CN109342111A - A kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity - Google Patents

A kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity Download PDF

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Publication number
CN109342111A
CN109342111A CN201811277003.4A CN201811277003A CN109342111A CN 109342111 A CN109342111 A CN 109342111A CN 201811277003 A CN201811277003 A CN 201811277003A CN 109342111 A CN109342111 A CN 109342111A
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micro
sampling
soil
extraction
allelochemical
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CN201811277003.4A
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王炎
赵敏
王宁
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Harbin Institute of Technology
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Harbin Institute of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/04Devices for withdrawing samples in the solid state, e.g. by cutting
    • G01N1/08Devices for withdrawing samples in the solid state, e.g. by cutting involving an extracting tool, e.g. core bit
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/062Preparation extracting sample from raw material

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The present invention provides a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity, belongs to secretions from plant roots and allelochemical sampling technique field.Drill bit is connect by screw thread with sampling pipe one end in the present invention, there is micropore on the tube wall of sampling pipe, studs is the two-sided threaded cap of seal rubber of the sampling pipe other end, one end of the sampling pipe other end and studs is connected through a screw thread, and the other end and the tail pipe of studs are connected through a screw thread, and the centre of tail pipe is provided with channel, tail pipe outer end is provided with end cover, sampling pipe uses high wellability aluminium oxide, and alternating temperature sinters micropore ceramics sampling pipe into repeatedly, and capillary aperture is 0.05-100um.The present invention has strong capillarity, and liquid flows into pipe from micropore, facilitates regular micro-extraction, the allelochemical in Qualitative and quantitative analysis soil.

