CN102954946A - Method for determining sulfur content of crude oil through infrared spectrometry - Google Patents
Method for determining sulfur content of crude oil through infrared spectrometry Download PDFInfo
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Abstract
The invention relates to a method for determining the sulfur content of crude oil through infrared spectrometry, which comprises the following steps: (1) collecting various crude oil samples, measuring the sulfur contents of the crude oil samples through a standard method, and establishing a sulfur content matrix Y; (2) determining infrared spectra of each collected crude oil sample at different temperatures, performing first-order or second-order differential treatment, selecting absorbency in characteristic spectrum regions of 745-1227 cm<-1> and 1516-1613 cm<-1> to form a three-dimensional spectrum matrix X(I*J*K), and establishing a correcting model by combining the three-dimensional spectrum matrix X(I*J*K) and the sulfur content matrix Y through a multidimensional partial least square method, wherein I is the number of the crude oil samples, J is the number of wavelength points in the characteristic spectrum regions, and K is the number of temperature change; and (3) determining infrared spectra of a crude oil sample to be measured at different temperatures under the identical conditions of the collected crude oil samples, performing first-order or second-order differential treatment, selecting absorbency in characteristic spectrum regions of 745-1227 cm<-1> and 1516-1613 cm<-1> to form a three-dimensional spectrum matrix Xun, and substituting in the correcting model established in the step (2) to obtain the sulfur content of the crude oil sample to be measured. The method provided by the invention has the advantages of high analysis speed, high test accuracy and good repetitiveness.
Description
Technical field
The present invention is a kind of method by the Forecast of Spectra sulfur content in crude oil, specifically, is a kind of method by infrared spectrum prediction sulfur content in crude oil.
Background technology
At present, the crude oil price of production and transaction alters a great deal on the Global Oil trade market, and except the density factor of crude oil, the sulfur content of crude oil height also is to cause crude oil to be worth a major reason that greatly reduces.The crude oil kind of China refinery processing is comparatively complicated, and most of refinery is all at the mixed crude oil of converting of processing.The fast detecting sulfur content in crude oil for optimizing charging, mediation, improves enterprise efficiency significant.
The Chinese Crude Oils sulfur content is generally lower, and the corrosion to environment in the defeated process of pipe is relatively gentle, can not cause great corrosion to oil pipeline.Most of imported crude oils are sulphur-bearing crude and sour crude, and its corrosivity generally is higher than domestic low-sulphur crude.Therefore, the crude oil in China pipeline must detect the content of various corrosivity sulphur-containing substances when carrying imported high sulfur crude oil and device charging, and it is significant.
The existence form of sulphur has the sulfur-containing organic compounds such as elementary sulfur, sulfuretted hydrogen and mercaptan, thioether, disulfide, thiophene in the crude oil, can in Crude Oil Processing, produce corrosion to processing unit (plant), these corrosivity sulphur-containing substances can record its relative content by standard method, and sulfur content is exactly to measure the content of these sulfur-containing organic compounds in crude oil under specified requirements.Although the corrosivity of crude oil not necessarily with the proportional relation of its sulfur content, the possibility that the high crude oil of sulfur content produces corrosion is also larger.
The existence of corrosivity sulphur-containing substance produces corrosion to equipment, brings hidden danger to production, causes certain difficulty to petroleum refining, in time obtains sulfur content in crude oil petroleum refining is had very important directive significance.Existing domestic and international test methods of sulphur contents adopts firing method, spectroscopic methodology, spectral method to obtain the total sulfur content of crude oil more, its result is comparatively accurate, but measuring speed is slow, method is too loaded down with trivial details, workload is large, cost is high, far can not satisfy the needs of practical application.Convert fundamental property data such as generally all needing in time to obtain sulfur content in crude oil in crude oil or the Oil Transportation Process in Pipeline refinery refining is mixed, original method can not satisfy the needs of Fast Evaluation.
