CN104215497A - Experimental device and method for extracting polycyclic aromatic hydrocarbons in enriched seawater - Google Patents
Experimental device and method for extracting polycyclic aromatic hydrocarbons in enriched seawater Download PDFInfo
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- CN104215497A CN104215497A CN201410480174.2A CN201410480174A CN104215497A CN 104215497 A CN104215497 A CN 104215497A CN 201410480174 A CN201410480174 A CN 201410480174A CN 104215497 A CN104215497 A CN 104215497A
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Abstract
The invention discloses an experimental device and method for extracting polycyclic aromatic hydrocarbons in enriched seawater. The experimental device comprises a vortex instrument, a magnetic extraction part, motors and mechanical arms, wherein a bearing table for bearing a sample container is formed above the vortex instrument; a magnet column and a glass sleeve of which the lower part is sealed are arranged in the magnetic extraction part; the magnet column stretches into the glass sleeve; the number of the motors is two; the mechanical arms are rotary telescopic mechanical arms, and totally two groups of mechanical arms are arranged; and the mechanical arms are driven by the motors to drive the magnet column and the glass sleeve to move up and down. The experimental device disclosed by the invention is high in degree of automation, high in working efficiency and high in stability and can provide reliable monitoring, prevention and control means for environmental protection and sudden disaster warning. The polycyclic aromatic hydrocarbon enrichment method provided on the experimental device is rapid, high-efficiency and high in timeliness, the field analysis capacity of marine environmental pollution is improved, and possible potential contamination and target transformation loss existing in the whole sampling and analyzing process are avoided.
Description
Technical field
The invention belongs to ocean monitoring technologytechnologies field, specifically, the extraction and enrichment method of Polynuclear Aromatic Hydrocarbons In Seawater relating to a kind of experimental provision for carrying out extracting and enriching to the palycyclic aromatic in seawater and propose based on described experimental provision.
Background technology
Palycyclic aromatic (Polycyclic Aromatic Hydrocarbons, PAHs) and derivant thereof are the important persistence organic pollutants (Persistent Organic Pollutants, POPs) of a class.Although PAHs absolute content is very low in ocean, due to its " three-induced effect " and bioaccumulation, to human health and the marine eco-environment, all there is huge potential hazard.1979 Environmental Protection Agency (Environmental Protection Agency, EPA) just 16 kinds of PAHs compounds are classified as the most serious organic contaminant.
Content in view of phosphorus AHs does not reach the detection limit of existing analytical instrument, and therefore sample needs the extraction concentration through complexity before testing, and this also becomes the bottleneck of PAHs analytical approach development.Conventional pretreatment process (liquid-liquid extraction (LLE), Solid-Phase Extraction (SPE)) consumes the time of whole analytic process 70-80%, there is larger time stickiness, and " contamination " problem in sampling and storage and transport process is difficult to overcome completely, therefore be difficult to reflect pollution level in real time, comprehensively, truly, use a large amount of organic solvent simultaneously, easily secondary pollution is caused to environment.
Along with the raising of scientific and technological level and environmental requirement, micro-extraction technique has had significant progress.Dispersive liquid-liquid microextraction (DLLME) technology have simple to operate, extraction equilibrium can be reached fast and the advantage such as consumption of organic solvent is few, but extractant needs to use density ratio water large and water-fast organic solvent; If select the solvent that density ratio water is little, then shift difficulty after extraction, this just becomes the bottleneck of the method development and application.And magnetic abstraction technique is simple to operate, analysis time is short, adsorption efficiency is high, desorption rate is fast, especially utilize magnetic fields, can quickly and easily extraction solvent is separated with sample solution and shift.If the characteristics and advantages of magnetic abstraction technique can be made full use of, make up the restriction of the extractant scope of application in DLLME technology and the shortcoming of transfer difficulty, a larger breakthrough will be realized in rapid extraction technology.
Summary of the invention
The object of the present invention is to provide a kind of experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater, extraction and enrichment fast can be realized to palycyclic aromatic in seawater sample, simple to operate, automaticity is high.
