CN109682789A - A kind of in-situ detection method of micro- frosting absorption pollutant - Google Patents
A kind of in-situ detection method of micro- frosting absorption pollutant Download PDFInfo
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- CN109682789A CN109682789A CN201811592752.6A CN201811592752A CN109682789A CN 109682789 A CN109682789 A CN 109682789A CN 201811592752 A CN201811592752 A CN 201811592752A CN 109682789 A CN109682789 A CN 109682789A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The present invention provides a kind of in-situ detection methods of micro- frosting absorption pollutant comprising following steps: (1) preparation has the nano silver colloidal sol of SERS effect；(2) liquor kalii iodide of the nano silver colloidal sol and 0.1mol/L that prepare in micro methanol, (1) step is successively added dropwise in the micro- frosting for being adsorbed with pollutant.(3) the drop convex surface highest point for making laser focus on extract liquor, enhance substrate and coagulant mixed liquor acquires Raman spectrum；(4) method for combining Chemical Measurement establishes the quick predict model of micro- frosting absorption pollutant using the peak height of organic pollutant raman characteristic peak and peak area as variable.This method synchronizes the extraction and signal enhancing process for realizing micro- frosting pollutant, step is simple, chemical reagent consumption is few, detection time is short, quick, the in situ detection that micro- frosting persistence organic pollutant can be achieved are with a wide range of applications in persistence organic pollutant monitoring field.
Description
Technical field
The invention belongs to environmental contaminants in situ detection fields, are related to a kind of original of micro- frosting absorption organic pollutant
Position detecting method, the specifically synchronous situ extracting for realizing micro- frosting organic pollutant and the enhancing for detecting signal, benefit
It is realized with Surface enhanced Raman spectroscopy (Surface Enhance Raman Spectroscopy, SERS) technology to micro- plastic table
The organic pollutant in face is in situ, quickly detects.
Background technique
Cause society's more and more extensive concern the problem of plastic garbage is assembled in marine environment in recent years.Plastics are extremely strong
Stability, cause it to be difficult as other substances the natural degradation under physics, chemistry and biological effect in the environment, therefore
Plastics can persistently have the time of upper a century in the environment, and lasting influence ecological environment around it.In environment
Plastics can occur under the compound influence UV sunlight radiation, mechanical damage, the weathering Erosion, biodegrade the effects of it is broken,
Partial size < 5mm micro plastic is formed, is defined as " micro- plastics " in most of document.
Micro- plastics are difficult to degrade in the natural environment, and higher specific surface area and hydrophobic performance, make it easily will be in environment
Heavy metal, persistence organic pollutant, antibiotic etc. be enriched in surface, and can be influenced by diffusion mobilities such as wind-force, ocean currents
The distribution on global of pollutant.The Polychlorinated biphenyls for having researched and analysed multiple micro- frostings of countries and regions littoral zone before has
The pollutants such as machine chloro pesticide, polycyclic aromatic hydrocarbon, nonyl phenol and heavy metal.The many kinds of complicated component of these polluters, except a huge sum of money
Belong to outer major part and belong to persistence organic pollutant, has the characteristics that persistence, high toxicity, biological accumulation and remote migration,
Significant threat is constituted to the ecosystem.On the other hand, micro- plastics have lesser volume, thus are easy by floating in marine environment
Travelling object, benthon, fish etc. are eaten by mistake.Micro- plastics can accumulate after being ingested in organism different parts, and then lead to biology
Body poisoning or intracorporeal organ are hurt, are blocked.In addition, micro- plastics of marine organisms cylinder accumulation and its persistence of carrying are organic
Pollutant will under biological magnification, by marine food chain high nutrition grade biology internal enrichment, even into human body
Threat is generated to its health.Therefore, a kind of persistence organic pollutant detection of rapidly and accurately micro- frosting absorption is found
Method is the task of top priority.Currently, the detection method of common micro- frosting harmful substance is largely divided into two parts: (1) micro-
The extraction of frosting harmful substance.The extracting method of existing micro- frosting harmful substance includes soxhlet extraction method, accelerates
Solvent extraction, microwave-assisted, ultrasound-assisted extraction method, supercritical fluid extraction etc., often need to be by various
Equipment, step is complicated, and needs to consume a large amount of reagents in extraction process, and certain pressure is caused to environment.(2) extraction of substance
Chemical component detection.The polluter dissolved in eluant, eluent is usually by high performance liquid chromatograph, inductively coupled plasma constitution
The instruments such as spectrometer, high resolution gas chromatography instrument carry out qualitative and quantitative analysis.It is complex for operation step, need to consume a large amount of reagents and consume
Duration, somewhat expensive.Therefore, it is very necessary to find a kind of conveniently in-situ detection method.
