CN101988895B - Method for predicting single-type crude oil content in mixed crude oil by near infrared spectrum - Google Patents
Method for predicting single-type crude oil content in mixed crude oil by near infrared spectrum Download PDFInfo
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Abstract
The invention provides a method for predicting the single-type crude oil content in mixed crude oil by near infrared spectrum, which comprises the following steps of: 1. respectively detecting the near infrared spectrum of single-type crude oil contained in the mixed crude oil, and adding the light absorbency vectors of the near infrared spectrum of the single-type crude oil according to the simulated content proportion of the single-type raw oil for forming the simulated spectrum for simulating the mixed crude oil; 2. carrying out second-order differential treatment on each simulated spectrum for simulating the crude oil, taking the light absorbency at an interval between 3800 and 7000 cm<-1> to be related to the simulated content of the single-type crude oil in the simulated mixed crude rod, and building a correcting module for predicting the single-type crude oil by the partial least square method; and 3. testing the correcting model of the near infrared spectrum of the mixed crude oil, carrying out second-order differential treatment, introducing the light absorbency at the interval between 3800 and 7000 cm<-1> into the correcting model for predicting the single-type crude oil, and obtaining the content of the single-type crude oil in the mixed crude oil. The method can be used for quick detecting the content of each single-type crude oil in the mixed crude oil through the near infrared spectrum of the single-type crude oil, and can easily realize the automatic generation of the near infrared spectrum correcting model.
Description
Technical field
The present invention is a kind of by single method of planting crude content in the spectroscopic data prediction hybrid crude oil, specifically, is a kind of by the method for crude content of the same race not in the near infrared spectrum prediction hybrid crude oil.
Background technology
Along with market to the continuous increase of oil product demand and the deficiency of domestic crude resources, refinery is being processed increasing imported crude oil and Crude oil from CNOOC, the oil variety of processing is on the increase.Because oil variety is many, batch is few, crude oil is mixed the situation ubiquity of refining.Crude oil rationally mix refining, not only can improve extracting rate, and, in the time of a kind of character incompatibility equipment of crude oil, can improve through the refining of mixing of crude oil, to improve treatment capacity and to improve product quality.Therefore, before advancing distilling apparatus, need measure the ratio of blending crude oil timely and accurately.In addition, in the crude oil pipeline course of conveying, the situation that several kinds of crude oil mix can appear also, therefore, and carrying terminal also to need the blending ratio of mensuration crude oil in time, so that obtain the character situation of the crude oil that receives.
At present, still do not have a kind of method of simple and feasible to come to measure rapidly and accurately the mixing proportion of multiple crude oil, can extrapolate single crude oil ratio of planting of commingled crude through a plurality of physical parameters such as density, sulfur content and viscosity etc.This method not only need be measured a plurality of physical parameters, and runs into physical parameter between crude oil when close, and it is bigger that it calculates that result and actual conditions depart from, and is difficult to satisfy the needs of practical application.Also can calculate the mixing proportion of crude oil through the crude oil fingerprint parameter that GC-MS records, but this needs expensive analytical equipment, also is not suitable for scene or on-line analysis.
The wavelength coverage of near infrared light (NIR) is 780～2526nm; Be because the anharmonicity of molecular vibration makes molecular vibration produce when the high level transition from ground state; What reflect is the frequency multiplication and the sum of fundamental frequencies absorption of hydrogeneous radicals X-H (X is C, N, O) vibration, is very suitable for the measurement of oil product physico-chemical parameter.As far back as the early stage nineties in last century; Near-infrared spectrum technique just is used to the express-analysis and the on-line analysis of crude oil; Can in 1 minute, measure the crucial physico-chemical property data of crude oil and blending crude oil, like true boiling point distillation curve (TBP), carbon residue, sulfur content and API degree etc.Obtain application in fields such as Crude Oil Transportation, crude oil trade, crude oil blendings, obtained remarkable economical and social benefit.