Shi Naijie is in " sulfur content in the Crude Oil Certified Reference Materials By Oxygen Bomb Combustion And Ion Chromatography " (chemical analysis metering, 2006,15 (1): 4～7) in the literary composition, adopt By Oxygen Bomb Combustion And-chromatography of ions that the sulfur content in the Crude Oil Certified Reference Materials has been carried out quantitative test.Investigate the sample combustion condition, verified the reliability of experimental technique, analyzed many empirical factors such as matrix in blank amount, the solution, apparatus measures value drift, absorption liquid to the impact of measurement result.
Lei Meng " 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 the literary composition, with voltage for disturbing mode outward, to obtain I. C. engine oil two dimension near infrared spectrum.Collect to 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.
Marcelo M.Sena etc. are at " N-way PLS applied to simultaneous spectrophotometric determination of acetylsalicylic acid; paracetamol and caffeine " { Journal ofPharmaceutical and Biomedical Analysis, Issue 34, Pages 27-34 (2004) } in the literary composition, with the pH value as conditional-variable, use multidimensional offset minimum binary method to set up acetylsalicylic acid, paracetamol, the calibration model of caffeine, predicting the outcome shows, prediction standard deviation (RESEP) is lower than the deviation that adopts offset minimum binary.
Summary of the invention
The purpose of this invention is to provide a kind of method by the infrared spectrum measurement sulfur content in crude oil, the method analysis speed is fast, and test is accurate, good reproducibility.
Method by the infrared spectrum measurement sulfur content in crude oil provided by the invention comprises the steps:
(1) collect various crude oil samples, measure the crude oil sample sulfur content with standard method, set up sulfur content matrix Y,
(2) each crude oil sample of measure collecting under different temperatures infrared spectrum and carry out single order or second-order differential is processed, get 745～1227cm
-1With 1516～1613cm
-1The absorbance of characteristic spectrum area consists of the three-dimensional light spectrum matrix
X(I * J * K), wherein I is the crude oil sample number, and J is that the wavelength of characteristic spectrum area is counted, and K is the temperature variation number, adopts N-way partial least square to set up calibration model with sulfur content matrix Y,
(3) under the condition identical with the crude oil sample of collecting, measure crude oil sample to be measured under different temperatures infrared spectrum and carry out single order or second-order differential is processed, get 745～1227cm
-1With 1516～1613cm
-1The absorbance of characteristic spectrum area consists of the three-dimensional light spectrum matrix
X Un, with the calibration model that its substitution (2) step sets up, obtain the sulfur content of crude oil sample to be measured.
The inventive method is by measuring the infrared spectrum of crude oil sample under different temperatures, spectrogram is carried out differential to be processed, select suitable diffuse reflectance infrared spectroscopy spectrum district, the absorbance that characteristic spectrum area is corresponding is associated with the sulfur content in crude oil that standard method records, set up calibration model 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.
Description of drawings
Fig. 1 is the schematic flow sheet that the present invention sets up calibration model.
Embodiment
The inventive method selects to have with sulfur content the infrared spectral region of good correlation, and namely wave number is 745～1227cm
-1With 1516～1613cm
-1The wave band interval as characteristic spectrum area, the crude oil sample of measuring under the selection different temperatures is in the absorbance of above-mentioned characteristic spectrum area, absorbance with various crude oil characteristic spectrum area under different temperatures is associated with the sulfur content of each crude oil sample again, set up forecast model, the absorbance of being measured under different temperatures by forecast model and unknown crude oil sample is again predicted its sulfur content.The inventive method is quick, accurate.
Infrared spectrum is owing to molecular vibration-rotational energy level transition produces.Traditionally, be wavelength 2500～25000nm (wave number 4000～400cm often
-1) the spectrum district infrared in being called, be called for short infrared region, be wavelength 780～2500nm (wave number 12820～4000cm
-1) the spectrum district be called the near-infrared region.The fundamental frequency of most organic compounds and many mineral compound molecular vibrations all appears at region of ultra-red, and this qualitative analysis and constituent analysis for organic constitution is very effective.Because the existence of fingerprint region, quantitatively have more cogency than near infrared spectrum in this zone to sulfur content in crude oil.Described wave number is the number of the unit centimetre ripple that contains, and wave number is the inverse of wavelength.
