CN112255348A - Pretreatment method for detecting content of dioxin in soil - Google Patents
Pretreatment method for detecting content of dioxin in soil Download PDFInfo
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- CN112255348A CN112255348A CN202011045404.4A CN202011045404A CN112255348A CN 112255348 A CN112255348 A CN 112255348A CN 202011045404 A CN202011045404 A CN 202011045404A CN 112255348 A CN112255348 A CN 112255348A
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- dioxin
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- 239000002689 soil Substances 0.000 title claims abstract description 69
- 238000002203 pretreatment Methods 0.000 title claims abstract description 17
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 title claims abstract 13
- 238000000605 extraction Methods 0.000 claims abstract description 94
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 239000010410 layer Substances 0.000 claims abstract description 44
- 238000005070 sampling Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000002222 matrix solid-phase dispersion Methods 0.000 claims abstract description 10
- 238000002386 leaching Methods 0.000 claims abstract description 9
- 238000001179 sorption measurement Methods 0.000 claims abstract description 8
- 239000003480 eluent Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000002344 surface layer Substances 0.000 claims abstract description 4
- 230000007246 mechanism Effects 0.000 claims description 92
- 238000003825 pressing Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 14
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 7
- 230000003139 buffering effect Effects 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 235000021314 Palmitic acid Nutrition 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N n-hexadecanoic acid Natural products CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- -1 palmitic acid modified florisil Chemical class 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 230000006978 adaptation Effects 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- MSBXTPRURXJCPF-DQWIULQBSA-N cucurbit[6]uril Chemical compound N1([C@@H]2[C@@H]3N(C1=O)CN1[C@@H]4[C@@H]5N(C1=O)CN1[C@@H]6[C@@H]7N(C1=O)CN1[C@@H]8[C@@H]9N(C1=O)CN([C@H]1N(C%10=O)CN9C(=O)N8CN7C(=O)N6CN5C(=O)N4CN3C(=O)N2C2)C3=O)CN4C(=O)N5[C@@H]6[C@H]4N2C(=O)N6CN%10[C@H]1N3C5 MSBXTPRURXJCPF-DQWIULQBSA-N 0.000 claims description 2
- KVGZZAHHUNAVKZ-UHFFFAOYSA-N 1,4-Dioxin Chemical compound O1C=COC=C1 KVGZZAHHUNAVKZ-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 230000009471 action Effects 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000003028 elevating effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010720 hydraulic oil Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002013 dioxins Chemical class 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention discloses a pretreatment method for detecting dioxin content in soil, which comprises the steps of sampling layer-by-layer soil samples from a surface layer to a deep layer of a selected place through a soil layer sampling device, and numbering and storing the soil samples of different depth layers independently; mixing and fully grinding a soil sample and the matrix solid phase dispersion adsorption composition; placing the ground soil sample mixture into an extraction column in an extraction device, leaching the extraction liquid from an opening at the top end of the extraction column, and collecting extraction leaching liquid from an opening at the bottom end of the extraction column; and (3) carrying out concentration treatment and chromatographic analysis on the collected extraction eluent by a concentration device: the method can be used for quickly and accurately extracting the dioxin in the soil.
Description
Technical Field
The invention belongs to the field of soil detection, and particularly relates to a pretreatment method for detecting the content of dioxin in soil.
Background
Because dioxin compounds are more in variety, the content in the environment is very low, existing matrixes are complex, and meanwhile, an analysis instrument is required to have a lower detection limit, the pretreatment of a sample before detection and the importance of the pretreatment are achieved.
The matrix solid phase dispersion is a new extraction and purification technology, and has the advantages that: the sample structure is broken and uniformly dispersed on the surface of the filler by depending on the descaling effect of mechanical shearing force and a dispersing agent and huge surface area, so that the pretreatment process in the traditional detection method is simplified, the loss of the object to be detected caused by sample homogenization, solution conversion, emulsification, concentration and the like is avoided, and the purification efficiency is improved. However, the commonly used dispersing agents for the matrix solid phase dispersion technology are silica gel, alumina, C18Florisil, etc., have greater limitations in selectivity.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides a pretreatment method for detecting the content of dioxin in soil, which can quickly and fully recover the dioxin in the soil.
