CN102252994A - Method for rapid detection of quality index of motor fuel - Google Patents
Method for rapid detection of quality index of motor fuel Download PDFInfo
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- CN102252994A CN102252994A CN2011101397378A CN201110139737A CN102252994A CN 102252994 A CN102252994 A CN 102252994A CN 2011101397378 A CN2011101397378 A CN 2011101397378A CN 201110139737 A CN201110139737 A CN 201110139737A CN 102252994 A CN102252994 A CN 102252994A
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Abstract
The invention discloses a method for rapid detection of quality index of motor fuel. The method comprises the following steps: collecting a certain amount of fuel samples as a training set; detecting mid-infrared absorption spectrum and quality index of the samples in the training set; establishing a linear equation between each quality index and absorbance by employing the technology of stepwise linear regression; for detection of quality index of an unknown fuel sample, detecting mid-infrared spectrum of the fuel sample at first, and then using a computer to automatically calculate each quality index of the fuel sample according to the established linear equation. According to the method provided in the invention, 15 quality indexes such as RON and MON of gasoline, 9 quality indexes such as cetane numbers and condensation points of diesel oil and 10 quality indexes such as freezing points and flash points of jet fuel can be rapidly detected through infrared spectrum. The method can be used outdoors and for on-site detection of fuel quality, ensuring safe and normal utilization of fuels; the method can also be used by a quality supervision department for on-site sampling observation of fuel quality, thereby improving supervision capacity of fuel quality and avoiding loss caused by unqualified fuels.
Description
Technical field
The present invention relates to a kind of method of fast measuring motor fuel quality index, specifically, relate to a kind of employing mid-infrared light spectral technology, in conjunction with each quality index of linear regression technique fast measuring diesel oil, gasoline or jet fuel progressively.
Background technology
Engine purposes difference causes its motor fuel of a great variety.Such as, diesel motor uses diesel fuel, petrol engine to use petrol power fuel, and aircraft engine uses jet fuel.Motor fuel quality direct relation engine operating condition.If the defective fuel of service property (quality), engine operation is unusual, even causes engine failure, therefore needs strict monitoring fuel mass.At present, following pattern is mainly adopted in the detection of motor fuel quality index: gather fuel sample from the refuelling station, be sent to quality testing department then and adopt standard method to measure each quality index, and then the result is fed back relevant law enforcement agency.This pattern exists sense cycle long, and the cost height is unfavorable for fuel mass is monitored.At present, still exist fuel mass to adulterate, to pretend to be excellent phenomenon.For this reason, press for fuel mass express-analysis technology, can the spot check fuel mass, improve the fuel mass monitoring ability.
Because near-infrared spectrum technique has quick, many property analysis and is fit to online nondestructive analysis characteristics, more and more is applied to petrochemical industry at present, has irreplaceable effect in fuel quality detection with aspect cracking down on counterfeit goods.Because near infrared spectrum belongs to molecular vibration spectrum, wavelength coverage is 700-2500nm, is molecule frequency multiplication and combination absorption frequently, and peak shape is a broad peak; A little less than the characteristic, only X-H group (X is C, O etc.) there is absorption; A little less than the signal, antijamming capability is strong.Have These characteristics just because of near infrared spectrum, thus must be by the Chemical Measurement and the computer technology in modern times, and near-infrared spectrum technique could well be used.Along with the fast development and the near infrared spectroscopy instrument adaptive capacity to environment of Chemical Measurement and computing machine are strong, low price has promoted the near-infrared spectrum technique fast development, has now become hydro carbons (C-H) fuel mass fast detecting and online process monitoring technique.
Middle infrared spectrum also belongs to molecular vibration spectrum, is the fundamental frequency absorption of molecular vibration, and wave-number range is 400-4000cm
-1(wavelength is 2.5 microns～25 microns).Define from it, middle infrared spectrum and near infrared spectrum are wavelength coverage.From the essence of its generation, can well find that the two spectrum shape characteristic has obvious difference, thereby the technology and the application that cause finally being adopted there is very big difference.Compare with near infrared spectrum, the middle infrared spectrum peak shape is a spike, and characteristic is strong, and all there is tangible absorption in all kinds of functional groups (comprising the non-X-H of X-H and other functional group); Signal is strong, and microcomponent or adjuvant all have absorption, identifies so the mid-infrared light spectral technology is mainly used in the unknown materials functional group in analytical chemistry field, belongs to one of " four compose greatly ", is used for the unknown materials chemical constitution and identifies.Because a little less than the adaptive capacity to environment of middle infrared spectrum instrument, the instrument costliness is so this technology also is difficult to the quality testing and the kind identification of petrochemical industry at present.
