CN110146559A - A kind of soil pollution detection method - Google Patents
A kind of soil pollution detection method Download PDFInfo
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- CN110146559A CN110146559A CN201910368283.8A CN201910368283A CN110146559A CN 110146559 A CN110146559 A CN 110146559A CN 201910368283 A CN201910368283 A CN 201910368283A CN 110146559 A CN110146559 A CN 110146559A
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- 238000001514 detection method Methods 0.000 title claims abstract description 28
- 238000003900 soil pollution Methods 0.000 title claims abstract description 20
- 239000002689 soil Substances 0.000 claims abstract description 86
- 238000001035 drying Methods 0.000 claims abstract description 36
- 239000000706 filtrate Substances 0.000 claims abstract description 30
- 238000001179 sorption measurement Methods 0.000 claims abstract description 19
- 238000005259 measurement Methods 0.000 claims abstract description 9
- 238000000909 electrodialysis Methods 0.000 claims abstract description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 60
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 58
- 239000000047 product Substances 0.000 claims description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 238000004090 dissolution Methods 0.000 claims description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000003480 eluent Substances 0.000 claims description 21
- 229920000642 polymer Polymers 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 238000002242 deionisation method Methods 0.000 claims description 8
- 239000003208 petroleum Substances 0.000 claims description 8
- 230000001376 precipitating effect Effects 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000502 dialysis Methods 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- 239000005457 ice water Substances 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000000178 monomer Substances 0.000 claims description 7
- 230000010494 opalescence Effects 0.000 claims description 7
- 239000008363 phosphate buffer Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 230000003068 static effect Effects 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 2
- 239000005864 Sulphur Substances 0.000 claims 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 241001062009 Indigofera Species 0.000 description 6
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 6
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 6
- 235000011130 ammonium sulphate Nutrition 0.000 description 6
- 230000005518 electrochemistry Effects 0.000 description 6
- 230000000977 initiatory effect Effects 0.000 description 6
- 238000003808 methanol extraction Methods 0.000 description 6
- 229920000767 polyaniline Polymers 0.000 description 6
- AUZRCMMVHXRSGT-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CC(C)CS(O)(=O)=O AUZRCMMVHXRSGT-UHFFFAOYSA-N 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 4
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 4
- 206010028980 Neoplasm Diseases 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000010871 livestock manure Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- AXFBAIOSECPASO-UHFFFAOYSA-N pentacyclo[6.6.2.02,7.04,16.011,15]hexadeca-1(14),2(7),3,5,8(16),9,11(15),12-octaene Chemical compound C1=C(C=C23)C4=C5C3=CC=CC5=CC=C4C2=C1 AXFBAIOSECPASO-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000003802 soil pollutant Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to Soil K+adsorption technical fields, and in particular to a kind of soil pollution detection method, comprising the following steps: S1 soil collection: the drying of S2 soil；S3: soil is ground up, sieved；S4: centrifugal filtration；S5: filtrate electrodialysis；S6: filtrate pH adjusting and electrochemical sensor impregnate drying；S7: electrochemical sensor peak current measurement；The present invention can be realized BaP content in soil and fast and accurately measure, and improve the detection efficiency of BaP in soil, have biggish application prospect, be suitable for further genralrlization application.
Description
Technical field
The present invention relates to Soil K+adsorption technical fields, and in particular to a kind of soil pollution detection method.
Background technique
Soil pollutant is broadly divided into inorganic pollution and organic pollutant two major classes.Inorganic pollution mainly includes
Acid, alkali, heavy metal, salt, radioactive element caesium, the compound of strontium, containing arsenic, selenium, compound of fluorine etc..Organic pollutant is main
Including organic agricultural chemicals, phenols, cyanide, petroleum, synthetic detergent, 3,4- BaP and by municipal sewage, sludge and barnyard manure
Bring harmful microorganism etc..It is excessive when containing hazardous substance in soil, more than the self-purification capacity of soil, the group of soil will be caused
It changes at, structure and function, microbial activities is suppressed, and harmful substance or its decomposition product gradually accumulate in the soil
It is absorbed by the body indirectly by " soil → plant → human body ", or by " soil → water → human body ", reaches and be detrimental to health
Degree, be exactly soil pollution.
