasonic transducer containment vessel 3 that elastic cord 2 links together is to be easy to the independent assortment structural relation that mutually breaks away from together with the structural relation between its content itself and the syringe 1; these ultrasonic transducer 5 its radiable ultrasonic frequency scopes are between 100KHz and 12MHz; and; higher-order of oscillation electric signal transmission cable 8, an end of this higher-order of oscillation electric signal transmission cable 8 see through ultrasonic transducer containment vessel 3 and are connected with described ultrasonic transducer 5.
The described ultrasonic transducer containment vessel 3 that sees through refers to the shell wall that penetrates by ultrasonic transducer containment vessel 3.
The frequency values arbitrarily selected of this scope between 100KHz and 12MHz all is the preferred frequency enforcement value that this case allows.
The structure of this embodiment can comprise higher-order of oscillation electric signal generator certainly, and the other end of described higher-order of oscillation electric signal transmission cable 8 can be connected with this higher-order of oscillation electric signal generator.Do not draw described higher-order of oscillation electric signal generator in the accompanying drawing.
Among implementing, these ultrasonic transducer 8 its radiable ultrasonic frequencies, further preferred practical range is between 300KHz and 12MHz; The ultrasonic frequency value of selecting arbitrarily between this 300KHz and 12MHz all is the described further preferred frequency values that this case allows enforcement.
Among implementing, this syringe filter 7, the aperture of the filter bores of its filter membrane can be the arbitrarily selected aperture between from 0.01 micron to several microns, and still, the preferred practical range in its filter membrane aperture of this syringe filter is between 0.05 micron and 1.00 microns; The filter membrane aperture value arbitrarily selected of scope between 0.05 micron and 1.00 microns all is the enforcement value in the described aperture of this case permission.Described syringe filter 7 with and interior filter membrane market all on sale, also can customize to relevant speciality producer.
Described syringe 1, its pattern is analogous to usual medical syringe; Described syringe 1 its enforcement material can be plastics, glass, metal, pottery, etc.; This syringe 1 its preferably to implement material be quartz glass material or stainless steel.
Described elastic cord, itself art-recognized meanings of this word is known; Described elastic cord market is on sale.
The structure of this device of this case can also comprise some annexes, described annex for example: the fixed mount that is used for fixing described syringe 1; Described annex is also for example: the filtrate receiver that is used for receiving filtrate that is connected with syringe filter 7; Described annex is more for example: with the negative pressure source equipment of described filtrate receiver and syringe filter 7 UNICOMs, this negative pressure source refers to any equipment that can make vacuum condition, and described negative pressure source specifically refers to the equipment of vacuum pump and so on; Known with regard to itself art-recognized meanings of vacuum pump one word in the vacuum technique field only; Etc..Do not draw described annex in the accompanying drawing.
Implement related syringe 1, its pattern is not limited to the pattern in the accompanying drawing; Described syringe 1 also can be the structure that its upper end open-mouth does not have the convex edge.
Implement related syringe 1, the pattern of its injection port is not limited to the pattern in the accompanying drawing.
Implement related syringe 1, make a general reference its similar function member.
Implement related syringe filter 7, be not limited to accompanying drawing legend structure, related syringe filter 7 general reference similar function members.
The implementation of this case is not limited to this case accompanying drawing legend.
Claims (5)
1. the PCBs wash-out device of the assisted and strengthened object desorb of physics and mass transfer; this PCBs refers to polychlorinated biphenyl; this application of installation detects its standby sample program in PCBs gas-matter coupling; the structure of this device comprises syringe; and; syringe filter; a port of this syringe filter and the injection port of this syringe are socketed mutually; it is characterized in that; the structure of this device also comprises ultrasonic transducer; and; the ultrasonic transducer containment vessel; this ultrasonic transducer containment vessel is a box or drum; described ultrasonic transducer is the inside that is installed in this ultrasonic transducer containment vessel; the both sides of this ultrasonic transducer containment vessel respectively are equiped with a ring; the installing mode of this ring on the ultrasonic transducer containment vessel is fixedly installing mode or hinged installing mode; and; elastic cord; this elastic cord is to have flexible ribbon; the two ends of this elastic cord are connected with two described rings respectively; the part of the remainder of this elastic cord holds and is fitted on the syringe outer wall surface; it pulls strength and causes this ultrasonic transducer containment vessel to be close on the outer wall surface of syringe to hold the described elastic cord that is fitted on the syringe outer wall surface; this is close to the bottom of the contiguous syringe of its locations of structures of ultrasonic transducer containment vessel on the syringe outer wall surface; and the ultrasonic transducer containment vessel that elastic cord links together is to be easy to the independent assortment structural relation that mutually breaks away from together with the structural relation between its content itself and the syringe; its radiable ultrasonic frequency scope of this ultrasonic transducer is between 100KHz and 12MHz; and; higher-order of oscillation electric signal transmission cable, an end of this higher-order of oscillation electric signal transmission cable see through the ultrasonic transducer containment vessel and are connected with described ultrasonic transducer.
2. the PCBs wash-out device of the assisted and strengthened object desorb of physics according to claim 1 and mass transfer, it is characterized in that, the structure of this device comprises higher-order of oscillation electric signal generator, and the other end of described higher-order of oscillation electric signal transmission cable is connected with this higher-order of oscillation electric signal generator.
3. the PCBs wash-out device of the assisted and strengthened object desorb of physics according to claim 1 and mass transfer is characterized in that, its radiable ultrasonic frequency scope of this ultrasonic transducer is between 300KHz and 12MHz.
4. the PCBs wash-out device of the assisted and strengthened object desorb of physics according to claim 1 and mass transfer is characterized in that the aperture of this its filter membrane of syringe filter is between 0.05 micron and 1.00 microns.
5. the PCBs wash-out device of the assisted and strengthened object desorb of physics according to claim 1 and mass transfer is characterized in that, its material of this syringe is quartz glass material or stainless steel.
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| CN201210440070XA CN102967677A (en) | 2012-10-25 | 2012-10-25 | PCBs (Polychlorinated Biphenyls) elution device for intensifying target object desorption and mass transfer based on physical assistance |
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| CN201210440070XA CN102967677A (en) | 2012-10-25 | 2012-10-25 | PCBs (Polychlorinated Biphenyls) elution device for intensifying target object desorption and mass transfer based on physical assistance |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111422862A (en) * | 2020-05-12 | 2020-07-17 | 上海理工大学 | Method for separating graphene quantum dots by using molecular sieve |
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Application publication date: 20130313 |