SERS is detection technique emerging in recent decades, and principle is in coarse gold, silver body structure surface, and the Raman of molecule is believed
It number will be increased dramatically.The synchronous situ extracting for realizing micro- frosting organic pollutant of this research and surface Raman increase
By force, and then by SERS technology the SERS signal for directly acquiring object realizes micro- frosting persistence organic pollutant
Situ extracting and detection.Compared to traditional micro- plastics detection method, this method has step simple, and chemical reagent consumption is few,
Detection time is short, it can be achieved that the advantages that micro- frosting pollutant in situ detection.
Summary of the invention
The purpose of the present invention is to provide a kind of situ extracting of micro- frosting organic pollutant and detection are integrated
Method.Existing detection method needs to separate organic pollutant from the surface of micro- plastics, then by corresponding analysis hand
Duan Jinhang qualitative and quantitative analysis.Compared with detection method it is different, the present invention directly micro- frosting carry out situ extracting and
Raman enhancing, is then acquired by signal of the SERS technology to persistence organic pollutant, realizes situ extracting and detection
Integration.The present invention reduces the use of chemical reagent, simplify detection program, it can be achieved that micro- frosting in situ detection.
The technical scheme is that
The in-situ detection method of micro- frosting absorption pollutant, steps are as follows:
(1) preparation of micro- plastics
The micro- plastics for being 0.1-5mm at partial size by plastic crushing, excessively different purpose sieves, and be added separately to configured
In isometric persistence organic pollutant solution and ultrapure water, 72h or more is shaken in 25 DEG C of constant water bath box, obtains persistence
The micro- plastics and blank control sample of organic pollutant pollution；
(2) preparation of nano silver colloidal sol
By 1.06 × 10-3The silver nitrate aqueous solution of mol/L is placed in the constant temperature blender with magnetic force of 100 DEG C of heating, and revolving speed is
1200~1400r/min；Taking mass fraction is 1% sodium citrate aqueous solution；According to sodium citrate aqueous solution and silver nitrate water
The volume ratio of solution is 1:50, and sodium citrate solution is added dropwise in the silver nitrate solution after boiling, keeps solution boiling
And continue to stir 1h, it is protected from light and is cooled to room temperature, obtain silver sol；
(3) synchronous to realize situ extracting and Raman enhancing
Firstly, the micro- plastics and blank control sample of the persistence organic pollutant pollution that filtration step (1) obtains respectively,
Micro- plastic grain therein is separated, is transferred on masking foil after natural drying at room temperature；Then, in micro- modeling of acquisition
Material sample surfaces be successively added dropwise the methanol of 5uL, the silver sol and 5uL that 5uL step (2) obtains 0.1mol/L potassium iodide it is ultrapure
Aqueous solution, the synchronous situ extracting for realizing micro- frosting persistence organic pollutant and Raman enhancing；At this point, different-grain diameter
There are two states with drop is mixed for micro- plastics: the first, micro- modeling that mixing drop will be covered on partial size and be within the scope of 2-5mm
Expect on surface；Second, micro- plastics of partial size 0.1-2mm will then swim in the edge of mixing drop；
(4) SERS spectra acquires
By micro- plastic sample undried in step (3), it is placed under micro laser Raman spectroscopy detector, makes laser as far as possible
It is radiated near the highest point on mixing drop convex surface, acquires SERS spectra；At this point, laser will for micro- plastic sample of 2-5mm
It is irradiated to micro- frosting through drop, and for micro- plastic sample of 0.1-2mm, laser then will transmit through drop and be radiated at aluminium foil
On paper；Parameter setting when Raman spectrum acquires are as follows: scanning range 500-2500cm-1, excitation wavelength 785nm, optical resolution
Rate 1um-1, laser power 20.6mW, time of integration 25s are integrated 3 times and are taken average spectral value；
(5) qualitative and quantitative analysis of Chemical Measurement Raman spectrum
It is qualitative with the presence or absence of pollutant progress of the pollutant characteristic peak to micro- frosting according to spectral signal obtained
Analysis；In conjunction with linear regression model (LRM)-Partial Least Squares, using peak height, peak area as variable, micro- frosting pollutant is established
Prediction model.