BaP is also known as benzo (α) pyrene, is a kind of common high activity indirect-acting carcinogen.It enters by breathing or diet
After in vivo, it is easy to and the DNA of people is combined, and has upset the synthesis program of human body protein.It plays in the activity of DNA
The role of one " trigger ": as long as the other BaP of extremely micro-nanogram level, so that it may change structure, direction and the function of DNA；
The DNA of BaP is combined, the cell of synthesis is no longer normal cell, but tumour, also has led to cancer.It in water body,
Residual is all easy in soil and crop.
Nowadays, it is many country also all carry out soil in BaP content investigation.The detection side of BaP content at present
Method higher cost, and detection time is longer.
Summary of the invention
In view of the above problems, the present invention provides a kind of soil pollution detection method, this kind of detection method can be realized soil
BaP content fast and accurately measures in earth, improves the detection efficiency of BaP in soil, before having biggish application
Scape.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of soil pollution detection method, comprising the following steps:
S1: selection Soil K+adsorption region, and soil collection is carried out in the region；
S2: it takes out in appropriate soil placement drying box and is dried；
S3: the pedotheque after drying being put into ball mill and is ground, and 150-200 mesh is crossed after grinding；
S4: the 20-30 times of deionized water solution measured of addition into the pedotheque after grinding, ultrasonic mixing 30-45min,
Then suspension is centrifuged, filtered, obtain clear filtrate；
S5: obtained clear filtrate is subjected to the ion in electrodialysis removing filtrate；
S6: 0.1M phosphate buffer is added into the filtrate after deionization, pH is adjusted to 7.0, then pass electrochemistry
Sensor is impregnated in above-mentioned solution, is taken out and is dried after impregnating 10-15min；
S7: the measurement of peak point current is carried out to the electrochemical sensor after drying using electrochemical analyser.
Preferably, soil collection method is as follows in S1:
A) prior to selecting multiple sample points in Soil K+adsorption region；
B) collecting soil sample is carried out at multiple sample points using snakelike method of layouting, when acquisition takes 0-25cm topsoil
Mixing sample；
C) soil of one group of sample point is taken individually to be detected, the soil of remaining sample point after mixing, by aggregate sample
It is detected.
Preferably, the water content after drying in S2 in soil should be less than 4%.
Preferably, electrochemical sensor described in S6 preparation method the following steps are included:
1) p styrene sulfonic acid, styrene are sequentially added into flask at room temperature, azodiisobutyronitrile is subsequently added into appropriate
Dimethylformamide, is stirred dissolution, and nitrogen is passed through into flask and excludes air, sealing, is then reacted in 85 DEG C of oil baths
Cooling blowing air, then settles out product using petroleum ether as precipitating reagent, repeatedly for three times after 12h；Products therefrom continue dissolution and
It dialyses in deionized water, freeze-drying obtains product A；
2) dimethylformamide stirring and dissolving is added to product A at room temperature, it is molten is configured to the polymer that concentration is 50mg/ml
Liquid is added dropwise to deionized water into polymer solution under conditions of being stirred continuously with the speed of 1-2ml/s, when in solution go out
Stop being added dropwise and continue to stir 5-8h after existing indigo plant opalescence, then to being added dropwise to a large amount of water in above-mentioned solution gradually with micella of being formed,
Stirring 3-5h is then continued to, solution is then encased in bag filter the 3-5d that dialyses, the dimethylformamide in solution is removed, connects
That the solution after dialysis is settled to 5mg/ml is stand-by；
3) solution of above-mentioned 5mg/ml is added in flask, nitrogen discharge air is passed through into flask, then to solution
Middle addition BaP, 2- acrylamide-2-methyl propane sulfonic and aniline are stirred dissolution, to add after completely dissolution into solution
Enter ammonium sulfate initiation aniline to be polymerize, mixed liquor reacts 15-18h in ice-water bath, then takes out reaction product, and respectively
Three times through methanol extraction, centrifuge separation, product B is obtained；
4) be added and eluent and be stirred into product B, room temperature it is static for 24 hours after, reuse eluent and clean 3-5 times,
The BaP being wrapped in long-chain molecule is eluted, the product after cleaning is uniformly applied on Au electrode, then again will
Au electrode carries out room temperature aeration-drying, and above-mentioned electrochemical sensor is made.
Preferably, 1:2.4-2.5 is added p styrene sulfonic acid described in step 1) in molar ratio with styrene, described
Azodiisobutyronitrile is the 1% of reaction monomers integral molar quantity.
