CN113655050A - Method for improving Raman spectrum detection limit of trace crude oil in light oil - Google Patents
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- 238000001237 Raman spectrum Methods 0.000 title claims abstract description 57
- 239000010779 crude oil Substances 0.000 title claims abstract description 46
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000001228 spectrum Methods 0.000 claims abstract description 24
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- 238000009499 grossing Methods 0.000 claims description 7
- 230000002159 abnormal effect Effects 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims 1
- 238000010238 partial least squares regression Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000007781 pre-processing Methods 0.000 abstract 1
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 238000001069 Raman spectroscopy Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
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- 238000004817 gas chromatography Methods 0.000 description 1
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- 238000001320 near-infrared absorption spectroscopy Methods 0.000 description 1
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Abstract
The invention discloses a method for improving Raman spectrum detection limit of trace crude oil in light oil, which comprises the steps of selecting different spectral bands with good linear characteristics in a Raman spectrum, obtaining a plurality of prediction models by adopting different preprocessing methods, predicting a spectrum to be detected and integrating prediction results to obtain a final prediction result. The method reduces the detection limit of the concentration of trace crude oil in the light oil to 1ppm, thereby more sensitively monitoring the condition of crude oil leaking to the light oil product in the industrial production process, improving the detection performance of Raman spectrum, being beneficial to early warning of fault conditions, stabilizing the product quality and ensuring the production safety.
Description
Technical Field
The invention relates to a trace detection method, in particular to a method for improving the Raman spectrum detection limit of trace crude oil in light oil.
Background
The refinery enterprises usually adopt crude oil and various light oils for heat exchange, but leakage is possible in the heat exchange process. Once the heat exchanger leaks, the crude oil can pollute the light oil, so that the product quality is reduced, and potential safety hazards are brought to production. The detection limit index of the crude oil content leaked to the light oil in the production is very high, even is as low as below 10ppm, and the detection difficulty is very high.
Compared with a gas chromatography method and a near infrared spectrometry method, the Raman spectrum is very sensitive to a dark color sample, particularly the crude oil has a very strong fluorescence background in the Raman spectrum, and the pure light oil of the refining enterprise is colorless transparent or yellowish liquid at normal temperature and pressure and has no fluorescence background. Therefore, crude oil detection in light oil is achieved by utilizing this characteristic of raman spectroscopy, which has recently begun to be studied and applied in industry.
However, according to the prior research results, the concentration of the trace crude oil detected by Raman spectroscopy is generally about 25ppm, such as the patent CN202010420057.2 of the applicant's prior application. For trace crude oil with concentration lower than the concentration, the peak intensity of the Raman spectrum is low, the Raman spectrum regions of the trace crude oil with different concentrations have small graduation, and the Raman spectrum detection precision can be adversely affected by manual operation, a spectrum instrument and the like. Therefore, it is necessary to improve the detection method of raman spectroscopy, further reduce the detection limit, and promote the application of raman spectroscopy in measuring crude oil leakage.
Disclosure of Invention
The invention discloses a method for improving Raman spectrum detection limit of trace crude oil in light oil, which can quickly identify the trace crude oil with concentration as low as 1ppm in the light oil.
The invention comprises the following steps:
and (3) acquiring a Raman spectrum of the sample off line, establishing a Raman spectrum detection model of the trace crude oil by adopting the highest peak and the secondary peak of the Raman spectrum, and detecting the concentration of the trace crude oil to be detected by using the model.
