CN110174392A - A kind of dactylogram building of high sense multi-component complex oil product and discrimination method - Google Patents
A kind of dactylogram building of high sense multi-component complex oil product and discrimination method Download PDFInfo
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Abstract
The dactylogram building of the present invention relates to a kind of high sense multi-component complex oil product based on Raman spectrum and discrimination method.Spectrum of the method to standard specimen and the acquisition of blind sample comprising fluorescence and Raman signatures, seek the synchronous correlation spectrum of the two dimension for calculating each standard specimen and blind sample, under conditions of retaining dactylogram main feature, after carrying out resampling to the synchronous related spectral data of above-mentioned two dimension, it is converted into one-dimension array；It is rejected using stepwise discriminatory method to unessential variable is differentiated, only the strong set of variables of reserve judgement ability；Intensity data corresponding to the set of variables preferably gone out is projected to new lower dimensional space, according to projection coordinate in new lower dimensional space, drafting column stack diagram is intuitively compared or drawing three-dimensional space projection figure fingerprint characteristic compares.The method of the present invention identification efficiency is high, mutually confirms with existing crude oil identification method, increases the accuracy and convincingness of crude oil identification.
Description
Technical field
A kind of the present invention relates to a kind of high sense discrimination method based on Raman spectrum, and in particular to multi-component complex oil
The dactylogram construction method of product, and the Oil spill identification method based on this dactylogram.
Background technique
In ocean petroleum transportation and offshore and gas development, oil spill accident happens occasionally.According to oil spilling sample and suspicious oil spilling
The physics in source, chemical fingerprint information carry out identification of tracing to the source, and can provide reliable science for the confirmation of responsibility of accident and law ruling
Foundation, and the important prerequisite of effective control way is taken in time.
On the basis of many years on-site law-enforcing and reference foreign technology, National Bureau of Oceanography was in publication " offshore spilled oil in 1997
Identification system specification " professional standard (HY 043-1997), using gas chromatography, infra-red sepectrometry and fluorescent spectrometry as
Three kinds of basic skills of Oil spill identification.2007, State Administration for Quality Supervision and Inspection and Quarantine and national standardization administration committee
The national proposed standard (GB/T 21247-2007) of " offshore spilled oil identification system specification " is issued, proposes the oil spilling of mode step by step
Identify principle: " firstly, carry out the screening of suspicious oil spilling source sample, using fluorescent spectrometry or infra-red sepectrometry as optional method,
Preliminary screening is carried out prior to gas chromatography, excludes the suspicious oil spilling sample of different cause；Then carry out gas-chromatography and
GC/MS Analysis is aided with the analysis of unimolecule hydrocarbon stable carbon isotope when necessary, is finally differentiated.All samples exist
It is carried out under the conditions of same analysis instrument, same analysis."
Raman spectrum have test is easy, amount of samples is small, without pretreatment, sample nondestructive wound, not by seawater interference, easily
In the portability the features such as, identifies field in oil sample and be with a wide range of applications.When using Raman spectroscopy oil sample, fluorescence jump
Moving can excite with Raman transition simultaneously.In general, fluorescence signal intensity is larger, spectral peak is smooth；Raman signal is relatively weak, and details is rich
It is rich.In the prior art, ZL201310347484.2 by simultaneously include fluorescence and Raman signal original Raman spectrum, as crude oil
Spectral fingerprint；Without the processing of any fluorescence background subtraction in fingerprint collecting, convert the spectral fingerprint data of extraction to more
Dimension space vector is identified.ZL201610647605.9 carries out successive Discrimination to the intensive variable in the one-dimensional finger print spectrum of crude oil
Analysis, so that the sense that crude oil identifies is improved.The existing method with Raman spectrum detection crude oil, measurement is accurate, convenient
Fast.
Crude oil identification is difficult point and hot spot in Oil spill identification research, and the complicated multiplicity of oil composition uses single detection side
Method is difficult to ensure the accuracy and convincingness of Oil spill identification, and in the world, crude oil identification generallys use a variety of detection method joints
It uses, especially in judicial expertise, needs that different discrimination methods is respectively adopted to identical oil spilling sample, obtained testing result
Mutually confirmation.Therefore researching and developing new high identification crude oil identification method has important practical value.