Preferably, the molar ratio of aniline described in step 3) and p styrene sulfonic acid segment in solution is 1:0.5-10；Institute
State aniline, BaP and 2- acrylamide-2-methyl propane sulfonic is 1:3-5:1 in molar ratio.
Preferably, by methanol, 8:2 is mixed eluent described in step 4) by volume with acetic acid.
Preferably, the smearing thickness of Au electrode surface wash products is 30-80 μm in step 4).
The utility model has the advantages that
1, the present invention can effectively avoid misleading of the specific region to Soil K+adsorption by specific soil sample method, protect
The accuracy for having demonstrate,proved Soil K+adsorption reduces the analysis time of soil, effectively increases Soil K+adsorption efficiency.
2, the electrochemical sensor in the present invention is built-up by Nano particles of polyaniline, by that will gather in preparation process
The BaP elution wrapped up in aniline nano particle, makes to leave on Nano particles of polyaniline and BaP molecular shape, size, electricity
Lotus distribution has complementary hole, and hole is enable to have preferable specific recognition ability and sensitivity to BaP, separately due to
The polyaniline of nanostructure has big specific surface area, therefore electrochemical sensor can be to BaP sensitivity with higher
With faster response speed；When BaP is combined with the hole on Nano particles of polyaniline, BaP and polyaniline nano
Strand in particle can have interaction, the electron transport ability of polyaniline be improved, to enhance the strong of electric signal
Degree；Peak current that electrochemical sensor detects can be carried out using this kind of characteristic corresponding with the concentration of BaP, facilitate benzene
And the detection of pyrene concentration.
3, it is able to carry out reuse through elution processing after electrochemical sensor detection in the present invention, reduces benzene in soil
And the testing cost of pyrene, there is biggish application prospect and commercial value.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of soil pollution detection method, comprising the following steps:
S1: selection Soil K+adsorption region, and soil collection is carried out in the region；
S2: it takes out in appropriate soil placement drying box and is dried；
S3: the pedotheque after drying being put into ball mill and is ground, and 150-200 mesh is crossed after grinding；
S4: the 20-30 times of deionized water solution measured of addition into the pedotheque after grinding, ultrasonic mixing 30-45min,
Then suspension is centrifuged, filtered, obtain clear filtrate；
S5: obtained clear filtrate is subjected to the ion in electrodialysis removing filtrate；
S6: 0.1M phosphate buffer is added into the filtrate after deionization, pH is adjusted to 7.0, then pass electrochemistry
Sensor is impregnated in above-mentioned solution, is taken out and is dried after impregnating 10-15min；
S7: the measurement of peak point current is carried out to the electrochemical sensor after drying using electrochemical analyser.
Soil collection method is as follows in S1:
A) prior to selecting multiple sample points in Soil K+adsorption region；
B) collecting soil sample is carried out at multiple sample points using snakelike method of layouting, when acquisition takes 0-25cm topsoil
Mixing sample；
C) soil of one group of sample point is taken individually to be detected, the soil of remaining sample point after mixing, by aggregate sample
It is detected.
Water content after drying in S2 in soil should be less than 4%.
In S6 electrochemical sensor preparation method the following steps are included:
1) p styrene sulfonic acid, styrene are sequentially added into flask at room temperature, azodiisobutyronitrile is subsequently added into appropriate
Dimethylformamide, is stirred dissolution, and nitrogen is passed through into flask and excludes air, sealing, is then reacted in 85 DEG C of oil baths
Cooling blowing air, then settles out product using petroleum ether as precipitating reagent, repeatedly for three times after 12h；Products therefrom continue dissolution and
It dialyses in deionized water, freeze-drying obtains product A；
2) dimethylformamide stirring and dissolving is added to product A at room temperature, it is molten is configured to the polymer that concentration is 50mg/ml
Liquid is added dropwise to deionized water into polymer solution under conditions of being stirred continuously with the speed of 1-2ml/s, when in solution go out
Stop being added dropwise and continue to stir 5-8h after existing indigo plant opalescence, then to being added dropwise to a large amount of water in above-mentioned solution gradually with micella of being formed,
Stirring 3-5h is then continued to, solution is then encased in bag filter the 3-5d that dialyses, the dimethylformamide in solution is removed, connects
That the solution after dialysis is settled to 5mg/ml is stand-by；
3) solution of above-mentioned 5mg/ml is added in flask, nitrogen discharge air is passed through into flask, then to solution
Middle addition BaP, 2- acrylamide-2-methyl propane sulfonic and aniline are stirred dissolution, to add after completely dissolution into solution
Enter ammonium sulfate initiation aniline to be polymerize, mixed liquor reacts 15-18h in ice-water bath, then takes out reaction product, and respectively
Three times through methanol extraction, centrifuge separation, product B is obtained；
4) be added and eluent and be stirred into product B, room temperature it is static for 24 hours after, reuse eluent and clean 3-5 times,
The BaP being wrapped in long-chain molecule is eluted, the product after cleaning is uniformly applied on Au electrode, then again will
Au electrode carries out room temperature aeration-drying, and above-mentioned electrochemical sensor is made.
