CN104502327A - Method for single particle surface pollutant site quantitative detection based on surface enhanced Raman spectrum - Google Patents
Method for single particle surface pollutant site quantitative detection based on surface enhanced Raman spectrum Download PDFInfo
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- CN104502327A CN104502327A CN201510014349.5A CN201510014349A CN104502327A CN 104502327 A CN104502327 A CN 104502327A CN 201510014349 A CN201510014349 A CN 201510014349A CN 104502327 A CN104502327 A CN 104502327A
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Abstract
The invention relates to a method for single particle surface pollutant site quantitative detection based on a surface enhanced Raman spectrum. The method comprises the step (a) of establishing a calibration curve of mass of pollutants adsorbed to particle surfaces and the surface enhanced Raman spectrum strength of the position of the pollutant characteristic peak; the step (b) of adopting a portable Raman spectrometer on the site to perform surface enhanced Raman spectrum detection on single particle surfaces used for adsorbing the pollutants and having the surface enhanced Raman spectrum activity, so as to obtain the surface enhanced Raman spectrum strength of the position of the pollutant characteristic peak; and the step (c) of contrasting the detected pollutant surface enhanced Raman spectrum characteristic peak strength and the calibration curve obtained in the step (a), so as to obtain the mass of the pollutants adsorbed to the particle surfaces.
Description
Technical field
The invention belongs to field of environment engineering technology, relate to a kind of pollutant SERS (Surface enhanced raman spectroscopy) in situ quantitation detection method of individual particle adsorption.
Background technology
In recent years, along with the industrialized fast development of China, for enhancing productivity or meeting the object of technological requirement, increasing porous particle is applied in commercial production as catalyst support, filtration aid, adsorbent etc.Because China's treatment technology is perfect not, these porous particles can carry or adsorb a large amount of hazardous contaminants after use is lost efficacy, if be directly discharged in environment, can cause serious environmental pollution.How quantitatively to detect the absorption of these solid particles surface or the pollutant that carries becomes the task of top priority.The main method that present stage is used for detecting porous particle surface contaminant has: the methods such as vapor-phase chromatography, gas chromatography combined with mass spectrometry, atomic absorption spectrum, infrared spectrum.But these methods can only realize in the lab to particle surface pollutant monitoring after a series of loaded down with trivial details pre-service such as being separated, concentrated, are difficult to meet on-the-spot quick, sensitive quantitative testing requirement.
Such as, Chinese patent application CN 102279231A discloses a kind of method to chlordiphenyl in qualitative detection soil or sediment, parachloroanilinum in soil or sediment is separated through steps such as extraction, purification, wash-outs by the method, and recycling gaschromatographic mass spectrometric analysis instrument carries out analysis to polystream amine and detects.Said method needs to carry out pre-service lock out operation to sample before detecting measured object, gas chromatograph-mass spectrometer could be utilized to carry out qualitative detection, need large component analysis sample and complex pretreatment, detection time is long, can not meet the requirement of on-the-spot Quantitative detection.
Such as, Chinese patent CN 101251479B discloses a kind of detection method of aluminium foil surface oleaginousness, the method utilizes hydrochloric acid to be taken off by the oil wash of aluminium foil surface, use carbon tetrachloride extraction again, finally adopt infrared spectrometer to survey oily software and calculate oil content by the absorbance at the stretching band place of oily substance.Said method need carry out the complicated operation such as wash-out, extraction to the oily substance of solid surface absorption, its oily substance content is recorded in laboratory environments again in conjunction with infrared spectrometer, need a large amount of sample pre-treatments work, and have larger operate miss to testing result.Be difficult to the requirement that satisfied on-the-spot particle surface pollutant accurate quantification detects.
Detection sensitivity is high, analysis speed is fast owing to having for SERS technology, easy and simple to handle, the advantages such as the little and Monitoring lower-cut of water interference is low, make it be widely used in the qualitative detection of the aspects such as material tests, environment measuring, chemical analysis and Biosample, but utilize the research of SERS technology to the quantitative detecting method of measured object to rarely have report.
Such as, Chinese patent application CN 102109467A discloses a kind of method utilizing Raman spectrum quantitatively to detect rhodamine 6G, the method utilizes the SERS substrate of " sandwich " system of preparation, and the SERS intensity of drawing in conjunction with early stage and the relation curve of rhodamine 6G concentration detect the concentration of rhodamine 6G.But said method is difficult to meet the requirement in production scene, the material of solid particles surface being carried out to quantitatively detection.