The sweep limit that the present invention measures the crude oil sample infrared spectrum is 4000～400cm
-1
The method of setting up calibration model is to select first dissimilar crude oil sample, such as the crude oil of different producing regions, different base genus, different viscosities, then uses standard method working sample sulfur content.The standard method of the present invention (1) used mensuration sulfur content in crude oil of step is the GB/T17040 standard method, i.e. the 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, generally choose right quantity and can contain the sample that institute might predicted value in the practical operation, preferably dissimilar crude oil sample quantity is 200～280.
Be the accuracy of check calibration model, generally will be divided into calibration set and checking collection with the sample that sulfur content is measured in standard method.The calibration set sample number is set up calibration model greater than checking collection sample number with the calibration set sample, and the calibration set sample is representative, and its sulfur content contains the sulfur content of all prediction samples.The checking collection will be verified to collect sample as unknown sample by collecting the sample composition of randomly drawing in the sample, verify the accuracy of calibration model.Checking collection sample size is less, is about to collect 1/3 of specimen total quantity.
After measuring the acid number of crude oil sample with standard method, with its infrared spectrum of determination of infrared spectroscopy, then the absorbance of selected wave band is carried out single order or second-order differential processing, disturb to eliminate.
The inventive method is all measured absorbance under the different temperatures to each crude oil sample, and the temperature of measuring the crude oil infrared spectrum is 30～60 ℃, and each to measure the temperature interval that changes be 5～10 ℃.Then the absorbance of the crude oil measured under the different temperatures is set up the three-dimensional light spectrum matrix
X, i.e. absorbance matrix, its size is counted by the wavelength of the used sample number of modeling, characteristic spectrum area and the temperature variation number of times determines.
The inventive method is set up the method signal of forecast model and the unknown crude oil sample sulfur content of prediction such as Fig. 1 with the calibration set sample.
The below is used for the absorbance matrix the present invention
XThe method that is associated with the N-PLS algorithm with sulfur content matrix Y briefly introduces as follows:
The principle of N-PLS algorithm is with three-dimensional matrice
X(I * J * K) is decomposed into three linear models:
(1) set up forecast model:
X(I * J * K) is the absorbance matrix, and I is the modeling sample number, and J is that the wavelength of characteristic spectrum area is counted, and K is the temperature variation number.Y (I * 1) is the concentration array of modeling sample, and the inventive method is sulfur content matrix Y.
(1) will
XExpand into two-dimensional matrix X
0(I * JK), namely according to the temperature variation order absorbance of measuring under the different temperatures is spliced successively forms a two-dimensional matrix X
0(I * JK);
(2) determine the maximal value of main cause subnumber, select one by one main cause subnumber f=1 ..., F;
(3) calculate Z (matrix of J * K), Z
f=X
F-1 TY;
(4) the Z matrix is carried out svd, [wk, s, wj]=svd (Z
f)
Make w
K=wk (:, 1), w
J=wj (:, 1);
(5) calculate
(JK×1)
(6) calculate t
f=X
F-1w
f(I * 1)
(7) calculate
(1×1)
(8) calculate u
f=y
F-1q
f(I * 1)
(9) calculate
T wherein
f=[t
1..., t
f];
(10) make X
f=X
F-1-t
fw
f,
(11) f=f+1 returns (3) step, obtains successively score and the load of each circulation.Then use the corresponding prediction residual quadratic sum of main gene number (PRESS) mapping, be called PRESS figure, 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 the calibration set total number of samples.
(12) preserve w
f, b
fAnd q
f, with to the unknown sample matrix
X UnCarry out concentration value (the present invention is sulfur content) prediction.