1:2.4 is added p styrene sulfonic acid in molar ratio with styrene in step 1), and azodiisobutyronitrile is reaction
The 1% of monomer integral molar quantity.
The molar ratio of aniline and p styrene sulfonic acid segment in solution is 1:0.5 in step 3)；Aniline, BaP and 2- third
Acrylamide -2- methyl propane sulfonic acid is 1:3:1 in molar ratio.
By methanol, 8:2 is mixed eluent by volume with acetic acid in step 4).
The smearing thickness of Au electrode surface wash products is 30-80 μm in step 4).
Embodiment 2:
A kind of soil pollution detection method, comprising the following steps:
S1: selection Soil K+adsorption region, and soil collection is carried out in the region；
S2: it takes out in appropriate soil placement drying box and is dried；
S3: the pedotheque after drying being put into ball mill and is ground, and 150-200 mesh is crossed after grinding；
S4: the 20-30 times of deionized water solution measured of addition into the pedotheque after grinding, ultrasonic mixing 30-45min,
Then suspension is centrifuged, filtered, obtain clear filtrate；
S5: obtained clear filtrate is subjected to the ion in electrodialysis removing filtrate；
S6: 0.1M phosphate buffer is added into the filtrate after deionization, pH is adjusted to 7.0, then pass electrochemistry
Sensor is impregnated in above-mentioned solution, is taken out and is dried after impregnating 10-15min；
S7: the measurement of peak point current is carried out to the electrochemical sensor after drying using electrochemical analyser.
Soil collection method is as follows in S1:
A) prior to selecting multiple sample points in Soil K+adsorption region；
B) collecting soil sample is carried out at multiple sample points using snakelike method of layouting, when acquisition takes 0-25cm topsoil
Mixing sample；
C) soil of one group of sample point is taken individually to be detected, the soil of remaining sample point after mixing, by aggregate sample
It is detected.
Water content after drying in S2 in soil should be less than 4%.
In S6 electrochemical sensor preparation method the following steps are included:
1) p styrene sulfonic acid, styrene are sequentially added into flask at room temperature, azodiisobutyronitrile is subsequently added into appropriate
Dimethylformamide, is stirred dissolution, and nitrogen is passed through into flask and excludes air, sealing, is then reacted in 85 DEG C of oil baths
Cooling blowing air, then settles out product using petroleum ether as precipitating reagent, repeatedly for three times after 12h；Products therefrom continue dissolution and
It dialyses in deionized water, freeze-drying obtains product A；
2) dimethylformamide stirring and dissolving is added to product A at room temperature, it is molten is configured to the polymer that concentration is 50mg/ml
Liquid is added dropwise to deionized water into polymer solution under conditions of being stirred continuously with the speed of 1-2ml/s, when in solution go out
Stop being added dropwise and continue to stir 5-8h after existing indigo plant opalescence, then to being added dropwise to a large amount of water in above-mentioned solution gradually with micella of being formed,
Stirring 3-5h is then continued to, solution is then encased in bag filter the 3-5d that dialyses, the dimethylformamide in solution is removed, connects
That the solution after dialysis is settled to 5mg/ml is stand-by；
3) solution of above-mentioned 5mg/ml is added in flask, nitrogen discharge air is passed through into flask, then to solution
Middle addition BaP, 2- acrylamide-2-methyl propane sulfonic and aniline are stirred dissolution, to add after completely dissolution into solution
Enter ammonium sulfate initiation aniline to be polymerize, mixed liquor reacts 15-18h in ice-water bath, then takes out reaction product, and respectively
Three times through methanol extraction, centrifuge separation, product B is obtained；
4) be added and eluent and be stirred into product B, room temperature it is static for 24 hours after, reuse eluent and clean 3-5 times,
The BaP being wrapped in long-chain molecule is eluted, the product after cleaning is uniformly applied on Au electrode, then again will
Au electrode carries out room temperature aeration-drying, and above-mentioned electrochemical sensor is made.
