CN102954946B - By the method for infrared spectrum measurement sulfur content in crude oil - Google Patents
By the method for infrared spectrum measurement sulfur content in crude oil Download PDFInfo
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Abstract
A kind of method by infrared spectrum measurement sulfur content in crude oil, comprise (1) and collect various crude oil sample, crude oil sample sulfur content is measured with standard method, set up sulfur content matrix Y, (2) measure each crude oil sample infrared spectrum at different temperatures collected and carry out single order or second-order differential process, getting 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1the absorbance of characteristic spectrum area forms three-dimensional light spectrum matrix <u>X</uGreatT.Gr eaT.GT (I × J × K), wherein I is crude oil sample number, J is that the wavelength of characteristic spectrum area is counted, K is temperature variation number, N-way partial least square is adopted to set up calibration model with sulfur content matrix Y, (3) with measure crude oil sample to be measured infrared spectrum at different temperatures under the identical condition of crude oil sample of collecting and carry out single order or second-order differential process, get 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1the absorbance of characteristic spectrum area forms three-dimensional light spectrum matrix <u>X</uGreatT.Gr eaT.GT
un, substituted into the calibration model that (2) step is set up, obtained the sulfur content of crude oil sample to be measured.The method analysis speed is fast, tests accurate, reproducible.
Description
Technical field
The present invention is a kind of method by Forecast of Spectra sulfur content in crude oil, specifically, is a kind of method being predicted sulfur content in crude oil by infrared spectrum.
Background technology
At present, on Global Oil trade market, the crude oil price of production and transaction alters a great deal, and except the density factor of crude oil, the sulfur content height of crude oil is also the major reason causing crude value greatly to reduce.The crude oil kind of refinery of China processing is comparatively complicated, and most of refinery all mixes in processing and converts crude oil.Quick detection sulfur content in crude oil, for optimization charging, mediation, improves enterprise efficiency significant.
Chinese Crude Oils sulfur content is general lower, relatively gentle to the corrosion of environment in the defeated process of pipe, can not cause great corrosion to oil pipeline.Most of imported crude oil is sulphur-bearing crude and sour crude, and its corrosivity is generally higher than domestic low-sulphur crude.Therefore, crude oil in China pipeline is when carrying imported high sulfur crude oil and device charging, and must detect the content of various corrosive sulphur material, it is significant.
In crude oil, the existence form of sulphur has the sulfur-containing organic compound such as elementary sulfur, sulfuretted hydrogen and mercaptan, thioether, disulfide, thiophene, corrosion can be produced to processing unit (plant) in Crude Oil Processing, these corrosive sulphur materials can record its relative content by standard method, and sulfur content is exactly under specified requirements, measure the content of these sulfur-containing organic compounds in crude oil.Although the corrosivity of crude oil is relation proportional with its sulfur content not necessarily, the possibility that the crude oil that sulfur content is high produces corrosion is also larger.
The existence of corrosive sulphur material produces corrosion to equipment, brings hidden danger, causes certain difficulty to petroleum refining, obtain sulfur content in crude oil in time and have very important directive significance to petroleum refining to production.Existing domestic and international test methods of sulphur contents many employings combustion method, spectroscopic methodology, spectral method obtain the total sulfur content of crude oil, its result is comparatively accurate, but measuring speed compared with slow, method is too loaded down with trivial details, workload is large, cost is high, far can not meet the needs of practical application.Generally all need to obtain the fundamental property data such as sulfur content in crude oil in time mixed the converting in crude oil or Oil Transportation Process in Pipeline of refinery's refining, original method can not meet the needs of Fast Evaluation.
In " in Crude Oil Certified Reference Materials By Oxygen Bomb Combustion And Ion Chromatography sulfur content ", (chemical analysis measures Shi Naijie, 2006,15 (1): 4 ~ 7), in a literary composition, By Oxygen Bomb Combustion-chromatography of ions is adopted to carry out quantitative test to the sulfur content in Crude Oil Certified Reference Materials.Investigate sample combustion condition, demonstrated the reliability of experimental technique, to analyze in blank amount, solution many empirical factors such as matrix, apparatus measures value drift, absorbing liquid to the impact of measurement result.