Analyze theoretically, middle infrared spectrum not only has absorption to the main hydrocarbon composition of fuel, and a small amount of non-hydrocarbons component and trace mineral supplement component all there is response, if combine so the mid-infrared light spectral technology learns a skill with stoichiometry, will realize the irrealizable function of near-infrared spectrum technique, measure such as manganese type additive level.
Summary of the invention
The object of the invention provides a kind of method of fast measuring motor fuel quality index, specifically, relates to a kind of employing mid-infrared light spectral technology, in conjunction with linear regression technique progressively, and the quality index of fast measuring diesel oil, gasoline and jet fuel.
Concrete steps are as follows:
The first step, collection has the motor fuel sample of some as training set;
Second step, the mid infrared absorption spectrum of mensuration training set sample;
In the 3rd step, adopt standard method to measure the quality index of training set sample;
In the 4th step, adopt linear regression technique progressively to set up the equation of linear regression of each quality index and middle infrared spectrum absorbance;
In the 5th step, for the mensuration of unknown fuel sample quality index, the user at first measures its infrared spectrum, is utilized the equation of spectrum and foundation then by computing machine, measures each quality index.
The described second step infrared spectrum measurement mode is a transmission mode.
The progressively equation of linear regression in described the 4th step is:
Wherein y is a quality index, k
iRegression coefficient for the i wavelength; A
iBe the absorbance of wavelength i, b is a coefficient, and m is the characteristic variable number.
It is as follows that described multiple linear regression equations is set up process:
(1) adopts the F check, estimate the conspicuousness of each wavelength quality index y.Select one to the most significant absorbance A of quality index (y)
1, set up simple regression equation: y=k
1A
1+ b
1, the computing formula of F is:
Wherein, Q
iBe the variance contribution of wavelength i to y.Q is the residual sum of square of all variablees, and n is the sample number;
(2) in remaining wavelength, select one then again to the significant absorbance A of y effect
2, by A
1And A
2Set up binary regression equation: y=k
1A
1+ k
2A
2+ b;
Whether (3) remarkable by the variable of F test evaluation introducing, i.e. whether check can improve the accuracy of model; If not remarkable, pick out this variable immediately; If still remarkable, then need repeat to introduce the 3rd variable, and then check the conspicuousness of this variable, if continue significantly then to repeat this step, till not having remarkable variable to introduce;
(4) utilize the absorbance of selected characteristic wavelength at last, set up relation with quality index:
Wherein y is a quality index, k
iRegression coefficient for the i variable; A
iBe the absorbance of wavelength i, b is a coefficient, and m is the characteristic variable number.
The quality index in described the 4th step comprises: the RON of gasoline, MON, anti-knock index, 10% evaporating temperature, 50% evaporating temperature, 90% evaporating temperature, the end point of distillation, saturated vapor pressure, benzene content, arene content, olefin(e) centent, saturated hydrocarbon content, oxygen content, manganese content and sulfur content; The cetane rating of diesel oil, condensation point, flash-point, density, kinematic viscosity, 10% recovered (distilled) temperature, 50% recovered (distilled) temperature, 90% recovered (distilled) temperature and 95% recovered (distilled) temperature; The freezing point of jet fuel, flash-point, density, initial boiling point, 10% recovered (distilled) temperature, 20% recovered (distilled) temperature, 50% recovered (distilled) temperature, 90% recovered (distilled) temperature, the end point of distillation and kinematic viscosity.
