CN102590175A - 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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- CN102590175A CN102590175A CN2012100392723A CN201210039272A CN102590175A CN 102590175 A CN102590175 A CN 102590175A CN 2012100392723 A CN2012100392723 A CN 2012100392723A CN 201210039272 A CN201210039272 A CN 201210039272A CN 102590175 A CN102590175 A CN 102590175A
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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 29
- 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 16
- 238000012360 testing method Methods 0.000 description 4
- 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
- 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
- 239000000203 mixture Substances 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 the 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, the home market increases rapidly the demand of gasoline, has brought immense pressure with environmental protection for the oil supply of China.The unique method that changes oil shortage, severe environmental pollution is exactly the dependence that reduces oil, exploitation green high-efficient cleaning substitute energy.Methanol gasoline is as the substitute of regular gasoline; Be a kind of " replace oil with coal " and the path can directly substitute regular gasoline, alleviate gasoline in short supply in; Good environmental benefit is arranged, the sustainable development of the national ecological economy, the progress of society are all had crucial meaning.
Methanol gasoline is the potpourri of methyl alcohol, gasoline and adjuvant.The methyl alcohol incorporation is generally 5%～30%.To mix 15% serves as at most, claims the M15 methanol gasoline.The calorific value of methyl alcohol is about the half the of gasoline, and under the prerequisite of not changing the motor car engine ratio of compression, methanol content must be fixed within the specific limits.If content is low excessively, then can cause the too low and infringement engine of octane value; Too high levels then can cause fuel value not enough, increases oil consumption, raises the cost.In the end of the year 2009, China has formally issued high-proportion methanol gasoline for vehicle product standard " Vehicular methanol petrol (M85) ", and requiring the content of methyl alcohol in methanol gasoline is about 85%.Shaanxi Province has popularized in an all-round way and has used the M15 methanol gasoline.In the provincial standard of national standard (M85) and each province; Like Hebei province's provincial standard " M30 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 the 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 complex equipments is not suitable for on-the-spot the detection.Simultaneously, vapor-phase chromatography also need be carried out interior mark.For this reason, need the measuring method quick and precisely of methanol content in the exploitation blend gasoline, it all has great important for the quality control of methanol gasoline with check.
Present method for quick mainly adopts near infrared spectrum and Raman spectrum analysis method.These class methods at first utilize near infrared or Raman spectrometer to obtain the spectroscopic data of oil product to be measured; Then with database in the spectrum of a large amount of training sample (oil sample that refers to known methanol content and corresponding spectrum) compare, and then estimate methanol content in the methanol gasoline.These class methods, measuring speed is fast, easy to use.But the subject matter that these two class methods exist is that needs are collected a large amount of different base oils, the training sample of different methanol contents, could guarantee the accuracy of detection to oil product methanol content to be measured like this.Simultaneously, because the molecule absorption characteristic of near infrared spectrum, measurement result is subject to other alcohols and disturbs.
Summary of the invention
The objective of the invention is to the deficiency to prior art, a kind of methanol gasoline methanol content rapid assay methods based on the Raman spectrum stack is provided, this method is easy, effective.
The objective of the invention is to realize through following technical scheme: a kind of methanol gasoline methanol content rapid assay methods based on the Raman spectrum linear superposition theorem, this method may further comprise the steps:
(1) methyl alcohol is added in a certain base oil methanol gasoline of configuration arbitrary volume content; Base oil uses the Raman spectrum of Raman spectrometer Fundamentals of Measurement oil, above-mentioned methanol gasoline and pure methyl alcohol; At first to the spectrum that obtains carry out smoothly, pre-service such as noise filtering, fluorescence background removal; Then base oil and methanol gasoline spectrum are carried out the normalization of stable hydrocarbon characteristic peak, obtain spectrum A and spectrum B; Pure methyl alcohol spectrum is carried out maximal value normalization, obtain spectrum C;
Said base oil refers to the regular price gasoline that does not contain methyl alcohol that mixed by catalytic gasoline, reformed gasoline and MTBE.