Further, above-mentioned plastic material is polyethylene, and persistence organic pollutant material is fluoranthene.
Further, the concentration of persistence organic pollutant solution is 20mg/L in above-mentioned steps (1).
Effect of the invention is with benefit: compared with traditional detection method, this method, which synchronizes, to be realized extraction and detected
Journey reduces the use of reagent in traditional separation process, reduces environmental pressure, simplifies detection program, save the time.
Detailed description of the invention
The micro- frosting organic pollutant in situ detection flow chart of Fig. 1.
The SERS spectra of the micro- frosting organic pollutant of Fig. 2.
Specific embodiment
A specific embodiment of the invention is described in detail below in conjunction with technical solution (and attached drawing).
(1) the micro- plastics for being adsorbed with environmental contaminants prepare
Certain density organic solution is configured, the present invention is illustrated by taking fluoranthene as an example.The micro- plastics of partial size < 5mm are taken,
It is dipped into fluoranthene ultra-pure water solution (20mg/L), simulates micro- plastics to the adsorption process of fluoranthene in environment water.It separately takes identical
Micro- plastics of equivalent amount are added, as blank control in the ultrapure water of volume.The fluoranthene solution and ultrapure water of micro- plastics will be contained
It is individually positioned in 25 DEG C of isothermal vibration incubator and continuously shakes 72h.
(2) preparation of nano silver colloidal sol solution
It weighs 18mg and analyzes pure silver nitrate, be settled to 100mL in volumetric flask with ultrapure water.Solution is put into 100mL cone
In shape bottle, it is placed on 100 DEG C of heated constant temperature magnetic stirring apparatus, revolving speed 1300r/min.Weigh the dissolution of 0.285g trisodium citrate
In 25mL ultrapure water, it is configured to the trisodium citrate aqueous solution that mass fraction is 1%, takes 2mL citric acid three sodium solution dropwise
In silver nitrate solution after being added to boiling, keeps solution to be boiling for stirring 1h, be protected from light and be cooled to room temperature.
(3) synchronous to realize situ extracting and Raman enhancing
Firstly, filtering persistence organic pollutant solution and ultrapure water respectively, micro- plastic grain therein is separated,
It is transferred on masking foil after natural drying at room temperature；Then, 5uL methanol is successively added dropwise on micro- plastic sample surface of acquisition
(AR), potassium iodide (KI) ultra-pure water solution of the 0.1mol/L of 5uL silver sol and 5uL, a step realize micro- frosting persistence
The situ extracting and Raman of organic pollutant enhance, as shown in Fig. 1 (a) (b), (c)；At this point, micro- plastics of different-grain diameter and mixed
Closing drop, there are two states: mixing drop is in partial size is covered on micro- frosting within the scope of 2-5mm, and partial size
Micro- plastics of 0.1-2mm will then swim in the edge of mixing drop；
(4) SERS spectra acquires
Micro- plastic sample undried in (3) is placed under micro laser Raman spectroscopy detector, and make laser as far as possible according to
It penetrates near the highest point on mixing drop convex surface, SERS spectra is acquired, as shown in Fig. 1 (d)；At this point, for micro- plastics of 2-5mm
Sample, laser will transmit through drop and is irradiated to micro- frosting, and for micro- plastic sample of 0.1-2mm, laser then will transmit through liquid
Drop is radiated on aluminium-foil paper；Parameter setting when Raman spectrum acquires are as follows: scanning range 500-2500cm-1, excitation wavelength
785nm, optical resolution 1um-1, laser power 20.6mW, time of integration 25s are integrated 3 times and are taken average spectral value.