The technical scheme is as follows: in order to achieve the purpose, the technical scheme of the invention is as follows:
a pretreatment method for detecting the content of dioxin in soil comprises the following steps:
s1: sampling: sampling the soil samples from the surface layer to the deep layer of the selected place layer by layer through a soil layer sampling device, and numbering and storing the soil samples of different depth layers independently;
s2: grinding: mixing and fully grinding a soil sample and the matrix solid phase dispersion adsorption composition;
s3: dissolving and extracting: placing the ground soil sample mixture into an extraction column in an extraction device, leaching the extraction liquid from an opening at the top end of the extraction column, and collecting extraction leaching liquid from an opening at the bottom end of the extraction column;
s4: concentrating the extract liquor: concentrating the collected extraction eluent by a concentration device until the extraction eluent is in a colloid state;
s5: and (3) chromatographic analysis: dissolving the substance to be detected with acetonitrile, filtering, separating with HRGC-HRMS, and qualitatively and quantitatively detecting the content of each component in the substance to be detected.
Further, the matrix solid phase dispersion adsorption composition comprises cucurbituril grafted acrylic acid, sulfonated carbon nanotubes, palmitic acid modified florisil and sandstone particles.
Further, the soil layer sampling device comprises a supporting vertical frame, a lifting mechanism, a rotary mechanism and a scraper, wherein the lifting mechanism is arranged at the top end of the supporting vertical frame, the rotary mechanism is arranged at the lifting end of the lifting mechanism, the scraper is arranged at the rotary end of the rotary mechanism, and the rotary surface of the scraper is arranged in parallel to the ground; the scraper rotates through the slewing mechanism and meanwhile downwards extends layer by layer through the lifting mechanism.
Furthermore, the lifting mechanism is a screw rod mechanism, the lifting mechanism comprises a screw rod and a sliding seat arranged on the screw rod, the bottom end of the screw rod is coaxially provided with a pre-anchor part, the pre-anchor part comprises a spiral auger blade, and the pre-anchor part is inserted below the ground through the rotation of the screw rod; still include connecting sleeve, the connecting sleeve clearance cover is established the outside of lead screw, just connecting sleeve's top axial fixity and circumference gyration set up on the slide, at least two the scraper blade circumference sets up on connecting sleeve's bottom.
Furthermore, the slide is T type swivel nut structure, connecting sleeve's top contains the connecting seat, the connecting seat contains the gyration recess with the slide adaptation, be provided with the spacing ring corresponding to the gyration recess on the top of connecting seat, the slide passes through the connecting seat and the spacing ring sets up in the gyration recess.
Further, the extraction device includes extraction post, filter plate, filtrating container, collection liquid container and supporting seat, be provided with collection liquid container on the supporting seat, the gyration is provided with filtrating container in the inner chamber of collection liquid container, the vertical interval in open-top of filtrating container is provided with the extraction post, the upper and lower both ends opening setting of extraction post, be provided with two filter plates, two along axial interval in the extraction post constitute sample holding chamber between the filter plate.
Furthermore, the extraction column comprises a fixed cylinder and a movable cylinder, the movable cylinder is arranged in the fixed cylinder in a sliding sealing and sealing manner or penetrates through the fixed cylinder, the movable cylinder is axially adjusted relative to the fixed cylinder, one filter plate is arranged in the fixed cylinder, and the other filter plate is arranged in the movable cylinder; the volume of the sample accommodating cavity is adjusted by axially adjusting the movable cylinder body relative to the fixed cylinder body.
Furthermore, a pressing mechanism is arranged in an opening at the top end of the extraction column, the pressing mechanism is pressed and covered above the filter plate at the top layer, and the filter plate at the top layer is pressed and covered to the sample accommodating cavity through the pressing mechanism;
the pressing mechanism comprises a pressing ring, the inner wall of the opening at the top end of the extraction column axially comprises a thread section, and the pressing ring is adjusted and arranged in the extraction column through threads; the filter plate gap at the top layer of the extraction column is arranged in the extraction column, and a telescopic spring is arranged between the compression ring and the filter plate at the top layer.
