CN113655050B - 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 58
- 239000010779 crude oil Substances 0.000 title claims abstract description 48
- 239000003921 oil Substances 0.000 title claims abstract description 38
- 238000001514 detection method Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000001228 spectrum Methods 0.000 claims description 34
- 238000009499 grossing Methods 0.000 claims description 8
- 230000002159 abnormal effect Effects 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 5
- 230000003595 spectral effect Effects 0.000 claims description 5
- 238000001069 Raman spectroscopy Methods 0.000 claims description 3
- 238000010238 partial least squares regression Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000012544 monitoring process Methods 0.000 abstract 1
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- 238000002329 infrared spectrum Methods 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012549 training Methods 0.000 description 1
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Abstract
The invention discloses a method for improving the detection limit of a trace crude oil Raman spectrum in light oil. 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 fault working 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
Crude oil and various light oils are often adopted by refining enterprises to exchange heat, but leakage is likely to occur in the heat exchange process. Once the heat exchanger leaks, crude oil can pollute light oil, so that the product quality is reduced, and potential safety hazards are brought to production. In the production, the requirement on the crude oil content detection limit index leaked into light oil is very high, even lower than 10ppm, and the detection difficulty is very high.
Compared with gas chromatography and near infrared spectrum detection methods, raman spectrum is very sensitive to dark samples, especially crude oil, has strong fluorescent background in Raman spectrum, and pure light oil of a refining enterprise is colorless transparent or yellowish liquid at normal temperature and normal pressure, and has no fluorescent background. Thus, the detection of crude oil in light oil is achieved by utilizing this characteristic of raman spectrum, and research and application have been started in industry in recent years.
However, from the current results of research, trace crude oil concentrations detected using raman spectroscopy are typically around 25ppm, as in applicant's prior application patent CN202010420057.2. For trace crude oil with concentration lower than the concentration, the peak intensity of the Raman spectrum is low, the Raman spectrum distinction of trace crude oil with different concentrations is small, and the manual operation, the spectrometer and the like can bring adverse effects to the detection precision of the Raman spectrum. Therefore, it is necessary to perfect the raman spectrum detection method, further reduce the detection limit, and promote the application of raman spectrum in measuring crude oil leakage.
Disclosure of Invention
The invention discloses a method for improving the Raman spectrum detection limit of trace crude oil in light oil, which can rapidly identify trace crude oil with the concentration as low as 1ppm in the light oil.
The invention comprises the following steps:
and acquiring a sample Raman spectrum offline, establishing a trace crude oil Raman spectrum detection model by adopting the highest peak and the sub-peak of the Raman spectrum, and detecting the concentration of the trace crude oil to be detected by using the model.
The detection model is established as follows:
(1) Preparing crude oil light oil mixed samples with different concentrations in an off-line manner, wherein the concentrations are 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm and 20ppm respectively, and preparing pure light oil samples which are not doped with 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 sub-peak of the Raman spectrum of the sample, wherein the wave number range of the peak is 165-590 cm -1 and 1405-1520 cm -1 respectively;
(4) Establishing a model M 1 by using standardized spectrum data with the wave number range of 165-590 cm -1 in the original Raman spectrum of the sample, and establishing a model M 2 by using standardized spectrum data with the wave number range of 1405-1520 cm -1 in the original Raman spectrum of the sample;
(5) Carrying out smoothing treatment on the original spectrum by adopting a Savitzky-Golay 3 times 17-point convolution smoothing algorithm to obtain a sample smooth spectrum, removing a nonlinear part in a spectrogram curve, and improving the signal to noise ratio of the spectrogram;
(6) Establishing a model M 3 by using standardized spectrum data with a wave number range of 165-590 cm -1 in a sample smooth Raman spectrum, and establishing a model M 4 by using spectrum data with a wave number range of 1405-1520 cm -1 in a sample original Raman spectrum;
after the model is established, the light oil is monitored on line by using the model, and the steps are as follows:
(1) Collecting Raman spectrum of light oil on line, wherein the spectrum wave number range is 55-3255 cm -1;
(2) Adopting a Savitzky-Golay 3 times 17-point convolution smoothing algorithm to carry out smoothing treatment on an original Raman spectrum of the light oil to be detected to obtain a smooth Raman spectrum;
(3) Intercepting spectrum data of which the wave number range of the original Raman spectrum and the smooth Raman spectrum of the light oil to be detected is 165-590 cm -1 and 1405-1520 cm -1, and carrying out standardized treatment to obtain an input of a model M 1、M2、M3、M4;
(4) Predicting the concentration of crude oil to be detected by using a model M 1、M2、M3、M4 to obtain an intermediate prediction result R 1、r2、r3、r4, solving the mean square error of the prediction result, screening out abnormal prediction results to obtain n (n is less than or equal to 4) prediction results R 1、R2,...,Rn, and finally obtaining the integrated result
The beneficial effects are that:
The invention discloses a method for improving the detection limit of trace crude oil Raman spectrum in light oil, which comprises the steps of selecting the highest peak and sub-peak wave number segments in the Raman spectrum of the light oil, training a plurality of models for prediction, screening out abnormal prediction results, and integrating the abnormal prediction results into final prediction results. The method establishes a plurality of models and performs integrated prediction, is favorable for screening abnormal data and reducing the influence of modeling errors, so that the detection precision of trace crude oil is improved, and the detection limit of crude oil leakage concentration can be reduced to 1ppm.