Lei Meng is at " research of two-dimentional Near-Infrared Spectra for Quantitative Analysis viscosity index of internal combustion engine oil performance " (petroleum refining and chemical industry, 2009,40 (4): 61 ~ 65) in a literary composition, with voltage for disturb mode outward, to obtain I. C. engine oil two dimension near infrared spectrum.Collect and set up multidimensional offset minimum binary (N-PLS) model combustion motor oil viscosity index from 35 I. C. engine oil samples of different manufacturers, different quality grade and carried out forecasting research.
MarceloM.Sena etc. are at " N-wayPLSappliedtosimultaneousspectrophotometricdetermina tionofacetylsalicylicacid, paracetamolandcaffeine " { JournalofPharmaceuticalandBiomedicalAnalysis, Issue34, Pages27-34 (2004) } in a literary composition, using pH value as conditional-variable, multidimensional deflected secondary air is used to set up acetylsalicylic acid, paracetamol, the calibration model of caffeine, predict the outcome and show, prediction standard deviation (RESEP) is lower than the deviation adopting offset minimum binary.
Summary of the invention
The object of this invention is to provide a kind of method by infrared spectrum measurement sulfur content in crude oil, the method analysis speed is fast, tests accurate, reproducible.
Method by infrared spectrum measurement sulfur content in crude oil provided by the invention, comprises the steps:
(1) collect various crude oil sample, measure crude oil sample sulfur content with standard method, set up sulfur content matrix Y,
(2) measure each crude oil sample infrared spectrum at different temperatures collected and carry out single order or second-order differential process, getting 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1the absorbance of characteristic spectrum area forms three-dimensional light spectrum matrix
x(I × J × K), wherein I is crude oil sample number, and J is that the wavelength of characteristic spectrum area is counted, and K is temperature variation number, adopts N-way partial least square to set up calibration model with sulfur content matrix Y,
(3) with measure crude oil sample to be measured infrared spectrum at different temperatures under the identical condition of crude oil sample of collecting and carry out single order or second-order differential process, get 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1the absorbance of characteristic spectrum area forms three-dimensional light spectrum matrix
x un, substituted into the calibration model that (2) step is set up, obtained the sulfur content of crude oil sample to be measured.
The inventive method is by measuring the infrared spectrum of crude oil sample at different temperatures, spectrogram is carried out differential process, select suitable diffuse reflectance infrared spectroscopy spectrum district, the sulfur content in crude oil that absorbance corresponding for characteristic spectrum area and standard method record is associated, calibration model is set up by multiple regression analysis, by calibration model, predict its sulfur content by crude oil sample to be measured in the absorbance of selected characteristic spectrum area.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet that the present invention sets up calibration model.
Embodiment
The inventive method selects the infrared spectral region having good correlation with sulfur content, and namely wave number is 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1wave band interval as characteristic spectrum area, the crude oil sample measured under selecting different temperatures is in the absorbance of above-mentioned characteristic spectrum area, again the absorbance of various crude oil characteristic spectrum area is at different temperatures associated with the sulfur content of each crude oil sample, set up forecast model, then the absorbance measured at different temperatures by forecast model and unknown crude oil sample predicts its sulfur content.The inventive method is quick, accurate.
Infrared spectrum produces due to molecular vibration-rotational energy level transition.Traditionally, be often 2500 ~ 25000nm (wave number 4000 ~ 400cm wavelength
-1) spectrum district be called in infrared, be called for short infrared region, be 780 ~ 2500nm (wave number 12820 ~ 4000cm wavelength
-1) spectrum district be called near-infrared region.The fundamental frequency of most organic compounds and many mineral compound molecular vibrations all appears at region of ultra-red, this qualitative analysis for organic constitution and constituent analysis very effective.Due to the existence of fingerprint region, in this region, than near infrared spectrum, cogency is had more to the quantitative of sulfur content in crude oil.Described wave number is the number of the ripple contained in unit centimetre, and wave number is the inverse of wavelength.
The sweep limit that the present invention measures crude oil sample infrared spectrum is 4000 ~ 400cm
-1.