Further, the enrichment facility includes support frame, third rotation mechanism, concentrated barrel and gentle stream board, concentrated barrel is closed containment structure, concentrated barrel uses the radial direction to rotate the setting as the axial on the support frame, third rotation mechanism sets up on the support frame and drives concentrated barrel intermittent type nature upset in the vertical plane and rotates, be provided with two gentle stream boards along the axial respectively interval in the concentrated barrel, the inner chamber of concentrated barrel separates into the collection liquid chamber that is located both ends and is located the concentrated chamber in the middle of through two gentle stream boards, it is provided with intake pipe and outlet duct to communicate concentrated chamber on the concentrated barrel.
The device further comprises a disturbance stirring mechanism and a driving mechanism, wherein the disturbance stirring mechanism is rotatably arranged on each flow buffering plate respectively, the disturbance stirring mechanism extends into the two liquid collecting cavities respectively, the driving mechanism is arranged in the concentration cavity, and the driving mechanism drives the disturbance stirring mechanism to rotate;
the driving mechanism comprises a supporting shaft, a blade rotor and a transmission assembly, wherein the supporting shaft is arranged between the two baffle plates in a distance and parallel to a rotating shaft of the stirring mechanism, the blade rotor is rotatably arranged on the supporting shaft and corresponds to the air outlet end of the air inlet pipe, and the blade rotor is driven by the transmission assembly to rotate the disturbance stirring mechanism.
Has the advantages that: according to the invention, the soil in the same place is sampled in a layered manner, and the steps of grinding, dissolving and extracting, extracting solution concentrating, chromatograph analyzing and the like are carried out on each soil sample, so that the overall detection process is optimized to a great extent, and the dioxin content in the soil can be detected quickly and accurately.
Drawings
FIG. 1 is a schematic perspective view of a soil layer sampling apparatus according to the present invention;
FIG. 2 is a schematic half-section view of a soil layer sampling apparatus of the present invention;
FIG. 3 is a partially enlarged schematic view of a lifting mechanism in the soil layer sampling apparatus of the present invention;
FIG. 4 is a perspective view of the whole structure of the extraction apparatus of the present invention;
FIG. 5 is a schematic half-sectional view of the overall structure of the extraction apparatus of the present invention;
FIG. 6 is a partially enlarged schematic view of a pressing mechanism of the extraction apparatus of the present invention;
FIG. 7 is a perspective view of the overall configuration of the thickener according to the present invention;
FIG. 8 is a schematic half-sectional view showing the overall structure of the thickener according to the present invention;
FIG. 9 is a schematic view of another embodiment of the concentrating device of the present invention;
FIG. 10 is a schematic view showing the internal structure of a concentrating chamber in the concentrating device of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
A pretreatment method for detecting the content of dioxin in soil comprises the following steps:
s1: sampling: sampling the soil samples layer by layer from the surface layer to the deep layer of the selected place through the soil layer sampling device 1, and numbering and storing the soil samples of different depth layers independently;
s2: grinding: mixing and fully grinding a soil sample and the matrix solid phase dispersion adsorption composition;
s3: dissolving and extracting: placing the ground soil sample mixture into an extraction column in an extraction device 2, leaching the extraction solution from an opening at the top end of the extraction column, and collecting the extraction leaching solution from an opening at the bottom end of the extraction column;
s4: concentrating the extract liquor: concentrating the collected extraction eluent by a concentration device 3 until the extraction eluent is in a colloid state;
s5: and (3) chromatographic analysis: dissolving the substance to be detected with acetonitrile, filtering, separating with HRGC-HRMS, and qualitatively and quantitatively detecting the content of each component in the substance to be detected.
The matrix solid-phase dispersion adsorption composition comprises cucurbit urils grafted acrylic acid, sulfonated carbon nanotubes, palmitic acid modified florisil and sandstone particles, wherein the weight ratio of the cucurbit urils grafted acrylic acid, the sulfonated carbon nanotubes to the palmitic acid modified florisil is 1: 0.5-1.2) of the above-mentioned inorganic particles, wherein the sand and stone particles are used for crushing soil particles during grinding, and the shearing force is increased so that the soil and the matrix solid phase dispersion adsorption composition can be sufficiently adsorbed. By sampling the soil in the same place in a layered manner, and grinding, dissolving and extracting, extracting solution concentrating, chromatograph analyzing and other steps are carried out on each soil sample, the overall detection process is optimized to a great extent, dioxin substances in the soil can be rapidly and fully recovered, and the dioxin content in the soil can be accurately detected.
