CN102879255A - Electrically-driven solid phase micro-extraction method and device thereof - Google Patents
Electrically-driven solid phase micro-extraction method and device thereof Download PDFInfo
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Abstract
The invention relates to an electrically-driven solid phase micro-extraction method and a device thereof. An integrated porous material prepared through treating an epoxy resin as a base material, diethylenetriamine as a curing agent and polyethylene glycol as a pore forming agent and utilizing an in-situ gradual polymerization process is adopted as a solid phase micro-extraction material, the form of the solid phase micro-extraction material to prepare a solid micro-extraction column is combined with a rotation-speed-adjustable motor, a stirring effect is realized through rotation, and simultaneously the solid phase micro-extraction material which is adopted as an electrical adsorption work electrode and a platinum wire electrode which is adopted as a counter electrode are combined with a high-voltage direct current power supply to realize an electric adsorption effect in order to complete the electrically-driven solid phase micro-extraction. The electrically-driven solid phase micro-extraction method combining the electric adsorption technology with the stirring technology effectively overcomes a disadvantage that magnetic stirring cannot be used in a small-volume solution and simultaneously reduces a disadvantage that the abrasion of a solid phase micro-extraction stirring bar is easy, so the service life can be prolonged; the integrated epoxy resin based porous polymer is treated as the adsorption material, so the extraction amount and the detection sensitivity are improved. The method has the advantages of simplicity, easy operation and high flexibility.
Description
Technical field
The present invention relates to a kind of electricity and drive acceleration solid phase micro-extraction method and device thereof, is the Preconcentration and Separation technology of various analysis, belongs to the laboratory applications category.
Background technology
Solid-phase microextraction (the Solid-phase micro-extraction that integrates sampling, extraction, enrichment, separation, sample introduction, SPME) become one of important Sample Pretreatment Technique, Solid-Phase Extraction (Solid-phase extraction with routine, SPE) technology is compared and can be shortened more significantly the sample pretreatment time, thereby improves analysis efficiency.For example, a complete SPE process usually needs to spend 30-60 minute, and the SPME process then can be reduced to 10-30 minute.But when in the face of large batch of sample analysis task, particularly with respect to being that achievable large-scale instrument is measured process in a few minutes even a few second, the time that further shortens SPME is still significant.In addition, also there is the relatively not high deficiency of a loading capacity less, sensitivity for analysis in the SPME technology.Although the stir bar sorptive extraction technology of exploitation can the Effective Raise loading capacity afterwards, but still existed the defective that stirring rod is is easily worn and torn, the life-span is short.Therefore, how when guaranteeing serviceable life, the extraction quantity that improves target analytes is conducive to reduce detectability, improves sensitivity, also is an important problem.
Electric field-enhanced technology has some patented claims in the fields such as chemical industry and water treatment, such as: the human hairs such as Yang Xia understand " electric field strengthened heat transmission and heat exchange machine " (publication number: CN101358818), " electric field-enhanced ozone equipment for treating water " (patent No.: ZL02251073.7) of Liu Zhongyang invention, " a kind of electric field-enhanced method for rapidly concentrating by film and the device " of the people such as Wan Yinhua invention (publication number: CN101596406), " electric field-enhanced assemble method and the device of compound polyelectrolyte film " (publication number: CN101157010) of the people such as Zhang Guojun invention.A branch of electric field-enhanced technology is electric adsorption technology (Electrosorption Technology, EST), refers in the situation that be added with voltage but electrochemical reaction does not occur the adsorption process that occurs at electrode.The EST technology also has research more, for example, Huang Zhangyan has invented " electro-adsorption demineralization water purifier " (patent No.: ZL200720193459.3), " solid phase micro-extraction extraction head take the single armed carbon nano-tube as coating and preparation method thereof " (publication number: CN101306351) of the people such as Li Quanlong invention, " electro-adsorption reinforced activated carbon fiber solid phase micro-extraction method " of Jia Jin equality people invention (publication number: CN101294937), " electric field-enhanced hollow fiber membrane liquid-phase micro extraction technique and device " (publication number: CN101670190) of the high people's invention of Guo Yu.Above research work has all proved by apply effectively Accelerative mass transfer process of electric field at extraction process, has shortened extraction time.