For solving the problems of the technologies described above, the present invention is achieved by the following technical solutions:
For an experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater, comprise vortex instrument, magnetic extraction portion, motor and mechanical arm; The plummer for carrying sampling receptacle is formed above described vortex instrument; In described magnetic extraction portion, be provided with the glass bushing of magnetic column and bottom sealing, described magnetic column extend in glass bushing; Described motor is provided with two, described mechanical arm is rotary and telescopic mechanical arm and is provided with two groups, wherein, first group of mechanical arm is connected between First motor and described glass bushing, First motor, by driving first group of mechanical arm rotary extension, stretches into drive glass bushing or shifts out described sampling receptacle; Second group of mechanical arm is connected to second between motor and magnetic column, and second motor, by driving second group of mechanical arm rotary extension, stretches into drive magnetic column or shift out described glass bushing.
Conveniently the installation of motor is laid, and described motor is supported on the top of vortex instrument by support, and the axis direction level of machine shaft; Described mechanical arm comprises the horizontal arm be connected with machine shaft and the vertical arm be connected with magnetic column or glass bushing, reversing arrangement is provided with between horizontal arm and vertical arm, be vertical arm rotation around vertical axis by horizontal arm around the rotational transform of horizontal axis by reversing arrangement, in described mechanical arm, only vertical arm is rotary and telescopic arm.
In order to carry out spacing to described sampling receptacle, avoid the vortex of vortex instrument to vibrate cause sampling receptacle to be toppled over or be shifted, the present invention is buckled with a case in the outer cup of described vortex instrument, the end face of case offers an opening, and the size of opening size and sampling receptacle is suitable, described sampling receptacle is just placed on the end face of vortex instrument through described opening.Thus, the end face of vortex instrument and the end face of case and opening thereof is utilized just to define the plummer with spacing base.
Conveniently sampling receptacle picking and placeing on plummer, is preferably supported on the top of described case by support by described motor, and is positioned at the position, corner of case; The side of described case is provided with guidance panel, the motor described in described guidance panel is connected by control circuit, controls motor and run.
In order to avoid seawater sample, in extraction experiments process, light degradation occurs, the precision of experimental result is caused to reduce, when choosing described sampling receptacle, preferably select the glass container with shading characteristic, such as brown glass container or outer wall are coated with the colorless glass container etc. of opaque medium.
In order to increase the magnetic pole adsorption area of magnetic column, described magnetic column preferably adopts and is formed by connecting by multiple button-shaped permanent magnet cross arrangement not of uniform size.
Based on the above-mentioned experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater, present invention also offers a kind of palycyclic aromatic extraction and enrichment method adopting described experimental provision to design, comprise the following steps:
A, sampling receptacle is placed on plummer, in sampling receptacle, adds a certain amount of seawater sample;
B, in sampling receptacle, add extractant and spreading agent, form emulsion fluid, open vortex instrument and make emulsion fluid vortex, until reach extraction equilibrium;
C, in sampling receptacle, add magnetic spe medium, vortex, after reaching adsorption equilibrium, close vortex instrument;
D, startup two motor in synchrony rotate forward, the magnetic portion of extraction is extend in sampling receptacle, utilizes magnetic column to be adsorbed on the tube wall of glass bushing, after upon adsorption by magnetic spe medium, start two motor in synchrony reversions, magnetic is extracted portion and shifts out from sampling receptacle;
E, change sampling receptacle, and add eluting solvent in sampling receptacle after replacing, then start two motor in synchrony and rotate forward, the magnetic portion of extraction is extend in the sampling receptacle after described replacing;
F, startup second motor reversal, shift out magnetic column, make magnetic spe medium be shed in eluting solvent from glass bushing from glass bushing, starts the vortex dispersion again of vortex instrument;
G, closedown vortex instrument, start second motor and rotate forward, stretched into by magnetic column in glass bushing, attract magnetic spe medium to be adsorbed onto on the tube wall of glass bushing;
H, startup two motor reversals, the portion that extracted by magnetic shifts out from the sampling receptacle after described replacing; Now, the solution in the sampling receptacle after replacing is solution to be measured, completes the extraction process to palycyclic aromatic in described seawater sample.
Preferably, described extractant preferably adopts octanol, and the volume ratio of described octanol and seawater sample is 1:2500-3000; Described spreading agent preferably adopts acetone, and the volume ratio of described acetone and seawater sample is 1:25-30; Described eluting solvent preferably adopts acetonitrile, and the volume ratio of described acetonitrile and seawater sample is 1:500-1000.