At geological exploration field, the research oily for the source of mixing has many reports, and the old equality of building is in " with the mathematical model of biomarker quantitative Analysis commingled crude oil sources " (geochemistry; Vol.36, No.2,205～214) in; Choose three typical end member crude oil; Adopt 18 commingled crudes of method preparation of artificial mixed typical case end member crude oil, then end member crude oil and commingled crude are carried out analysis tests such as full oil carbon isotope, total hydrocarbon chromatogram and stable hydrocarbon chromaticness, utilize the absolute content of the biomarker in the crude oil; Adopt the method for multiple linear regression to set up mathematical model, the shared ratio of end member crude oil in the prediction hybrid crude oil.
Jin Guangxing etc. are in " the control Inner Mongol two connects the immixture of the key factor-different oil sources crude oil of its oil field oil enrichment of basin Da Er " (modern geology; Vol.19; No.3,425～431) in, ripe crude oil in its oil field of Da Er and low ripe crude oil are carried out artificial mixed; Miscella is carried out Physical Property Analysis and stratographic analysis, judge by oil density, viscosity, group composition and biomarker whether the oil that the exploration oil well is got is to mix source oil.
Summary of the invention
The purpose of this invention is to provide a kind of by different single methods of planting crude content in the near infrared spectrum prediction hybrid crude oil; This method can be set up forecast model through measuring single near infrared spectrum of planting crude oil, predicts each single content of crude oil of planting in the miscella of being made up of two or more crude oil.
Provided by the invention by the method for crude content of the same race not in the near infrared spectrum prediction hybrid crude oil, comprise the steps:
(1) measure single near infrared spectrum of planting crude oil respectively, each single absorbance vector of planting the near infrared spectrum of crude oil carried out adduction by its simulation content proportion, form the spectrum of simulation commingled crude,
(2) spectrum with each simulation commingled crude carries out the second-order differential processing, gets 3800～7000cm
-1Interval absorbance is associated with the simulation content of single kind crude oil in the corresponding simulating commingled crude, sets up the single calibration model of planting crude oil of prediction with PLS,
(3) measure the near infrared spectrum of commingled crude and carry out second-order differential and handle, get 3800～7000cm
-1The interval single calibration model of planting crude oil of absorbance substitution prediction obtains this list kind content of crude oil in the commingled crude.
The inventive method is measured single near infrared spectrum of planting crude oil earlier; Set up the spectrum of simulation commingled crude with each single near infrared light spectrum analog mixing proportion of planting crude oil, get treated simulated spectra and be associated and set up calibration model in the absorbance of specific region and corresponding single content of crude oil of planting.Near infrared spectrum by commingled crude gets final product single content of crude oil of planting in prediction hybrid or the blending crude oil through calibration model.The inventive method is set up calibration model need not carry out actual contaminated product preparation, has saved human and material resources, but each single kind content of crude oil in several kinds of blends of crudes of fast measuring, and have higher accuracy.
Description of drawings
Fig. 1 is the near infrared spectrum of crude oil A and crude oil B.
41 spectrum of simulating miscellas that Fig. 2 obtains for the near infrared spectrum by crude oil A and crude oil B.
The reality of the crude oil A content that Fig. 3 obtains with the leaving-one method validation-cross for binary system-predict the outcome.
Fig. 4 is the near infrared spectrum of crude oil C, crude oil D and crude oil E.
66 spectrum of simulating miscellas that Fig. 5 obtains for the near infrared spectrum by crude oil C, crude oil D and crude oil E.
The reality of the crude oil C content that Fig. 6 obtains with the leaving-one method validation-cross for ternary system-predict the outcome.
The reality of the crude oil D content that Fig. 7 obtains with the leaving-one method validation-cross for ternary system-predict the outcome.