Description

A kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity
Technical field
The present invention relates to a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity, belongs to plant Root exudates and allelochemical sampling technique field.
Background technique
The release approach of plant allelochemicals specifically includes that root system secretion outwardly, the misty rain leaching of plant and volatilization; The decomposition of plant or residuum under soil physiochemical effects, microbial action;Pollen transmission and seed are sprouted.For research root system secretion Species and concentration, the influence that root exudates is generated of the environmental factors such as stress, allelochemical and allelopathic in root exudates Effect etc., people have devised the collection method of many root exudates, mainly have: hydroponics collection, matrix culture (vermiculite Training, sand culture, agar training) it collects, earth culture collection, automatically continuously collection etc..Traditional allelochemical extracting and developing method, which exists, to be lacked It owes, the confidence level for the result of study for causing it to obtain is had a greatly reduced quality.The hydroponics of root exudates are collected, matrix culture is received Collection, soil-solution Combined culture collecting method, filter paper collecting method, grows case cultivation at earth pillar elution collections, does not account for point Secretion enters the soil physiochemical effects after soil, the compound occurred after microbial action conversion and concentration variation, these Method is not suitable as the sampling method of allelochemical.
Although the in situ sampling technology of the soil liquid, this field of ecology is studied almost without being applied to allelopathic so far In, but its important research means for having become the subjects such as soil, plant nutrient, ecological environment, how effectively to extract the soil liquid Have become an important technical problem.Establish a kind of non-disturbance in situ sampling of efficient, highly sensitive soil allelochemical Technology, and can be connect with micro-extraction technique, concatenated operation that realization is sampled, extraction, is concentrated, sample introduction is seamless makes it by high score It distinguishes highly sensitive to be detected, it is extremely important to the type, content and release approach of correct understanding allelochemical.Only get allelopathic clear The real source of substance could determine the true donor and receptor of allelochemical, can just simulate the change of nature necessary being Feel phenomenon and its mechanism, and is applied in production practices.
Summary of the invention
The purpose of the present invention is to solve the above-mentioned problems of the prior art, using soil capillarity as principle, use The micropore ceramics such as high wellability aluminium oxide are that raw material prepares small-sized soil liquid sampling pipe, and it is appropriate that sampling pipe is retained in soil Position, netted poromerics have the micropore of a large amount of 1.5um or so, each small micropore can be understood as an independence Capillary, indwelling has strong capillarity in soil, and when the soil liquid is diffused into sampling pipe surface, liquid is from micro- It is flowed into pipe in hole, to facilitate regular micro-extraction, the allelochemical in Qualitative and quantitative analysis soil, and then one kind is provided and is based on Soil allelochemical in situ sampling-micro-extraction device of capillarity.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity, comprising: drill bit, sampling pipe, double Header stud, channel, tail pipe and end cover;
Wherein, drill bit is connect by screw thread with sampling pipe one end, has micropore on the tube wall of sampling pipe, and studs is to adopt One end of the two-sided threaded cap of seal rubber of the sample pipe other end, the sampling pipe other end and studs is connected through a screw thread, double end The other end of stud is connected through a screw thread with tail pipe, and the centre of tail pipe is provided with channel, and tail pipe outer end is provided with end cover.
The sampling pipe uses high wellability aluminium oxide, and alternating temperature sinters micropore ceramics sampling pipe, capillary aperture into repeatedly 0.05-100um, internal diameter 5-10mm, outer diameter 10-20mm, wall thickness 2-5mm, long 3-14cm, tube wall adsorption volume 3.54- 33.84cm3, hollow volume 1.18-12.02cm3
When described device is applied to solid phase microextraction, it is reserved with aperture on end cover, is passed through for Solid Phase Extraction fiber, no In use, the aperture on end cover is blocked by small rubber screw.
The Solid Phase Extraction fiber is telescopic to be set in micro-extraction protection needle tubing, and micro-extraction protection needle tubing can successively lead to Cross end cover, channel and studs.