At present, the electrode material that adopts in the electric adsorption technology is mainly porous conductive material: graphite, active carbon powder and NACF and modified active carbon fiber (Afkhami, A., Madrakian, T.; Amini, A.; Karimi, Z., Journal of Hazardous Materials, 2008,150,408-412; Huang, C.-C.; Su, Y.-J; Journal of Hazardous Materials, 2010,175,477-483; Park, S.-J.; Park, B.-J.; Ryu, S.-K..Carbon 1999, (37), 1223-1226; Swiatkowski, A.; Pakula, M.; Biniak, S.; Walczyk, M..Carbon, 2004,423057-3069), charcoal-aero gel (Gabelich, C.J., Tran, T.D., Suffet, I.H., Environmental Science and Technology 2002,36 (13), 3010-3019) etc.Because the good electrode material of this class electric conductivity has larger specific surface area, can provide electrostatic double layer as much as possible (to look into the woods that shakes, Yu Yixiong, Luo Yatian, Xu Shunhong, Lee analyse and, Sichuan chemical industry, 2005,8 (1), 52-55), (Alkire, the R.C. such as Alkire, Eisinger, R.S., Journal of the Electrochemical Society, 1983,130 (1), 85-93) proved that also the energy that stores in the electrostatic double layer is directly proportional with the amount of absorption, they have also proved energy and the bed sectional area of storing in the electrostatic double layer simultaneously, and length and electric potential difference are proportional.Therefore, by selecting suitable electrode material, not only extraction time can be shortened by applying electric field, adsorbance can also be increased simultaneously.
Although above-mentioned employee's card understands that applying electric field can accelerate the extraction rate of solid-phase microextraction and increase loading capacity, but still have following relative deficiency part: the electrostatic double layer major part of (1) porous electrode is not to form at electrode surface, but in the hole, form, and the thickness of the aperture of many porous electrodes and electrostatic double layer difference on the order of magnitude is not too large, when namely being equal to or less than 10nm, then again because the aperture is too little, cause the space that " eclipsing effects " (Yin Guangjun can occur, Chen Fuming, water technology, 2003,29 (2), 63-65) be unfavorable on the contrary the generation of electrostatic double layer.(2) existing electric sorbing material is mainly various C sills, and kind is single, is difficult to the sorption extraction of competent diversified target analytes.(3) apply voltage higher, it is faster that the rate of adsorption improves, and the voltage that applies in the existing electric adsorption process is many within several volts, has been subject to certain limitation for the raising of the rate of adsorption.(4) in the existing electricity absorption solid phase micro-extraction technique, also can be subject to certain limitation by using magnetic stirring apparatus that solution is stirred the method that improves mass transfer rate, particularly in the very little situation of liquor capacity, in addition, stir the damage that easily also easily causes the solid-phase micro-extraction fibre head with magneton.Based on the problems referred to above, develop a greater variety of porous electrode sorption extraction materials, increase voltage, conversion solution alr mode is a job very with practical value.
Summary of the invention
First technical matters to be solved by this invention provides a kind of electricity and drives solid phase micro-extraction method, improves adsorptive power and the speed of solid-phase microextraction, and then improves analysis efficiency and the detection sensitivity of solid-phase microextraction.
Second technical matters to be solved by this invention provides a kind of electricity and drives solid-phase micro-extracting device, improves adsorptive power and the speed of solid-phase microextraction, and then improves analysis efficiency and the detection sensitivity of solid-phase microextraction.
The present invention solves the technical scheme that above-mentioned first technical matters adopts: a kind of electricity drives solid phase micro-extraction method, it is characterized in that adopting with tinsel as the solid-phase microextraction post of inner core preparation as working electrode, with platinum electrode as to electrode, solid-phase microextraction post and platinum electrode are immersed in the sample solution, but the tinsel in the solid-phase microextraction post is connected on the motor of adjusting rotary speed, realize the rotation of solid-phase microextraction post by motor, be connected respectively to the tinsel in the solid-phase microextraction post and platinum electrode on two terminals can regulating direct supply by wire simultaneously, realize electric suction-operated by the electric field that produces, and the coating sorbing material of described solid-phase microextraction post is to adopt the epoxy resin-matrix porous polymer, thereby make the voltage of direct supply between 10V～30KV, after solid-phase microextraction finishes, disable motor also disconnects direct supply, take out the solid-phase microextraction post, carry out subsequent treatment.