(5) qualitative and quantitative analysis of Chemical Measurement Raman spectrum
It whether there is fluoranthene characteristic peak (563cm according to spectral signal obtained-1, 672cm-1, 798cm-1, 1099cm-1,
1267cm-1, 1414cm-1, 1456cm-1, 1610cm-1) qualitative analysis is carried out, in conjunction with the peak height and peak area of fluoranthene characteristic peak,
The prediction model that micro- frosting fluoranthene is established using the method for offset minimum binary, realize fluoranthene in micro- plastic sample it is quick,
Quantitative detection.
Claims (3)
1. the in-situ detection method of micro- frosting absorption pollutant, which is characterized in that steps are as follows:
(1) preparation of micro- plastics
The micro- plastics for being 0.1-5mm at partial size by plastic crushing, excessively different purpose sieves, and it is added separately to configured Deng bodies
In long-pending persistence organic pollutant solution and ultrapure water, 72h or more is shaken in 25 DEG C of constant water bath box, it is organic to obtain persistence
The micro- plastics and blank control sample of contaminants；
(2) preparation of nano silver colloidal sol
By 1.06 × 10-3The silver nitrate aqueous solution of mol/L is placed in the constant temperature blender with magnetic force of 100 DEG C of heating, revolving speed 1200
~1400r/min；Taking mass fraction is 1% sodium citrate aqueous solution；According to sodium citrate aqueous solution and silver nitrate aqueous solution
Volume ratio be 1:50, by sodium citrate solution be added dropwise to boiling after silver nitrate solution in, keep solution boil and hold
Continuous stirring 1h, is protected from light and is cooled to room temperature, obtain silver sol；
(3) synchronous to realize situ extracting and Raman enhancing
Firstly, the micro- plastics and blank control sample of the persistence organic pollutant pollution that filtration step (1) obtains respectively, by it
In micro- plastic grain separate, be transferred on masking foil after natural drying at room temperature；Then, in micro- plastic-like of acquisition
Product surface be successively added dropwise the methanol of 5uL, the silver sol and 5uL that 5uL step (2) obtains 0.1mol/L potassium iodide it is ultrapure water-soluble
Liquid, the synchronous situ extracting for realizing micro- frosting persistence organic pollutant and Raman enhancing；At this point, micro- modeling of different-grain diameter
There are two states with drop is mixed for material: the first, mix micro- plastic table that drop will be covered on partial size and be within the scope of 2-5mm
On face；Second, micro- plastics of partial size 0.1-2mm will then swim in the edge of mixing drop；
(4) SERS spectra acquires
By micro- plastic sample undried in step (3), it is placed under micro laser Raman spectroscopy detector, irradiates laser as far as possible
Near the highest point on mixing drop convex surface, SERS spectra is acquired；At this point, for micro- plastic sample of 2-5mm, laser be will transmit through
Drop is irradiated to micro- frosting, and for micro- plastic sample of 0.1-2mm, laser then will transmit through drop and be radiated at aluminium-foil paper
On；Parameter setting when Raman spectrum acquires are as follows: scanning range 500-2500cm-1, excitation wavelength 785nm, optical resolution
1um-1, laser power 20.6mW, time of integration 25s are integrated 3 times and are taken average spectral value；
(5) qualitative and quantitative analysis of Chemical Measurement Raman spectrum
Qualitative analysis is carried out with the presence or absence of pollutant of the pollutant characteristic peak to micro- frosting according to spectral signal obtained；
In conjunction with linear regression model (LRM)-Partial Least Squares, using peak height, peak area as variable, the prediction of micro- frosting pollutant is established
Model.
2. the in-situ detection method of micro- frosting absorption pollutant according to claim 1, which is characterized in that described
Plastic material is polyethylene, and persistence organic pollutant material is fluoranthene.
3. the in-situ detection method of micro- frosting absorption pollutant according to claim 1, which is characterized in that step
(1) concentration of persistence organic pollutant solution is 20mg/L in.