When described device is applied to liquid-phase micro-extraction, the doughnut for bending to U-shaped, U-shaped are provided in sampling pipe Two ends of doughnut be connected with hollow stainless steel filament, reserve that there are two holes on end cover, it is thin for hollow stainless steel Silk passes through, and two ends are usually sealed with special rubber cap.
The end of the hollow stainless steel filament is respectively connected with microsyringe.
Also reserved one is used to connect the insertion hole of cleaning syringe on the end cover.
The invention has the benefit that
Micropore quantity, the gross area can guarantee and rely on capillarity between soil capillary on present invention sampling tube wall, Moisture is realized automatically into pipe, certain time in pipe indwelling to soil, pipe is interior to be full of the soil liquid, effectively separation in situ Potential allelochemical in Enriching soil realizes non-disturbance in-situ sampling;And it is connect with micro-extraction technique, realizes allelopathic Extracting substances;Sampling, extraction, concentration, sample introduction serial operation, enable acquired sample by the detection of high-resolution high sensitivity, It is extremely important to the type, content and release approach of correct understanding allelochemical;For quantitative analysis, self-induction action, allelopathy Evaluation provide theoretical basis.
Detailed description of the invention
Fig. 1 is that a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity of the present invention is applied to admittedly The structural schematic diagram of phase extraction.
Fig. 2 is that a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity of the present invention is applied to liquid The structural schematic diagram of phase extraction.
Appended drawing reference in figure, 1 is drill bit, and 2 be sampling pipe, and 3 be studs, and 4 be channel, and 5 be tail pipe, and 6 be sealing End cap, 7 be doughnut, and 8 be microsyringe, and 9 be Solid Phase Extraction fiber, and 10 protect needle tubing for micro-extraction, and 11 be cleaning note Emitter, 12 be hollow stainless steel filament.
Specific embodiment
Below in conjunction with attached drawing, the present invention is described in further detail: the present embodiment is being with technical solution of the present invention Under the premise of implemented, give detailed embodiment, but protection scope of the present invention is not limited to following embodiments.
As depicted in figs. 1 and 2, a kind of soil allelochemical based on capillarity involved in the present embodiment is adopted in situ Sample-micro-extraction device, comprising: drill bit 1, sampling pipe 2, studs 3, channel 4, tail pipe 5 and end cover 6;
Wherein, drill bit 1 is connect by screw thread with 2 one end of sampling pipe, has micropore, studs 3 on the tube wall of sampling pipe 2 For the two-sided threaded cap of seal rubber of 2 other end of sampling pipe, one end of 2 other end of sampling pipe and studs 3 is connected by screw thread It connects, the other end and the tail pipe 5 of studs 3 are connected through a screw thread, and the centre of tail pipe 5 is provided with channel 4, the setting of 5 outer end of tail pipe There is end cover 6.
The sampling pipe 2 uses high wellability aluminium oxide, and alternating temperature sinters micropore ceramics sampling pipe, capillary aperture into repeatedly 0.05-100um, internal diameter 5-10mm, outer diameter 10-20mm, wall thickness 2-5mm, long 3-14cm, tube wall adsorption volume 3.54- 33.84cm3, hollow volume 1.18-12.02cm3
When described device is applied to solid phase microextraction, it is reserved with aperture on end cover 6, is passed through for Solid Phase Extraction fiber 9, When not in use, the aperture on end cover 6 is blocked by small rubber screw.
The Solid Phase Extraction fiber 9 is telescopic to be set in micro-extraction protection needle tubing 10, and micro-extraction protects needle tubing 10 can Pass sequentially through end cover 6, channel 4 and studs 3.
When described device is applied to liquid-phase micro-extraction, the doughnut 7, U for bending to U-shaped is provided in sampling pipe 2 7 two ends of doughnut of shape are connected with hollow stainless steel filament 12, reserve on end cover 6 there are two hole, for it is hollow not Rust steel filament 12 passes through, and two ends are usually sealed with special rubber cap.
The end of the hollow stainless steel filament 12 is respectively connected with microsyringe 8.
Also reserved one is used to connect the insertion hole of cleaning syringe 11 on the end cover 6.
Embodiment 1
As shown in Figure 1 and Figure 2, drill bit 1 is connect by screw thread with sampling pipe 2, the other end of sealing double end spiral shell of sampling pipe 2 Column 3 is connect with tail pipe 5, and 5 outer end of tail pipe is provided with end cover 6;When applied to solid phase microextraction, the soil based on capillarity The channel 4 being arranged among aperture and tail pipe 5 is reserved with all on allelochemical in situ sampling-micro-extraction device end cover 6 Pass through for Solid Phase Extraction fiber 9;When applied to liquid-phase micro-extraction, the soil allelochemical in situ sampling-based on capillarity Micro-extraction device puts in one in sampling pipe 2 bends to U-shaped doughnut 7, microsyringe 8 is connected when extraction, at this time Channel 4 is used as the insertion channel of cleaning syringe 11.Wherein, sampling pipe 2 be both the soil liquid collector and micro- extraction The protection sleeve pipe in the place and extracting fiber that take, and since situ sampling device wants the depth of soil of indwelling different, so The length needs of tail pipe 5 are adjusted according to practical operation, achieve the purpose that micro-extraction is facilitated to operate.