As preferably, the rotational speed of described motor is at 1～600rpm, the control Faradaic current in 1mA, extraction time 1～60 minute.
As improvement, the coating sorbing material of described solid-phase microextraction post is as matrix material take epoxy resin, diethylenetriamine is hardening agent, polyglycol is that pore-foaming agent utilizes the progressively monoblock type epoxy resin-matrix porous polymer for preparing of polymerization of original position, wherein the mass ratio of epoxy resin, diethylenetriamine and polyglycol is 4: 0.5～1.5: 6～10, and the coating thickness of described solid-phase microextraction post is 0.01～0.5mm.
As improvement, described tinsel adopts to have electric conductivity and has certain physical strength and the material of stability, comprise stainless steel wire, copper wire, iron wire or platinum filament, described diameter wiry is at 0.2～2.0mm, length is between 1.0～20cm, and after the metal-wire cleaning drying at the glue-line of surface parcel skim 0.01～0.5mm or the wall thickness that is nested with one deck and mates with selected wire diameter 0.01～0.5mm kapillary, tinsel is sealed for subsequent use.
Improve again, the preparation process of described solid-phase microextraction post is: heat first the polyglycol fusing, add the epoxy resin mixing, add again diethylenetriamine after the cooling, be poured in the container behind the mixing, aforementioned treated tinsel is dipped vertically in the reaction liquid, reserve one section outside reactant liquor, 50-100 ℃ of reaction 16-30h after the sealing, polymerization is finished after washing and is removed pore-foaming agent and place deionized water for subsequent use, and obtaining coating thickness is the solid-phase microextraction post of 0.01～0.5mm, and the epoxide equivalent value of described epoxy resin is 0.43～0.47, the preferred E-44 of described epoxy resin, described polyglycol are PEG1000～2000.
Improve, described control Faradaic current is realized with interior by the following method at 1mA again: access one adjustable rheostat between wire and direct supply; Perhaps platinum electrode is inserted an other container that buffer solution is housed, and be connected to form conductive path with sample solution by salt bridge; Perhaps salt bridge replaces with the kapillary that is full of buffer solution, controls Faradaic current in 1mA by regulating capillary diameter and length and buffer solution.
Further improve, be provided with a magnetic stir bar in the described sample solution, control stirring rate at 1～600rpm by the magnetic stirring apparatus that is placed on container bottom.
Further preferred, the rotational speed 300～500rpm of described motor, supply voltage are at 50～500V, and the control Faradaic current is at 0.01～0.1mA, and extraction time was at 5～15 minutes.
Described subsequent treatment is: after stopping extraction, change corresponding desorbed solution according to the characteristic of target analytes, apply identical rotational speed and the electric field opposite with when extraction resolved, 1～30 minute parsing time, desorbed solution detects with analytical instrument.
At last, the stirring rate of described magnetic stir bar is preferably 300～500rpm.
The present invention solves the technical scheme that above-mentioned second technical matters adopt: a kind of electricity drives solid-phase micro-extracting device, the container and the working electrode that comprise load sample solution, to electrode, it is characterized in that described working electrode adopts with the solid-phase microextraction post of tinsel as the inner core preparation, and the coating sorbing material of solid-phase microextraction post is to adopt the epoxy resin-matrix porous polymer, be platinum electrode to electrode, described solid-phase microextraction post and platinum electrode immerse in the sample solution, tinsel in the described solid-phase microextraction post and platinum electrode are wired to respectively on two terminals can regulating high-voltage DC power supply, but the tinsel in the described solid-phase microextraction post of while is connected with the motor of adjusting rotary speed.
Or,
A kind of electricity drives solid-phase micro-extracting device, the container and the working electrode that comprise load sample solution, to electrode, it is characterized in that described working electrode adopts with the solid-phase microextraction post of tinsel as the inner core preparation, and the coating sorbing material of solid-phase microextraction post is to adopt the epoxy resin-matrix porous polymer, be platinum electrode to electrode, described solid-phase microextraction post immerses in the sample solution, described platinum electrode immerses in the buffer solution, described buffer solution and sample solution are connected to form conductive path by salt bridge, tinsel in the described solid-phase microextraction post and platinum electrode are wired to respectively on two terminals can regulating high-voltage DC power supply, but the tinsel in the described solid-phase microextraction post of while is connected with the motor of adjusting rotary speed.
