CN110793947B - Correction method for reducing influence of soil type on polycyclic aromatic hydrocarbon fluorescence working curve - Google Patents
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- 239000002689 soil Substances 0.000 title claims abstract description 97
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000011159 matrix material Substances 0.000 claims abstract description 32
- 238000002189 fluorescence spectrum Methods 0.000 claims abstract description 19
- 238000001228 spectrum Methods 0.000 claims abstract description 15
- 230000003595 spectral effect Effects 0.000 claims abstract description 8
- 238000007689 inspection Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 9
- GYFAGKUZYNFMBN-UHFFFAOYSA-N Benzo[ghi]perylene Chemical group C1=CC(C2=C34)=CC=C3C=CC=C4C3=CC=CC4=CC=C1C2=C43 GYFAGKUZYNFMBN-UHFFFAOYSA-N 0.000 description 36
- TXVHTIQJNYSSKO-UHFFFAOYSA-N BeP Natural products C1=CC=C2C3=CC=CC=C3C3=CC=CC4=CC=C1C2=C34 TXVHTIQJNYSSKO-UHFFFAOYSA-N 0.000 description 18
- 238000005516 engineering process Methods 0.000 description 8
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthene Chemical compound C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 5
- 125000005605 benzo group Chemical group 0.000 description 4
- 230000005284 excitation Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 description 3
- CSHWQDPOILHKBI-UHFFFAOYSA-N peryrene Natural products C1=CC(C2=CC=CC=3C2=C2C=CC=3)=C3C2=CC=CC3=C1 CSHWQDPOILHKBI-UHFFFAOYSA-N 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 238000000985 reflectance spectrum Methods 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 239000006004 Quartz sand Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 150000002979 perylenes Chemical class 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- -1 cyclic aromatic hydrocarbons Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
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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
- G01N21/64—Fluorescence; Phosphorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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Abstract
The invention belongs to the field of detection methods, relates to detection of polycyclic aromatic hydrocarbons in soil, and particularly relates to a correction method for reducing influence of soil types on a polycyclic aromatic hydrocarbon fluorescence working curve, which comprises the following steps of 1: selecting a plurality of soil samples of different types, and preparing a plurality of soil samples of polycyclic aromatic hydrocarbons with different concentrations aiming at the soil samples; step 2: establishing a corresponding polycyclic aromatic hydrocarbon concentration matrix C; and step 3: scanning and preparing a fluorescence spectrum and a near-infrared diffuse reflection spectrum of the soil sample; and 4, step 4: selecting a quantitative fluorescence band M; and 5: selecting a near infrared diffuse reflection spectral band N; step 6: obtaining a corresponding fluorescence intensity matrix F; and 7: obtaining a corresponding near-infrared diffuse reflection intensity matrix S; and 8: obtaining a corrected fluorescence intensity matrix F of each soil samplec(ii) a And step 9: and establishing a correction working curve.
Description
Technical Field
The invention belongs to the field of detection methods, relates to detection of polycyclic aromatic hydrocarbons in soil, and particularly relates to a correction method for reducing the influence of soil types on a polycyclic aromatic hydrocarbon fluorescence working curve.
Background
As is known, Polycyclic Aromatic Hydrocarbons (PAHs) have carcinogenicity, and soil is used as an important environmental medium, the pollution problem of the polycyclic aromatic hydrocarbons is particularly serious, the sustainable development of the soil is seriously influenced, and the soil needs to be repaired and treated on the premise that the distribution and the concentration of the polycyclic aromatic hydrocarbons in the soil need to be determined.
The fluorescence spectrum technology has been widely applied to the detection of polycyclic aromatic hydrocarbons in soil due to the advantages of high sensitivity, good selectivity, rapid realization, on-site detection and the like. The Chinese patent application publication No. CN 106442447A discloses a method for reducing the influence of the soil particle size on the polycyclic aromatic hydrocarbon working curve and realizing effective correction of the influence of the soil particle size on the PAHs fluorescence intensity through Rayleigh scattering light intensity. The invention provides and establishes a correction method for reducing the influence of soil types on PAHs fluorescence.
However, besides the soil particle size, the fluorescence intensity of PAHs is also seriously affected by factors such as soil properties, (categories, components) and the like, so that the application of the technology in soil PAHs pollutant detection is restricted, and a correction method for reducing the influence of soil categories on the polycyclic aromatic hydrocarbon working curve is established.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a correction method for reducing the influence of the soil type on the polycyclic aromatic hydrocarbon fluorescence working curve, which combines a fluorescence spectrum technology and a near-infrared diffuse reflection spectrum technology, provides theoretical and experimental basis for the field detection of polycyclic aromatic hydrocarbons in soil.