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Cited By (10)
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| CN110227282A (en) * | 2019-07-09 | 2019-09-13 | 浙江工业大学 | A kind of application of waste and old agricultural polyethylene mulch in absorption hydrophobic organic pollutant |
| CN110865135A (en) * | 2019-10-30 | 2020-03-06 | 河南大学 | Method for measuring capacity of micro plastic for adsorbing soil organic chlorine pesticide |
| CN110907429A (en) * | 2019-12-31 | 2020-03-24 | 广东海洋大学 | Surface enhanced Raman spectroscopy detection method for micro/nano plastic |
| CN111220732A (en) * | 2020-01-22 | 2020-06-02 | 大连理工大学 | SERS detection method for persistent organic pollutants in water body based on micro-plastics |
| CN113495066A (en) * | 2020-12-14 | 2021-10-12 | 广东石油化工学院 | Method for carrying out sensitive SERS (surface enhanced Raman Scattering) detection on micro-plastic by gold-assembled sponge with bowl-shaped structure |
| CN113670779A (en) * | 2021-07-26 | 2021-11-19 | 杭州娃哈哈集团有限公司 | Method for detecting and evaluating distribution of micro-plastics in packaged drinking water based on infrared imaging technology |
| CN113933261A (en) * | 2021-11-15 | 2022-01-14 | 中国计量科学研究院 | Method for detecting micro-plastic in sediment based on solubility parameter calculation |
| CN115259586A (en) * | 2021-04-29 | 2022-11-01 | 暨南大学 | Method for extracting micro-plastic from sludge and application |
| US11635385B2 (en) | 2021-06-29 | 2023-04-25 | Jimei University | Characteristic information extraction method, and rapid detection method and system of organic pollutants in complex system |
| CN116223427A (en) * | 2023-03-24 | 2023-06-06 | 胜科纳米(苏州)股份有限公司 | Method for analyzing surface dispersed pollutants by adopting infrared spectrum |
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| CN110227282A (en) * | 2019-07-09 | 2019-09-13 | 浙江工业大学 | A kind of application of waste and old agricultural polyethylene mulch in absorption hydrophobic organic pollutant |
| CN110865135A (en) * | 2019-10-30 | 2020-03-06 | 河南大学 | Method for measuring capacity of micro plastic for adsorbing soil organic chlorine pesticide |
| CN110907429A (en) * | 2019-12-31 | 2020-03-24 | 广东海洋大学 | Surface enhanced Raman spectroscopy detection method for micro/nano plastic |
| CN110907429B (en) * | 2019-12-31 | 2023-09-19 | 广东海洋大学 | Surface enhanced Raman spectrum detection method for micro/nano plastic |
| CN111220732A (en) * | 2020-01-22 | 2020-06-02 | 大连理工大学 | SERS detection method for persistent organic pollutants in water body based on micro-plastics |
| CN113495066A (en) * | 2020-12-14 | 2021-10-12 | 广东石油化工学院 | Method for carrying out sensitive SERS (surface enhanced Raman Scattering) detection on micro-plastic by gold-assembled sponge with bowl-shaped structure |
| CN115259586A (en) * | 2021-04-29 | 2022-11-01 | 暨南大学 | Method for extracting micro-plastic from sludge and application |
| US11635385B2 (en) | 2021-06-29 | 2023-04-25 | Jimei University | Characteristic information extraction method, and rapid detection method and system of organic pollutants in complex system |
| CN113670779A (en) * | 2021-07-26 | 2021-11-19 | 杭州娃哈哈集团有限公司 | Method for detecting and evaluating distribution of micro-plastics in packaged drinking water based on infrared imaging technology |
| CN113933261A (en) * | 2021-11-15 | 2022-01-14 | 中国计量科学研究院 | Method for detecting micro-plastic in sediment based on solubility parameter calculation |
| CN116223427A (en) * | 2023-03-24 | 2023-06-06 | 胜科纳米(苏州)股份有限公司 | Method for analyzing surface dispersed pollutants by adopting infrared spectrum |
| CN116223427B (en) * | 2023-03-24 | 2023-12-19 | 胜科纳米(苏州)股份有限公司 | Method for analyzing surface dispersed pollutants by adopting infrared spectrum |
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