As improvement, the sorbing material of described solid-phase microextraction post is as matrix material take epoxy resin, diethylenetriamine is hardening agent, polyglycol is pore-foaming agent, be 4: 0.5～1.5: 6～10 to prepare the monoblock type epoxy resin-matrix porous polymer that obtains in mass ratio with epoxy resin, diethylenetriamine and polyglycol, the coating thickness of described solid-phase microextraction post is 0.01～0.5mm.
Improve, described tinsel adopts to have electric conductivity and has certain physical strength and the material of stability, comprises stainless steel wire, copper wire, iron wire or platinum filament again, and described diameter wiry is at 0.2～2.0mm, and length is between 1.0～20cm.
Further improve, the rotational speed of described motor is at 1～600rpm, and the voltage of direct supply is at 1～30KV.
At last, described electricity drives solid-phase micro-extracting device and also comprises magnetic stir bar and magnetic stirring apparatus, and described magnetic stir bar is arranged in the sample solution, and described magnetic stirring apparatus is supported in container bottom, and the rotation of control magnetic stir bar.
Compared with prior art, the invention has the advantages that:
(1) electric adsorption technology and stirring technique are united two into one forms electricity and drive mode of operation, by with the motor coupling solid-phase microextraction post can being rotated, carrying out finishing stirring when electricity adsorbs in solution example.Effectively overcome the shortcoming that in small size solution, is difficult to use magnetic agitation, reduced simultaneously the shortcoming that the solid-phase microextraction post is easy to wear and tear, thereby can increase the service life.
(2) develop a kind of Novel electric sorbing material---monoblock type epoxy resin-matrix porous polymer, having broken through existing electric sorbing material all is restrictions of hole, C Quito material (activated charcoal, carbon fiber, carbon nano-tube, carbon aerogels etc.).When adopting this electric sorbing material simultaneously, apply voltage and also can bring up to tens to hundreds of volts from several volts, be conducive to further utilize the efficient of high electric field acceleration mass transfer.In addition, monoblock type epoxy resin-matrix porous polymer has the larger fixing characteristics that extract mutually volume and the distribution of micron/nano diplopore, can either overcome the space " eclipsing effects " that on the common porous electrode because aperture causes, can have larger loading capacity again, and then improve analyzing and testing sensitivity.
(3) preparation method is easy, easily operation, and dirigibility is high, is easy to assemble according to actual needs and adjust, and adapts to the extraction testing requirement of more actual samples and target analytes.For example: the large or larger sample of target molecule volume for viscosity can apply simultaneously self rotating of outside magnetic agitation and solid-phase microextraction post, otherwise can apply a kind of alr mode even adopt the static extracting pattern; For the solution of high conductivity, in order to reduce or to suppress Faradaic current and can adopt salt bridge to consist of path.
The present invention is under the jurisdiction of the concentration and separation technology in the sample pre-treatments, can be widely used in the actual sample analyzing and testing in the fields such as environmental monitoring, food security, medical and health, has stronger actual application value.
Description of drawings
Fig. 1 (a), Fig. 1 (b) are solid-phase microextraction post of the present invention and cross-sectional structure figure;
Fig. 2 (a), (b), (c) show respectively be the fixedly phase monoblock type material of solid-phase microextraction post in enlargement factor 5000,10000,20000 o'clock scanning electron microscope diagram;
Fig. 3 A, 3B are the structural representations that electricity of the present invention drives solid-phase micro-extracting device, and A is for using outside magnetic stirring apparatus but do not use the device of salt bridge; B is for using salt bridge but do not use the device of outside magnetic stirring apparatus, and wherein 1 is motor, and 2 is tinsel, and 3 is the solid-phase microextraction post, the 4th, sample solution, 5 is container, and 6 is stirring parts, and 7 is magnetic stirring apparatus, 8 is high-voltage DC power supply, and 9 is platinum electrode, and 10 is salt bridge, and 11 is buffer solution;
Fig. 4 be among the embodiment 2 voltage on the impact of cupric ion adsorption.
Embodiment
Embodiment is described in further detail the present invention below in conjunction with accompanying drawing.