(2) spectrum B is expressed as the weighted algebraic sum of base oil spectrum A, pure methyl alcohol spectrum C, sets up the linear Superposition Formula of the corresponding spectrum of this base oil:
B=k1[(1-m)A]+k2(mC)?+E ；
In the formula, m is the concentration of volume percent of methyl alcohol in the methanol gasoline, and E is the spectral measurement error, k1=a, and k2=aK, a are systematic parameter, K is the relative raman scattering intensity of methyl alcohol in methanol gasoline,
Utilize least square method then, can get k1, k2, utilize K=k2/k1, can get key parameter K in the linear Superposition Formula of spectrum, deposit spectrum A and parameter K in spectra database at last;
(3) select different base oils, repeat step 1 and 2, can set up the linear Superposition Formula of the corresponding spectrum of different base oils thus, and one comprises the spectrum of various base oils and the spectra database of parameter K thereof;
(4), methanol content also unknown to be measured oil sample unknown for base oil types uses Raman spectrometer to measure its spectrum; At first to this spectrum carry out smoothly, 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 the spectrum Superposition Formula, D=k3A+k4KC+E, k3=a (1-m) wherein, k4=am uses least square method to estimate k3, k4; The coefficient k 3 of estimation error minimum, k4 utilize k3, k4 to calculate m as final estimation coefficient in the selection all situations, obtain the methanol content in this methanol gasoline sample thus.
The invention has the beneficial effects as follows; The methanol gasoline methanol content rapid assay methods measuring speed that the present invention is based on the Raman spectrum linear superposition theorem is fast; Analysis precision is high, and required demarcation sample reduces significantly, for methanol gasoline provides a kind of detection means easily in the popularization process of China.
Description of drawings
Fig. 1 is certain refinery base oil spectrum;
Fig. 2 refinery M20 spectrum;
Fig. 3 is pure methyl alcohol spectrum;
Fig. 4 handles certain refinery base oil spectrum of back;
Fig. 5 handles certain refinery M20 spectrum of back;
Fig. 6 handles the pure methyl alcohol spectrum in back;
Fig. 7 gasoline mediation station base oil spectrum;
Fig. 8 gasoline mediation station M30 spectrum;
Fig. 9 handles certain gasoline mediation station base oil spectrum of back;
Figure 10 handles certain gasoline mediation station M30 spectrum of back;
Figure 11 partial test sample spectra;
Figure 12 handles rear section specimen spectrum.
Embodiment
The present invention is based on the methanol gasoline methanol content rapid assay methods of Raman spectrum linear superposition theorem, may further comprise the steps:
1, methyl alcohol is added in a certain base oil 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.At first to the spectrum that obtains carry out smoothly, pre-service such as noise filtering, fluorescence background removal.Then base oil and methanol gasoline spectrum are carried out the normalization of stable hydrocarbon characteristic peak, obtain spectrum A and spectrum B; Pure methyl alcohol spectrum is carried out maximal value normalization, obtain spectrum C.
2, spectrum B is expressed as the weighted algebraic sum of base oil spectrum A, pure methyl alcohol spectrum C, sets up the linear Superposition Formula of the corresponding spectrum of this base oil:
B=k1[(1-m)A]+k2(mC)?+E ；
In the formula, m is the concentration of volume percent of methyl alcohol in the methanol gasoline, and E is the spectral measurement error, k1=a, and k2=aK, a are systematic parameter, K is the relative raman scattering intensity of methyl alcohol in methanol gasoline,
Utilize least square method then, can get k1, k2, utilize K=k2/k1, can get key parameter K in the linear Superposition Formula of spectrum, deposit spectrum A and parameter K in spectra database at last.
3, select different base oils, repeat step 1 and 2, can set up the linear Superposition Formula of the corresponding spectrum of different base oils thus, and one comprises the spectrum of various base oils and the spectra database of parameter K thereof.
4,, methanol content also unknown to be measured oil sample unknown for base oil types uses Raman spectrometer to measure its spectrum.At first to this spectrum carry out smoothly, 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 the spectrum Superposition Formula, D=k3A+k4KC+E, k3=a (1-m) wherein, k4=am uses least square method to estimate k3, k4.The coefficient k 3 of estimation error minimum, k4 utilize k3, k4 to calculate m as final estimation coefficient in the selection all situations, obtain the methanol content in this methanol gasoline sample thus.
Below in conjunction with accompanying drawing and instance, further specify the present invention.
Embodiment 1:
The example spectra test condition is: laser instrument centre wavelength is 785nm, pops one's head in to be InPhotonics Raman probe, and spectrometer uses the U.S. QE65000 of marine optics company type spectrometer.Set spectrometer 10s integral time, gather and make even for 10 times all.