1:2.5 is added p styrene sulfonic acid in molar ratio with styrene in step 1), and azodiisobutyronitrile is reaction
The 1% of monomer integral molar quantity.
The molar ratio of aniline and p styrene sulfonic acid segment in solution is 1:10 in step 3)；Aniline, BaP and 2- third
Acrylamide -2- methyl propane sulfonic acid is 1:4:1 in molar ratio.
By methanol, 8:2 is mixed eluent by volume with acetic acid in step 4).
The smearing thickness of Au electrode surface wash products is 30-80 μm in step 4).
Embodiment 3:
A kind of soil pollution detection method, comprising the following steps:
S1: selection Soil K+adsorption region, and soil collection is carried out in the region；
S2: it takes out in appropriate soil placement drying box and is dried；
S3: the pedotheque after drying being put into ball mill and is ground, and 150-200 mesh is crossed after grinding；
S4: the 20-30 times of deionized water solution measured of addition into the pedotheque after grinding, ultrasonic mixing 30-45min,
Then suspension is centrifuged, filtered, obtain clear filtrate；
S5: obtained clear filtrate is subjected to the ion in electrodialysis removing filtrate；
S6: 0.1M phosphate buffer is added into the filtrate after deionization, pH is adjusted to 7.0, then pass electrochemistry
Sensor is impregnated in above-mentioned solution, is taken out and is dried after impregnating 10-15min；
S7: the measurement of peak point current is carried out to the electrochemical sensor after drying using electrochemical analyser.
Soil collection method is as follows in S1:
A) prior to selecting multiple sample points in Soil K+adsorption region；
B) collecting soil sample is carried out at multiple sample points using snakelike method of layouting, when acquisition takes 0-25cm topsoil
Mixing sample；
C) soil of one group of sample point is taken individually to be detected, the soil of remaining sample point after mixing, by aggregate sample
It is detected.
Water content after drying in S2 in soil should be less than 4%.
In S6 electrochemical sensor preparation method the following steps are included:
1) p styrene sulfonic acid, styrene are sequentially added into flask at room temperature, azodiisobutyronitrile is subsequently added into appropriate
Dimethylformamide, is stirred dissolution, and nitrogen is passed through into flask and excludes air, sealing, is then reacted in 85 DEG C of oil baths
Cooling blowing air, then settles out product using petroleum ether as precipitating reagent, repeatedly for three times after 12h；Products therefrom continue dissolution and
It dialyses in deionized water, freeze-drying obtains product A；
2) dimethylformamide stirring and dissolving is added to product A at room temperature, it is molten is configured to the polymer that concentration is 50mg/ml
Liquid is added dropwise to deionized water into polymer solution under conditions of being stirred continuously with the speed of 1-2ml/s, when in solution go out
Stop being added dropwise and continue to stir 5-8h after existing indigo plant opalescence, then to being added dropwise to a large amount of water in above-mentioned solution gradually with micella of being formed,
Stirring 3-5h is then continued to, solution is then encased in bag filter the 3-5d that dialyses, the dimethylformamide in solution is removed, connects
That the solution after dialysis is settled to 5mg/ml is stand-by；
3) solution of above-mentioned 5mg/ml is added in flask, nitrogen discharge air is passed through into flask, then to solution
Middle addition BaP, 2- acrylamide-2-methyl propane sulfonic and aniline are stirred dissolution, to add after completely dissolution into solution
Enter ammonium sulfate initiation aniline to be polymerize, mixed liquor reacts 15-18h in ice-water bath, then takes out reaction product, and respectively
Three times through methanol extraction, centrifuge separation, product B is obtained；
4) be added and eluent and be stirred into product B, room temperature it is static for 24 hours after, reuse eluent and clean 3-5 times,
The BaP being wrapped in long-chain molecule is eluted, the product after cleaning is uniformly applied on Au electrode, then again will
Au electrode carries out room temperature aeration-drying, and above-mentioned electrochemical sensor is made.
1:2.4 is added p styrene sulfonic acid in molar ratio with styrene in step 1), and azodiisobutyronitrile is reaction
The 1% of monomer integral molar quantity.
