CN102590175B - Raman spectrum superposition-based method for quickly determining content of methanol in methanol gasoline - Google Patents
Raman spectrum superposition-based method for quickly determining content of methanol in methanol gasoline Download PDFInfo
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- CN102590175B CN102590175B CN201210039272.3A CN201210039272A CN102590175B CN 102590175 B CN102590175 B CN 102590175B CN 201210039272 A CN201210039272 A CN 201210039272A CN 102590175 B CN102590175 B CN 102590175B
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 372
- 239000003502 gasoline Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000001237 Raman spectrum Methods 0.000 title claims abstract description 15
- 238000001228 spectrum Methods 0.000 claims abstract description 116
- 239000002199 base oil Substances 0.000 claims abstract description 52
- 238000005259 measurement Methods 0.000 claims abstract description 14
- 239000003921 oil Substances 0.000 claims description 16
- 238000001069 Raman spectroscopy Methods 0.000 claims description 14
- 238000010606 normalization Methods 0.000 claims description 12
- 239000004215 Carbon black (E152) Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 229930195733 hydrocarbon Natural products 0.000 claims description 8
- 150000002430 hydrocarbons Chemical class 0.000 claims description 8
- 238000003556 assay Methods 0.000 claims description 6
- 230000003595 spectral effect Effects 0.000 claims description 5
- 230000009897 systematic effect Effects 0.000 claims description 4
- 238000012545 processing Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003822 preparative gas chromatography Methods 0.000 description 2
- 238000012549 training Methods 0.000 description 2
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a Raman spectrum superposition-based method for quickly determining the content of methanol in methanol gasoline. The Raman spectrum superposition-based method comprises the following steps of: firstly, measuring a base oil spectrum, a pure methanol spectrum and a methanol gasoline spectrum with known methanol content; secondly, obtaining a spectrum superposing formula according to data and storing base oil and a corresponding spectrum superposition parameter in a spectrum database; and constructing the spectrum database and then estimating the content of the methanol from the methanol gasoline spectrum with the unknown methanol content by using the spectrum superposition formula. The invention provides the spectrum superposition formula from a view of spectrum soft processing as well as the formula-based method for quickly determining the content of the methanol in the methanol gasoline. According to the method, the quantity of samples required to be calibrated can be greatly reduced in the application process, the labor capacity of calibrating works is reduced and the problem that the measurement for low-content methanol is inaccurate or even cannot be measured in the traditional method is overcome; and in addition, the measurement precision of the unknown methanol gasoline prepared from the base oil can also be maintained.
Description
Technical field
The invention belongs to Chemical Measurement field, relate to the spectral measurement method of material in a kind of potpourri, relate in particular to the measuring method of methanol content in a kind of methanol gasoline.
Background technology
Along with China's rapid development of economy, the quick increase of automobile use amount, home market increases rapidly the demand of gasoline, and the oil of Yi Gei China is supplied with environmental protection and has been brought immense pressure.The unique method that changes oil shortage, severe environmental pollution is exactly the dependence reducing oil, developing green high-efficiency cleaning substitute energy.Methanol gasoline is as the substitute of regular gasoline, be a kind of " replace oil with coal " and path, can directly substitute regular gasoline, alleviate gasoline in short supply in, have good environmental benefit, to the sustainable development of the national ecological economy, society progress all tool be of great significance.
Methanol gasoline is the potpourri of methyl alcohol, gasoline and adjuvant.Methyl alcohol incorporation is generally 5%～30%.Take and mix 15% as at most, claim M15 methanol gasoline.The calorific value of methyl alcohol is about half of gasoline, is not changing under the prerequisite of motor car engine ratio of compression, and methanol content must be fixed within the specific limits.If content is too low, can cause octane value too low and infringement engine; Too high levels, can cause fuel value inadequate, increases oil consumption, raises the cost.The end of the year 2009, China has formally promulgated high-proportion methanol gasoline for vehicle product standard < < Vehicular methanol petrol (M85) > >, and requiring the content of methyl alcohol in methanol gasoline is 85% left and right.Shaanxi Province has popularized in an all-round way and has used M15 methanol gasoline.In the provincial standard of national standard (M85) and each province, as the provincial standard < < M30 of Hebei province Vehicular methanol petrol > >, < < Vehicular methanol petrol component oil > >, Shanxi Province provincial standard DB14/T 92-2002, the provincial standard DB33/T 756.2-2009 of Zhejiang Province etc., have done strict requirement to the methanol content in methanol gasoline.