Preferably, described magnetic spe medium is magnetic nano-particle, and the preparation method of described magnetic nano-particle is:
Get ferric chloride hexahydrate, ethylene glycol, sodium acetate, polyglycol mix, react in a kettle., after terminating, be cooled to room temperature, obtain magnetic nano-particle through centrifuging, then divide three washing magnetic nano-particles, after drying with ethanol, be placed in crucible and calcine, carry out drying process;
Carry out surface-functionalized to magnetic nano-particle: take the magnetic nano-particle of above-mentioned drying, octadecyl trichlorosilane alkane, solvent toluene fully stir in a nitrogen atmosphere, proceed to reaction kettle for reaction again, after cooling product is used toluene, washed with methanol successively, afterwards 40 DEG C of dryings again.
Further, in described step a, again join in described sampling receptacle, to improve the accuracy of detection after the glass fiber filter being 0.45 μm filters by described seawater sample use aperture.
Compared with prior art, advantage of the present invention and good effect are: the present invention is specially for the palycyclic aromatic design extracting and enriching experimental provision that content in seawater is less, can the extract and separate of realize target pollutant and the full-automation of the whole process of enrichment, be particularly suitable for the extracting and enriching of palycyclic aromatic in batch seawater sample.Compared to traditional hand sample preprocess method, this device can reach better accuracy and reappearance, significantly improve the efficiency of pre-treatment, eliminate manually-operated error, make the chance of experimenter's contact target pollutant and organic solvent greatly reduce simultaneously, and then make the security of pretreatment process higher.Extracting and enriching experimental provision of the present invention has high-level efficiency, high automation degree, high stability, the feature such as portable, easy to operate, has both saved the time, and has again reduced cost, and can monitor preventions reliably for environmental protection and burst fire-disaster early warning provide.The palycyclic aromatic extraction and enrichment method that this experimental provision proposes is simple, quick, efficient, by force ageing, substantially increase the on-the site analysis ability of marine environmental pollution, effectively reduce transport retain costs, simultaneously, avoid from sampling the potential contamination and object conversion loss analyzing and may exist whole process, there is stronger practicality.
After reading the detailed description of embodiment of the present invention by reference to the accompanying drawings, the other features and advantages of the invention will become clearly.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of embodiment of the experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater proposed by the invention;
Fig. 2 is the structural representation of a kind of embodiment in magnetic extraction portion in Fig. 1;
Fig. 3 is the workflow diagram of a kind of embodiment of palycyclic aromatic extraction and enrichment method proposed by the invention;
Fig. 4 is in the extracting and enriching process of palycyclic aromatic, the motion process schematic diagram in magnetic extraction portion.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.
The present embodiment is in order to accelerate the extracting and enriching speed of Polynuclear Aromatic Hydrocarbons In Seawater, improve the processing flux of sample, the problems such as the pollution avoiding water sample potential in transportation and character change, propose a kind of method adopting palycyclic aromatic in magnetic extracting process enriching seawater, by adopting the palycyclic aromatic in magnetic spe medium adsorbing seawater sample, to realize Rapid Extraction to it and enrichment.
For realizing above-mentioned purpose of design, first the present embodiment devises a kind of experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater, to realize the robotization of extracting and enriching process.
Shown in Figure 1, the experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater (hereinafter referred to as experimental provision) of the present embodiment is primarily of part compositions such as vortex instrument 1, plummer 3, sampling receptacle 4, magnetic extraction portion 5, mechanical arm 6 and motors 7.Wherein, vortex instrument 1 can select at present matured product on the market, also can designed, designed as required.In the present embodiment, preferably adopt working method to be circumference concussion, and concussion rotating speed is the vortex instrument of 500 ~ 2500rpm, to meet the extracting and enriching requirement of palycyclic aromatic.Certainly, also can on experimental provision design operation panel 2, changed the concussion rotating speed of vortex instrument 1 by control circuit, to meet the vortex demand of different experiments.