The molar ratio of aniline and p styrene sulfonic acid segment in solution is 1:3.5 in step 3)；Aniline, BaP and 2- third
Acrylamide -2- methyl propane sulfonic acid is 1:5:1 in molar ratio.
By methanol, 8:2 is mixed eluent by volume with acetic acid in step 4).
The smearing thickness of Au electrode surface wash products is 30-80 μm in step 4).
Embodiment 4:
A kind of soil pollution detection method, comprising the following steps:
S1: selection Soil K+adsorption region, and soil collection is carried out in the region；
S2: it takes out in appropriate soil placement drying box and is dried；
S3: the pedotheque after drying being put into ball mill and is ground, and 150-200 mesh is crossed after grinding；
S4: the 20-30 times of deionized water solution measured of addition into the pedotheque after grinding, ultrasonic mixing 30-45min,
Then suspension is centrifuged, filtered, obtain clear filtrate；
S5: obtained clear filtrate is subjected to the ion in electrodialysis removing filtrate；
S6: 0.1M phosphate buffer is added into the filtrate after deionization, pH is adjusted to 7.0, then pass electrochemistry
Sensor is impregnated in above-mentioned solution, is taken out and is dried after impregnating 10-15min；
S7: the measurement of peak point current is carried out to the electrochemical sensor after drying using electrochemical analyser.
Soil collection method is as follows in S1:
A) prior to selecting multiple sample points in Soil K+adsorption region；
B) collecting soil sample is carried out at multiple sample points using snakelike method of layouting, when acquisition takes 0-25cm topsoil
Mixing sample；
C) soil of one group of sample point is taken individually to be detected, the soil of remaining sample point after mixing, by aggregate sample
It is detected.
Water content after drying in S2 in soil should be less than 4%.
In S6 electrochemical sensor preparation method the following steps are included:
1) p styrene sulfonic acid, styrene are sequentially added into flask at room temperature, azodiisobutyronitrile is subsequently added into appropriate
Dimethylformamide, is stirred dissolution, and nitrogen is passed through into flask and excludes air, sealing, is then reacted in 85 DEG C of oil baths
Cooling blowing air, then settles out product using petroleum ether as precipitating reagent, repeatedly for three times after 12h；Products therefrom continue dissolution and
It dialyses in deionized water, freeze-drying obtains product A；
2) dimethylformamide stirring and dissolving is added to product A at room temperature, it is molten is configured to the polymer that concentration is 50mg/ml
Liquid is added dropwise to deionized water into polymer solution under conditions of being stirred continuously with the speed of 1-2ml/s, when in solution go out
Stop being added dropwise and continue to stir 5-8h after existing indigo plant opalescence, then to being added dropwise to a large amount of water in above-mentioned solution gradually with micella of being formed,
Stirring 3-5h is then continued to, solution is then encased in bag filter the 3-5d that dialyses, the dimethylformamide in solution is removed, connects
That the solution after dialysis is settled to 5mg/ml is stand-by；
3) solution of above-mentioned 5mg/ml is added in flask, nitrogen discharge air is passed through into flask, then to solution
Middle addition BaP, 2- acrylamide-2-methyl propane sulfonic and aniline are stirred dissolution, to add after completely dissolution into solution
Enter ammonium sulfate initiation aniline to be polymerize, mixed liquor reacts 15-18h in ice-water bath, then takes out reaction product, and respectively
Three times through methanol extraction, centrifuge separation, product B is obtained；
4) be added and eluent and be stirred into product B, room temperature it is static for 24 hours after, reuse eluent and clean 3-5 times,
The BaP being wrapped in long-chain molecule is eluted, the product after cleaning is uniformly applied on Au electrode, then again will
Au electrode carries out room temperature aeration-drying, and above-mentioned electrochemical sensor is made.
1:2.5 is added p styrene sulfonic acid in molar ratio with styrene in step 1), and azodiisobutyronitrile is reaction
The 1% of monomer integral molar quantity.
The molar ratio of aniline and p styrene sulfonic acid segment in solution is 1:6.5 in step 3)；Aniline, BaP and 2- third
Acrylamide -2- methyl propane sulfonic acid is 1:5:1 in molar ratio.
By methanol, 8:2 is mixed eluent by volume with acetic acid in step 4).
The smearing thickness of Au electrode surface wash products is 30-80 μm in step 4).