Summary of the invention
To be used in combination with crude oil identification method in the prior art, improves oil sample and identify accuracy and convincingness, this hair
It is bright provide it is a kind of by two-dimensional correlation spectra, data resampling, Stepwise Discriminatory Analysis, lower dimensional space projection combine, carry out it is more
Complicated components sample mirror method for distinguishing.
For achieving the above object, the invention adopts the following technical scheme:
A kind of building of multi-component complex oil sample dactylogram and discrimination method, include the following steps,
(1) to the standard specimen of Known Species and blind sample to be identified, parallel sample is acquired respectively；For each oil sample, use
Raman spectrometer measures a series of spectroscopic datas comprising fluorescence and Raman information under different shooting conditions；
(2) spectroscopic data measured under different shooting conditions is subjected to interpolation processing, makes all spectroscopic data abscissas one
One is corresponding, seeks the synchronous correlation spectrum of the two dimension for calculating each standard specimen and blind sample；
(3) under conditions of retaining dactylogram main feature, the synchronous related spectral data of above-mentioned two dimension is adopted again
Sample；The upper triangular matrix or inferior triangular flap in two-dimension spectrum matrix after extracting resampling, is converted into one-dimension array；
(4) it is based on above-mentioned one-dimension array, intensive variable is screened using stepwise discriminatory method analysis, is rejected to differentiation not
Important variable, only the strong set of variables of reserve judgement ability is as preferred variable group；According to " similar deviation is minimum, deviation between class
It is maximum " principle construction allusion quotation then discriminant function group；Based on allusion quotation then discriminant function group, by intensity corresponding to the set of variables preferably gone out
Data projection is to new lower dimensional space；
(5) according to projection coordinate in new lower dimensional space, drafting column stack diagram is intuitively compared or drawing three-dimensional space is thrown
Shadow figure fingerprint characteristic compares, and can identify blind sample.
A kind of above-mentioned multi-component complex oil sample dactylogram building and discrimination method, step (5) column stack diagram intuitively compare
In similar sample, then drawing three-dimensional space projection figure fingerprint characteristic compare.
A kind of above-mentioned multi-component complex oil sample dactylogram constructs and discrimination method, excitation wavelength used in step (1)
For two or more in 532nm, 514.5nm, 488nm, 457.9nm, 638nm, 632.8nm, 785nm, all spectrum
Data without the processing of any fluorescence background deduction, are standardized all spectroscopic datas, so that all spectrograms
Maximum of intensity is identical, and minimum value is also identical.
A kind of above-mentioned multi-component complex oil sample dactylogram constructs and discrimination method, and attenuator is set as 0.1% in step (1)
And 1% one or more, object lens 10 × or 50 ×, detection range 50-6000cm-1Or 200-6000cm-1。
A kind of above-mentioned multi-component complex oil sample dactylogram building and discrimination method, in step (3) to two-dimensional spectrum data into
When row resampling, the data break of two-dimension spectrum is 1-80cm-1。
Under preferable case, the data break of above-mentioned two-dimension spectrum is 20-40cm-1。
A kind of above-mentioned multi-component complex oil sample dactylogram constructs and discrimination method, and stepwise discriminatory method is selected from step (4)
Wilk ' s lambda, non-explained variance, Mahalanobis generalised distance, minimum F value or Rao ' s V.