Therefore, for being difficult to the present situation realizing the detection of solid particles surface pollutant in situ quantitation, this area, in the urgent need to developing one fast and accurately, is applicable to the individual particle surface contaminant quantitative detecting method of production scene.
Summary of the invention
The invention provides a kind of individual particle surface contaminant in situ quantitation detection method based on Surface enhanced raman spectroscopy of novelty, thus solve problems of the prior art.
The invention provides a kind of individual particle surface contaminant in situ quantitation detection method based on Surface enhanced raman spectroscopy, the method comprises:
A () sets up the quality of a particle surface adsorption fouling thing and the calibration curve of pollutant characteristic peak place Surface enhanced raman spectroscopy intensity, comprise the following steps: (1) adsorbs the pollutant of variable concentrations in waste water with the porous particle with SERS-Activity prepared; (2) Pollutants in Wastewater concentration change before and after the absorption of gas chromatography combined with mass spectrometry technical Analysis is adopted, accurately to record the pollutant quality of the porous particle adsorption with SERS-Activity; (3) with Surface enhanced raman spectroscopy direct-detection particle surface pollutant to obtain corresponding Surface enhanced raman spectroscopy spectrogram, thus obtain characteristic peak place Surface enhanced raman spectroscopy intensity; (4) set up a calibration curve in conjunction with above-mentioned two kinds of testing results, prepare for subsequent field quantitatively detects particle surface pollutant;
B () scene adopts the individual particle surface of Portable Raman spectrometer to the adsorption fouling thing with SERS-Activity to carry out Surface enhanced raman spectroscopy detection, thus obtain pollutant characteristic peak place Surface enhanced raman spectroscopy intensity; And
C the pollutant Surface-Enhanced Raman Scattering Characteristics peak intensity detected contrasts with the calibration curve obtained in above-mentioned steps (a) by (), can obtain the pollutant quality of particle surface absorption.
In one preferred embodiment, described in there is the porous particle finishing of SERS-Activity noble metal nano particles, the particle diameter of described noble metal nano particles is 70-100nm.
Another preferred embodiment in, described noble metal nano particles is silver nano-grain, and particle diameter is 70nm.
Another preferred embodiment in, described porous particle is selected from activated charcoal porous particle, polymer resin porous particle, activated alumina porous particle, zeolite and molecular sieve.
Another preferred embodiment in, described porous particle is activated alumina porous particle, and its specific grain surface amasss as 371.14m
2/ g.
Another preferred embodiment in, described pollutant be have Surface enhanced raman spectroscopy response water-soluble substances.
Another preferred embodiment in, the laser intensity in described Surface enhanced raman spectroscopy testing process is less than 30mW, and integral time is less than 30s.
Another preferred embodiment in, described pollutant characteristic peak energy enough represents specific functional groups or the chemical bond of this material itself.
Another preferred embodiment in, described calibration curve is the double logarithmic curve of the pollutant quality that pollutant characteristic peak intensity and particle surface adsorb.
Another preferred embodiment in, the Detection job of the individual particle adsorption pollutant detected reaches 7.8ng.
Accompanying drawing explanation
According to carrying out following detailed description by reference to the accompanying drawings, object of the present invention and feature will become more obvious, in accompanying drawing:
Fig. 1 is the individual particle surface contaminant in situ quantitation characterization processes FB(flow block) based on Surface enhanced raman spectroscopy according to an embodiment of the invention.
Fig. 2 Al of silver nano-grain that has been modifying according to an embodiment of the invention
2o
3the scanning electron microscope (SEM) photograph of particle surface.
Fig. 3 be according to an embodiment of the invention with 3 × 10
-4the biphenylamine of M is the SERS spectrogram of target molecule on 22 points of porous particle surface random selecting with SERS activity.
Fig. 4 is the SERS spectrogram with the biphenylamine of the porous particle adsorption of SERS activity different quality according to an embodiment of the invention.
Fig. 5 is the quality and the biphenylamine characteristic peak place (976cm that adsorb biphenylamine according to the unit mass particle surface of the foundation of an embodiment of the invention
-1) calibration curve of SERS intensity.