Embodiment 5:
A kind of soil pollution detection method, comprising the following steps:
S1: selection Soil K+adsorption region, and soil collection is carried out in the region；
S2: it takes out in appropriate soil placement drying box and is dried；
S3: the pedotheque after drying being put into ball mill and is ground, and 150-200 mesh is crossed after grinding；
S4: the 20-30 times of deionized water solution measured of addition into the pedotheque after grinding, ultrasonic mixing 30-45min,
Then suspension is centrifuged, filtered, obtain clear filtrate；
S5: obtained clear filtrate is subjected to the ion in electrodialysis removing filtrate；
S6: 0.1M phosphate buffer is added into the filtrate after deionization, pH is adjusted to 7.0, then pass electrochemistry
Sensor is impregnated in above-mentioned solution, is taken out and is dried after impregnating 10-15min；
S7: the measurement of peak point current is carried out to the electrochemical sensor after drying using electrochemical analyser.
Soil collection method is as follows in S1:
A) prior to selecting multiple sample points in Soil K+adsorption region；
B) collecting soil sample is carried out at multiple sample points using snakelike method of layouting, when acquisition takes 0-25cm topsoil
Mixing sample；
C) soil of one group of sample point is taken individually to be detected, the soil of remaining sample point after mixing, by aggregate sample
It is detected.
Water content after drying in S2 in soil should be less than 4%.
In S6 electrochemical sensor preparation method the following steps are included:
1) p styrene sulfonic acid, styrene are sequentially added into flask at room temperature, azodiisobutyronitrile is subsequently added into appropriate
Dimethylformamide, is stirred dissolution, and nitrogen is passed through into flask and excludes air, sealing, is then reacted in 85 DEG C of oil baths
Cooling blowing air, then settles out product using petroleum ether as precipitating reagent, repeatedly for three times after 12h；Products therefrom continue dissolution and
It dialyses in deionized water, freeze-drying obtains product A；
2) dimethylformamide stirring and dissolving is added to product A at room temperature, it is molten is configured to the polymer that concentration is 50mg/ml
Liquid is added dropwise to deionized water into polymer solution under conditions of being stirred continuously with the speed of 1-2ml/s, when in solution go out
Stop being added dropwise and continue to stir 5-8h after existing indigo plant opalescence, then to being added dropwise to a large amount of water in above-mentioned solution gradually with micella of being formed,
Stirring 3-5h is then continued to, solution is then encased in bag filter the 3-5d that dialyses, the dimethylformamide in solution is removed, connects
That the solution after dialysis is settled to 5mg/ml is stand-by；
3) solution of above-mentioned 5mg/ml is added in flask, nitrogen discharge air is passed through into flask, then to solution
Middle addition BaP, 2- acrylamide-2-methyl propane sulfonic and aniline are stirred dissolution, to add after completely dissolution into solution
Enter ammonium sulfate initiation aniline to be polymerize, mixed liquor reacts 15-18h in ice-water bath, then takes out reaction product, and respectively
Three times through methanol extraction, centrifuge separation, product B is obtained；
4) be added and eluent and be stirred into product B, room temperature it is static for 24 hours after, reuse eluent and clean 3-5 times,
The BaP being wrapped in long-chain molecule is eluted, the product after cleaning is uniformly applied on Au electrode, then again will
Au electrode carries out room temperature aeration-drying, and above-mentioned electrochemical sensor is made.
1:2.4 is added p styrene sulfonic acid in molar ratio with styrene in step 1), and azodiisobutyronitrile is reaction
The 1% of monomer integral molar quantity.
The molar ratio of aniline and p styrene sulfonic acid segment in solution is 1:8.5 in step 3)；Aniline, BaP and 2- third
Acrylamide -2- methyl propane sulfonic acid is 1:3:1 in molar ratio.
By methanol, 8:2 is mixed eluent by volume with acetic acid in step 4).
The smearing thickness of Au electrode surface wash products is 30-80 μm in step 4).
Data Detection:
The electrochemical sensor prepared using each embodiment is respectively to 0.0004mM；0.015mM；0.035mM；0.080mM；
0.5mM；0.8mM；1.5mM；The BaP of 2mM carries out the measurement of peak point current, and testing result is as follows:
Wherein peak current and BaP concentration meet linear equation: ip (μ A)=15.82*C+4.462, wherein C: BaP
Concentration (mM).