In the above-mentioned computing method, symbol
Represent the Kronecker product (Kronecker product) of matrix, matrix A (I * J) and Matrix C (Kronecker product of M * N) is expressed as:
(2) prediction sample sulfur content
Spectrum matrix for some unknown crude oil samples
X Un(1 * J * K) calculates by following steps and to predict the outcome:
(1) will
X UnExpand into two-dimensional matrix X
Un 0(1 * JK), namely according to temperature conditions variation order the absorbance of measuring under the different temperatures is spliced successively, form a two-dimensional matrix X
Un 0(1 * JK);
(2) call the w that has preserved
f, b
fAnd q
f
(3) calculate t
f=X
Un F-1w
f, X
f=X
Un F-1-t
fw
f, f=1 ..., F;
(4) calculate
T wherein
f=[t
1..., t
f].
The used crude oil sample of the inventive method modeling has been contained 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 of collecting in the example are measured its sulfur content according to GB/T 17040 methods, are used for setting up calibration model.
GB/T 17040 methods are expressed as the repeatability of measurement result: the result's of twice repeated test difference can not surpass 0.02894 (x+0.1691), to being expressed as of repeatability result: the different operating person.In the different experiments chamber, the result's that same sample is measured difference can not surpass 0.1215 (x+0.05555).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) measures the crude oil sample sulfur content with standard method
Collect 280 of the crude oil samples of each major production areas, measure its sulfur content with GB/T 17040 methods.Collecting wherein, 240 of representational crude oil samples form calibration set.
(2) set up calibration model with the calibration set sample
Infrared spectrum with Thermo Nicolet-6700 Fourier transformation infrared spectrometer measurement update collection sample.Measuring annex is 45 ℃ of ZnSe ATR of Thermo company temperature-changeable crystal pond.
Measuring method is: specimen is poured in the ZnSe ATR absorption of sample pond, be warming up to 30 ℃, carry out spectral scan take air as reference after 2 minutes, scanning times is 64 times.Adopt spectral limit: 650～4000cm
-1Resolution is 8cm
-1
Be warming up to successively 40 ℃, 50 ℃, 60 ℃ and stablize after 2 minutes and carry out Infrared spectrum scanning, each sample determination time is 20 minutes.The spectrum that obtains is carried out the single order differential process, get 745～1227cm
-1With 1516～1613cm
-1Absorbance in the characteristic spectrum area after the single order differential is processed forms the three-dimensional light spectrum matrix
X(I * J * K), wherein I is calibration set crude oil sample number, and J is that the characteristic spectrum area wavelength is counted, and K is temperature variation number, herein K=4.
The sulfur content of measuring with GB/T 17040 methods corresponding to each crude oil sample forms sulfur content matrix Y.Will with N-way partial least square (N-PLS)
XBe associated with Y, set up the sulfur content in crude oil calibration model.Calculate prediction residual quadratic sum (PRESS) minimum value and determine that the best main cause subnumber of N-PLS is 7, set up the ASSOCIATE STATISTICS parameter that model uses and see Table 1.
Wherein,
In the following formula, m is checking collection total number of samples, y
I, actualBe standard method measured value, y
I, predictedBe predicted value.
(3) reliability of checking calibration model
Choose at random 40 unknown samples and form the checking collection, measure its infrared spectrum at 30 ℃, 40 ℃, 50 ℃, 60 ℃, carry out the single order differential and process, get 745～1227cm
-1With 1516～1613cm
-1The absorbance of characteristic spectrum area forms the three-dimensional light spectrum matrix
X Un, be launched into again two-dimensional matrix
X Un 0, the substitution calibration model obtains the sulfur content predicted value of crude oil sample.Checking collection ASSOCIATE STATISTICS parameter sees Table 1, and the comparative result of predicted value and GB/T 17040 method measured values sees Table 2.