As shown in Figure 1, device is applied to the development of solid phase microextraction: on soil liquid situ sampling device, end cover 6 On be reserved with aperture, the Solid Phase Extraction fiber 9 after lengthening, under the protection of micro-extraction protection needle tubing 10, across the double of rubber mass Header stud 3 stretches out Solid Phase Extraction fiber 9 after being inserted into sampling pipe 2;After completing extraction, Solid Phase Extraction fiber 9 is shunk, micro- extraction is extracted Device is taken, the instruments sample introduction such as GC-MS is directly used in.Aperture on end cover 6 is blocked by small rubber screw, sampling pipe 2 after In continuous indwelling soil.
As shown in Fig. 2, device is applied to the development of liquid-phase micro-extraction: putting in 1 and bent in U-shaped in sampling pipe 2 Hollow fiber 7 can inject several microlitres to several tens of microliters extraction phase (or receiving phase), the hollow fibre of U-shaped in it according to its length and internal diameter Two ends of dimension 7 are connected with hollow stainless steel filament 12, and two holes reserved by end cover 6, one end is inlet opening, The other end is fluid hole, and two ends of hollow stainless steel filament 12 are usually sealed with special rubber cap;Inlet opening one when extraction End connection microsyringe 8 injects extraction phase, and other end fluid hole is exported as extraction phase.It is not infused in two end certain lengths Enter extract liquor, is used for fluid column vibration mass transfer.The microsyringe 8 of one end applies pressure after the completion of extraction, and reception is mutually pumped into another The microsyringe 8 at end, the sample introduction for instruments such as GC-MS.In addition one is also reserved on end cover 6 for connecting cleaning note The insertion hole of emitter 11, to clean syringe entrance.
Embodiment 2
Using capsicum as model plant, soil allelochemical in situ sampling-micro-extraction device based on capillarity is placed in In five pottings of A, B, C, D, E, E is the soil that basin does not plant capsicum, is compareed as processing.Transplantation of seedlings first three days, every basin are daily Hereafter moisturizing 2L mends 1L water daily, facilitates absorption of the pipe to the soil liquid, continuous culture is collected after three weeks, sampling experiment: Gu Phase extraction, by the Solid Phase Extraction fiber 9 after lengthening, under the protection of micro-extraction protection needle tubing 10, across the double end of rubber mass Stud 3 stretches out extracting fiber 9 after being inserted into sampling pipe 2, after completing extraction, shrinks back extracting fiber 9, extracts micro-extraction device, directly It connects and is used for the instruments sample introductions such as GC-MS, the aperture on end cover 6 is blocked by small rubber screw, and sampling pipe 2 continues indwelling soil In;Liquid-phase micro-extraction puts in one in sampling pipe 2 and bends to U-shaped doughnut 7, injects 20 microlitres of extraction phases, in U-shaped Two ends of hollow fiber 7 are connected with hollow stainless steel filament 12, two holes reserved by end cover 6, one when extraction End connection microsyringe 8 injects extraction phase, and the other end is exported as extraction phase.Extraction is not injected into two end certain lengths Liquid is used for fluid column vibration mass transfer.The microsyringe 8 of one end applies pressure after the completion of extraction, receives and is mutually pumped into the micro- of the other end Measure sample injector 8, the sample introduction for instruments such as GC-MS.Liquid phase test result peak, which is concentrated, appears in 2min or so, peak area compared with Greatly, it was found that, the time of occurrence at peak is different, and peak area is also different, and the substance detected is different.The testing result of GC-MS Potential allelochemical (ketone, alcohols, phthalate, the adipic acid esters, phenol of the secretion of 31 kinds of capsicum root systems have been determined Class, aromatic hydrocarbon, alkane, alkene).
The foregoing is only a preferred embodiment of the present invention, these specific embodiments are all based on the present invention Different implementations under general idea, and scope of protection of the present invention is not limited thereto, it is any to be familiar with the art Technical staff in the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, should all cover of the invention Within protection scope.Therefore, the scope of protection of the invention shall be subject to the scope of protection specified in the patent claim.