The method setting up calibration model first selectes dissimilar crude oil sample, as the crude oil of Different producing area, different base genus, different viscosities, then uses standard method working sample sulfur content.The standard method of the present invention (1) step mensuration sulfur content in crude oil used is GB/T17040-2008 standard method, i.e. energy-dispersion X-ray fluorescence spectrometry.The quantity of selected crude oil sample is more, and institute's positive model for school building is more accurate, reliable.But for reducing workload in practical operation, generally choose right quantity and can contain the sample of likely predicted value, preferably dissimilar crude oil sample quantity is 200 ~ 280.
For checking the accuracy of calibration model, generally the sample measuring sulfur content with standard method is divided into calibration set and checking collection.Calibration set sample number is greater than checking collection sample number, and set up calibration model with calibration set sample, calibration set sample is representative, and its sulfur content contains the sulfur content of all prediction samples.Checking collection, by collecting the sample composition randomly drawed in sample, using checking collection sample as unknown sample, verifies the accuracy of calibration model.Checking collection sample size is less, is about and collects 1/3 of test sample total quantity.
After the acid number measuring crude oil sample with standard method, with its infrared spectrum of determination of infrared spectroscopy, then single order or second-order differential process are carried out, to eliminate interference to the absorbance of selected wave band.
The inventive method all measures the absorbance under different temperatures to each crude oil sample, and the temperature measuring crude oil infrared spectrum is 30 ~ 60 DEG C, and each temperature interval measuring change is 5 ~ 10 DEG C.Then the absorbance of the crude oil measured under different temperatures is set up three-dimensional light spectrum matrix
x, i.e. absorbance matrix, its size is counted by the wavelength of modeling sample number used, characteristic spectrum area and temperature variation number of times determines.
The inventive method calibration set sample sets up the method signal of forecast model and the unknown crude oil sample sulfur content of prediction as Fig. 1.
Below the present invention is used for absorbance matrix
xbriefly introduce as follows with the method that sulfur content matrix Y N-PLS algorithm is associated:
It is by three-dimensional matrice that N-PLS calculates ratio juris
x(I × J × K) is decomposed into trilinear model:
wherein t is score vector, w
jand w
kfor two load vectors of correspondence, F is main cause subnumber, e
ijkfor residual error battle array.Identical with conventional P LS, N-PLS, while decomposed spectrum battle array, also decomposes concentration array (the present invention is sulfur content matrix Y), and by iteration, two decomposable processes is united two into one, with validation-cross determination main gene.Specific algorithm is:
(1) forecast model is set up:
x(I × J × K) is absorbance matrix, and I is modeling sample number, and J is that the wavelength of characteristic spectrum area is counted, and K is temperature variation number.The concentration array that y (I × 1) is modeling sample, the inventive method is sulfur content matrix Y.
(1) will
xexpand into two-dimensional matrix X
0(I × JK), namely splices the absorbance measured under different temperatures successively according to temperature variation order, forms a two-dimensional matrix X
0(I × JK);
(2) determine the maximal value of main cause subnumber, select main cause subnumber f=1 one by one ..., F;
(3) Z (J × K) matrix is calculated, Z
f=X
f-1 ty;
(4) svd is carried out to Z matrix, [wk, s, wj]=svd (Z
f)
Make w
k=wk (:, 1), w
j=wj (:, 1);
(5) calculate
(JK×1)
(6) t is calculated
f=X
f-1w
f; (I × 1)
(7) calculate
(1×1)
(8) u is calculated
f=y
f-1q
f; (I × 1)
(9) calculate
wherein T
f=[t
1..., t
f];
(10) X is made
f=X
f-1-t
fw
f,
(11) f=f+1, returns (3) step, obtains score and the load of each circulation successively.Then use corresponding prediction residual quadratic sum (PRESS) mapping of main gene number, be called that PRESS schemes, the minimum point of corresponding PRESS figure is best main cause subnumber,
wherein y* is the predicted value that validation-cross obtains, and y is measured value, and n is calibration set total number of samples.