The technical scheme adopted by the invention is as follows:
1. a correction method for reducing the influence of soil type on a polycyclic aromatic hydrocarbon fluorescence working curve is characterized by comprising the following steps: the method comprises the following steps:
step 1: selecting a plurality of soil samples of different types, and preparing a plurality of soil samples of polycyclic aromatic hydrocarbons with different concentrations aiming at the soil samples;
step 2: establishing a corresponding polycyclic aromatic hydrocarbon concentration matrix C according to the soil samples with different concentrations of polycyclic aromatic hydrocarbons in the step 1;
and step 3: scanning the fluorescence spectrum and the near-infrared diffuse reflection spectrum of each soil sample prepared in the step 1 to obtain the fluorescence spectrum and the near-infrared diffuse reflection spectrum of each soil sample;
and 4, step 4: selecting a quantitative fluorescence band M for establishing a polycyclic aromatic hydrocarbon working curve for the fluorescence spectrum in the step 3;
and 5: selecting a near infrared diffuse reflection spectral band N for correcting the working curve for the near infrared diffuse reflection spectrum in the step 3;
step 6: extracting the fluorescence intensity of the quantitative fluorescence band M in the step 4 to obtain a corresponding fluorescence intensity matrix F;
and 7: extracting the intensity of the near-infrared diffuse reflection spectral band N in the step 5 to obtain a corresponding near-infrared diffuse reflection intensity matrix S;
and 8: the fluorescence intensity matrix F extracted in step 6 is corrected by the near-infrared diffuse reflection intensity matrix S extracted in step 7, i.e.
Obtaining a corrected fluorescence intensity matrix F of each soil samplec；
And step 9: the corrected fluorescence intensity matrix F obtained according to step 7cAnd establishing a polycyclic aromatic hydrocarbon concentration matrix C established in the step 2, and establishing a correction working curve for quantitatively analyzing the polycyclic aromatic hydrocarbon concentration in the soil.
Furthermore, the soil samples in the step 1 are preferably three or more, and each soil sample meets the corresponding requirements of GBW07412a approved by the State quality supervision, inspection and quarantine headquarters.
The invention has the advantages and positive effects that:
according to the invention, a plurality of different types of soil samples are randomly adopted, and different concentrations of cyclic aromatic hydrocarbons are added to different soil samples to prepare corresponding soil samples, so that a plurality of experimental samples are formed. Then combining the fluorescence spectrum technology with the near infrared diffuse reflection spectrum technology, and respectively selecting characteristic spectral bandsEstablishing corresponding intensity matrixes F and S, correcting through the matrixes, and adopting
Formula, calculating to obtain a corrected fluorescence intensity matrix F of the soil samplecAnd then, a corresponding correction working curve is established by combining with the known polycyclic aromatic hydrocarbon concentration matrix C, and the method can quickly and effectively realize the correction of the influence of the soil type on the PAHs fluorescence working curve, thereby providing theoretical and experimental basis for the application of the fluorescence spectrum technology to polycyclic aromatic hydrocarbon detection in the field soil.
Drawings
FIG. 1 is a graph showing fluorescence spectra of various soil samples of different concentrations of benzo [ ghi ] perylene under excitation of light having a wavelength of 390 nm;
FIG. 2 is a near infrared diffuse reflectance spectrum of various soil samples of differing concentrations of benzo [ ghi ] perylene;
FIG. 3 is a plot of benzo [ ghi ] perylene fluorescence work in soil after calibration;
FIG. 4 is a plot of the benzo [ ghi ] perylene fluorescence working curve in soil prior to calibration.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
Polycyclic aromatic hydrocarbons are organic compounds formed by connecting two or more benzene rings, and include more than 150 compounds such as anthracene, benzo [ ghi ] perylene, fluoranthene, etc., and the benzo [ ghi ] perylene is taken as an example, and the calibration method of the present invention is explained in detail with reference to the accompanying drawings.
2. A correction method for reducing the influence of soil type on a polycyclic aromatic hydrocarbon fluorescence working curve is characterized by comprising the following steps: the method comprises the following steps:
step 1: selecting a plurality of soil samples of different types, and preparing a plurality of soil samples of polycyclic aromatic hydrocarbons with different concentrations aiming at the soil samples;
in this embodiment, the soil sample in step 1 is obtained by respectively selecting yellow cotton soil in shanxi, haii moisture soil, and mixed soil of 10% of haii moisture soil and quartz sand, taking a standard substance for analyzing active ingredients of soil, and performing drying and grinding operations. The soil sample meets the corresponding requirements of GBW07412a approved by the State quality supervision, inspection and quarantine Bureau, and is purchased from the China center for Standard substances.