Embodiment
The single near infrared spectrum of planting crude oil of the inventive method collection; Utilize the method for spectrum simulation that single absorbance of planting the near infrared spectrum of crude oil is carried out adduction by single kind crude oil blending ratio of simulation; Form various single simulated spectra of planting the different commingled crude of crude content; Simulated spectra is carried out second-order differential handle, choose 3800～7000cm
-1Interval absorbance is associated with corresponding single simulation content of planting crude oil, sets up certain single calibration model of planting crude oil in the commingled crude.Like this, measure the near infrared spectrum of actual commingled crude and carry out the second-order differential processing, choose 3800～7000cm
-1Interval absorbance substitution calibration model can obtain this list kind content of crude oil in the tested oil sample.The inventive method can very easily realize the automatic generation of near infrared spectrum calibration model by each single content of crude oil of planting in its commingled crude of near infrared spectrum quick test of single kind crude oil, is very suitable for on-line analysis.
Plant crude oil A for list and plant crude oil B with the mixed commingled crude that obtains of converting of the ratio (mass ratio) of m: n with list; If the near infrared spectrum of known crude oil A and crude oil B; Then according to Lambert-Beer's law, the absorbance of commingled crude near infrared spectrum should be each single absorbance of planting crude oil and converts the absorbance that obtains behind the ratio adduction in mixing.If want single content of crude oil of planting in the prediction hybrid crude oil; Only need the absorbance of crude oil A and crude oil B near infrared spectrum is carried out adduction by several predetermined ratios; Can obtain the theoretical spectral of a series of simulation commingled crudes; Select the characteristic wavelength district then, single crude content of planting that the absorbance of simulation commingled crude is corresponding with it is associated, and obtains calibration model (calibration curve) through least square fitting.
For the commingled crude sample of reality, only need to measure its near infrared spectrum, through the spectral manipulation same with modeling, can be through the calibration model of having built, each single content of crude oil of planting in the fast prediction commingled crude.In fact; Because crude oil is a kind of and complicated potpourri; And exist to mix and to convert reasons such as effect and apparatus measures error, can there be certain difference with the simulation mixed spectra that Theoretical Calculation obtains in the near infrared spectrum of the actual commingled crude that records, i.e. the substantial deviation Lambert-Beer's law.The method of setting up simple calibration curve can not be predicted the outcome accurately, must adopt characteristic wavelength binding factor regretional analysis such as principal component regression, offset minimum binary method, sets up calibration model.
The inventive method divided for three steps carried out single prediction of planting crude content in the mixed crude; The first step is set up different single spectrum of planting the simulation mixed crude of crude content earlier; Second step handled the spectrum of simulation mixed crude; The interval absorbance of selected characteristic is set up the single calibration model of planting crude content of prediction; The near infrared spectrum of the fixed actual mixed crude of the 3rd pacing; To its spectrum carry out with the same processing of modeling after; With the absorbance substitution calibration model of characteristic interval, can dope single content of crude oil of planting in the actual oil sample.
Preferably contain two or three single crude oil of planting in the described commingled crude of the inventive method.If when containing two kinds of list kind crude oil in the miscella, change wherein a kind of single simulation content of planting crude oil, can obtain the spectrum of a series of simulation commingled crudes, set up the calibration model of predicting this kind crude oil.If when containing three kinds of list kind crude oil in the miscella, then need change the simulation content of three kinds of crude oil, obtain the spectrum of a series of simulation commingled crudes, set up the wherein calibration model of two kinds of crude oil of prediction respectively.
Particularly, the method for the spectrum of foundation simulation commingled crude is:
When described commingled crude contained two kinds of list kind crude oil, the absorbance vector of the spectrum of simulation commingled crude was calculated by formula (I):
S
Q＝a％×S
A+b％×S
B， (I)
In the formula (I), S
Q, S
AAnd S
BBe respectively the absorbance vector of simulation commingled crude, crude oil A and crude oil B, a% and b% are respectively the analog-quality percentage composition of crude oil A and crude oil B, the spectrum of simulating commingled crude is carried out second-order differential handle, and get 3800～7000cm
-1Interval absorbance is associated with the analog-quality percentage composition of crude oil A in the corresponding simulating commingled crude, sets up the calibration model of prediction crude oil A content with PLS.