Drawings
FIG. 1 is a flow chart of spectrum detection of trace crude oil in light oil according to the invention;
FIG. 2 is a raw spectral plot of batch A, 5ppm samples of the inventive example;
FIG. 3 is a spectrum of the smoothed spectrum of FIG. 2;
FIG. 4 is a graph showing the spectra of different crude oil concentrations for batch A samples according to an embodiment of the present invention.
Detailed description of the preferred embodiments
The effect of the method in analyzing trace crude oil in light oil will be described by specific operation flow with reference to the accompanying drawings and specific examples. The present embodiment is implemented on the premise of the technical solution of the present invention, but the scope of protection 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 industrial processes. The detection flow is shown in fig. 1. The method comprises the steps of configuring crude oil and kerosene mixed samples with different concentrations through a laboratory, scanning Raman spectra and carrying out relevant pretreatment, so as to establish a plurality of models, integrating prediction results of the models to obtain final prediction results, and configuring other two groups of mixed oil as samples to be tested to test the prediction effects of the models.
The method comprises the following steps:
(1) Preparing 3 batches of crude oil and kerosene mixed samples respectively:
batch a: 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm, 20ppm;
batch B samples: 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm, 20ppm;
batch C: 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm, 20ppm;
(2) And scanning the samples by adopting a Raman spectrometer to obtain Raman spectra of the samples within the range of 55-3255 cm -1, wherein each sample is scanned by 2 spectra. Specific raman spectra are shown in fig. 2;
(3) Each stretch-draw Raman spectrum is subjected to convolution smoothing by adopting Savitzky-Golay for 3 times at 17 points, and the smoothed spectrogram is shown in figure 3;
(4) The spectra of different crude oil concentrations for lot a samples were observed as shown in fig. 4. It is evident that the spectrum in the range of 55 to 3255cm -1 is gradually inclined upward as the crude oil concentration increases, which is caused by the increase in fluorescence background, and that the higher the crude oil concentration is, the greater the fluorescence intensity is. In the graph, the highest peak and the second peak, namely the wave number ranges of spectra of 165-590 cm -1 and 1405-1520 cm -1 show a nearly linear superposition change relation between the concentration of trace crude oil and the fluorescence intensity, so that the two spectra are suitable for establishing a regression model of low-concentration mixed light oil;
(6) Carrying out standardization treatment on an original spectrum band and a smooth spectrum band of samples A within the range of 55-3255 cm -1, respectively intercepting spectra of the wave numbers within 165-590 cm -1 and 1405-1520 cm -1, establishing a partial least square model M 1 by using the original spectra of samples A within the wave numbers within 165-590 cm -1, establishing a partial least square model M 2 by using the original spectra of samples A within the wave numbers within 1405-1520 cm -1, establishing a partial least square model M 3 by using the smooth spectra of samples A within the wave numbers within 165-590 cm -1, and establishing a partial least square model M 4 by using the smooth spectra of samples A within the wave numbers within 1405-1520 cm -1;
(7) Predicting the samples of the batch B and the batch C by using the 4 partial least squares models in the step (6), wherein the mean square error MSE of the 4 models is less than 0.25, so that abnormal prediction results are avoided, and the final integrated result is that The predicted results for each sample are shown in tables 1 and 2, respectively;
Table 1B batch sample prediction results (content unit is ppm)
Table 2C batch sample prediction results (content unit is ppm)
According to the analysis, the invention extracts the spectrum section with better linear characteristic in the Raman spectrum, respectively models and predicts the integration, and realizes the accurate detection of the trace crude oil in the mixed light oil with the concentration of 1-20 ppm. The detection limit of detecting trace crude oil by Raman spectrum is further reduced, so that the condition that crude oil leaks into light oil products in the industrial production process can be monitored more sensitively by Raman spectrum, early warning of fault working conditions is facilitated, product quality is stabilized, and production safety is guaranteed.