This patent has following benefit: the present invention utilizes various chemical compositions of fuel and adjuvant to have the characteristic absorption peak characteristics at middle infrared spectrum, adopts the progressively absorbance of linear regression technique screening characteristic wavelength, sets up the equation of linear regression of fuel mass index.When detecting the fuel mass index, only need in several minutes, to measure its middle infrared spectrum, utilize the equation of linear regression of being set up then, can in several minutes, once measure tens of kinds of quality index of fuel simultaneously, tens of kinds of quality index of gasoline, diesel oil and jet fuel be can realize, thereby fuel mass index detection speed and ability improved greatly.Can be used for the field on the one hand, the fast detecting fuel mass is guaranteed with oil quality and safety; Can be used for quality supervised department on the other hand, on-the-spot quick check fuel, the monitoring ability that improves the quality is avoided the loss of using defective fuel to bring.
Description of drawings
Fig. 1 gasoline sample mid infrared absorption spectrum;
Fig. 2 diesel samples mid infrared absorption spectrum figure;
No. 3 jet fuel samples of Fig. 3 mid infrared absorption spectrum figure.
Embodiment
The step of assay method of the present invention is as follows:
The first step, collection has the motor fuel sample of some as training set;
Second step, the mid infrared absorption spectrum of mensuration training set sample;
In the 3rd step, adopt standard method to measure the quality index of training set sample;
In the 4th step, adopt linear regression technique progressively to set up the equation of linear regression of each quality index and middle infrared spectrum absorbance;
The 5th step, for the mensuration of unknown fuel sample quality index, at first measure its infrared spectrum, utilize the equation of linear regression of spectrum and the foundation of the 4th step then by computing machine, measure each quality index.
The described second step infrared spectrum measurement mode is a transmission mode.
The progressively equation of linear regression in described the 4th step is:
Wherein y is a quality index, k
iRegression coefficient for the i wavelength; A
iBe the absorbance of wavelength i, b is a coefficient, and m is the characteristic variable number.
It is as follows that described multiple linear regression equations is set up process:
(1) adopts the F check, estimate the conspicuousness of each wavelength quality index y.Select one to the most significant absorbance A of quality index (y)
1, set up simple regression equation: y=k
1A
1+ b
1, the computing formula of F is:
Wherein, Q
iBe the variance contribution of wavelength i to y.Q is the residual sum of square of all variablees, and n is the sample number;
(2) in remaining wavelength, select one then again to the significant absorbance A of y effect
2, by A
1And A
2Set up binary regression equation: y=k
1A
1+ k
2A
2+ b;
Whether (3) remarkable by the variable of F test evaluation introducing, i.e. whether check can improve the accuracy of model; If not remarkable, pick out this variable immediately; If still remarkable, then need repeat to introduce the 3rd variable, and then check the conspicuousness of this variable, if continue significantly then to repeat this step, till not having remarkable variable to introduce;
(4) utilize the absorbance of selected characteristic wavelength at last, set up relation with quality index:
Wherein y is a quality index, k
iRegression coefficient for the i variable; A
iBe the absorbance of wavelength i, b is a coefficient, and m is the characteristic variable number.
The quality index in described the 4th step comprises: the RON of gasoline, MON, anti-knock index, 10% evaporating temperature, 50% evaporating temperature, 90% evaporating temperature, the end point of distillation, saturated vapor pressure, benzene content, arene content, olefin(e) centent, saturated hydrocarbon content, oxygen content, manganese content and sulfur content; The cetane rating of diesel oil, condensation point, flash-point, density, kinematic viscosity, 10% recovered (distilled) temperature, 50% recovered (distilled) temperature, 90% recovered (distilled) temperature and 95% recovered (distilled) temperature; The freezing point of jet fuel, flash-point, density, initial boiling point, 10% recovered (distilled) temperature, 20% recovered (distilled) temperature, 50% recovered (distilled) temperature, 90% recovered (distilled) temperature, the end point of distillation and kinematic viscosity.
Below by concrete example in detail the present invention, but the present invention is not limited to this.
Example 1: the fast measuring of quality of gasoline index
1) collects the training set sample
Collect 202 samples of gasoline from each refinery of China, gasoline comprises No. 90 motor petrol, No. 93 motor petrol, No. 97 motor petrol, No. 90 ethanol petrols, No. 93 ethanol petrols and No. 97 ethanol petrols, has covered China's gasoline oil sample substantially.