Fig. 6 is the SERS spectrogram of the biphenylamine according to the active porous particle surface absorption of the SERS of the Site Detection of an embodiment of the invention.
Embodiment
Present inventor have passed through extensive and deep research, for being difficult to the present situation realizing the detection of solid particles surface pollutant in situ quantitation in prior art, utilize Surface enhanced raman spectroscopy technology and detection method thereof, have developed a kind of method that porous particle surface contaminant that can be applicable to production scene quantitatively detects, the method can realize particle surface pollutant in situ quantitation accurately and rapidly with less sample and detect, thus compensate for the deficiencies in the prior art.
Technical conceive of the present invention is as follows:
Utilize the porous particle with SERS activity quantitatively to detect individual particle surface contaminant, comprise the following steps:
A () sets up the quality of a particle surface adsorption fouling thing and the calibration curve of pollutant characteristic peak place SERS intensity, concrete steps are as follows: (1) adsorbs the pollutant of variable concentrations in waste water by certain liquid-solid ratio with the porous particle with SERS activity prepared; (2) Pollutants in Wastewater concentration change before and after the absorption of gas chromatography combined with mass spectrometry technical Analysis is adopted, accurately to record the quality of the porous particle adsorption pollutant with SERS activity; (3) corresponding SERS spectrogram is obtained to obtain characteristic peak place SERS intensity with SERS direct-detection particle surface pollutant; (4) testing result in conjunction with above-mentioned two kinds of technology sets up a calibration curve, prepares for subsequent field quantitatively detects particle surface pollutant;
B () scene adopts Portable Raman spectrometer to carry out SERS detection to the individual particle surface being adsorbed with pollutant with SERS activity, thus obtain pollutant characteristic peak place SERS intensity; And
C the pollutant SERS characteristic peak intensity detected contrasts with the calibration curve obtained in above-mentioned steps (a) by (), can obtain the pollutant quality of particle surface absorption.
In the present invention, have the functionalization porous particle finishing of SERS activity noble metal nano particles, the particle diameter of noble metal nano particles is preferably 70-100nm.
Preferably, described in be modified at porous particle surface noble metal nano particles be silver nano-grain, particle diameter is about 70 nanometers.
In the present invention, described porous particle includes, but are not limited to: activated charcoal porous particle, polymer resin porous particle, activated alumina porous particle, zeolite and molecular sieve.
Preferably, described porous particle is activated alumina porous particle, and its specific grain surface amasss as 371.14m
2/ g.
In the present invention, described pollutant is the water-soluble substances with SERS response.
In the present invention, the laser intensity in described SERS testing process should be less than 30mW, and integral time is less than 30s, is radiated at for a long time on pollutant causes pollutant generation sex change to cause characteristic peak occur skew or disappear to prevent laser facula.
In the present invention, described pollutant characteristic peak energy enough represents specific functional groups or the chemical bond of this material itself.
In the present invention, described calibration curve is the double logarithmic curve of pollutant characteristic peak intensity and particle surface adsorb pollutants amount.
In an illustrative embodiments, the individual particle surface contaminant in situ quantitation detection method based on Surface enhanced raman spectroscopy comprises the following steps:
I () has the preparation of the porous particle of SERS activity: SnCl porous particle being immersed in 0.01 ~ 0.05M
2with a period of time in the mixed solution of the HCl of 0.01 ~ 0.05M, to make Sn
2+ion deposition, on porous particle, then takes out particle and uses distilled water, acetone rinsing multipass successively; Again 70 DEG C of dryings; Then the liquor argenti nitratis ophthalmicus that particle puts into 0.01 ~ 0.05M is soaked a few minutes, make silver nano-grain be deposited on particle surface, rinse with the purging method identical with preceding step subsequently and dry; Repeat above-mentioned steps several times, make silver nano-grain be deposited over porous particle surface; By the AgNO with silver nano-grain seed of above-mentioned process
3particle immerses the AgNO containing 1 milliliter of 10 ~ 30mM
3with in the ascorbic acid mixed solution of 2 milliliters of 100 ~ 300mM; After soaking a period of time, take out porous particle and use deionized water rinsing 3 times low temperature dryings for subsequent use;
(ii) mix with the waste water of the pollutant containing variable concentrations by certain liquid-solid volume ratio with the porous particle with SERS activity prepared, adsorbed rear taking-up, low temperature drying;
(iii) Pollutants in Wastewater concentration change before and after the absorption of rear employing gas chromatography combined with mass spectrometry technical Analysis has been adsorbed, accurately to record the quality of porous particle adsorption pollutant;
(iv) with Portable Raman optical spectrum direct-detection particle surface pollutant, corresponding SERS spectrogram is obtained;
V () sets up the quality of an individual particle adsorption pollutant and the calibration curve of pollutant characteristic peak place SERS intensity in conjunction with the testing result of above-mentioned two kinds of technology;
(vi) the on-the-spot Portable Raman spectrometer that adopts carries out SERS detection to the individual particle surface being adsorbed with pollutant with SERS activity, thus obtains pollutant characteristic peak place SERS intensity; And
(vii) the pollutant SERS characteristic peak intensity of detection is contrasted with the calibration curve that above-mentioned steps 1 obtains, obtain the pollutant quality of particle surface absorption.