Preparation Example 1
1) pre-service of tinsel 2: get one section stainless steel wire (30mm * 1.2mm i.d.) and clean up, drying is coated with skim with commercially available epoxy resin tackifier later, and is rear for subsequent use until solidifying fully.
2) preparation of solid-phase microextraction post 3: get 4.0g PEG-1540 heating and make its fusing, add 2.0g epoxy resin mixing 2min, add again the 0.5g diethylenetriamine after being cooled to room temperature, obtain homogeneous through the abundant mixing of 2min, transparent thick liquid, it is poured into (polypropylene material in the disposable syringe of 1mL, bore is 5mm approximately), filling liquid length is 10～15mm approximately, with aforesaid treated stainless steel wire 2 be dipped vertically into reaction liquid in, reserve one section outside reactant liquor, sealing is placed in 60 ℃ of baking ovens reacts 24h, and the solid-phase microextraction post 3 for preparing is taken out from container.
3) aftertreatment of solid-phase microextraction post 3: solid-phase microextraction post 3 cyclic washing in 40 ℃ of deionized waters of the polymerization that step (2) is obtained, to removing pore-foaming agent fully, and press required size and excise unnecessary part, obtain epoxy resin base polyalcohol integral formula material and be the fixing sorption extraction stirring rod of phase, solid-phase microextraction post 3 pictorial diagram and structural representation thereof are seen Fig. 1; The electron scanning micrograph of sorbing material is seen Fig. 2.
Application Example 2
Preparation copper ion standard solution, regulating pH=6 is placed in the small beaker, insert the solid-phase microextraction post 3 by embodiment 1 preparation, connect experimental provision by Fig. 3 (A), solid-phase microextraction post 3 is as negative pole, platinum electrode 9 is done anodal, connects high-voltage DC power supply 8, regulates the rotating speed 500rmin of magnetic stirring apparatus 7 under room temperature
-1Lower sorption extraction 20min takes out solid-phase microextraction post 3, with the HNO of 2mL 5%
3Resolve 10min, eluent intermediate ion concentration is measured with atomic emission spectrum (ICP-AES), measures wavelength and selects 327.393nm.
When Fig. 4 is control same current (1mA), apply different magnitudes of voltage to the impact of adsorption efficiency.As can be seen from Fig., in the situation that other conditions are identical, added negative potential is higher on the electrode, and its adsorbance is also just larger, and adsorption efficiency is also higher.By the actual sample mark-on is tested, recovery of standard addition is between 95%-105%, and the relative standard deviation of repeated experiments is less than 8%.
Application Example 3
Preparation saccharin sodium standard solution, regulating pH=6 is placed in the small beaker, insert the solid-phase microextraction post 3 by embodiment 1 preparation, connect experimental provision by Fig. 3 (B), salt bridge 10 adopts commercially available agar-saturated KCl glass salt bridge, and solid-phase microextraction post 3 is as anodal, and platinum electrode 9 is made negative pole, connect high-voltage DC power supply 8 regulation voltages to 300V, the rotating speed of regulating electric machine 1 is 200rmin
-1, sorption extraction 10min under room temperature takes out solid-phase microextraction post 3, with 2mL 0.03mol/L Na
2CO
3Resolve 15min with the mixed liquor (volume ratio is 90: 10) of methyl alcohol, eluent carries out analyzing and testing with molecular fluorescence photometer (excitation wavelength 270nm, emission wavelength 470nm).Experimental result shows, the method can be used for the analyzing and testing of organic molecule.The recovery of standard addition of actual sample is more than 90%.
Can obtain electricity of the present invention from above embodiment and drive solid phase micro-extraction method, easily operation, dirigibility is high, be easy to assemble according to actual needs and adjust, the extraction testing requirement that adapts to more actual samples and target analytes, the actual sample analyzing and testing that can be widely used in the fields such as environmental monitoring, food security, medical and health, extraction quantity is large simultaneously, and the recovery of standard addition of sample is high.