(12) w is preserved
f, b
fand q
f, with to unknown sample matrix
x uncarry out concentration value (the present invention is sulfur content) prediction.
In above-mentioned computing method, symbol
represent the Kronecker product (Kroneckerproduct) of matrix, matrix A (I × J) is expressed as with the Kronecker product of Matrix C (M × N):
(2) sample sulfur content is predicted
For the spectrum matrix of some unknown crude oil samples
x un(1 × J × K), is calculated by following steps and predicts the outcome:
(1) will
x unexpand into two-dimensional matrix X
un 0(1 × JK), namely splices the absorbance measured under different temperatures successively according to temperature conditions change order, forms a two-dimensional matrix X
un 0(1 × JK);
(2) w preserved is called
f, b
fand q
f;
(3) t is calculated
f=X
un f-1w
f, X
f=X
un f-1-t
fw
f, f=1 ..., F;
(4) calculate
wherein T
f=[t
1..., t
f].
The inventive method modeling crude oil sample used covers the crude oil kind of global major production areas, therefore, and the sulfur content of major production areas, available the inventive method fast prediction whole world crude oil.
Below by example in detail the present invention, but the present invention is not limited to this.
The various crude oil samples collected in example, measure its sulfur content according to GB/T17040 method, for setting up calibration model.
The repeatability of GB/T17040 method to measurement result is expressed as: the difference of the result of twice repeated test can not more than 0.02894 (x+0.1691), to being expressed as of repeatability result: different operating person.In different experiments room, can not more than 0.1215 (x+0.05555) to the difference of the result that same sample measures.Wherein, x is the arithmetic mean of twice test findings, quality %.
Example 1
Set up sulfur content in crude oil infrared spectrum calibration model and verify.
(1) crude oil sample sulfur content is measured with standard method
Collect the crude oil sample 280 of each major production areas, measure its sulfur content by GB/T17040 method.Collect wherein representational crude oil sample 240 composition calibration set.
(2) calibration model is set up with calibration set sample
With the infrared spectrum of ThermoNicolet-6700 Fourier transformation infrared spectrometer measurement update collection sample.Measuring annex is Thermo company 45 DEG C of ZnSeATR temperature-changeable crystal ponds.
Measuring method is: poured into by test sample in ZnSeATR absorption of sample pond, be warming up to 30 DEG C, and be that reference carries out spectral scan with air after 2 minutes, scanning times is 64 times.Adopt spectral limit: 650 ~ 4000cm
-1; Resolution is 8cm
-1.
Be warming up to 40 DEG C, 50 DEG C, 60 DEG C successively to stablize after 2 minutes and carry out Infrared spectrum scanning, each sample determination time is 20 minutes.The spectrum obtained is carried out first differential process, gets 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1absorbance composition three-dimensional light spectrum matrix in characteristic spectrum area after first differential process
x(I × J × K), wherein I is calibration set crude oil sample number, and J is that characteristic spectrum area wavelength is counted, and K is temperature variation number, herein K=4.
Sulfur content matrix Y is formed by the sulfur content that the GB/T17040 method that each crude oil sample is corresponding measures.Will with N-way partial least square (N-PLS)
xbe associated with Y, set up sulfur content in crude oil calibration model.Computational prediction residual sum of squares (RSS) (PRESS) minimum value determines that the best main cause subnumber of N-PLS is 7, and Modling model pertinent statistical parameters used is in table 1.
Wherein,
In above formula, m is checking collection total number of samples, y
i, actualfor standard method measured value, y
i, predictedfor predicted value.
(3) reliability of calibration model is verified
Random selecting 40 unknown sample composition checking collection, measure it at the infrared spectrum of 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, carry out first differential process, get 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1the absorbance composition three-dimensional light spectrum matrix of characteristic spectrum area
x un, then be launched into two-dimensional matrix
x un 0, substitute into calibration model, obtain the sulfur content predicted value of crude oil sample.Checking collection pertinent statistical parameters is in table 1, and the comparative result of predicted value and GB/T17040 method measured value is in table 2.