In this embodiment, a certain amount of benzo [ ghi ] perylene powder (analytically pure, purchased from shanghai haohong biomedical science and technology limited) is dissolved in dichloromethane, shaken to prepare a solution, the solution is drained by a glass rod and poured into the soil sample, and the soil sample is placed in a fume hood, after the dichloromethane is completely volatilized, the air-dried benzo [ ghi ] perylene soil sample is ground to ensure that benzo [ ghi ] perylene is uniformly mixed in the soil, and a corresponding soil sample is prepared.
Step 2: establishing a corresponding benzo [ ghi ] perylene concentration matrix C according to the soil samples of different benzo [ ghi ] perylenes in the step 1;
in this example, 10 different types of soil samples of benzo [ ghi ] perylene at different concentrations were prepared: the benzo [ ghi ] perylene concentrations C were 0.4mg/g, 0.6mg/g, 0.8mg/g, 1.0mg/g, 1.2mg/g, 1.4mg/g, 1.6mg/g, 1.8mg/g, 2.0mg/g, and 2.2mg/g, respectively. Wherein the soil used by the samples of 0.4mg/g, 0.6mg/g and 1.2mg/g is Shanxi yellow cotton soil; the soil used by the samples of 0.8mg/g, 1.0mg/g, 1.6mg/g and 2.0mg/g is Anhui moisture soil; the soil used for the samples of 1.4mg/g, 1.8mg/g and 2.2mg/g was a mixed soil of Anhui moisture soil and 10% quartz sand.
And step 3: scanning the fluorescence spectrum and the near-infrared diffuse reflection spectrum prepared by each soil sample prepared in the step 1 to obtain the fluorescence spectrum and the near-infrared diffuse reflection spectrum of each soil sample;
in this example, an LS-55 fluorescence spectrophotometer manufactured by perkin elmer, usa was used to scan the fluorescence spectrum of the prepared soil sample, and the fluorescence spectrum of each sample was obtained.
The instrument parameters were set as follows: the wavelength of an excitation light source is 390nm, the wavelength range of a fluorescence spectrum is 400-650 nm, the widths of slits of an excitation monochromator and an emission monochromator are respectively 10nm and 10nm, the voltage of a photomultiplier is 650, and the scanning speed is 1000 nm/min.
As shown in figure 1, the benzo [ ghi ] perylene has two obvious characteristic fluorescence peaks in soil, the positions of the two obvious characteristic fluorescence peaks are 487nm and 510nm respectively, and the quantitative characteristic band M for preparing a quantitative analysis benzo [ ghi ] perylene fluorescence working curve is 487nm according to the fluorescence spectrum.
Meanwhile, a Fourier near-infrared spectrometer produced by Perkin Elmer company in America is adopted to scan the near-infrared diffuse reflection spectrum of the prepared soil sample, and the near-infrared diffuse reflection spectrum of each sample is obtained.
The instrument parameter settings were as follows: scanning range 12000-4000cm-1Resolution of 8cm-1Each sample was scanned 64 times and the spectra averaged.
As shown in FIG. 2, different concentrations of benzo [ ghi ] can be seen]The perylene different types of soil samples are 12000-4000cm-1The intensity of the diffuse reflectance spectrum of the range is different, and the value for correcting the benzo [ ghi ] is determined according to the near infrared diffuse reflectance spectrum]The near infrared diffuse reflection spectral band N of the perylene fluorescence working curve is 5220cm-1。
And 4, step 4: selecting a fluorescence band M for establishing a quantitative analysis benzo [ ghi ] perylene working curve for the fluorescence spectrum in the step 3;
and 5: selecting a near infrared diffuse reflection spectral band N for correcting the working curve for the near infrared diffuse reflection spectrum in the step 3;
step 6: extracting the fluorescence intensity of 10 benzo [ ghi ] perylene soil samples in the step 4 at 487nm to obtain a corresponding fluorescence intensity matrix F;
and 7: extraction of 10 benzo [ ghi ] s from step 5]Perylenes soil samples at 5220cm-1Obtaining a corresponding near-infrared diffuse reflection intensity matrix S according to the intensity of the infrared light;
and 8: correcting the fluorescence intensity matrix F extracted in the step 6 through the near-infrared diffuse reflection intensity matrix S extracted in the step 7 by a formula
Obtaining a corrected fluorescence intensity matrix F of 10 soil samplesc；
And step 9: the corrected fluorescence intensity matrix F obtained according to step 7cAnd establishing a polycyclic aromatic hydrocarbon concentration matrix C established in the step 2, establishing a horizontal and vertical axis as FcThe calibration operation curve is established with the vertical axis and the horizontal axis C (as shown in fig. 3).