In each class standard, the official method of measuring methanol content comprises vapor-phase chromatography and fractionating process.These two kinds of methods are measured accurately, but complicated operation, sense cycle is long, and equipment is complicated, is not suitable for Site Detection.Meanwhile, vapor-phase chromatography also needs to carry out interior mark.For this reason, need to develop the quick and precisely measuring method of methanol content in blend gasoline, it has vital meaning for quality control and the check of methanol gasoline.
Current method for quick mainly adopts near infrared spectrum and Raman spectrum analysis method.First these class methods utilize near infrared or Raman spectrometer to obtain the spectroscopic data of oil product to be measured, then compare with the spectrum of training sample a large amount of in database (oil sample that refers to known methanol content and corresponding spectrum), and then estimate methanol content in methanol gasoline.These class methods, measuring speed is fast, easy to use.But the subject matter that these two class methods exist is need to collect a large amount of different base oils, the training sample of different methanol contents, like this accuracy of detection of guarantee to oil product methanol content to be measured.Meanwhile, due to the molecule absorption characteristic of near infrared spectrum, measurement result is subject to other alcohols and disturbs.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of content of methanol in methanol gasoline rapid assay methods based on Raman spectrum stack is provided, the method is easy, effective.
The object of the invention is to be achieved through the following technical solutions: a kind of content of methanol in methanol gasoline rapid assay methods based on Raman spectrum linear superposition theorem, the method comprises the following steps:
(1) methyl alcohol is added in a certain base oil to the methanol gasoline of configuration arbitrary volume content; Base oil is used the Raman spectrum of Raman spectrometer Fundamentals of Measurement oil, above-mentioned methanol gasoline and pure methyl alcohol; First to the spectrum obtaining carry out smoothly, the pre-service such as noise filtering, fluorescence background removal; Then base oil and methanol gasoline spectrum are carried out to the normalization of stable hydrocarbon characteristic peak, obtain spectrum A and spectrum B; Pure methyl alcohol spectrum is carried out to maximal value normalization, obtain spectrum C;
Described base oil refer to be mixed by catalytic gasoline, Reformed Gasoline and MTBE not containing the regular price gasoline of methyl alcohol.
(2) spectrum B is expressed as to the weighted algebraic sum of base oil spectrum A, pure methyl alcohol spectrum C, sets up the linear Superposition Formula of spectrum that this base oil is corresponding:
B=k1[(1-m)A]+k2(mC) +E ；
In formula, m is the concentration of volume percent of methyl alcohol in methanol gasoline, and E is spectral measurement error, k1=a, and k2=aK, a is systematic parameter, K is the relative raman scattering intensity of methyl alcohol in methanol gasoline,
Then utilize least square method, can obtain k1, k2, utilize K=k2/k1, can obtain key parameter K in the linear Superposition Formula of spectrum, finally deposit spectrum A and parameter K in spectra database;
(3) select different base oils, repeat step 1 and 2, can set up thus the linear Superposition Formula of spectrum corresponding to different base oils, and the spectra database of spectrum that comprises various base oils and parameter K thereof;
(4) also unknown oil sample to be measured of, methanol content unknown for base oil types, is used Raman spectrometer to measure its spectrum; First to this spectrum carry out smoothly, the pre-service such as noise filtering, fluorescence background removal, and carry out stable hydrocarbon normalization, obtain spectrum D;
(5) from spectra database, select different base oil spectrum A and correlation parameter K thereof, utilize spectrum Superposition Formula, D=k3A+k4KC+E, k3=a (1-m) wherein, k4=am is used least square method to estimate k3, k4; In selection all situations, the coefficient k 3 of estimation error minimum, k4, as final estimation coefficient, utilize k3, k4 to calculate m, obtain thus the methanol content in this methanol gasoline sample.
The invention has the beneficial effects as follows, the content of methanol in methanol gasoline rapid assay methods measuring speed that the present invention is based on Raman spectrum linear superposition theorem is fast, analysis precision is high, and required demarcation sample significantly reduces, for methanol gasoline provides a kind of detection means easily in the extension process of China.
Accompanying drawing explanation
Fig. 1 is certain refinery base oil spectrum;
Fig. 2 refinery M20 spectrum;
Fig. 3 is pure methyl alcohol spectrum;
Certain refinery base oil spectrum after Fig. 4 processes;
Certain refinery M20 spectrum after Fig. 5 processes;
Fig. 6 processes rear pure methyl alcohol spectrum;
Fig. 7 gasoline mediation station base oil spectrum;
Fig. 8 gasoline mediation station M30 spectrum;
Certain gasoline mediation station base oil spectrum after Fig. 9 processes;
Certain gasoline mediation station M30 spectrum after Figure 10 processes;
Figure 11 partial test sample spectra;
Figure 12 processes rear section test sample spectra.