In the said method; Two kinds of single modulation amounts of planting a certain crude oil A in the crude oil are preferably a fixed value; Promptly press the fixed value content of increasing or decreasing crude oil A gradually; Preferably change the analog-quality percentage composition of crude oil A, with the spectrum of the different simulation commingled crude of the analog-quality percentage composition that obtains a series of crude oil A by the modulation amount of 0.5～4.0 quality %.
When described commingled crude contained three kinds of list kind crude oil, the absorbance vector of the spectrum of simulation commingled crude was calculated by formula (II):
S
Q＝c％×S
C+d％×S
D+e％×S
E (II)
In the formula (II), S
Q, S
C, S
DAnd S
EBe respectively the absorbance vector of simulation commingled crude, crude oil C, crude oil D and crude oil E; C%, d% and e% are respectively the analog-quality percentage composition of crude oil C, crude oil D and crude oil E; Spectrum to the simulation commingled crude carries out the second-order differential processing, gets 3800～7000cm
-1Interval absorbance is associated with the analog-quality percentage composition of crude oil C and crude oil D in the corresponding simulating commingled crude respectively, sets up the calibration model of predicting crude oil C and crude oil D content respectively with PLS.
In the said method, preferably press three kinds of single simulation content of planting crude oil of ternary phase diagram modulation, three kinds of single preferred 1～20 quality % of modulation amount that plant crude oil, more preferably 5～15 quality %.
Behind the spectrum of the simulation commingled crude that obtains different single kind crude contents, it to be carried out second-order differential handle, 3800～7000cm is chosen in the influence of elimination baseline wander etc.
-1Spectrum range, the absorbance that this is interval and corresponding single simulation content of planting crude oil are formed calibration set, set up calibration model with the offset minimum binary method.The value of the prediction residual quadratic sum (PRESS) that the best main gene employing leaving-one method validation-cross process of offset minimum binary method obtains is chosen.Leaving-one method validation-cross process is following: to a certain main cause subnumber; From the calibration set sample, choose a sample and be used for prediction, set up calibration model, predict the measured value of this sample with remaining sample; Then; This sample is put back to calibration set, from the calibration set sample, choose another one again and be used for prediction, repeat said process.Through modeling and prediction repeatedly, all once and only predicted once until all calibration set samples by prediction, then obtain the PRESS value of corresponding this factor number:
Y wherein
iBe the practical measurement value of i sample,
Be the predicted value that i sample validation-cross process obtains, n is the sample number of calibration set.
Accuracy to the calibration model set up needs verify with single known commingled crude of crude content of planting of preparation.Concrete verification method is: the different single miscellas of planting crude contents of preparation, measure the near infrared spectrum of miscella again, and carry out getting 3800～7000cm after second-order differential handles
-1The calibration model that interval absorbance substitution the inventive method (2) step sets up, the single crude content of planting that obtains predicting is by single accuracy of planting the deviation checking calibration model of content of crude oil and its content in the commingled crude of preparation of prediction.
The inventive method is the ratio of fast measuring blending crude oil accurately, can be used for fields such as Crude Oil Transportation and crude oil blending with the crucial physico-chemical property data of the blending crude oil of measuring.
Pass through example in detail the present invention below, but the present invention is not limited to this.
Used near infrared spectrometer and the condition determination of working sample is following in the instance:
Near infrared spectrometer: Thermo AntarisII ft-nir spectrometer, spectrum wave-number range 3800～10000cm
-1, resolution 8cm
-1, accumulation scanning times 64 times, transmission measurement mode.
Instance 1
Foundation is mixed single calibration model of planting crude content in the miscella of converting by two kinds of crude oil.
(1) measures single near infrared spectrum of planting crude oil
Get two kinds of intermediate base crude oil A and B, its main character is seen table 1, and the near infrared spectrum of mensuration is seen Fig. 1.