Below method of the present invention is described with reference to the accompanying drawings in detail.
Fig. 1 is the individual particle surface contaminant in situ quantitation characterization processes FB(flow block) based on Surface enhanced raman spectroscopy according to an embodiment of the invention.As shown in Figure 1, this technological process is as follows: preparation has the porous particle of SERS activity; With the pollutant in porous particle planar water; GC-MS (gas chromatography combined with mass spectrometry technology) detects solution concentration change before and after absorption; Particle surface pollutant SERS detects; Set up calibration curve; Portable Raman spectrometer individual particle surface contaminant Site Detection; And contrast obtains the quality of individual particle adsorption pollutant.
The major advantage of method of the present invention is:
1) porous particle with SERS activity prepared as adsorbent, as SERS substrate, directly can obtain the SERS spectrogram of particle surface material again in actual production by Portable Raman optical spectrum;
2) detect in conjunction with the fast qualitative analysis utilizing of Raman spectrum and the accurate quantitative analysis of gaschromatographic mass spectrometry, by the calibration curve of the quality and pollutant characteristic peak place SERS intensity of setting up particle surface adsorption fouling thing, the quality of the pollutant of particle surface absorption can be obtained accurately and rapidly in production scene;
3) measure and analysis time short, amount of samples is few, and it is convenient, accurate to detect, and can realize the quantitative detection of production scene SERS active porous particle surface pollutant.
Embodiment
The present invention is set forth further below in conjunction with specific embodiment.But, should be understood that these embodiments only do not form limitation of the scope of the invention for illustration of the present invention.The test method of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.Except as otherwise noted, all number percent and number are by weight.
embodiment 1: in situ quantitation detects the active A l having modified silver nano-grain
2
o
3
the biphenylamine of particle surface absorption
(I) there is the preparation of the porous particle of SERS activity
By Al
2o
3particle is immersed in the SnCl of 0.02M
2with in the mixed solution of the HCl of 0.01M 2 minutes, to make Sn
2+ion deposition is at Al
2o
3on, take out particle and use distilled water, acetone rinsing multipass successively, then 70 DEG C of dryings; Then particle put into 0.02M liquor argenti nitratis ophthalmicus soak 2 minutes, make silver nano-grain be deposited on particle surface, rinse with the purging method identical with preceding step subsequently and dry; Repeat above-mentioned steps 6 times, make silver nano-grain be deposited over alumina surface; Again by the AgNO with silver nano-grain seed of above-mentioned process
3particle immerses the AgNO containing 1 milliliter of 10mM
3with in the ascorbic acid mixed solution of 2 milliliters of 100mM; Soak after 25 minutes, take out Al
2o
3for subsequent use with deionized water rinsing 3 times low temperature dryings; Al
2o
3the scanning electron microscope of particle surface as shown in Figure 2; Fig. 3 shows with 3 × 10
-4the biphenylamine of M is that target molecule is at the Al with SERS activity
2o
3sERS spectrogram on 22 points of porous particle surface random selecting, shows the relation between Raman shift and raman scattering intensity, fully confirms the repeatability of SERS " substrate " and the accuracy of testing result;
(II) mix with the waste water of the pollutant containing variable concentrations by the liquid-solid volume ratio of the porous particle with SERS activity prepared by 4:6, upon adsorption complete after taking-up, under nitrogen protection low temperature drying;
(III) Pollutants in Wastewater concentration change before and after the absorption of rear employing gas chromatography combined with mass spectrometry technical Analysis has been adsorbed, accurately to record the quality of porous particle adsorption pollutant;
(IV) with Portable Raman spectrometer direct-detection Al
2o
3the pollutant of particle surface, obtains corresponding SERS spectrogram, as shown in Figure 4;