Above vortex instrument 1, form plummer 3, described plummer 3 is for carrying sampling receptacle 4.In order to realize the spacing of plummer 3 pairs of sampling receptacles 4, avoiding sampling receptacle 4 to topple in vortex process or the problem such as displacement, preferably on plummer 3, designing spacing base 10.As a kind of preferred design of described plummer 3, the present embodiment designs a case 8 in the outside of vortex instrument 1, at the end face of case 8, an opening 9 is set, the size designing the size of described opening 9 and sampling receptacle 4 is suitable, namely the size of opening 9 should slightly larger than the size of sampling receptacle 4, ensureing that the bottom of sampling receptacle 4 can pass through opening 9 and be placed on the basis of the end face of vortex instrument 1, limit the horizontal shift of sampling receptacle 4 as much as possible.Between the end face and the end face of vortex instrument 1 of case 8, form certain difference in height, described difference in height, more preferably greater than 3cm, just can form the plummer 3 that has spacing base 10 thus.
Because described experimental provision is used for extraction and the enrichment of palycyclic aromatic, in order to avoid the seawater sample containing palycyclic aromatic, in experimentation, light degradation occurs, the present embodiment is when selecting described sampling receptacle 4, preferred employing has the glass container of shading characteristic, and such as brown glass container or outer wall are coated with the colorless glass container etc. of opaque medium (as tinfoil).
Motor 7 is placed in the top of vortex instrument 1, conveniently sampling receptacle 4 picking and placeing on plummer 3, preferably selects the position of a corner to hold up a support 11 at the end face of case 8, motor 7 is arranged on the top of support 11, and machine shaft in horizontal direction, for junctor mechanical arm 6.In the present embodiment, described mechanical arm 6 is provided with two groups, in order to realize the independent driving to two groups of mechanical arms 6, described motor 7 is provided with two, a motor 6 drives one group of mechanical arm 6 to rotate, and by mechanical arm 6 is designed to rotary and telescopic structure, is elevated to drive magnetic extraction portion 5.
The conveniently absorption of magnetic spe medium and disengaging, the present embodiment is provided with magnetic column 5-1 and glass bushing 5-2 two parts in described magnetic extraction portion 5, shown in composition graphs 1, Fig. 2.Wherein, glass bushing 5-2 is bottom sealing, open-topped transparent hollow tube, and the position closing on top at glass bushing 5-2 is provided with pipe clamp 5-3, and pipe clamp 5-3 connects first group of mechanical arm 6-1, is connected the rotating shaft of First motor 7 by first group of mechanical arm 6-1.Extend into by magnetic column 5-1 in glass bushing 5-2, the top of magnetic column 5-1 connects second group of mechanical arm 6-2, is connected the rotating shaft of second motor 7 by second group of mechanical arm 6-2.
In order to the rotating shaft of motor 7 is become mechanical arm 6 elevating movement vertically around the rotational transform of horizontal direction axis, the present embodiment is provided with a horizontal arm and a vertical arm, see Fig. 1 in each group mechanical arm 6-1,6-2.Horizontal arm is connected the rotating shaft of motor 7, vertical arm connects magnetic column 5-1 or glass bushing 5-2, installs reversing arrangement, such as tumbler gear or cross balladeur train etc. between horizontal arm and vertical arm.When the axis of rotation of motor 7, horizontal arm is driven to rotate around the axis of horizontal direction, by reversing arrangement, described rotation is passed to vertical arm, and reversing arrangement Rotation With Changing to effect under, become vertical arm around the rotation of vertical direction axis around the rotational transform of horizontal direction axis horizontal arm.Described vertical arm is designed to rotary and telescopic structure, by driving vertical arm clockwise or rotate counterclockwise, control vertical arm extend or shorten, and then utilize the flexible glass bushing 5-2 that drives of vertical arm to stretch into or shift out sampling receptacle 4, or magnetic column 5-1 is driven to stretch into or shift out described glass bushing 5-2.
In the present embodiment, in order to increase the magnetic pole adsorption area of magnetic column 5-1, button-shaped permanent magnet cross arrangement not of uniform size is preferably adopted to be connected to form described magnetic column 5-1.As shown in Figure 2, can select multiple large-sized button-shaped permanent magnet 5-1-2 and multiple undersized button-shaped permanent magnet 5-1-1, small one and large one cross arrangement forms described magnetic column 5-1.
In the center of spacing base 10 of design plummer 3 and the center of sampling receptacle 4, mechanical arm 6-2, the axle axle center of vertical arm and the axle center of magnetic column 5-1 are in same radial line, to ensure that magnetic extraction portion 5 can stretch into and shift out described sampling receptacle 4 exactly.