Table 1
Table 2
Example 2
Press the method for example 1 and collect crude oil sample, measure the crude oil sample sulfur content with standard method, measure each sample at 30 ℃, 40 ℃, 50 ℃, 60 ℃ infrared spectrum, different is spectrum to be carried out second-order differential process, and gets 745～1227cm
-1With 1516～1613cm
-1Absorbance in the characteristic spectrum area after second-order differential is processed forms the three-dimensional light spectrum matrix
X, then with the Y matrix with the related calibration model of setting up of N-PLS method, the absorbance of the characteristic spectrum area of processing through second-order differential with checking collection sample again forms the three-dimensional light spectrum matrix
X Un, the substitution calibration model obtains the sulfur content predicted value of crude oil sample.Calibration set and checking collection ASSOCIATE STATISTICS parameter see Table 3, and the predicted value of checking collection sample and the comparative result of GB/T 17040 method measured values see Table 4.
Table 3
Table 4
Claims (7)
1. method by the infrared spectrum measurement sulfur content in crude oil comprises the steps:
(1) collect various crude oil samples, measure the crude oil sample sulfur content with standard method, set up sulfur content matrix Y,
(2) each crude oil sample of measure collecting under different temperatures infrared spectrum and carry out single order or second-order differential is processed, get 745～1227cm
-1With 1516～1613cm
-1The absorbance of characteristic spectrum area consists of the three-dimensional light spectrum matrix
X(I * J * K), wherein I is the crude oil sample number, and J is that the wavelength of characteristic spectrum area is counted, and K is the temperature variation number, adopts N-way partial least square to set up calibration model with sulfur content matrix Y,
(3) under the condition identical with the crude oil sample of collecting, measure crude oil sample to be measured under different temperatures infrared spectrum and carry out single order or second-order differential is processed, get 745～1227cm
-1With 1516～1613cm
-1The absorbance of characteristic spectrum area consists of the three-dimensional light spectrum matrix
X Un, with the calibration model that its substitution (2) step sets up, obtain the sulfur content of crude oil sample to be measured.
2. the sweep limit that in accordance with the method for claim 1, it is characterized in that measuring the crude oil sample infrared spectrum is 4000～400cm
-1
3. in accordance with the method for claim 1, it is characterized in that it is GB/T 17040 that the standard method of crude oil sample sulfur content is decided in (1) pacing.
4. in accordance with the method for claim 1, it is characterized in that the various crude oil samples that will collect are divided into calibration set and checking collection, the calibration set sample number is set up calibration model greater than checking collection sample number with the calibration set sample, with 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 acid number of all prediction crude oil samples.
6. in accordance with the method for claim 4, it is characterized in that verifying that the collection sample is by collecting the sample composition of randomly drawing in the sample.
7. in accordance with the method for claim 1, the temperature that it is characterized in that measuring the crude oil sample infrared spectrum is 30～60 ℃, and each to measure the temperature interval that changes be 5～10 ℃.
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| 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 |
| CN115406857A (en) * | 2022-09-07 | 2022-11-29 | 山东天厚石油科技有限责任公司 | Crude oil organic chloride detection device and method for petroleum production |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103364368A (en) * | 2013-07-12 | 2013-10-23 | 南京富岛信息工程有限公司 | Rapid detection method for properties of mixed crude oil |
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| CN105044050A (en) * | 2015-07-07 | 2015-11-11 | 中国农业大学 | Rapid quantitative analysis method for metallic elements in crop straw |
| CN105486658A (en) * | 2015-11-19 | 2016-04-13 | 江南大学 | Near-infrared physical property parameter measuring method without measuring point temperature compensation |
| WO2017084119A1 (en) * | 2015-11-19 | 2017-05-26 | 江南大学 | Near-infrared physical parameter measuring method having measuring-point-free temperature compensation function |
| WO2017084118A1 (en) * | 2015-11-19 | 2017-05-26 | 江南大学 | Method for correcting measuring-point-free temperature compensation model during online application of near infrared spectrum analyzer |
| 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 |
| CN115406857A (en) * | 2022-09-07 | 2022-11-29 | 山东天厚石油科技有限责任公司 | Crude oil organic chloride detection device and method for petroleum production |
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