As shown in fig. 1 to 3, the soil layer sampling device 1 includes a supporting stand 1.1, a lifting mechanism 1.2, a swing mechanism 1.3 and a scraper 1.4, the supporting stand 1.1 includes a top plate 1.10 and a plurality of fixing rods 1.11 circumferentially distributed below the top plate 1.10, the fixing rods 1.11 are located on an outer ring of the scraper 1.4, the bottom end of the fixing rod 1.11 is a tip, and the fixing rod 1.11 is used for being inserted into the ground for fixing. The lifting mechanism 1.2 is arranged at the top end of the supporting vertical frame 1.1, the slewing mechanism 1.3 is arranged at the lifting end of the lifting mechanism 1.2, the scraper 1.4 is arranged at the slewing end of the slewing mechanism 1.3, and the slewing surface of the scraper 1.4 is arranged in parallel to the ground; the scraper 1.4 rotates through the rotating mechanism 1.3 and simultaneously downwards extends layer by layer through the lifting mechanism 1.2. When ground soil is scraped in the gyration of scraper blade 1.4, be used for getting rid of the soil and the debris on shallow table earlier, descend through elevating system 1.2 afterwards, dig the hole to same position region with the successive layer, until the soil degree of depth that needs the sampling, simultaneously, the scraper blade is under the high-speed gyration action of slewing mechanism, the soil that is scraped out is thrown away to outer lane and subaerial through centrifugal force, also can suspend the gyration and the lift of scraper blade and carry out the manual work and clear away, and the soil layer surface that is located the inner circle is comparatively level and smooth, can obtain the soil sample on same soil layer, in order to guarantee to detect the accuracy.
Elevating system 1.2 is screw rod mechanism, elevating system 1.2 includes that lead screw 1.5 is in with the setting slide 1.6 on the lead screw 1.5, lead screw 1.5 rotate the setting on the roof that supports grudging post 1.1, just the top of lead screw is provided with the hydraulic oil motor, carries out the gyration through hydraulic power unit and rotates, perhaps is driving motor, it is provided with guide bar 1.15 in vertical to support grudging post 1.1, slide 1.6 slides on guide bar 1.15 through connecting plate 1.18 direction. The bottom end of the screw rod 1.5 is coaxially provided with a pre-anchor part 1.7, the pre-anchor part 1.7 comprises an axial spiral auger blade 1.8, and the pre-anchor part 1.7 is inserted below the ground through the rotation of the screw rod 1.8. When the support stand 1.1 is placed and fixed, the fixing rod can be quickly inserted into the ground through the rotary action of the lead screw and the pre-anchor 7 because the fixing rod needs to be inserted into the ground, and the labor intensity of workers is saved.
Still include connecting sleeve 1.12, connecting sleeve 1.12 clearance cover is established the outside of lead screw 1.5, just connecting sleeve 1.12's top axial fixity and circumference gyration set up on slide 1.6, at least two scraper blade 1.4 circumference sets up on connecting sleeve 1.12's bottom. The connecting sleeve 1.12 and the sliding seat 1.6 rotate relatively, so that the scraper 1.4 can have independent rotating speed to rotate at high speed, and the sliding seat 1.6 can perform slow lifting action.
The sliding seat 1.6 is of a T-shaped threaded sleeve structure, the bottom end is large, the top end is small, the top end of the connecting sleeve 1.12 comprises a connecting seat 1.13, the connecting seat 1.13 comprises a rotary groove matched with the sliding seat 1.6, a limiting ring 1.14 is arranged on the top end of the connecting seat 1.13 corresponding to the rotary groove, and the sliding seat 1.6 is arranged in the rotary groove through the connecting seat 1.13 and the limiting ring 1.14.
The rotary mechanism 1.3 is arranged on the sliding seat 1.6, a driving gear 1.16 is arranged on the rotary mechanism 1.3 in a rotary mode, a gear tooth portion 1.17 is arranged on the wall of an outer ring of the connecting seat 1.13, and the gear tooth portion 1.17 is in meshing transmission with the driving gear 1.16. The slewing mechanism 1.3 is a hydraulic oil motor, and has large torsion and good stability.