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 like Fig. 1, Fig. 2, shown in Figure 3.At first to the spectrum that obtains carry out smoothly, pre-service such as noise filtering, fluorescence background removal.Then base oil and methanol gasoline spectrum are carried out the normalization of stable hydrocarbon characteristic peak, obtain spectrum A and spectrum B, respectively like Fig. 4, shown in Figure 5.Pure methyl alcohol spectrum is carried out maximal value normalization, obtain spectrum C, as shown in Figure 6;
2, spectrum B is expressed as the weighted algebraic sum of base oil spectrum A, pure methyl alcohol spectrum C, sets up the linear Superposition Formula of the corresponding spectrum of this base oil:
B=k1[(1-m)A]+k2(mC)?+E ；
In the formula, m is the concentration of volume percent of methyl alcohol in the methanol gasoline, and E is the spectral measurement error, k1=a, and k2=aK, a are systematic parameter, K is the relative raman scattering intensity of methyl alcohol in methanol gasoline,
Utilize least square method then, can get k1, k2, utilize K=k2/k1, can get key parameter K=1.333 in the linear Superposition Formula of spectrum, deposit spectrum A and parameter K in spectra database at last.
3, select the base oil at certain gasoline mediation station, dispose the methanol gasoline (being designated as M30) of methanol content 30%, repeat the step of (1), (2), wherein corresponding K=1.7932.Shown in the base oil at this gasoline mediation station, the Raman spectrum of M30 such as Fig. 7, Fig. 8.Shown in base oil after the processing, M30 spectrum such as Fig. 9, Figure 10.
Can set up the corresponding spectrum Superposition Formula of different base oils thus, 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%.As, methanol content also unknown testing sample unknown as base oil types respectively, use Raman spectrometer to measure its spectrum above methanol gasoline, Figure 11 is the spectrum of sample segment wherein.At first to this spectrum carry out smoothly, 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 the spectrum Superposition Formula, D=k3A+k4KC+E, k3=a (1-m) wherein, k4=am uses least square method to estimate k3, k4.The coefficient k 3 of estimation error minimum, k4 utilize k3, k4 to calculate m as final estimation coefficient in the selection all situations, obtain the methanol content in this methanol gasoline sample thus.Test result is 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 |
Annotate: data are methyl alcohol volume content in the methanol gasoline in the table.
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 | ? |
Annotate: data are methyl alcohol volume content in the methanol gasoline in the table.
Claims (1)
1. methanol gasoline methanol content rapid assay methods based on the Raman spectrum linear superposition theorem is characterized in that this method may further comprise the steps:
(1) methyl alcohol is added in a certain base oil 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; At first to the spectrum that obtains carry out smoothly, pre-service such as noise filtering, fluorescence background removal; Then base oil and methanol gasoline spectrum are carried out the normalization of stable hydrocarbon characteristic peak, obtain spectrum A and spectrum B; Pure methyl alcohol spectrum is carried out maximal value normalization, obtain spectrum C;
(2) spectrum B is expressed as the weighted algebraic sum of base oil spectrum A, pure methyl alcohol spectrum C, sets up the linear Superposition Formula of the corresponding spectrum of this base oil:
B=k1[(1-m)A]+k2(mC)?+E ；
In the formula, m is the concentration of volume percent of methyl alcohol in the methanol gasoline, and E is the spectral measurement error, k1=a, and k2=aK, a are systematic parameter, K is the relative raman scattering intensity of methyl alcohol in methanol gasoline,
Utilize least square method then, can get k1, k2, utilize K=k2/k1, can get key parameter K in the linear Superposition Formula of spectrum, deposit spectrum A and parameter K in spectra database at last;
(3) select different base oils, repeat step 1 and 2, can set up the linear Superposition Formula of the corresponding spectrum of different base oils thus, and one comprises the spectrum of various base oils and the spectra database of parameter K thereof;
(4), methanol content also unknown to be measured oil sample unknown for base oil types uses Raman spectrometer to measure its spectrum; At first to this spectrum carry out smoothly, 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 the spectrum Superposition Formula, D=k3A+k4KC+E, k3=a (1-m) wherein, k4=am uses least square method to estimate k3, k4; The coefficient k 3 of estimation error minimum, k4 utilize k3, k4 to calculate m as final estimation coefficient in the selection all situations, obtain the methanol content in this methanol gasoline sample thus.
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