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (8)
1. a kind of soil pollution detection method, which comprises the following steps:
S1: selection Soil K+adsorption region, and soil collection is carried out in the region；
S2: it takes out in appropriate soil placement drying box and is dried；
S3: the pedotheque after drying being put into ball mill and is ground, and 150-200 mesh is crossed after grinding；
S4: the 20-30 times of deionized water solution measured of addition into the pedotheque after grinding, ultrasonic mixing 30-45min, then
Suspension is centrifuged, is filtered, clear filtrate is obtained；
S5: obtained clear filtrate is subjected to the ion in electrodialysis removing filtrate；
S6: 0.1M phosphate buffer is added into the filtrate after deionization, pH is adjusted to 7.0, then by electrochemical sensor
It is impregnated in above-mentioned solution, takes out and be dried after impregnating 10-15min；
S7: the measurement of peak point current is carried out to the electrochemical sensor after drying using electrochemical analyser.
2. a kind of soil pollution detection method according to claim 1, it is characterised in that: soil collection method is such as in S1
Under:
A) prior to selecting multiple sample points in Soil K+adsorption region；
B) collecting soil sample is carried out at multiple sample points using snakelike method of layouting, when acquisition takes the mixed of 0-25cm topsoil
Close sample；
C) soil of one group of sample point is taken individually to be detected, after mixing, aggregate sample is carried out for the soil of remaining sample point
Detection.
3. a kind of soil pollution detection method according to claim 1, it is characterised in that: containing in soil after being dried in S2
Water should be less than 4%.
4. a kind of soil pollution detection method according to claim 1, it is characterised in that: electrochemical sensor described in S6
Preparation method the following steps are included:
1) p styrene sulfonic acid, styrene are sequentially added into flask at room temperature, azodiisobutyronitrile is subsequently added into appropriate diformazan
Base formamide, is stirred dissolution, and nitrogen is passed through into flask and excludes air, sealing, after then reacting 12h in 85 DEG C of oil baths
Cooling blowing air, then settles out product using petroleum ether as precipitating reagent, repeatedly for three times；Products therefrom continues dissolution and in deionization
It dialyses in water, freeze-drying obtains product A；
2) dimethylformamide stirring and dissolving is added to product A at room temperature, is configured to the polymer solution that concentration is 50mg/ml,
Under conditions of being stirred continuously, deionized water is added dropwise into polymer solution with the speed of 1-2ml/s, it is blue when occurring in solution
Stop being added dropwise and continue to stir 5-8h after opalescence, then to being gradually added dropwise to a large amount of water in above-mentioned solution with micella of being formed, then
Continue to stir 3-5h, solution is then encased in bag filter the 3-5d that dialyses, remove the dimethylformamide in solution, then will
It is stand-by that solution after dialysis is settled to 5mg/ml；
3) solution of above-mentioned 5mg/ml is added in flask, nitrogen discharge air is passed through into flask, is then added into solution
Enter BaP, 2- acrylamide-2-methyl propane sulfonic and aniline and be stirred dissolution, to which sulphur is added into solution after completely dissolution
Sour ammonium causes aniline and is polymerize, and mixed liquor reacts 15-18h in ice-water bath, then takes out reaction product, and respectively through first
Alcohol precipitating, centrifuge separation three times, obtain product B；
4) be added and eluent and be stirred into product B, room temperature it is static for 24 hours after, reuse eluent and clean 3-5 times, will wrap
The BaP being rolled in long-chain molecule is eluted, and the product after cleaning is uniformly applied on Au electrode, then again by Au electricity
Pole carries out room temperature aeration-drying, and above-mentioned electrochemical sensor is made.
5. a kind of soil pollution detection method according to claim 4, it is characterised in that: to styrene described in step 1)
1:2.4-2.5 is added sulfonic acid in molar ratio with styrene, and the azodiisobutyronitrile is reaction monomers integral molar quantity
1%.
6. a kind of soil pollution detection method according to claim 4, it is characterised in that: aniline described in step 3) with it is molten
The molar ratio of p styrene sulfonic acid segment is 1:0.5-10 in liquid；The aniline, BaP and 2- acrylamide -2- methyl-prop sulphur
Acid is 1:3-5:1 in molar ratio.
7. a kind of soil pollution detection method according to claim 4, it is characterised in that: eluent described in step 4) by
8:2 is mixed methanol by volume with acetic acid.
8. a kind of soil pollution detection method according to claim 4, it is characterised in that: Au electrode surface is clear in step 4)
The smearing thickness for washing product is 30-80 μm.
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