Claims (7)
1. A method for improving the detection limit of a raman spectrum of a trace crude oil in a light oil, which is characterized by respectively modeling the highest peak and the next highest peak of the raman spectrum and integrating the prediction result, comprising the following steps:
(1) Preparing crude oil light oil mixed samples with different concentrations in an off-line manner, and preparing a pure light oil sample without crude oil;
(2) Measuring Raman spectrum of each sample, wherein the spectrum wave number range is a 1～a2cm-1;
(3) Selecting the highest peak and the sub-peak of the Raman spectrum of the sample, and recording the wave number range of the sample as b 1～b2cm-1 and c 1～c2cm-1 respectively;
(4) Establishing a model M 1 by using standardized spectrum data with a wave number range of b 1～b2cm-1 in the original Raman spectrum of the sample, and establishing a model M 2 by using standardized spectrum data with a wave number range of c 1～c2cm-1 in the original Raman spectrum of the sample;
(5) Smoothing the original Raman spectrum of the sample to obtain a smooth Raman spectrum of the sample, establishing a model M 3 by using standardized spectrum data with a wave number range of b 1～b2cm-1 in the smooth Raman spectrum of the sample, and establishing a model M 4 by using standardized spectrum data with a wave number range of c 1～c2cm-1 in the smooth Raman spectrum of the sample;
(6) The Raman spectrum of the light oil is collected on line, and the spectrum range is a 1～a2cm-1;
(7) Smoothing spectral data with the wave number range of a 1～a2cm-1 in the spectrum to be detected to obtain a smooth Raman spectrum, intercepting the original Raman spectrum and the spectral data with the wave number range of b 1～b2cm-1 and c 1～c2cm-1 in the smooth Raman spectrum, and carrying out standardized processing on the spectral data, wherein the distribution is used as the input of a model M 1、M2、M3、M4;
(8) Predicting the concentration of crude oil to be detected by using a model M 1、M2、M3、M4 to obtain an intermediate prediction result r 1、r2、r3、r4;
(9) Solving the mean square error of the predicted result and screening out the abnormal predicted result to obtain n which is less than or equal to 4 predicted results R 1、R2,...,Rn, wherein the final integrated result is
2. The method for improving the raman spectrum detection limit of trace crude oil in light oil according to claim 1, wherein the raman spectrum range a 1～a2cm-1 is measured to be 55-3255 cm -1.
3. The method for improving the detection limit of the raman spectrum of the trace crude oil in the light oil according to claim 1, wherein the wave number range b 1～b2cm-1 of the highest peak of the raman spectrum is 165-590 cm -1, and the wave number range c 1～c2cm-1 of the sub-peak is 1405-1520 cm -1.
4. The method for improving the detection limit of the raman spectrum of the trace crude oil in the light oil according to claim 1, wherein the original spectrum is smoothed by using a Savitzky-Golay 3-order 17-point convolution smoothing algorithm.
5. A method of improving the raman spectral limit of trace amounts of crude oil in light oil according to claim 1, characterized by using partial least squares regression modeling.
6. The method for improving the raman spectrum detection limit of trace crude oil in light oil according to claim 1, wherein the concentration of the crude oil light oil mixed samples with different concentrations is 1ppm, 2ppm, 3ppm, 4ppm, 5ppm, 10ppm and 20ppm respectively.
7. The method for improving the raman spectrum detection limit of trace crude oil in light oil according to claim 1, wherein the mean square error threshold value when screening out abnormal samples is 0.25.
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