Embodiment
The content of methanol in methanol gasoline rapid assay methods that the present invention is based on Raman spectrum linear superposition theorem, comprises the following steps:
1, methyl alcohol is added in a certain base oil to the methanol gasoline of configuration arbitrary volume content; Use the Raman spectrum of Raman spectrometer Fundamentals of Measurement oil, above-mentioned methanol gasoline and pure methyl alcohol.First to the spectrum obtaining carry out smoothly, the pre-service such as noise filtering, fluorescence background removal.Then base oil and methanol gasoline spectrum are carried out to the normalization of stable hydrocarbon characteristic peak, obtain spectrum A and spectrum B; Pure methyl alcohol spectrum is carried out to maximal value normalization, obtain spectrum C.
2, spectrum B is expressed as to the weighted algebraic sum of base oil spectrum A, pure methyl alcohol spectrum C, sets up the linear Superposition Formula of spectrum that this base oil is corresponding:
B=k1[(1-m)A]+k2(mC) +E ；
In formula, m is the concentration of volume percent of methyl alcohol in methanol gasoline, and E is spectral measurement error, k1=a, and k2=aK, a is systematic parameter, K is the relative raman scattering intensity of methyl alcohol in methanol gasoline,
Then utilize least square method, can obtain k1, k2, utilize K=k2/k1, can obtain key parameter K in the linear Superposition Formula of spectrum, finally deposit spectrum A and parameter K in spectra database.
3, select different base oils, repeat step 1 and 2, can set up thus the linear Superposition Formula of spectrum corresponding to different base oils, and the spectra database of spectrum that comprises various base oils and parameter K thereof.
4, also unknown oil sample to be measured of, methanol content unknown for base oil types, is used Raman spectrometer to measure its spectrum.First to this spectrum carry out smoothly, the pre-service such as noise filtering, fluorescence background removal, and carry out stable hydrocarbon normalization, obtain spectrum D.
5, from spectra database, select different base oil spectrum A and correlation parameter K thereof, utilize spectrum Superposition Formula, D=k3A+k4KC+E, k3=a (1-m) wherein, k4=am is used least square method to estimate k3, k4.In selection all situations, the coefficient k 3 of estimation error minimum, k4, as final estimation coefficient, utilize k3, k4 to calculate m, obtain thus the methanol content in this methanol gasoline sample.
Below in conjunction with accompanying drawing and example, further illustrate the present invention.
Embodiment 1:
Example spectra test condition is: laser instrument centre wavelength is 785nm, pops one's head in as InPhotonics Raman probe, and spectrometer uses the U.S. QE65000 of marine optics company type spectrometer.Set spectrometer 10s integral time, gather and be averaged for 10 times.
1, for certain refinery base oil, the methanol gasoline (being designated as M20) of configuration methanol content 20%.Use Raman spectrometer Fundamentals of Measurement oil, the methanol gasoline of known methyl alcohol volume content and the Raman spectrum of pure methyl alcohol.Respectively as shown in Figure 1, Figure 2, Figure 3 shows.First to the spectrum obtaining carry out smoothly, the pre-service such as noise filtering, fluorescence background removal.Then base oil and methanol gasoline spectrum are carried out to the normalization of stable hydrocarbon characteristic peak, obtain spectrum A and spectrum B, respectively as shown in Figure 4, Figure 5.Pure methyl alcohol spectrum is carried out to maximal value normalization, obtain spectrum C, as shown in Figure 6;
2, spectrum B is expressed as to the weighted algebraic sum of base oil spectrum A, pure methyl alcohol spectrum C, sets up the linear Superposition Formula of spectrum that this base oil is corresponding:
B=k1[(1-m)A]+k2(mC) +E ；
In formula, m is the concentration of volume percent of methyl alcohol in methanol gasoline, and E is spectral measurement error, k1=a, and k2=aK, a is systematic parameter, K is the relative raman scattering intensity of methyl alcohol in methanol gasoline,
Then utilize least square method, can obtain k1, k2, utilize K=k2/k1, can obtain key parameter K=1.333 in the linear Superposition Formula of spectrum, finally deposit spectrum A and parameter K in spectra database.
3, select the base oil at certain gasoline mediation station, configure the methanol gasoline (being designated as M30) of methanol content 30%, repeat the step of (1), (2), wherein corresponding K=1.7932.This gasoline be in harmonious proportion the base oil at station, the Raman spectrum of M30 as shown in Fig. 7, Fig. 8.Base oil after processing, M30 spectrum are as shown in Fig. 9, Figure 10.
Can set up thus the spectrum Superposition Formula that different base oils are corresponding, and a spectra database that comprises various base oils and correlation parameter K.