Claims (11)
1. an electricity drives solid phase micro-extraction method, it is characterized in that adopting with tinsel as the solid-phase microextraction post of inner core preparation as working electrode, with platinum electrode as to electrode, solid-phase microextraction post and platinum electrode are immersed in the sample solution, but the tinsel in the solid-phase microextraction post is connected on the motor of adjusting rotary speed, realize the rotation of solid-phase microextraction post by motor, be connected respectively to the tinsel in the solid-phase microextraction post and platinum electrode on two terminals can regulating direct supply by wire simultaneously, realize electric suction-operated by the electric field that produces, and the coating sorbing material of described solid-phase microextraction post is to adopt the epoxy resin-matrix porous polymer, thereby make the voltage of direct supply between 10V～30KV, after solid-phase microextraction finishes, disable motor also disconnects direct supply, take out the solid-phase microextraction post, carry out subsequent treatment.
2. electricity according to claim 1 drives solid phase micro-extraction method, it is characterized in that the rotational speed of described motor at 1～600rpm, controls Faradaic current in 1mA, extraction time 1～60 minute.
3. electricity according to claim 1 and 2 drives solid phase micro-extraction method, the coating sorbing material that it is characterized in that described solid-phase microextraction post is as matrix material take epoxy resin, diethylenetriamine is hardening agent, polyglycol is that pore-foaming agent utilizes the progressively monoblock type epoxy resin-matrix porous polymer for preparing of polymerization of original position, wherein the mass ratio of epoxy resin, diethylenetriamine and polyglycol is 4: 0.5～1.5: 6～10, and the coating thickness of described solid-phase microextraction post is 0.01～0.5mm.
4. electricity according to claim 1 and 2 drives solid phase micro-extraction method, it is characterized in that described tinsel adopts stainless steel wire, copper wire, iron wire or platinum filament, described diameter wiry is at 0.2～2.0mm, length is between 1.0～20cm, and after the metal-wire cleaning drying at the glue-line of surface parcel skim 0.01～0.5mm or the wall thickness that is nested with one deck and mates with selected wire diameter at the kapillary of 0.01～0.5mm, tinsel is sealed for subsequent use.
5. electricity according to claim 3 drives solid phase micro-extraction method, the preparation process that it is characterized in that described solid-phase microextraction post is: heat first the polyglycol fusing, add the epoxy resin mixing, add again diethylenetriamine after the cooling, be poured in the container behind the mixing, aforementioned treated tinsel is dipped vertically in the reaction liquid, reserve one section outside reactant liquor, 50-100 ℃ of reaction 16-30h after the sealing, polymerization is finished after washing and is removed pore-foaming agent and place deionized water for subsequent use, and obtaining coating thickness is the solid-phase microextraction post of 0.01～0.5mm.
6. electricity according to claim 1 and 2 drives solid phase micro-extraction method, it is characterized in that described control Faradaic current realizes with interior by the following method at 1mA: access one adjustable rheostat between wire and direct supply; Perhaps platinum electrode is inserted an other container that buffer solution is housed, and be connected to form conductive path with sample solution by salt bridge; Perhaps salt bridge replaces with the kapillary that is full of buffer solution, controls Faradaic current in 1mA by regulating capillary diameter and length and buffer solution.
7. electricity according to claim 2 drives solid phase micro-extraction method, it is characterized in that the rotational speed 300～500rpm of described motor, and supply voltage is at 50～500V, and the control Faradaic current is at 0.01～0.1mA, and extraction time was at 5～15 minutes.
8. electricity according to claim 1 drives solid phase micro-extraction method, it is characterized in that described subsequent treatment is: after stopping extraction, change corresponding desorbed solution according to the characteristic of target analytes, apply identical rotational speed and the electric field opposite with when extraction resolved, 1～30 minute parsing time, desorbed solution detects with analytical instrument.
9. an electricity drives solid-phase micro-extracting device, the container and the working electrode that comprise load sample solution, to electrode, it is characterized in that described working electrode adopts with the solid-phase microextraction post of tinsel as the inner core preparation, and the coating sorbing material of solid-phase microextraction post is to adopt the epoxy resin-matrix porous polymer, be platinum electrode to electrode, described solid-phase microextraction post and platinum electrode immerse in the sample solution, tinsel in the described solid-phase microextraction post and platinum electrode are wired to respectively on two terminals can regulating direct supply, but the tinsel in the described solid-phase microextraction post of while is connected with the motor of adjusting rotary speed;
Or, the container and the working electrode that comprise load sample solution, to electrode, it is characterized in that described working electrode adopts with the solid-phase microextraction post of tinsel as the inner core preparation, and the coating sorbing material of solid-phase microextraction post is to adopt the epoxy resin-matrix porous polymer, be platinum electrode to electrode, described solid-phase microextraction post immerses in the sample solution, described platinum electrode immerses in the buffer solution, described buffer solution and sample solution are connected to form conductive path by salt bridge, tinsel in the described solid-phase microextraction post and platinum electrode are wired to respectively on two terminals can regulating direct supply, but the tinsel in the described solid-phase microextraction post of while is connected with the motor of adjusting rotary speed.