Described guidance panel 2 is arranged on the anterior side of case 8, operates to facilitate experimenter.Guidance panel 2 is connected motor 7 and vortex instrument 1 by control circuit, controls the start and stop of motor 7 rotating and vortex instrument 1 and the adjustment of concussion rotating speed with the operation of experimentally personnel.
Experimental provision conveniently described in experimenter's remote control, the present embodiment can also design communication module further on described guidance panel 2, for the Computer link with outside, specifically can with the mode of wired or radio communication and compunication, transmission data.In a computer by running corresponding application program, realize the manipulation that experimental provision complete machine is run.
Below in conjunction with the experimental provision shown in Fig. 1, Fig. 2, the extraction and enrichment method of Polynuclear Aromatic Hydrocarbons In Seawater is explained in detail, shown in composition graphs 3, Fig. 4, comprises the following steps:
(1) sampling receptacle 4 is placed in the spacing base 10 on plummer 3, in sampling receptacle 4, adds a certain amount of seawater sample;
In the present embodiment, in order to improve the accuracy of detection of palycyclic aromatic, before seawater sample being joined in sampling receptacle 4, preferably first seawater sample is filtered, after the glass fiber filter of 0.45 μm can be adopted to filter seawater sample, then join in sampling receptacle 4.
For the volume of the seawater sample joined in sampling receptacle 4, according to how many preliminary judgements of the palycyclic aromatic probably contained in seawater sample can determine, content higher position can add a little seawater sample less, content is low just can be added into a little seawater sample, to guarantee to be extracted into enough palycyclic aromatics, to meet the testing requirement in later stage.
(2) in sampling receptacle 4, add extractant and spreading agent, form emulsion fluid, open vortex instrument and make emulsion fluid vortex, to accelerate to reach extraction equilibrium;
In this step, the disposable mode added fast should be adopted for extractant and adding of spreading agent, and the mode not adopting instillation or slowly add.For described extractant, octanol can be adopted, and the volume ratio of octanol and seawater sample preferably controls at 1:2500-3000.For described spreading agent, acetone can be adopted, and the volume ratio of acetone and seawater sample preferably controls at 1:25-30, to meet extraction requirement better.
(3) in sampling receptacle 4, add magnetic spe medium, vortex, after reaching adsorption equilibrium, close vortex instrument 1;
In the present embodiment, preferably adopt magnetic nano-particle as described magnetic spe medium.Described magnetic nano-particle can adopt following methods to be prepared from:
Get ferric chloride hexahydrate, ethylene glycol, sodium acetate, polyglycol mix, react in a kettle., after terminating, be cooled to room temperature, obtain magnetic nano-particle through centrifuging, then divide three washing magnetic nano-particles, after drying with ethanol, be placed in crucible and calcine, carry out drying process;
Carry out surface-functionalized to magnetic nano-particle: take the magnetic nano-particle of above-mentioned drying, octadecyl trichlorosilane alkane, solvent toluene fully stir in a nitrogen atmosphere, proceed to reaction kettle for reaction again, after cooling product is used toluene, washed with methanol successively, afterwards 40 DEG C of dryings again.
Wherein, in the process of the described magnetic nano-particle of preparation, the mass ratio of described ferric chloride hexahydrate, sodium acetate, polyglycol is preferably 1-1.5:3.5-4:1.2-1.8, ferric chloride hexahydrate, sodium acetate, polyglycol are joined in ethylene glycol, formed in mixed solution, wherein, the concentration of ferric chloride hexahydrate in described mixed solution is 0.03-0.04g/mL.
Magnetic nano-particle is being carried out in the process of surface-functionalized process, the magnetic nano-particle of described drying and the mass ratio of octadecyl trichlorosilane alkane are preferably 1:2-3, described magnetic nano-particle and octadecyl trichlorosilane alkane are joined in solvent toluene and forms mixed solution, wherein, the concentration of magnetic nano-particle in this mixed solution should control at 0.005-0.015g/mL.
In this step, usual vortex can reach adsorption equilibrium in 2 minutes.
(4) start two motors 7 synchronously to rotate forward, magnetic being extracted portion 5 extend in sampling receptacle 4, magnetic column 5-1 is utilized to be adsorbed on the tube wall of glass bushing 5-2 by magnetic spe medium, after upon adsorption, start two motors 7 synchronously to reverse, magnetic is extracted portion 5 to shift out from sampling receptacle 4, and then the magnetic spe medium being adsorbed with palycyclic aromatic is shifted out from the solution sampling receptacle 4.