As shown in fig. 4 to 6, the extraction device 2 includes an extraction column 2.1, filter plates 2.2, a filtrate container 2.3, a liquid collection container 2.4 and a support base 2.5, the liquid collection container 2.4 is arranged on the support base 2.5, the filtrate container 2.3 is rotatably arranged in an inner cavity of the liquid collection container 2.4, the extraction columns 2.1 are vertically arranged above top openings of the filtrate container 2.3 at intervals, openings are arranged at upper and lower ends of the extraction column 2.1, an extraction liquid for leaching is introduced into top openings of the extraction column 2.1, two filter plates 2.2 are axially arranged in the extraction column 2.1 at intervals, a sample accommodating cavity 2.6 is formed between the two filter plates 2.2, a soil sample is placed in the sample accommodating cavity 2.6, and is compressed by the two filter plates 2.2. Drip washing extraction is carried out soil sample through the extraction post, promotes the sufficiency of its extraction, and carries out centrifugal filtration to mixed solution after the extraction, further promotes the purity of extraction mixed solution, gets rid of mud, and the preface unifies, simple structure, convenient operation promotes the whole efficiency of soil extraction.
The filtrate container 2.3 and the liquid collecting container 2.4 are both of a cylindrical structure with an open top end, the side wall of the filtrate container 2.3 is provided with a plurality of filter holes 2.7, the bottom of the filtrate container 2.3 is provided with a rotary driving mechanism 2.9, the rotary driving mechanism 2.9 is a driving motor arranged below the mounting seat 2.5, and the filtrate container 2.3 is arranged at an interval on the annular wall of the liquid collecting container 2.4 and forms a filtrate cavity 2.8; the extraction mixture solution passing through the extraction column 2.1 is filtered through a filtrate vessel 2.3, after extraction, the mixture solution in the filtrate vessel is filtered through centrifugal rotation of the filtrate vessel 2.4.
As shown in fig. 5 and fig. 6, the extraction column 2.1 includes a fixed cylinder 2.11 and a movable cylinder 2.12, the movable cylinder 2.12 is slidably and hermetically sealed or inserted into the fixed cylinder 2.11, the movable cylinder 2.12 is axially adjusted relative to the fixed cylinder 2.11, one filter plate 2.2 is arranged in the fixed cylinder 2.12, and the other filter plate 2.2 is arranged in the movable cylinder 2.12; through the axial adjustment of the movable cylinder 2.12 relative to the fixed cylinder 2.11 is used for adjusting the volume of the sample accommodating cavity 2.6, the overall height of the extraction column can be reduced, and the application range of the extraction column can be widened through the lifting adjustment.
Support seat 2.5 is last to be provided with backup pad 2.13 adjacent to extraction post 2.1, fixed barrel 2.11 is fixed to be set up on backup pad 2.13, activity barrel 2.12 passes through guide bar 2.14 direction slip setting on backup pad 2.13, backup pad 2.13 has seted up the guide way corresponding guide bar 2.14, just be provided with locking regulating part 2.15 on the guide bar 2.14, locking regulating part 2.15 is the bolt.
As shown in fig. 5 and 6, a pressing mechanism 2.16 is arranged in the top opening of the extraction column 2.1, the pressing mechanism 2.16 is pressed above the top filter plate 2.2, the top filter plate 2.2 is pressed towards one side of the sample accommodating cavity 2.6 through the pressing mechanism 2.16 so as to press the soil sample placed in the extraction column, the pressing mechanism 2.16 comprises a pressing ring 2.18, the inner wall of the top opening of the extraction column 2.1 axially comprises a thread section 2.19, and the pressing ring 2.18 is arranged in the extraction column in a thread adjusting manner.
The filter plate 2.2 that is located the top layer of extraction post is the clearance activity setting in the extraction post, and the filter plate and the extraction post of bottom are fixed to be set up, be provided with expanding spring 2.20 between the filter plate 2.2 of clamp ring 2.18 and top layer, compress tightly the soil sample through the filter plate and the expanding spring 2.20 of top layer, and the soil sample when the drip washing runs off, filter plate 2.2 compensates downwards through expanding spring's reset action, and the soil sample still keeps the compression state during.