The establishment process of the detection model is as follows:
(1) preparing mixed samples of crude oil and light oil with different concentrations in an off-line mode, wherein the concentrations of the mixed samples are 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm and 20ppm respectively, and preparing pure light oil samples without being doped with the crude oil;
(2) measuring the Raman spectrum of each sample and carrying out standardization treatment, wherein the spectrum wave number range is 55-3255 cm-1；
(3) Selecting the highest peak and the secondary peak of the Raman spectrum of the sample, wherein the wave number ranges of the peak and the secondary peak are 165-590 cm respectively-1And 1405-1520 cm-1；
(4) The original Raman spectrum of the sample has the wave band range of 165-590 cm-1The standardized spectral data of (A) is modeled1The original Raman spectrum of the sample is used, and the wave band range is 1405-1520 cm-1The standardized spectral data of (A) is modeled2；
(5) Smoothing the original spectrum by adopting a Savitzky-Golay 3-time 17-point convolution smoothing algorithm to obtain a sample smoothed spectrum, removing a nonlinear part in a spectrogram curve, and improving the signal-to-noise ratio of the spectrogram;
(6) the range of the wave band in the smooth Raman spectrum of the sample is 165-590 cm-1The standardized spectral data of (A) is modeled3The original Raman spectrum of the sample is used, and the wave band range is 1405-1520 cm-1Spectral data of (2) establishing a model M4；
After the model is established, the model is used for carrying out on-line monitoring on the light oil, and the steps are as follows:
(1) the Raman spectrum of the light oil is collected on line, and the spectrum wave number range is 55-3255 cm-1；
(2) Smoothing the original Raman spectrum of the light oil to be measured by adopting a Savitzky-Golay 3-time 17-point convolution smoothing algorithm to obtain a smoothed Raman spectrum;
(3) the range of the original Raman spectrum and the smooth Raman spectrum of the light oil to be detected is cut out and ranges from 165 cm to 590cm-1And 1405-1520 cm-1Is normalized as a model M1、M2、M3、M4The input of (1);
(4) using model M1、M2、M3、M4The concentration of the crude oil to be measured is predicted to obtain an intermediate prediction result r1、r2、r3、r4Calculating the mean square error of the prediction result and screening the abnormal prediction result to obtain n (n is less than or equal to 4) prediction results R1、R2,...,RnThe final integrated result is
Has the advantages that:
the invention discloses a method for improving Raman spectrum detection limit of trace crude oil in light oil, which trains a plurality of models for prediction by selecting the highest peak and the second highest peak wave number in Raman spectrum of light oil, and screens out abnormal prediction results to be integrated into a final prediction result. The method establishes a plurality of models and carries out integrated prediction, is favorable for screening abnormal data and reducing the influence of modeling errors, thereby improving the detection precision of trace crude oil and reducing the detection limit of crude oil leakage concentration to 1 ppm.
Drawings
FIG. 1 is a flow chart of the spectral detection of trace crude oil in light oil according to the present invention;
FIG. 2 is a raw spectrum of batch A, 5ppm sample according to an exemplary embodiment of the present invention;
FIG. 3 is a graph of the smoothed spectrum of FIG. 2;
FIG. 4 is a spectrum of different crude concentrations for batch A samples according to an embodiment of the present invention.
Detailed description of the preferred embodiment
The following describes the effect of the method in analyzing trace crude oil in light oil by a specific operation flow with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical solution of the present invention, but the scope of the present invention is not limited to the following embodiments.
The invention takes the analysis process in a laboratory as an example, and is also suitable for online detection in the industrial process. The detection process is shown in FIG. 1. Crude oil and kerosene mixed samples with different concentrations are configured in a laboratory, Raman spectra are scanned and relevant pretreatment is carried out, a plurality of models are built according to the Raman spectra, prediction results of the models are integrated to obtain final prediction results, and the other two groups of mixed oil are configured to serve as samples to be tested so as to test the prediction effect of the models.
The method specifically comprises the following steps:
(1) 3 batches of crude oil and kerosene mixed samples were prepared:
batch a samples: 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm, 20 ppm;
sample batch B: 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm, 20 ppm;
sample batch C: 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm, 20 ppm;
(2) aiming at the samples, scanning by adopting a Raman spectrometer to obtain 55-3255 cm of each sample-1Raman spectra in the range, 2 spectra were scanned per sample. The specific raman spectrum is shown in fig. 2;
(3) each tensioman spectrum is smoothed by adopting Savitzky-Golay 3 times 17-point convolution, and the smoothed spectrogram is shown in figure 3;
(4) and (4) observing the spectrum of the A batch of samples with different crude oil concentrations, as shown in figure 4. The concentration of the crude oil is obviously increased, and the concentration is 55-3255 cm-1The spectra within the range are gradually tilted upward, which is caused by the increase in fluorescence background, and it is found that the higher the crude oil concentration, the greater the fluorescence intensity. The highest peak and the second highest peak in the figure, namely the wave number range is 165-590 cm-1And 1405-1520 cm-1The spectrum of (1) shows a change relation close to linear superposition between the concentration of the trace crude oil and the fluorescence intensity, so that the two sections of spectra are suitable for establishing a regression model of the low-concentration mixed light oil;
(6) for batch A, samples are 55-3255 cm-1Standardizing the original spectral band and the smooth spectral band in the range, and respectively intercepting the wave number range of 165-590 cm-1And 1405-1520 cm-1The wave number of the sample A is 165-590 cm-1Partial least square model M is established by the original spectrum1The wave number of the sample A is 1405-1520 cm-1Partial least square model M is established by the original spectrum2Using A lot of samples with wave number ranging from 165 to e590cm-1Partial least square model M is established by the smooth spectrum3The wave number of the sample A is 1405-1520 cm-1Partial least square model M is established by the smooth spectrum4；
(7) Predicting samples of batch B and batch C by using 4 partial least squares models in step (6) due to Mean Square Error (MSE) of 4 models<0.25, so there is no abnormal prediction result, and the final integrated result is
The predicted results of each sample are shown in tables 1 and 2, respectively;
TABLE 1B batch sample prediction results (content in ppm)
TABLE 2C predicted results for lots of samples (in ppm content)
According to the analysis, the spectrum band with good linear characteristic in the Raman spectrum is extracted, and modeling is respectively carried out to carry out integrated prediction, so that the accurate detection of the trace crude oil in the mixed light oil of 1-20 ppm is realized. The detection limit of the Raman spectrum for detecting the trace crude oil is further reduced, so that the Raman spectrum can more sensitively monitor the condition that the crude oil leaks to the light oil product in the industrial production process, the early warning of fault conditions is facilitated, the product quality is stabilized, and the production safety is guaranteed.