Claims (7)

1. a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity characterized by comprising drill bit (1), sampling pipe (2), studs (3), channel (4), tail pipe (5) and end cover (6);
Wherein, drill bit (1) is connect by screw thread with sampling pipe (2) one end, has micropore, double end spiral shell on the tube wall of sampling pipe (2) Column (3) is the two-sided threaded cap of seal rubber of sampling pipe (2) other end, one end of sampling pipe (2) other end and studs (3) It is connected through a screw thread, the other end and the tail pipe (5) of studs (3) are connected through a screw thread, and the centre of tail pipe (5) is provided with channel (4), tail pipe (5) outer end is provided with end cover (6).
2. a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity according to claim 1, It is characterized in that, the sampling pipe (2) uses high wellability aluminium oxide, and alternating temperature sinters micropore ceramics sampling pipe, pore into repeatedly Diameter 0.05-100um, internal diameter 5-10mm, outer diameter 10-20mm, wall thickness 2-5mm, long 3-14cm, tube wall adsorption volume 3.54- 33.84cm3, hollow volume 1.18-12.02cm3
3. a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity according to claim 1, It is characterized in that, when described device is applied to solid phase microextraction, end cover is reserved with aperture on (6), for Solid Phase Extraction fiber (9) Pass through, when not in use, the aperture on end cover (6) is blocked by small rubber screw.
4. a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity according to claim 3, It is characterized in that, the Solid Phase Extraction fiber (9) is telescopic to be set in micro-extraction protection needle tubing (10), and micro-extraction protects needle tubing (10) end cover (6), channel (4) and studs (3) can be passed sequentially through.
5. a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity according to claim 1, It is characterized in that, when described device is applied to liquid-phase micro-extraction, is provided with the doughnut for bending to U-shaped in sampling pipe (2) (7), (7) two ends of the doughnut of U-shaped are connected with hollow stainless steel filament (12), on end cover (6) reserve there are two Hole passes through for hollow stainless steel filament (12), and two ends are usually sealed with special rubber cap.
6. a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity according to claim 5, It is characterized in that, the end of the hollow stainless steel filament (12) is respectively connected with microsyringe (8).
7. a kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity according to claim 5, It is characterized in that, also reserved one is used to connect the insertion hole of cleaning syringe (11) on the end cover (6).
CN201811277003.4A 2018-10-30 2018-10-30 A kind of soil allelochemical in situ sampling-micro-extraction device based on capillarity Pending CN109342111A (en)

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CN109765077A (en) * 2019-02-28 2019-05-17 中国科学院南京土壤研究所 A kind of root exudates sampler and sampling system
CN110514768A (en) * 2019-08-29 2019-11-29 河海大学 The ceramic tube sampler and the method for sampling acquired for polar organic matter in underground water
CN110887960A (en) * 2019-12-02 2020-03-17 电子科技大学 Urine test strip quantitative detection system and method based on machine vision
CN111076964A (en) * 2019-12-27 2020-04-28 中国科学院生态环境研究中心 In-situ collection device and method for soluble substances
CN111167152A (en) * 2019-12-25 2020-05-19 云南中烟工业有限责任公司 Method for measuring non-volatile organic acid and fatty acid in tobacco by micro extraction separation-gas chromatography
CN114570183A (en) * 2022-03-01 2022-06-03 西安热工研究院有限公司 Derivatization reaction device of urea hydrolysis sediment

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CN109765077A (en) * 2019-02-28 2019-05-17 中国科学院南京土壤研究所 A kind of root exudates sampler and sampling system
CN110514768A (en) * 2019-08-29 2019-11-29 河海大学 The ceramic tube sampler and the method for sampling acquired for polar organic matter in underground water
CN110887960A (en) * 2019-12-02 2020-03-17 电子科技大学 Urine test strip quantitative detection system and method based on machine vision
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CN111167152B (en) * 2019-12-25 2022-02-01 云南中烟工业有限责任公司 Method for measuring non-volatile organic acid and fatty acid in tobacco by micro extraction separation-gas chromatography
CN111076964A (en) * 2019-12-27 2020-04-28 中国科学院生态环境研究中心 In-situ collection device and method for soluble substances
CN111076964B (en) * 2019-12-27 2021-04-06 中国科学院生态环境研究中心 In-situ collection device and method for soluble substances
CN114570183A (en) * 2022-03-01 2022-06-03 西安热工研究院有限公司 Derivatization reaction device of urea hydrolysis sediment

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Application publication date: 20190215