10. electricity according to claim 9 drives solid-phase micro-extracting device, the sorbing material that it is characterized in that described solid-phase microextraction post is as matrix material take epoxy resin, diethylenetriamine is hardening agent, polyglycol is pore-foaming agent, be 4: 0.5～1.5: 6～10 to prepare the monoblock type epoxy resin-matrix porous polymer that obtains in mass ratio with epoxy resin, diethylenetriamine and polyglycol, the coating thickness of described solid-phase microextraction post is 0.01～0.5mm.
11. electricity according to claim 9 drives solid-phase micro-extracting device, it is characterized in that described tinsel adopts stainless steel wire, copper wire, iron wire or platinum filament, described diameter wiry is at 0.2～2.0mm, and length is between 1.0～20cm.
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| CN103245532A (en) * | 2013-04-23 | 2013-08-14 | 上海市刑事科学技术研究院 | Scene sampler for toxicants in water body and using method |
| CN103463833A (en) * | 2013-10-03 | 2013-12-25 | 中华人民共和国济宁出入境检验检疫局 | Stirring rod adsorptive extraction device |
| CN103616275A (en) * | 2013-12-09 | 2014-03-05 | 嘉兴市产品质量监督检验所 | Trace metal ion electric concentration sample treatment method and trace metal ion electric concentration sample treatment device |
| CN103616275B (en) * | 2013-12-09 | 2016-01-20 | 嘉兴市产品质量监督检验所 | A kind of trace metal ion electricity enriched sample disposal route and device thereof |
| CN104266890A (en) * | 2014-10-17 | 2015-01-07 | 太原理工大学 | Method for quickly extracting composite educt from heat-resisting austenitic stainless steel at normal temperature |
| US10324012B2 (en) | 2015-08-20 | 2019-06-18 | King Fahd University Of Petroleum And Minerals | Method for detecting and quantifying haloether contamination in aqueous samples by flow assisted electro-enhanced solid-phase microextraction |
| US10466148B2 (en) | 2015-08-20 | 2019-11-05 | King Fahd University Of Petroleum And Minerals | Use of platinum wire electrode and synthetic fiber for flow assisted electro-enhanced solid phase microextraction |
| US10429282B2 (en) | 2015-08-20 | 2019-10-01 | King Fahd University Of Petroleum And Minerals | Detection of organic halide compounds using close loop flow assisted electro-enhanced solid-phase microextraction |
| CN106237653A (en) * | 2016-08-16 | 2016-12-21 | 福州大学 | Hand-held is from ultrasound wave solid-phase microextraction rod and using method thereof |
| CN106237653B (en) * | 2016-08-16 | 2018-05-04 | 福州大学 | Hand-held is from ultrasonic wave solid phase microextraction rod and its application method |
| CN106902772A (en) * | 2017-03-29 | 2017-06-30 | 青岛贞正分析仪器有限公司 | Novel chelate resin solid-phase extraction muddler and preparation method thereof |
| CN106902772B (en) * | 2017-03-29 | 2019-10-18 | 青岛贞正分析仪器有限公司 | Chelating resin solid-phase extraction muddler and preparation method thereof |
| CN107589186A (en) * | 2017-08-30 | 2018-01-16 | 浙江清华长三角研究院 | One kind power-up membrane extraction device and its application method |
| CN108355378A (en) * | 2018-02-08 | 2018-08-03 | 云南警官学院 | A kind of head space microcirculation solid-phase micro-extracting device |
| CN108760425A (en) * | 2018-05-30 | 2018-11-06 | 重庆第二师范学院 | A kind of graphite oxide alkenyl pretreating device and its application in food inspection |
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