(2) set up calibration model
Crude oil A that provides by table 2 and the simulation content of crude oil B with the near infrared spectrum adduction of crude oil A and crude oil B, obtain 41 simulated spectra.The method of adduction is: the simulation content of establishing crude oil A and crude oil B is respectively a quality % and b quality %, and the near infrared spectrum absorbance vector of known crude oil A and crude oil B is S
AAnd S
B, then mix by a quality % crude oil A and b quality % crude oil B and the absorbance vector of spectrum of simulation commingled crude Q calculate by formula (I),
S
Q＝a％×S
A+b％×S
B， (I)
During calculating, each data point of spectral absorbance vector is spaced apart the resolution of instrument, is 8 wave numbers, down together.The absorbances vector of 41 simulation commingled crudes that crude oil A that will provide by table 2 and the simulation cubage of B obtain is arranged from small to large and is drawn by its corresponding wave number, and the spectrum of 41 simulation commingled crudes that obtain are seen Fig. 2.
The spectrum of above-mentioned 41 simulation commingled crudes is carried out the second-order differential processing, the interval 3800～7000cm of chosen spectrum
-1Absorbance form independent variable (X) matrix of spectrum; The simulation content of the crude oil A that each simulated spectra is corresponding is as dependent variable (Y) matrix; Set up the calibration model of predicting crude oil A content with the offset minimum binary method, the main cause subnumber is used the leaving-one method validation-cross, and value is 4; The PRESS value is 0.0011, and actual value-predicted value result that leaving-one method validation-cross process obtains sees Fig. 3.
(3) checking
Crude oil A and two kinds of crude oil of crude oil B are evenly mixed by the actual content that table 3 provides, obtain 4 oil samples.Gather the near infrared spectrum of these 4 oil samples by measuring single condition of planting crude oil, handle the interval 3800～7000cm of chosen spectrum through second-order differential
-1The calibration model set up of absorbance substitution dope the content of crude oil A, the content of crude oil B is (content of 100%-crude oil A).Table 3 provided by two kinds of content of crude oil of A, B of near infrared spectrum prediction and with the deviation of actual content.Can find out that the content of near-infrared spectrum method prediction and the absolute value of the bias between the actual content are less than 2.0 quality %.
Table 1
Table 2
Table 3
Instance 2
Foundation is mixed single calibration model of planting crude content in the miscella of converting by three kinds of crude oil.
(1) measures single near infrared spectrum of planting crude oil
Get crude oil C, crude oil D and three kinds of crude oil of crude oil E, its character is seen table 4, and the near infrared spectrum of mensuration is seen Fig. 4.
(2) set up calibration model
If the simulation commingled crude is made up of the crude oil C of c quality %, the crude oil D of d quality % and the crude oil E of e quality %, the simulation content value that provides according to table 5 is by the spectrum of the simulation commingled crude of crude oil C, crude oil D and the crude oil E of formula (II) calculating different content.
S
Q＝c％×S
C+d％×S
D+e％×S
E (II)
In the formula (II), S
C, S
DAnd S
EBe respectively the absorbance vector of crude oil C, crude oil D and crude oil E, S
QAbsorbance vector for the simulation commingled crude.The absorbance vector of 66 simulation commingled crudes that will obtain by the simulation cubage that table 5 provides is arranged from small to large by its corresponding wave number and is drawn, and the spectrum of 66 simulation commingled crudes that obtain is seen Fig. 5.
Spectrum to 66 simulation commingled crudes carries out the second-order differential processing respectively, chooses 3800～7000cm
-1The absorbance of spectrum range; It is formed independent variable (X) matrix; Be dependent variable (Y) matrix with the crude oil C of simulation commingled crude spectrum correspondence and the content of crude oil D respectively; Set up two calibration sets of prediction crude oil C and crude oil D content, set up two calibration models predicting crude oil C, crude oil D content respectively with the offset minimum binary method, best main gene adopts the leaving-one method validation-cross to be chosen for 4 respectively; The PRESS value is 0.0014, the reality of crude oil C that leaving-one method validation-cross process obtains and crude oil D content-predict the outcome and see Fig. 6 and Fig. 7 respectively.