Claims (7)
1. A method for improving the Raman spectrum detection limit of trace crude oil in light oil is characterized in that the highest peak and the secondary peak of a Raman spectrum are respectively modeled, and the prediction results are integrated, and the method comprises the following steps:
(1) preparing mixed samples of crude oil and light oil with different concentrations in an off-line manner, and preparing pure light oil samples without being mixed with the crude oil;
(2) measuring the Raman spectrum of each sample, wherein the spectral wavenumber range is a1～a2cm-1；
(3) Selecting the highest peak and the second highest peak of the Raman spectrum of the sample, and recording the wave number ranges of the peaks as b1～b2cm-1And c1～c2cm-1；
(4) Using a sample with a range of b in original Raman spectrum1～b2cm-1The normalized spectral data of (a) is modeled as M1Using a sample having a range of wavelengths c in the original Raman spectrum1～c2cm-1The normalized spectral data of (a) is modeled as M2；
(5) Smoothing the original Raman spectrum of the sample to obtain a smooth Raman spectrum of the sample, wherein the smooth Raman spectrum of the sample has a wave band range of b1～b2cm-1The normalized spectral data of (a) is modeled as M3Using a sample with a smooth Raman spectrum having a wavelength range of c1～c2cm-1The normalized spectral data of (a) is modeled as M4；
(6) Collecting the Raman spectrum of the light oil on line, wherein the spectrum range is a1～a2cm-1；
(7) The range of the wave number band in the spectrum to be measured is a1～a2cm-1Smoothing the spectrum data to obtain a smooth Raman spectrum, and intercepting the original Raman spectrum and the smooth Raman spectrum with the wave band range of b1～b2cm-1And c1～c2cm-1Is normalized and the distribution is used as a model M1、M2、M3、M4The input of (1);
(8) using model M1、M2、M3、M4Carrying out the concentration measurement of the crude oilPredicting to obtain intermediate prediction result r1、r2、r3、r4；
(9) Solving the mean square error of the prediction result and screening out the abnormal prediction result to obtain n, n is less than or equal to 4 prediction results R1、R2,...,RnThe final integrated result is
2. The method for improving the Raman spectrum detection limit of the trace crude oil in the light oil according to claim 1, wherein the Raman spectrum range a is determined1～a2cm-1Is 55-3255 cm-1。
3. The method for improving the Raman spectrum detection limit of the trace crude oil in the light oil as claimed in claim 1, wherein the wavenumber range b of the highest peak of the Raman spectrum is selected1～b2cm-1Is 165-590 cm-1Wave number range of the second peak c1～c2cm-1Is 1405-1520 cm-1。
4. The method for improving the Raman spectrum detection limit of the trace crude oil in the light oil as recited in claim 1, wherein the original spectrum is smoothed by Savitzky-Golay 3-times 17-point convolution smoothing algorithm.
5. The method for improving the Raman spectrum detection limit of the trace crude oil in the light oil according to claim 1, wherein partial least squares regression modeling is used.
6. The method for improving the Raman spectrum detection limit of the trace crude oil in the light oil as claimed in claim 1, wherein the crude oil light oil mixed samples with different concentrations are 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm and 20ppm respectively.
7. The method for improving the Raman spectrum detection limit of the trace crude oil in the light oil according to claim 1, wherein the mean square error threshold value when the abnormal samples are screened is 0.25.
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