Under preferable case, above-mentioned stepwise discriminatory method is Wilk ' s lambda method, and discrimination standard is the value of statistic F, works as F
Greater than FIntoWhen, retain the variable；When F value is less than FIt deletesWhen, reject the variable；Wherein, FIntoGreater than FIt deletes, FIntoFor 5.84-
1.84 FIt deletesFor 4.71-0.71；It is further preferable that FIntoIt is 3.84, FIt deletesIt is 2.71.
Calculation specifications in relation to Wilk ' s lambda and statistic F value are as follows:
For total sum of squares of deviations；
The sum of squares of deviations between group；
To organize interior sum of squares of deviations；
Wilk ' s lambda=SSE/SST；
MSA=SSA/ (m-1) is sum of squares of deviations between average group；
MSE=SSA/ (n-m), for sum of squares of deviations in average group；
F=MSA/MSE；
Wherein, n is total sample size, and m is the number of levels for controlling variable, XikFor i-th of horizontal lower k-th of sample value, niFor
I-th of horizontal sample size of variable is controlled,For i-th of mean value under horizontal,For observed quantity mean value.
Beneficial effects of the present invention: discrimination method of the invention can be obtained more richer than one-dimensional spectrum using two spectrum
Sample characteristic information, to improve identification precision；Using resampling technology, the discriminatory analysis based on two-dimension spectrum information is made to exist
It is more simple and efficient under conditions of retaining sample main feature information；Two-dimension spectrum information is projected by lower dimensional space and is carried out
" concentration " can make the fingerprint characteristic difference of different sample rooms more intuitive significant, be conducive to improve identification；Identification of the invention
Method is complementary to one another and confirms with existing crude oil identification method, improves accuracy and convincingness that crude oil identifies.
Detailed description of the invention
The synchronous related Raman spectrum of two dimension of Fig. 1 without resampling；A. the blind sample _ 1# of standard specimen _ 1#, b.；
The synchronous related Raman of two dimension after Fig. 2 resampling composes (sampling step length 5cm-1)；A. the blind sample of standard specimen _ 1#, b. _
1#；
The synchronous related Raman of two dimension after Fig. 3 resampling composes (sampling step length 10cm-1)；A. the blind sample of standard specimen _ 1#, b. _
1#；
The synchronous related Raman of two dimension after Fig. 4 resampling composes (sampling step length 20cm-1)；A. the blind sample of standard specimen _ 1#, b. _
1#；
The synchronous related Raman of two dimension after Fig. 5 resampling composes (sampling step length 40cm-1)；A. the blind sample of standard specimen _ 1#, b. _
1#；
The synchronous related Raman spectrum of two dimension of Fig. 6 without resampling；A. the blind sample _ 2# of standard specimen _ 2#, b.；
The synchronous related Raman of two dimension after Fig. 7 resampling composes (sampling step length 5cm-1)；A. the blind sample of standard specimen _ 2#, b. _
2#；
The synchronous related Raman of two dimension after Fig. 8 resampling composes (sampling step length 10cm-1)；A. the blind sample of standard specimen _ 2#, b. _
2#；
The synchronous related Raman of two dimension after Fig. 9 resampling composes (sampling step length 20cm-1)；A. the blind sample of standard specimen _ 2#, b. _
2#；
The synchronous related Raman of two dimension after Figure 10 resampling composes (sampling step length 40cm-1)；A. standard specimen _ 2#, b. are blind
Sample _ 2#；
Center of gravity stack diagram (the F of Figure 11 standard specimen and blind sample chaacteristic fingerprint spectrum in lower dimensional space projection coordinateThe upper limit=3.84, FLower limit
=2.71)；
Center of gravity perspective view (the F of Figure 12 standard specimen and blind sample chaacteristic fingerprint spectrum in lower dimensional space coordinate planeThe upper limit=3.84, FLower limit
=2.71).
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Embodiment 1
The present embodiment uses 15 kinds of crude oil standard specimens, comes from Sinopec Beijing Research Institute of Petro-Chemical Engineering.Crude oil standard specimen
And blind sample is respectively by 1-15# number consecutively, such as table 1.