(V) calibration curve of characteristic peak place intensity in the quality of an individual particle adsorption pollutant and pollutant SERS spectrogram is set up in conjunction with the testing result of above-mentioned two kinds of technology, as shown in Figure 5, Fig. 5 shows the relation between the logarithm of raman scattering intensity and the logarithm of quality;
(VI) the porous particle surface directly utilizing Portable Raman spectrometer to record to have modified silver nano-grain in production scene, record spectrogram as shown in Figure 6, Fig. 6 shows the relation between Raman shift and raman scattering intensity, 976cm in Fig. 6
-1the SERS intensity at characteristic peak place is 7273CPS, and the calibration curve in contrast Fig. 5 can show that the biphenylamine quality of single porous particle adsorption is 7.8ng, namely completes the Quantitative detection of the pollutant to SERS active particle adsorption.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after having read above-mentioned instruction content of the present invention.
Claims (10)
1., based on an individual particle surface contaminant in situ quantitation detection method for Surface enhanced raman spectroscopy, the method comprises:
A () sets up the quality of a particle surface adsorption fouling thing and the calibration curve of pollutant characteristic peak place Surface enhanced raman spectroscopy intensity, comprise the following steps: (1) adsorbs the pollutant of variable concentrations in waste water with the porous particle with SERS-Activity prepared; (2) Pollutants in Wastewater concentration change before and after the absorption of gas chromatography combined with mass spectrometry technical Analysis is adopted, accurately to record the pollutant quality of the porous particle adsorption with SERS-Activity; (3) with Surface enhanced raman spectroscopy direct-detection particle surface pollutant to obtain corresponding Surface enhanced raman spectroscopy spectrogram, thus obtain characteristic peak place Surface enhanced raman spectroscopy intensity; (4) set up a calibration curve in conjunction with above-mentioned two kinds of testing results, prepare for subsequent field quantitatively detects particle surface pollutant;
B () scene adopts the individual particle surface of Portable Raman spectrometer to the adsorption fouling thing with SERS-Activity to carry out Surface enhanced raman spectroscopy detection, thus obtain pollutant characteristic peak place Surface enhanced raman spectroscopy intensity; And
C the pollutant Surface-Enhanced Raman Scattering Characteristics peak intensity detected contrasts with the calibration curve obtained in above-mentioned steps (a) by (), can obtain the pollutant quality of particle surface absorption.
2. the method for claim 1, is characterized in that, described in there is the porous particle finishing of SERS-Activity noble metal nano particles, the particle diameter of described noble metal nano particles is 70-100nm.
3. method as claimed in claim 2, it is characterized in that, described noble metal nano particles is silver nano-grain, and particle diameter is 70nm.
4. the method according to any one of claim 1-3, is characterized in that, described porous particle is selected from activated charcoal porous particle, polymer resin porous particle, activated alumina porous particle, zeolite and molecular sieve.
5. method as claimed in claim 4, it is characterized in that, described porous particle is activated alumina porous particle, and its specific grain surface amasss as 371.14m
2/ g.
6. the method according to any one of claim 1-3, is characterized in that, described pollutant is the water-soluble substances with Surface enhanced raman spectroscopy response.
7. the method according to any one of claim 1-3, is characterized in that, the laser intensity in described Surface enhanced raman spectroscopy testing process is less than 30mW, and integral time is less than 30s.
8. the method according to any one of claim 1-3, is characterized in that, described pollutant characteristic peak energy enough represents specific functional groups or the chemical bond of this material itself.
9. the method according to any one of claim 1-3, is characterized in that, described calibration curve is the double logarithmic curve of the pollutant quality that pollutant characteristic peak intensity and particle surface adsorb.
10. the method according to any one of claim 1-3, is characterized in that, the Detection job of the individual particle adsorption pollutant detected reaches 7.8ng.
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Application publication date: 20150408 |