As shown in fig. 7 to 10, the concentration device 3 includes a support frame 3.1, a third revolving mechanism 3.2, a concentration cylinder 3.3 and a baffle plate 3.6, the concentration cylinder 3.3 is a closed cylinder container structure, the concentration cylinder 3.3 is disposed on the support frame 3.1 by revolving in the radial direction as the axial direction, the third revolving mechanism 3.2 is disposed on the support frame 3.1 and drives the concentration cylinder 3.3 to intermittently revolve in the vertical plane, the third revolving mechanism 3.2 is a revolving mechanism such as a motor, a rotating cylinder, etc., two baffle plates 3.6 are disposed in the concentration cylinder 3.3 at intervals along the axial direction, the baffle plates 3.6 are circular plate-shaped structures, the inner cavity of the concentration cylinder 3.3 is divided into a liquid collection cavity 3.8 at two ends and a concentration cavity 3.9 in the middle by the two baffle plates 3.6, the concentration cylinder 3.3 is communicated with the concentration cavity 3.9 and is provided with an air inlet pipe 3.4 and an air outlet pipe 3.5, hot air flows flow through the air inlet pipe 3.4 and the air outlet pipe 3.5, the temperature is 40-50 ℃, nitrogen or purified air is preferred to prevent other impurities from being introduced, extraction liquid in the concentration cylinder 3.3 is overturned through the third rotary mechanism 3.2, so that the extraction liquid circularly flows in the two liquid collecting cavities 3.8, in the flowing process of the extraction liquid, water vapor evaporation is carried out through the hot air flow introduced into the concentration cavity, the extraction liquid is carried out to the outside of a concentration container, the extraction liquid is concentrated, and the extraction liquid can be concentrated quickly and efficiently.
The flow slowing plate 3.6 comprises at least one group of liquid outlets 3.7 in the air flow direction, the liquid outlets 3.7 are linear through groove structures along the turning axis direction, and the liquid level path of the outflow extraction liquid is perpendicular to the air flow direction so as to fully concentrate the extraction liquid.
A plurality of separating blocks 3.10 are arranged in the liquid outlet 3.7 along the length direction, the liquid outlet 3.7 is divided into a plurality of liquid outlet through holes 3.11 which are mutually independent through the plurality of separating blocks 3.10, the extract liquid flows downwards through the liquid outlet through holes 3.11, and hot air flows through channels among the liquid outlet through holes, so that the sufficient and efficient concentration of the extract liquid can be further accelerated.
As shown in the attached drawing 9, the drying device further comprises a drying component 3.12, an air source component 3.13 and a heating component 3.14, the air inlet pipe 3.4 is communicated with the air outlet end of the air source component 3.13 through a hose, the air source component 3.13 comprises an air pump and an air storage bottle, the heating component 3.14 is arranged on the pipeline of the air inlet pipe 3.4, the air flow is heated through the heating component 3.14, the drying component 3.12 is arranged on the pipeline of the air outlet pipe 5 through a hose 3.15, and when the hot air flow carries water vapor through the concentration cavity 3.9, the hot air flow is dried and purified through the drying component 3.12. The gas outlet end of the gas outlet pipe 3.5 is communicated with the gas inlet end of the gas source component 3.13 through a gas pipe, and the gas source component 3.13 and the concentration cylinder 3.3 form a gas flow loop, so that gas is recycled, energy is saved, and waste heat is effectively recovered.
As shown in fig. 10, the device further comprises a disturbance stirring mechanism 3.20 and a driving mechanism 3.21, wherein the disturbance stirring mechanism 3.20 is rotatably arranged on each flow buffering plate 3.6, the disturbance stirring mechanism 3.20 extends into the two liquid collecting cavities 3.8, the driving mechanism 3.21 is arranged in the concentration cavity 3.9, and the driving mechanism 3.21 drives the disturbance stirring mechanism 3.20 to rotate. The extraction liquid in the two liquid collecting cavities 3.8 is stirred by the stirring mechanism 3.20 to prevent the extraction liquid from precipitating.
Actuating mechanism 3.21 includes back shaft 3.24, paddle rotor 3.22 and drive assembly, back shaft 3.24 interval and the revolving axle setting that is on a parallel with rabbling mechanism are between two buffer plate 3.6, it is provided with paddle rotor 3.22 to rotate on the back shaft 3.24, paddle rotor 3.22 sets up corresponding to the end of giving vent to anger of intake pipe 3.4, and the air current drive paddle rotor 3.22 that intake pipe 3.4 flows rotates, paddle rotor 3.22 passes through the drive assembly drive disturbance rabbling mechanism 3.20 rotates the setting, and it need not extra power supply, and the structure is ingenious, and occupation space is little.