1 crude oil of table number and title
| Serial number | Crude title |
| 1 | Horsepower cloth |
| 2 | Jie Nuo |
| 3 | It is sub- in poem |
| 4 | Section strangles |
| 5 | South Sinkiang mixing |
| 6 | Rich Buddhist nun's lightweight |
| 7 | Yunnan mixing |
| 8 | South Sinkiang -1 |
| 9 | South Sinkiang -2 |
| 10 | Breathe out state |
| 11 | Lucky drag-line |
| 12 | Oman |
| 13 | Basra weight |
| 14 | Ke Laowei |
| 15 | Card human relations |
The spectral fingerprint of each oil sample is acquired using Horiba JY XploRA microscopic confocal Raman spectrometer, acquires 4
The above parallel sample.Detection range is 50-3200cm-1, attenuator is set as 0.1%, aperture and slit be respectively 500 μm and
200 μm, object lens 10 ×, CCD detector temperature is -70 DEG C, time for exposure 1s, and each spectrogram is 30 times cumulative.Exciting light is 532nm
When, grating 2400T, when exciting light is 785nm, grating 1200T, all samples use identical test condition, spectrum number
According to without the processing of any fluorescence background deduction.Cube interpolation processing, step-length 1cm are carried out to each spectroscopic data-1, make to own
Spectroscopic data abscissa corresponds, then is standardized, and maximum value is set as 100, minimum value is set as 0.Then, it uses
Data calculation two-dimensional correlation spectra after standardization, and resampling is carried out to two-dimensional correlation spectra, retaining, dactylogram is main
Under conditions of feature, reduce the data volume of two-dimension spectrum；Extract upper triangular matrix after resampling in two-dimension spectrum matrix or
Inferior triangular flap is converted into one-dimension array with matlab by same rule.
Fig. 1 is standard specimen _ 1# related Raman spectrum synchronous with the two dimension of blind sample _ 1# without resampling；By standard specimen _ 1# and blind
The synchronous Raman spectrum of sample _ 1# two dimension carries out resampling, and step-length is respectively 5cm-1、10cm-1、20cm-1、40cm-1。
Fig. 2 is again that sampling step length is 5cm-1When obtained standard specimen _ 1# related Raman synchronous with the two dimension of blind sample _ 1# compose,
As can be seen that compared to Figure 1, the fingerprint characteristic of 1# oil sample is effectively maintained.
Fig. 3 is again that sampling step length is 10cm-1When obtained standard specimen _ 1# related Raman synchronous with the two dimension of blind sample _ 1# compose,
As can be seen that compared to Figure 1, the fingerprint characteristic of 1# oil sample is also effectively maintained.
Fig. 4 is again that sampling step length is 20cm-1When obtained standard specimen _ 1# related Raman synchronous with the two dimension of blind sample _ 1# compose,
As can be seen that compared to Figure 1, the fingerprint characteristic of 1# oil sample is also effectively maintained.
Fig. 5 is again that sampling step length is 40cm-1When obtained standard specimen _ 1# related Raman synchronous with the two dimension of blind sample _ 1# compose,
As can be seen that compared to Figure 1, the primary fingerprint feature of 1# oil sample is also preferably retained.
Fig. 6 is standard specimen _ 2# related Raman spectrum synchronous with the two dimension of blind sample _ 2# without resampling；By standard specimen _ 2# and blind
The synchronous Raman spectrum of sample _ 2# two dimension carries out resampling, and step-length is respectively 5cm-1、10cm-1、20cm-1、40cm-1。
Fig. 7 is again that sampling step length is 5cm-1When obtained standard specimen _ 2# related Raman synchronous with the two dimension of blind sample _ 2# compose,
As can be seen that the fingerprint characteristic of 2# oil sample is effectively maintained compared with Fig. 6.
Fig. 8 is again that sampling step length is 10cm-1When obtained standard specimen _ 2# related Raman synchronous with the two dimension of blind sample _ 2# compose,
As can be seen that the fingerprint characteristic of 2# oil sample is also effectively maintained compared with Fig. 6.
Fig. 9 is again that sampling step length is 20cm-1When obtained standard specimen _ 2# related Raman synchronous with the two dimension of blind sample _ 2# compose,
As can be seen that the fingerprint characteristic of 2# oil sample is also effectively maintained compared with Fig. 6.
Figure 10 is again that sampling step length is 40cm-1When obtained standard specimen _ 2# related Raman synchronous with the two dimension of blind sample _ 2#
Spectrum, it can be seen that compared with Fig. 6, the primary fingerprint feature of 2# oil sample is also preferably retained.