2) measure training set sample infrared spectrum
Adopt TENSOR 27 mid-infrared light spectrometers to measure training set sample mid infrared absorption spectrum, spectral range: 600cm
-1～4000cm
-1The transmission sample pond, the 0.1mm light path, spectrogram is seen Fig. 1.
3) adopt standard method to measure each quality index of gasoline.Table 1 has been listed unit, standard method, the repeatability requirement of each quality index of gasoline, and each quality index measured value scope of training set sample sees Table 2.
Table 1
Table 2
4) adopt progressively that linear regression method comes the preferred feature wavelength, and set up quality of gasoline index (y) and this characteristic wavelength absorbance (A
i) relation: y=k
iA
i+ b.Table 3 has been listed characteristic wavelength i, the k of part quality index such as arene content, olefin(e) centent and saturated hydrocarbon content
iAnd b.
Table 3
5) estimate the multiple linear regression equations precision of analysis
The gasoline sample of selecting 20 known quality indexs is measured its middle infrared spectrum as unknown sample, utilizes 4 then) regression coefficient calculate each quality index, and with actual value relatively, the results are shown in Table 4.This method error at measurment is lower than or approaches the repeatability requirement of table 1, can adopt method of the present invention to measure RON, MON, anti-knock index, 10% evaporating temperature, 50% evaporating temperature, 90% evaporating temperature, the end point of distillation, saturated vapor pressure, sulfur content, benzene content, arene content, olefin(e) centent, saturated hydrocarbon content, oxygen content and the manganese content of gasoline, the monitoring quality of gasoline.
Table 4
Example 2: the fast detecting of diesel quality index
1) collects the training set sample
Collect 262 samples of diesel oil from each refinery of China, diesel oil comprises No. 0 light diesel fuel ,-No. 10 light diesel fuels and-No. 35 light diesel fuels, has covered China's diesel oil oil sample substantially.
2) measure training set sample infrared spectrum
Adopt TENSOR 27 mid-infrared light spectrometers to measure training set sample mid infrared absorption spectrum, spectral range: 600cm
-1～4000cm
-1The transmission sample pond, the 0.1mm light path, spectrogram is seen Fig. 2.
3) adopt standard method to measure each quality index of diesel oil.Table 5 has been listed unit, standard method, the repeatability requirement of each quality index of diesel oil, and each quality index measured value scope of training set sample sees Table 6.
Table 5
| Character | Unit | Standard method | The repeatability requirement |
| Cetane rating | GB/T386 | 3.3 | |
| Condensation point | ℃ | GB/ |
4 |
| Flash-point | ℃ | GB/T?261 | 4 |
| Density | g/cm 3 | GB/T1884 | 0.0005 |
| Kinematic viscosity | mm 2/s | GB/ |
3％ |
| 10% recovered (distilled) temperature | ℃ | GB/T6536 | 7 |
| 50% recovered (distilled) temperature | ℃ | GB/T6536 | 8.5 |
| 90% recovered (distilled) temperature | ℃ | GB/T6536 | 9.5 |
| 95% recovered (distilled) temperature | ℃ | GB/T6536 | 9.5 |
Table 6
| Character | Unit | Scope |
| Cetane rating | 37.9～73.5 | |
| Condensation point | ℃ | -60～0 |
| Flash-point | ℃ | 43～98 |
| Density | Kg/m3 | 0.8739～0.7887 |
| Kinematic viscosity | mm 2/s | 1.884～6.11 |
| 10% recovered (distilled) temperature | ℃ | 176～247 |
| 50% recovered (distilled) temperature | ℃ | 203～287 |
| 90% recovered (distilled) temperature | ℃ | 247～354 |
| 95% recovered (distilled) temperature | ℃ | 271～369 |
4) adopt progressively that linear regression method comes the preferred feature wavelength, and set up diesel quality index (y) and this characteristic wavelength absorbance (A
i) relation: y=k
iA
i+ b.Table 7 has been listed characteristic wavelength i, the k of part quality index such as condensation point, flash-point and kinematic viscosity
iSee Table 7 with b.