4, use the methanol gasoline of certain refinery base oil compounding methanol content 40%, 60%, 80%; Use the methanol gasoline of certain gasoline mediation station base oil compounding methanol content 0%, 5%, 10%, 15%, 20%, 30%, 40%, 50%, 60%, 70%.Using above methanol gasoline as also unknown testing sample of, methanol content unknown as base oil types respectively, use Raman spectrometer to measure its spectrum, Figure 11 is the spectrum of sample segment wherein.First to this spectrum carry out smoothly, the pre-service such as noise filtering, fluorescence background removal, and carry out stable hydrocarbon normalization, obtain corresponding spectrum D, Figure 12 is the spectrum of sample segment wherein.
5, from spectra database, select different base oil spectrum A and correlation parameter K thereof, utilize spectrum Superposition Formula, D=k3A+k4KC+E, k3=a (1-m) wherein, k4=am is used least square method to estimate k3, k4.In selection all situations, the coefficient k 3 of estimation error minimum, k4, as final estimation coefficient, utilize k3, k4 to calculate m, obtain thus the methanol content in this methanol gasoline sample.Test result is as shown in Table 1 and Table 2:
Table 1: base oil is taken from the sample measurement result of refinery
| Actual value | 40 | 60 | 80 |
| Calculated value | 39.71 | 57.97 | 78.08 |
| Error | 0.29 | 2.03 | 1.92 |
Note: in table, data are methyl alcohol volume content in methanol gasoline.
Table 2: base oil is got the 1 sample measurement result from gasoline mediation station.
| |
0 | 5 | 10 | 15 | 20 |
| Calculated |
0 | 5.07 | 9.02 | 12.91 | 19.08 |
| Error | 0 | -0.07 | 0.98 | 2.19 | 0.92 |
| Actual value | 30 | 40 | 50 | 60 | |
| Calculated value | 30.00 | 36.94 | 48.28 | 56.68 | |
| |
0 | 3.16 | 1.72 | 3.32 |
Note: in table, data are methyl alcohol volume content in methanol gasoline.
Claims (1)
1. the content of methanol in methanol gasoline rapid assay methods based on Raman spectrum linear superposition theorem, is characterized in that, the method comprises the following steps:
(1) methyl alcohol is added in a certain base oil to the methanol gasoline of configuration arbitrary volume content; Use the Raman spectrum of Raman spectrometer Fundamentals of Measurement oil, above-mentioned methanol gasoline and pure methyl alcohol; First the spectrum obtaining is carried out to pre-service, described pre-service comprises smoothly, noise filtering, fluorescence background are removed; Then base oil and methanol gasoline spectrum are carried out to the normalization of stable hydrocarbon characteristic peak, obtain spectrum A and spectrum B; Pure methyl alcohol spectrum is carried out to maximal value normalization, obtain spectrum C;
(2) spectrum B is expressed as to the weighted algebraic sum of base oil spectrum A, pure methyl alcohol spectrum C, sets up the linear Superposition Formula of spectrum that this base oil is corresponding:
B=k1[(1-m)A]+k2(mC) +E ；
In formula, m is the concentration of volume percent of methyl alcohol in methanol gasoline, and E is spectral measurement error, k1=a, and k2=aK, a is systematic parameter, K is the relative raman scattering intensity of methyl alcohol in methanol gasoline,
Then utilize least square method, can obtain k1, k2, utilize K=k2/k1, can obtain key parameter K in the linear Superposition Formula of spectrum, finally deposit spectrum A and parameter K in spectra database;
(3) select different base oils, repeat step 1 and 2, can set up thus the linear Superposition Formula of spectrum corresponding to different base oils, and the spectra database of spectrum that comprises various base oils and parameter K thereof;
(4) also unknown oil sample to be measured of, methanol content unknown for base oil types, is used Raman spectrometer to measure its spectrum; First this spectrum is carried out to pre-service, described pre-service comprises smoothly, noise filtering, fluorescence background are removed, and carries out stable hydrocarbon normalization, obtains spectrum D;
(5) from spectra database, select different base oil spectrum A and correlation parameter K thereof, utilize spectrum Superposition Formula, D=k3A+k4KC+E, k3=a (1-m) wherein, k4=am is used least square method to estimate k3, k4; In selection all situations, the coefficient k 3 of estimation error minimum, k4, as final estimation coefficient, utilize k3, k4 to calculate m, obtain thus the methanol content in this methanol gasoline sample.
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| CN104267018B (en) * | 2014-10-27 | 2018-01-23 | 武汉四方光电科技有限公司 | The processing method of gas concentration signal in a kind of Raman gas analyzer |
| CN106198482B (en) * | 2015-05-04 | 2019-07-05 | 清华大学 | The method for whether being added with Western medicine in detection health care product based on Raman spectrum |
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