Comparison diagram 1 and Fig. 6, Fig. 2 and Fig. 7, Fig. 3 and Fig. 8, Fig. 4 and Fig. 9, Fig. 5 and Figure 10, it can be seen that in resampling
In dactylogram comparison afterwards, obvious embodiment is still can be obtained in the difference of 1# oil sample and 2# oil sample.On the other hand, the finger after resampling
In line spectrum, data variable number is substantially reduced, and the data processing work amount of corresponding discriminatory analysis can be made to mitigate significantly.
Use resampling step-length for 20cm-1Synchronize related fingerprint modal data, by Stepwise Discriminatory Analysis reject to oil
Sample identifies unessential data, the strong preferred variable group of reserve judgement ability；The method of discrimination used is Wilk ' s lambda
Method, discrimination standard are the value of statistic F, when F value is greater than FIntoWhen=3.84, retain the variable；When F value is less than FIt deletes=2.71
When, reject the variable；Spss software is reused, is then differentiated according to " similar deviation is minimum, and deviation is maximum between class " principle construction allusion quotation
Group of functions, using allusion quotation, then discriminant function projects the strong preferred variable group of discriminating power to lower dimensional space, by oil sample main feature
Difference " concentration " is to the most significant several dimension variables of cumulative proportion in ANOVA.
In lower dimensional space, the variance contribution of the most significant dimension variable of variance contribution ratio is as shown in table 2, and variance contribution ratio is most
The accumulative variance contribution ratio of first three significant dimension variable, can be more fully anti-using the coordinate of preceding three-dimensional up to 99.8%
Reflect the feature difference between variety classes sample.
The dimension variable variance contribution percentage of 2 lower dimensional space of table
| Dimension variable | Variance contribution % | Accumulation contribution % |
| 1 | 95.2 | 95.2 |
| 2 | 3.5 | 98.7 |
| 3 | 1.1 | 99.8 |
| 4 | 0.2 | 100.0 |
By coordinate mean value of all parallel samples of the standard specimen of 1-15# oil sample in new three-dimensional space, marked as this kind
The barycentric coodinates of sample.Similarly, coordinate of all parallel samples of the blind sample of 1-15# oil sample in new three-dimensional space is equal
Value, the barycentric coodinates as this kind of blind sample.By the most significant preceding three-dimensional barycentric coodinates of variance contribution, it is depicted as column stack diagram,
As a result as shown in figure 11.In Figure 11, characteristic difference is obvious between 15 kinds of crude oil standard specimen product, and the dactylogram according to blind sample and standard specimen is straight
Comparison is connect, realizes the accurate identification of 15 kinds of blind samples.
For 7#, 8#, 9#, 12#, 13# more similar in Figure 11, the center of gravity of each standard specimen and blind sample is drawn in three two dimensions
The projection of coordinate plane.As shown in figure 12, the difference of 7#, 8#, 9#, 12#, 13# can be recognized obviously by intuitively comparing.
Dactylogram building of the present invention and discrimination method can cooperate with other discrimination methods, significantly improve identification effect
Rate, accuracy and convincingness.Novel finger print spectrum building of the present invention and discrimination method are in the art work, historical relic, jewelry, criminal investigation
The Nondestructive Identification of material evidence, before the fields such as genunie medicinal materials, the place of production discriminating of marine product, medical conditions diagnosis are also widely used
Scape.
For any person skilled in the art, without departing from the scope of the technical proposal of the invention, all
Many possible changes and modifications are made to technical solution of the present invention using the technology contents of the disclosure above, or are revised as equivalent
The equivalent embodiment of variation.Therefore, anything that does not depart from the technical scheme of the invention, according to the technical essence of the invention to
Any simple modifications, equivalents, and modifications that upper embodiment is done should all be still fallen within the scope of protection of the technical scheme of the present invention.