(3) checking
Crude oil C, crude oil D and three kinds of crude oil of crude oil E are evenly mixed by the actual content that table 6 provides, prepare 5 and mix oil sample.Measure the near infrared spectrum of 5 commingled crude samples by measuring single condition of planting crude oil, it is carried out second-order differential handle, choose 3800～7000cm
-1The absorbance of spectrum range, the calibration model of crude oil C, crude oil D is predicted in substitution respectively, dopes the content of crude oil C and crude oil D respectively, the content of crude oil E is (100%-crude oil C content-crude oil C content), predicts content and sees table 6 with the deviation of actual content.Can know that by table 6 absolute value of the bias is less than 2.5 quality % between single kind content of crude oil of the inventive method prediction and the actual content.
Table 4
Table 5
Table 6
Claims (8)
1. the method by single kind crude content in the near infrared spectrum prediction hybrid crude oil comprises the steps:
(1) measure single near infrared spectrum of planting crude oil respectively, each single absorbance vector of planting the near infrared spectrum of crude oil carried out adduction by its simulation content proportion, form the spectrum of simulation commingled crude,
(2) spectrum with each simulation commingled crude carries out the second-order differential processing, gets 3800～7000cm
-1Interval absorbance is associated with the simulation content of single kind crude oil in the corresponding simulating commingled crude, sets up the single calibration model of planting crude oil of prediction with PLS,
(3) measure the near infrared spectrum of commingled crude and carry out second-order differential and handle, get 3800～7000cm
-1The interval single calibration model of planting crude oil of absorbance substitution prediction obtains this list kind content of crude oil in the commingled crude.
2. according to the described method of claim 1, it is characterized in that containing in the described commingled crude two or three kind of single crude oil of planting.
3. according to the described method of claim 1, it is characterized in that the absorbance vector of the spectrum of simulation commingled crude is calculated by formula (I) when described commingled crude contains two kinds of list kind crude oil:
S
Q＝a％×S
A+b％×S
B， (I)
In the formula (I), S
Q, S
AAnd S
BBe respectively the absorbance vector of simulation commingled crude, crude oil A and crude oil B, a% and b% are respectively the analog-quality percentage composition of crude oil A and crude oil B, the spectrum of simulating commingled crude is carried out second-order differential handle, and get 3800～7000cm
-1Interval absorbance is associated with the analog-quality percentage composition of crude oil A in the corresponding simulating commingled crude, sets up the calibration model of prediction crude oil A content with PLS.
4. according to the described method of claim 3, it is characterized in that changing the analog-quality percentage composition of crude oil A by the modulation amount of 0.5～4.0 quality %.
5. according to the described method of claim 1, it is characterized in that the absorbance vector of the spectrum of simulation commingled crude is calculated by formula (II) when described commingled crude contains three kinds of list kind crude oil:
S
Q＝c％×S
C+d％×S
D+e％×S
E (II)
In the formula (II), S
Q, S
C, S
DAnd S
EBe respectively the absorbance vector of simulation commingled crude, crude oil C, crude oil D and crude oil E; C%, d% and e% are respectively the analog-quality percentage composition of crude oil C, crude oil D and crude oil E; Spectrum to the simulation commingled crude carries out the second-order differential processing, gets 3800～7000cm
-1Interval absorbance is associated with the analog-quality percentage composition of crude oil C and crude oil D in the corresponding simulating commingled crude respectively, sets up the calibration model of predicting crude oil C and crude oil D content respectively with PLS.
6. according to the described method of claim 5, it is characterized in that by three kinds of single simulation content of planting crude oil of ternary phase diagram modulation.
7. according to the described method of claim 6, it is characterized in that three kinds of single modulation amounts of planting the simulation content of crude oil are 1～20 quality %.
8. according to the described method of claim 1, it is characterized in that preparing different single miscellas of planting crude contents, measure the near infrared spectrum of miscella again, carry out getting 3800～7000cm after second-order differential handles
-1The calibration model that interval absorbance substitution (2) step sets up, the single crude content of planting that obtains predicting is by single accuracy of planting the deviation checking calibration model of content of crude oil and its content in the commingled crude of preparation of prediction.
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| EP1703272A1 (en) * | 2005-03-16 | 2006-09-20 | BP Chemicals Limited | Measuring near infra-red spectra using a demountable NIR transmission cell |
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