Table 1
Table 2
Example 2
Collect crude oil sample by the method for example 1, measure crude oil sample sulfur content with standard method, measure each sample at the infrared spectrum of 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, carry out second-order differential process unlike to spectrum, get 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1absorbance composition three-dimensional light spectrum matrix in characteristic spectrum area after second-order differential process
x, then associate with Y matrix N-PLS method and set up calibration model, then form three-dimensional light spectrum matrix with checking collection sample through the absorbance of the characteristic spectrum area of second-order differential process
x un, substitute into calibration model, obtain the sulfur content predicted value of crude oil sample.Calibration set and checking collection pertinent statistical parameters are in table 3, and the predicted value of checking collection sample and the comparative result of GB/T17040 method measured value are in table 4.
Table 3
Table 4
Claims (6)
1., by a method for infrared spectrum measurement sulfur content in crude oil, comprise the steps:
(1) collect various crude oil sample, measure crude oil sample sulfur content with standard method, set up sulfur content matrix Y,
(2) measure each crude oil sample infrared spectrum at different temperatures collected and carry out single order or second-order differential process, getting 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1the absorbance of characteristic spectrum area forms three-dimensional light spectrum matrix
x(I × J × K), wherein I is crude oil sample number, and J is that the wavelength of characteristic spectrum area is counted, and K is temperature variation number, adopts N-way partial least square to set up calibration model with sulfur content matrix Y,
(3) with measure crude oil sample to be measured infrared spectrum at different temperatures under the identical condition of crude oil sample of collecting and carry out single order or second-order differential process, get 745 ~ 1227cm
-1with 1516 ~ 1613cm
-1the absorbance of characteristic spectrum area forms three-dimensional light spectrum matrix
x un, substituted into the calibration model that (2) step is set up, obtained the sulfur content of crude oil sample to be measured,
The temperature measuring crude oil sample infrared spectrum is 30 ~ 60 DEG C, and each temperature interval measuring change is 5 ~ 10 DEG C.
2. in accordance with the method for claim 1, it is characterized in that the sweep limit measuring crude oil sample infrared spectrum is 4000 ~ 400cm
-1.
3. in accordance with the method for claim 1, it is characterized in that the standard method that crude oil sample sulfur content is determined in (1) pacing is GB/T17040-2008.
4. in accordance with the method for claim 1, it is characterized in that the various crude oil samples collected being divided into calibration set and checking collection, calibration set sample number is greater than checking collection sample number, sets up calibration model with calibration set sample, by the accuracy of checking collection sample checking calibration model.
5. in accordance with the method for claim 4, it is characterized in that the sulfur content of calibration set sample contains the sulfur content of all prediction crude oil samples.
6. in accordance with the method for claim 4, it is characterized in that checking collection sample is by collecting the sample composition randomly drawed in sample.
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| CN103364368B (en) * | 2013-07-12 | 2015-04-15 | 南京富岛信息工程有限公司 | Rapid detection method for properties of mixed crude oil |
| CN105044050A (en) * | 2015-07-07 | 2015-11-11 | 中国农业大学 | Rapid quantitative analysis method for metallic elements in crop straw |
| CN105300923B (en) * | 2015-11-19 | 2018-02-13 | 江南大学 | Without measuring point model of temperature compensation modification method during a kind of near-infrared spectrometers application on site |
| CN105486658B (en) * | 2015-11-19 | 2018-09-28 | 江南大学 | A kind of near-infrared physical parameter measurement method with no measuring point temperature compensation function |
| CN112326594A (en) * | 2020-10-27 | 2021-02-05 | 安徽同心新材料科技有限公司 | Method for establishing quantitative model for rapidly detecting sulfur content in C5 oil product |
| CN115406857B (en) * | 2022-09-07 | 2023-06-27 | 山东天厚石油科技有限责任公司 | Crude oil organic chlorine detection device and method for petroleum production |
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| CN100498293C (en) * | 2004-12-28 | 2009-06-10 | 中国石油化工股份有限公司 | Method for measuring content of dialkene in C10-C13 positive formation hydrocarbon through spectrum of infrared light |
| CN101726451A (en) * | 2008-10-21 | 2010-06-09 | 冯新泸 | Method for measuring viscosity index of internal combustion engine oil |
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