Claims (9)
1. a kind of multi-component complex oil sample dactylogram building and discrimination method, which comprises the following steps:
(1) to the standard specimen of Known Species and blind sample to be identified, parallel sample is acquired respectively；For each oil sample, using Raman
Spectrometer measures a series of spectroscopic datas comprising fluorescence and Raman information under different shooting conditions；
(2) spectroscopic data measured under different shooting conditions is subjected to interpolation processing, keeps all spectroscopic data abscissas one a pair of
It answers, seeks the synchronous correlation spectrum of the two dimension for calculating each standard specimen and blind sample；
(3) under conditions of retaining dactylogram main feature, resampling is carried out to the synchronous related spectral data of above-mentioned two dimension；It mentions
The upper triangular matrix or inferior triangular flap in two-dimension spectrum matrix after taking resampling, is converted into one-dimension array；
(4) it is based on above-mentioned one-dimension array, intensive variable is screened using stepwise discriminatory method analysis, is rejected inessential to differentiating
Variable, only the strong set of variables of reserve judgement ability is as preferred variable group；According to " similar deviation is minimum, and deviation is maximum between class "
Principle construction allusion quotation then discriminant function group；Based on allusion quotation then discriminant function group, by intensity data corresponding to the set of variables preferably gone out
It projects to new lower dimensional space；
(5) according to projection coordinate in new lower dimensional space, drafting column stack diagram intuitively compares or drawing three-dimensional space projection figure
Fingerprint characteristic compares, and can identify blind sample.
2. a kind of multi-component complex oil sample dactylogram building according to claim 1 and discrimination method, it is characterised in that: step
Suddenly (5) column stack diagram intuitively compare in similar sample, then drawing three-dimensional space projection figure fingerprint characteristic compare.
3. a kind of multi-component complex oil sample dactylogram building according to claim 1 and discrimination method, it is characterised in that: step
Suddenly in excitation light wave a length of 532nm, 514.5nm, 488nm, 457.9nm, 638nm, 632.8nm, 785nm used in (1)
Two or more, all spectroscopic datas without the processing of any fluorescence background deduction, are marked all spectroscopic datas
Quasi-ization processing, so that the maximum of intensity of all spectrograms is identical, minimum value is also identical.
4. a kind of multi-component complex oil sample dactylogram building according to claim 1 and discrimination method, it is characterised in that: step
Suddenly in (1) attenuator be set as 0.1% and 1% one or more, object lens 10 × or 50 ×, detection range 50-
6000cm-1Or 200-6000cm-1。
5. a kind of multi-component complex oil sample dactylogram building according to claim 1 and discrimination method, it is characterised in that: step
When carrying out resampling to two-dimensional spectrum data in (3) suddenly, the data break of two-dimension spectrum is 1-80cm-1。
6. a kind of multi-component complex oil sample dactylogram building according to claim 5 and discrimination method, it is characterised in that: institute
Stating data break is 20-40cm-1。
7. a kind of multi-component complex oil sample dactylogram building according to claim 1 and discrimination method, it is characterised in that: step
Suddenly stepwise discriminatory method is selected from Wilk ' s lambda, non-explained variance, Mahalanobis generalised distance, minimum F value or Rao ' in (4)
sV。
8. a kind of multi-component complex oil sample dactylogram building according to claim 7 and discrimination method, it is characterised in that: by
Step diagnostic method is Wilk ' s lambda method, and discrimination standard is the value of statistic F, when F is greater than FIntoWhen, retain the variable；When F value
Less than FIt deletesWhen, reject the variable；Wherein, FIntoGreater than FIt deletes, FIntoFor 5.84-1.84, FIt deletesFor 4.71-0.71.
9. a kind of multi-component complex oil sample dactylogram building according to claim 8 and discrimination method, it is characterised in that: institute
State FIntoIt is 3.84, FIt deletesIt is 2.71.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113640331A (en) * | 2020-04-27 | 2021-11-12 | 华东师范大学 | Edible oil type identification and quality detection method based on nuclear magnetic resonance technology |
| CN113640331B (en) * | 2020-04-27 | 2023-09-15 | 华东师范大学 | Edible oil type identification and quality detection method based on nuclear magnetic resonance technology |
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