(5) change sampling receptacle 4, and add eluting solvent in sampling receptacle 4 after replacing, then start two motors 7 and synchronously rotate forward, magnetic is extracted portion 5 extend into described replacing after sampling receptacle 4 in;
In the present embodiment, described eluting solvent can adopt acetonitrile, and the volume ratio of described acetonitrile and seawater sample preferably controls at 1:500-1000.
(6) start second motor 7 to reverse, magnetic column 5-1 is shifted out from glass bushing 5-2, makes magnetic spe medium be shed in eluting solvent from glass bushing 5-2, start vortex instrument 1 vortex again, palycyclic aromatic is distributed in eluting solvent fast, to accelerate desorption process.
(7) close vortex instrument 1, start second motor 7 and rotate forward, magnetic column 5-1 is extend into again in glass bushing 5-2, attract magnetic spe medium to make on its tube wall being again adsorbed onto glass bushing 5-2.
(8) after treating the absorption of magnetic spe medium, start two motors 7 and reverse, magnetic being extracted portion 5 from the sampling receptacle after described replacing 4 shifts out.
Now, the solution stayed in the sampling receptacle 4 after described replacing is the solution to be measured containing palycyclic aromatic to be measured, thus, just completes the extraction process to palycyclic aromatic in described seawater sample.
(9) described solution micropipettor to be measured is shifted out, after its volume of precise, just can carry out subsequent analysis.
Such as, described solution to be measured can be transferred to the injection port of the detecting instruments such as gas chromatography (GC) or gas chromatograph-mass spectrometer (GCMS), heating and gasifying in detecting instrument, gas be sucked analytic unit and carry out detection analysis.
In the present embodiment, when arrive adsorption equilibrium can obtain by experiment, namely the surplus of target contaminant in sample solution can be detected in advance by experiment under certain environment, and with the concentration of target contaminant and time for coordinate axis draws adsorption equilibrium curve.Carry out in the process of target contaminant extracting and enriching at employing experimental provision, only according to adsorption equilibrium curve, need can determine the time of adsorption equilibrium, also can determine according to this adsorption equilibrium curve the time that vortex disperses.
Certainly, the above is only a kind of preferred implementation of the present invention, should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. for an experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater, it is characterized in that: comprise vortex instrument, magnetic extraction portion, motor and mechanical arm; The plummer for carrying sampling receptacle is formed above described vortex instrument; In described magnetic extraction portion, be provided with the glass bushing of magnetic column and bottom sealing, described magnetic column extend in glass bushing; Described motor is provided with two, described mechanical arm is rotary and telescopic mechanical arm and is provided with two groups, wherein, first group of mechanical arm is connected between First motor and described glass bushing, First motor, by driving first group of mechanical arm rotary extension, stretches into drive glass bushing or shifts out described sampling receptacle; Second group of mechanical arm is connected to second between motor and magnetic column, and second motor, by driving second group of mechanical arm rotary extension, stretches into drive magnetic column or shift out described glass bushing.
2. the experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater according to claim 1, is characterized in that: described motor is supported on the top of vortex instrument by support, and the axis direction level of machine shaft; Described mechanical arm comprises the horizontal arm be connected with machine shaft and the vertical arm be connected with magnetic column or glass bushing, reversing arrangement is provided with between horizontal arm and vertical arm, be vertical arm rotation around vertical axis by horizontal arm around the rotational transform of horizontal axis by reversing arrangement, in described mechanical arm, only vertical arm is rotary and telescopic arm.
3. the experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater according to claim 1, it is characterized in that: be buckled with a case in the outer cup of described vortex instrument, the end face of case offers an opening, and the size of opening size and sampling receptacle is suitable, described sampling receptacle is just placed on the end face of vortex instrument through described opening.
4. the experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater according to claim 3, is characterized in that: described motor is supported on the top of described case by support, and is positioned at the position, corner of case; The side of described case is provided with guidance panel, the motor described in described guidance panel is connected by control circuit, controls motor and run.
5. the experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater according to claim 1, is characterized in that: described sampling receptacle is the glass container with shading characteristic.
6. the experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater according to any one of claim 1 to 5, is characterized in that: described magnetic column is formed by connecting by multiple button-shaped permanent magnet cross arrangement not of uniform size.