Table 7
5) estimate the multiple linear regression equations precision of analysis
The diesel samples of selecting 20 known quality indexs is measured its middle infrared spectrum as unknown sample, utilizes 4 then) regression coefficient calculate each quality index, and with actual value relatively, the results are shown in Table 8.This method error at measurment is lower than or approaches the repeatability requirement of table 5, shows cetane rating, condensation point, flash-point, density, kinematic viscosity, 10% recovered (distilled) temperature, 50% recovered (distilled) temperature, 90% recovered (distilled) temperature and 95% recovered (distilled) temperature that can adopt method of the present invention to measure diesel oil.
Table 8
No. 33 jet fuel quality testings of example
1) collects the training set sample
Collect 105 samples of No. 3 jet fuels from each refinery of China, covered No. 3 jet fuel oil samples of China substantially.
2) measure training set sample infrared spectrum
Adopt TENSOR 27 mid-infrared light spectrometers to measure training set sample mid infrared absorption spectrum, spectral range: 600cm
-1～4000cm
-1The transmission sample pond, the 0.1mm light path, spectrogram is seen Fig. 3.
3) adopt standard method to measure each quality index of No. 3 jet fuels.Table 9 has been listed unit, standard method, the repeatability requirement of No. 3 each quality index of jet fuel, and each quality index measured value scope of training set sample sees Table 10.
Table 9
| Character | Unit | Standard method | The repeatability requirement |
| Freezing point | ℃ | GB/T386 | 2.6 |
| Flash-point | ℃ | GB/ |
4 |
| Density | g/cm 3 | GB/T1884 | 0.0005 |
| Initial boiling point | ℃ | GB/T6536 | 8.5 |
| 10% recovered (distilled) temperature | ℃ | GB/T6536 | 7 |
| 20% recovered (distilled) temperature | ℃ | GB/T6536 | 8.5 |
| 50% recovered (distilled) temperature | ℃ | GB/T6536 | 8.5 |
| 90% recovered (distilled) temperature | ℃ | GB/T6536 | 9.5 |
| The end point of distillation | ℃ | GB/T6536 | 9.5 |
| Kinematic viscosity | mm 2/s | GB/ |
3％ |
Table 10
| Character | Unit | Scope |
| Freezing point | ℃ | -82～-48 |
| Flash-point | ℃ | 41～56 |
| Density | g/cm 3 | 0.7782～0.8045 |
| Initial boiling point | ℃ | 145～168 |
| 10% recovered (distilled) temperature | ℃ | 163.5～177.5 |
| 20% recovered (distilled) temperature | ℃ | 167.5～182.5 |
| 50% recovered (distilled) temperature | ℃ | 175.5～192.5 |
| 90% recovered (distilled) temperature | ℃ | 185.5～225 |
| The end point of distillation | ℃ | 204.5～259 |
| Kinematic viscosity | mm 2/s | 1.38～1.768 |
4) adopt progressively that linear regression method comes the preferred feature wavelength, and set up quality of gasoline index (y) and this characteristic wavelength absorbance (A
i) relation: y=k
iA
i+ b, characteristic wavelength i, the k of part quality index such as freezing point, flash-point, density and kinematic viscosity
iSee Table 11 with b.
Table 11
5) estimate the multiple linear regression equations precision of analysis
No. 3 jet fuels selecting 20 known quality indexs are measured its middle infrared spectrum as unknown sample, utilize 4 then) regression coefficient calculate each quality index, and with actual value relatively, the results are shown in Table 12.This method error at measurment is lower than or approaches the repeatability requirement of table 9, shows freezing point, flash-point, density, initial boiling point, 10% recovered (distilled) temperature, 20% recovered (distilled) temperature, 50% recovered (distilled) temperature, 90% recovered (distilled) temperature, the end point of distillation and the kinematic viscosity that can adopt method of the present invention to measure jet fuel.