Fc＝6.58+5.37C (2)
For comparison, a working curve was established for the uncorrected fluorescence intensity matrix F at 487nm for different concentrations of benzo [ ghi ] perylene in different types of soil samples and the benzo [ ghi ] perylene concentration matrix C in soil (as shown in fig. 4), with the equation:
F＝238.00+161.33C (3)
comparing the working curves before and after correction to find that: correcting the complex correlation coefficient R of the working curve20.885, root mean square error of 1.16; complex correlation coefficient R of uncorrected working curve20.755, and a root mean square error of 54.61. From the above results, it can be seen that: the correction method applied by the patent can effectively reduce the soil type p-benzo [ ghi]Influence of the perylene fluorescence working curve.
Experiments prove that for different types of soil, for any polycyclic aromatic hydrocarbon in the soil, including pyrene, phenanthrene, fluoranthene and the like, the influence of the different types of soil on the quantitative analysis polycyclic aromatic hydrocarbon working curve can be reduced by the correction method established by the application.
Claims (2)
1. A correction method for reducing the influence of soil type on a polycyclic aromatic hydrocarbon fluorescence working curve is characterized by comprising the following steps: the method comprises the following steps:
step 1: selecting a plurality of soil samples of different types, and preparing a plurality of soil samples of polycyclic aromatic hydrocarbons with different concentrations aiming at the soil samples;
and 2, step: establishing a corresponding polycyclic aromatic hydrocarbon concentration matrix C according to the soil samples with different concentrations of polycyclic aromatic hydrocarbons in the step 1;
and step 3: scanning the fluorescence spectrum and the near-infrared diffuse reflection spectrum of each soil sample prepared in the step 1 to obtain the fluorescence spectrum and the near-infrared diffuse reflection spectrum of each soil sample;
and 4, step 4: selecting a quantitative fluorescence band M for establishing a polycyclic aromatic hydrocarbon working curve for the fluorescence spectrum in the step 3;
and 5: selecting a near infrared diffuse reflection spectral band N for correcting the working curve for the near infrared diffuse reflection spectrum in the step 3;
step 6: extracting the fluorescence intensity of the quantitative fluorescence band M in the step 4 to obtain a corresponding fluorescence intensity matrix F;
and 7: extracting the intensity of the near-infrared diffuse reflection spectral band N in the step 5 to obtain a corresponding near-infrared diffuse reflection intensity matrix S;
and 8: the fluorescence intensity matrix F extracted in step 6 is corrected by the near-infrared diffuse reflection intensity matrix S extracted in step 7, i.e.
Obtaining a corrected fluorescence intensity matrix F of each soil samplec；
And step 9: the corrected fluorescence intensity matrix F obtained according to step 8cAnd establishing a polycyclic aromatic hydrocarbon concentration matrix C established in the step 2, and establishing a correction working curve for quantitatively analyzing the polycyclic aromatic hydrocarbon concentration in the soil.
2. The calibration method for reducing the influence of soil type on the polycyclic aromatic hydrocarbon fluorescence working curve according to claim 1, wherein the calibration method comprises the following steps: the soil sample in the step 1 meets the corresponding requirements of GBW07412a approved by the State quality supervision, inspection and quarantine headquarters.
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Non-Patent Citations (4)
| Title |
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| Correction for the effect of soil types on the fluorescence intensity of polycyclic aromatic hydrocarbons;Tao Lei等;《Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy》;20210409;第257卷;第119807-1-6页 * |
| Determination of Total Petroleum Hydrocarbon (TPH) and Polycyclic Aromatic Hydrocarbon (PAH) in Soils: A Review of Spectroscopic and Nonspectroscopic Techniques;REUBEN NWOMANDAH OKPARANMA等;《Applied Spectroscopy Reviews》;20130313;第48卷(第6期);第458-486页 * |
| Feasibility of the simultaneous determination of polycyclic aromatichydrocarbons based on two-dimensional fluorescencecorrelation spectroscopy;Renjie Yang等;《Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy》;20170921;第190卷;第342-346页 * |
| 土壤粒径大小对蒽荧光特性的影响及校正;杨仁杰等;《光学精密工程》;20161115;第24卷(第11期);第2665-2671页 * |
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