7., based on a palycyclic aromatic extraction and enrichment method for the experimental provision for extracting and enriching Polynuclear Aromatic Hydrocarbons In Seawater described in claim any one of claim 1 to 6, comprise the following steps:
A, sampling receptacle is placed on plummer, in sampling receptacle, adds a certain amount of seawater sample;
B, in sampling receptacle, add extractant and spreading agent, form emulsion fluid, open vortex instrument and make emulsion fluid vortex, until reach extraction equilibrium;
C, in sampling receptacle, add magnetic spe medium, vortex, after reaching adsorption equilibrium, close vortex instrument;
D, startup two motor in synchrony rotate forward, the magnetic portion of extraction is extend in sampling receptacle, utilizes magnetic column to be adsorbed on the tube wall of glass bushing, after upon adsorption by magnetic spe medium, start two motor in synchrony reversions, magnetic is extracted portion and shifts out from sampling receptacle;
E, change sampling receptacle, and add eluting solvent in sampling receptacle after replacing, then start two motor in synchrony and rotate forward, the magnetic portion of extraction is extend in the sampling receptacle after described replacing;
F, startup second motor reversal, shift out magnetic column, make magnetic spe medium be shed in eluting solvent from glass bushing from glass bushing, starts the vortex dispersion again of vortex instrument;
G, closedown vortex instrument, start second motor and rotate forward, stretched into by magnetic column in glass bushing, attract magnetic spe medium to be adsorbed onto on the tube wall of glass bushing;
H, startup two motor reversals, the portion that extracted by magnetic shifts out from the sampling receptacle after described replacing; Now, the solution in the sampling receptacle after replacing is solution to be measured, completes the extraction process to palycyclic aromatic in described seawater sample.
8. palycyclic aromatic extraction and enrichment method according to claim 7, is characterized in that: described extractant is octanol, and the volume ratio of described octanol and seawater sample is 1:2500-3000; Described spreading agent is acetone, and the volume ratio of described acetone and seawater sample is 1:25-30; Described eluting solvent is acetonitrile, and the volume ratio of described acetonitrile and seawater sample is 1:500-1000.
9. palycyclic aromatic extraction and enrichment method according to claim 7, is characterized in that: described magnetic spe medium is magnetic nano-particle, and the preparation method of described magnetic nano-particle is:
Get ferric chloride hexahydrate, ethylene glycol, sodium acetate, polyglycol mix, react in a kettle., after terminating, be cooled to room temperature, obtain magnetic nano-particle through centrifuging, then divide three washing magnetic nano-particles, after drying with ethanol, be placed in crucible and calcine, carry out drying process;
Carry out surface-functionalized to magnetic nano-particle: take the magnetic nano-particle of above-mentioned drying, octadecyl trichlorosilane alkane, solvent toluene fully stir in a nitrogen atmosphere, proceed to reaction kettle for reaction again, after cooling product is used toluene, washed with methanol successively, afterwards 40 DEG C of dryings again.
10. the palycyclic aromatic extraction and enrichment method according to any one of claim 7 to 9, it is characterized in that: in described step a, after the glass fiber filter being 0.45 μm by described seawater sample use aperture filters, then join in described sampling receptacle.
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| CN107255689A (en) * | 2017-06-28 | 2017-10-17 | 中国科学院青岛生物能源与过程研究所 | A kind of array dynamic scatter solid-phase extraction device and extracting process |
| 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 |
| CN109115555A (en) * | 2018-10-15 | 2019-01-01 | 浙江省海洋水产研究所 | A kind of bay aromatic hydrocarbon enrichment facility |
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| CN105498290A (en) * | 2015-12-23 | 2016-04-20 | 中国科学院地球化学研究所 | Separation device for polycyclic aromatic hydrocarbon solid-liquid suspension system and separation method |
| CN107255689A (en) * | 2017-06-28 | 2017-10-17 | 中国科学院青岛生物能源与过程研究所 | A kind of array dynamic scatter solid-phase extraction device and extracting process |
| 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 |
| CN109115555A (en) * | 2018-10-15 | 2019-01-01 | 浙江省海洋水产研究所 | A kind of bay aromatic hydrocarbon enrichment facility |
| CN109115555B (en) * | 2018-10-15 | 2021-02-19 | 浙江省海洋水产研究所 | Bay aromatic hydrocarbon enrichment facility |
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