Table 12
Claims (7)
1. the method for a fast measuring motor fuel quality index comprises the steps:
The first step, collection has the motor fuel sample of some as training set;
Second step, the mid infrared absorption spectrum of mensuration training set sample;
In the 3rd step, adopt standard method to measure the quality index of training set sample;
In the 4th step, adopt linear regression technique progressively to set up the equation of linear regression of each quality index and middle infrared spectrum absorbance;
The 5th step, for the mensuration of unknown fuel sample quality index, at first measure its infrared spectrum, utilize the equation of linear regression of spectrum and the foundation of the 4th step then by computing machine, measure each quality index.
2. in accordance with the method for claim 1, it is characterized in that the described second step infrared absorption spectrometry mode is a transmission mode.
3. in accordance with the method for claim 1, it is characterized in that described the 4th step equation of linear regression is:
Wherein y is a quality index, k
iRegression coefficient for the i wavelength; A
iBe the absorbance of wavelength i, b is a coefficient, and m is the characteristic variable number.
4. it is as follows in accordance with the method for claim 3, to it is characterized in that described multiple linear equation is set up process:
(1) adopts the F check, estimate the conspicuousness of each wavelength, select one the most significant absorbance A of y to quality index (y)
1, set up simple regression equation: y=k
1A
1+ b
1, the F computing formula is:
Wherein, Q
iBe the variance contribution of wavelength i to y, Q is the residual sum of square of all variablees, and n is the sample number;
(2) in remaining wavelength, select one then again to the significant absorbance A of y effect
2, by A
1And A
2Set up binary linear regression equation: y=k
1A
1+ k
2A
2+ b;
Whether (3) remarkable by the variable of F test evaluation introducing, i.e. whether check can improve the accuracy of model; If not remarkable, pick out this variable immediately; If still remarkable, then need repeat to introduce the 3rd variable, and then check the conspicuousness of this variable, if continue significantly then to repeat this step, till not having remarkable variable to introduce;
(4) utilize the absorbance of selected characteristic wavelength at last, set up relation with quality index:
Wherein y is a quality index, k
iRegression coefficient for the i wavelength; A
iBe the absorbance of wavelength i, b is a coefficient, and m is the characteristic variable number.
5. in accordance with the method for claim 1, it is characterized in that described the 4th step quality index comprises: the RON of gasoline, MON, anti-knock index, 10% evaporating temperature, 50% evaporating temperature, 90% evaporating temperature, the end point of distillation, saturated vapor pressure, benzene content, arene content, olefin(e) centent, saturated hydrocarbon content, oxygen content, manganese content and sulfur content;
6. in accordance with the method for claim 1, it is characterized in that described the 4th step quality index comprises: the cetane rating of diesel oil, condensation point, flash-point, density, kinematic viscosity, 10% recovered (distilled) temperature, 50% recovered (distilled) temperature, 90% recovered (distilled) temperature and 95% recovered (distilled) temperature;
7. in accordance with the method for claim 1, it is characterized in that described the 4th step quality index comprises: the freezing point of jet fuel, flash-point, density, initial boiling point, 10% recovered (distilled) temperature, 20% recovered (distilled) temperature, 50% recovered (distilled) temperature, 90% recovered (distilled) temperature, the end point of distillation and kinematic viscosity.
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| AT16342U1 (en) * | 2018-02-20 | 2019-07-15 | Evk Di Kerschhaggl Gmbh | Method for determining the quality of substitute fuels |
| CN112676193A (en) * | 2019-10-18 | 2021-04-20 | 李和伟 | Application of spectrum detection in detecting quality of modified membrane cloth, detection method and detection equipment |
| CN114354534A (en) * | 2021-12-30 | 2022-04-15 | 中国航空油料有限责任公司 | Method for establishing aviation kerosene property prediction model by utilizing binary linear classifier |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104093963A (en) * | 2012-01-04 | 2014-10-08 | 罗地亚运作公司 | Method for diagnosing the malfunctioning of a device for adding an additive into a fuel for a vehicle, and system for implementing said method |
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| CN112676193A (en) * | 2019-10-18 | 2021-04-20 | 李和伟 | Application of spectrum detection in detecting quality of modified membrane cloth, detection method and detection equipment |
| CN114354534A (en) * | 2021-12-30 | 2022-04-15 | 中国航空油料有限责任公司 | Method for establishing aviation kerosene property prediction model by utilizing binary linear classifier |
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