The transmission assembly includes action wheel 3.25, drive belt 3.23 and follower 3.26, it sets up with coaxial and relatively fixed of paddle rotor 3.22 to rotate wheel 3.25, the coaxial setting of follower 3.26 is in rabbling mechanism's pivot, the follower passes through drive belt follow-up and action wheel 3.25.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (10)
1. A pretreatment method for detecting the content of dioxin in soil is characterized by comprising the following steps: the method comprises the following steps:
s1: sampling: sampling layer-by-layer soil samples from a surface layer to a deep layer of a selected place through a soil layer sampling device (1), and numbering and storing the soil samples of different depth layers independently;
s2: grinding: mixing and fully grinding a soil sample and the matrix solid phase dispersion adsorption composition;
s3: dissolving and extracting: placing the ground soil sample mixture into an extraction column in an extraction device (2), leaching the extraction liquid from an opening at the top end of the extraction column, and collecting the extraction leaching liquid from an opening at the bottom end of the extraction column;
s4: concentrating the extract liquor: concentrating the collected extraction eluent by a concentration device (3) until the extraction eluent is in a colloid state;
s5: and (3) chromatographic analysis: dissolving the substance to be detected with acetonitrile, filtering, separating with HRGC-HRMS, and qualitatively and quantitatively detecting the content of each component in the substance to be detected.
2. The pretreatment method for detecting the content of dioxin in soil according to claim 1, characterized in that: the matrix solid phase dispersion adsorption composition comprises cucurbituril grafted acrylic acid, sulfonated carbon nanotubes, palmitic acid modified florisil and sandstone particles.
3. The pretreatment method for detecting the content of dioxin in soil according to claim 1, characterized in that: the soil layer sampling device (1.1) comprises a supporting vertical frame (1.1), a lifting mechanism (1.2), a rotary mechanism (1.3) and a scraper (1.4), wherein the lifting mechanism (1.2) is arranged at the top end of the supporting vertical frame (1.1), the rotary mechanism (1.3) is arranged at the lifting end of the lifting mechanism (1.2), the scraper (1.4) is arranged at the rotary end of the rotary mechanism (1.3), and the rotary surface of the scraper (1.4) is arranged in parallel to the ground; the scraper (1.4) rotates through the rotating mechanism (1.3) and simultaneously downwards extends layer by layer through the lifting mechanism (1.2).
4. The pretreatment method for detecting the content of dioxin in soil according to claim 3, characterized in that: the lifting mechanism (1.2) is a screw rod mechanism, the lifting mechanism (1.2) comprises a screw rod (1.5) and a sliding seat (1.6) arranged on the screw rod (1.5), a pre-anchor piece (1.7) is coaxially arranged at the bottom end of the screw rod (1.5), the pre-anchor piece (1.7) comprises a spiral auger blade (1.8), and the pre-anchor piece (1.7) is inserted below the ground through the rotation of the screw rod (1.8); still include connecting sleeve (1.12), connecting sleeve (1.12) clearance cover is established the outside of lead screw (1.5), just the top axial fixity and the circumference gyration of connecting sleeve (1.12) set up on slide (1.6), at least two scraper blade (1.4) circumference sets up on the bottom of connecting sleeve (1.12).
5. The pretreatment method for detecting the content of dioxin in soil according to claim 4, characterized in that: slide (1.6) are T type swivel nut structure, the top of connecting sleeve (1.12) contains connecting seat (1.13), connecting seat (1.13) contain with the gyration recess of slide (1.6) adaptation, be provided with spacing ring (1.14) corresponding to the gyration recess on the top of connecting seat (1.13), slide (1.6) set up in the gyration recess through connecting seat (1.13) and spacing ring (1.14).
6. The pretreatment method for detecting the content of dioxin in soil according to claim 1, characterized in that: extraction device (2.2) are including extraction post (2.1), filter plate (2.2), filtrate container (2.3), collection liquid container (2.4) and supporting seat (2.5), be provided with collection liquid container (2.4) on supporting seat (2.5), the gyration is provided with filtrate container (2.3) in the inner chamber of collection liquid container (2.4), the vertical interval in top opening top of filtrate container (2.3) is provided with extraction post (2.1), the upper and lower both ends opening setting of extraction post (2.1), be provided with two filter plates (2.2) along axial interval in extraction post (2.1), two constitute sample holding chamber (2.6) between filter plate (2.2).
7. The pretreatment method for detecting the content of dioxin in soil according to claim 6, characterized in that: the extraction column (2.1) comprises a fixed cylinder body (2.11) and a movable cylinder body (2.12), the movable cylinder body (2.12) is arranged in the fixed cylinder body (2.11) in a sliding sealing and sealing mode or penetrates through the fixed cylinder body, the movable cylinder body (2.12) is axially adjusted relative to the fixed cylinder body (2.11), one filter plate (2.2) is arranged in the fixed cylinder body (2.12), and the other filter plate (2.2) is arranged in the movable cylinder body (2.12); the volume of the sample containing cavity (2.6) is adjusted by the axial adjustment of the movable cylinder (2.12) relative to the fixed cylinder (2.11).
8. The pretreatment method for detecting the content of dioxin in soil according to claim 7, characterized in that: a pressing mechanism (2.16) is arranged in an opening at the top end of the extraction column (2.1), the pressing mechanism (2.16) is pressed above the filter plate at the top layer, and the filter plate (2.2) at the top layer is pressed towards the sample accommodating cavity through the pressing mechanism (2.16);
the pressing mechanism (2.16) comprises a pressing ring (2.18), the inner wall of the top opening of the extraction column (2.1) axially comprises a threaded section (2.19), and the pressing ring (2.18) is arranged in the extraction column in a threaded adjusting mode; the filter plate (2.2) at the top layer of the extraction column is arranged in the extraction column in a clearance mode, and a telescopic spring (2.20) is arranged between the compression ring (2.18) and the filter plate (2.2) at the top layer.
9. The pretreatment method for detecting the content of dioxin in soil according to claim 1, characterized in that: the concentrating device (3.3) comprises a support frame (3.1), a third rotating mechanism (3.2), a concentrating cylinder body (3.3) and a flow buffering plate (3.6), the concentrating cylinder body (3.3) is of a closed container structure, the concentrating cylinder body (3.3) is arranged on the support frame (3.1) in an axially rotating mode in the radial direction, the third rotating mechanism (3.2) is arranged on the support frame (3.1) and drives the concentrating cylinder body (3.3) to intermittently overturn and rotate in a vertical plane, two flow buffering plates (3.6) are arranged in the concentrating cylinder body (3.3) at intervals in the axial direction, an inner cavity of the concentrating cylinder body (3.3) is separated into a liquid collecting cavity (3.8) located at two ends and a concentrating cavity (3.9) located in the middle through the two flow buffering plates (3.6), and the concentrating cavity (3.9) is communicated with the concentrating cylinder body (3.3.3) and is provided with an air inlet pipe (3.4) and an air outlet pipe (3.
10. The pretreatment method for detecting the content of dioxin in soil according to claim 9, characterized in that: the device is characterized by further comprising a disturbance stirring mechanism (3.20) and a driving mechanism (3.21), wherein the disturbance stirring mechanism (3.20) is rotatably arranged on each flow buffering plate (3.6) respectively, the disturbance stirring mechanism (3.20) extends into the two liquid collecting cavities (3.8) respectively, the driving mechanism (3.21) is arranged in the concentration cavity (3.9), and the driving mechanism (3.21) drives the disturbance stirring mechanism (3.20) to rotate;
actuating mechanism (3.21) are including back shaft (3.24), paddle rotor (3.22) and drive assembly, back shaft (3.24) interval and the revolving axle setting that is on a parallel with rabbling mechanism are between two gentle stream boards (3.6), it is provided with paddle rotor (3.22) to rotate on back shaft (3.24), paddle rotor (3.22) are corresponding to the end setting of giving vent to anger of intake pipe (3.4), paddle rotor (3.22) are through the drive assembly drive disturbance rabbling mechanism (3.20) rotate the setting.
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Application publication date: 20210122 |