CN1727877A - Method for measuring character data of gasoline from near infrared light spectrum - Google Patents
Method for measuring character data of gasoline from near infrared light spectrum Download PDFInfo
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- CN1727877A CN1727877A CNA2004100711194A CN200410071119A CN1727877A CN 1727877 A CN1727877 A CN 1727877A CN A2004100711194 A CNA2004100711194 A CN A2004100711194A CN 200410071119 A CN200410071119 A CN 200410071119A CN 1727877 A CN1727877 A CN 1727877A
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- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000001228 spectrum Methods 0.000 title claims description 28
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 11
- 238000004364 calculation method Methods 0.000 claims abstract description 7
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 41
- 238000012360 testing method Methods 0.000 claims description 30
- 238000010521 absorption reaction Methods 0.000 claims description 21
- 239000006096 absorbing agent Substances 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical group C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract 1
- 125000003342 alkenyl group Chemical group 0.000 abstract 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 abstract 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 238000011160 research Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000010276 construction Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 230000005477 standard model Effects 0.000 description 2
- 241001269238 Data Species 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 238000000611 regression analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
A method for determining data of gasoline property by near infrared spectrum includes determining near infrared spectrum of gasoline sample to be determined ; calculating out peak area corresponding to each following absorptive waveband as benzol ring C - H of 872.8 - 879.8nm , methyl C - H of 904.8 -907.8nm and 909.8 - 916.8 nm , methylene C - H of 932.8 - 934.8 nm and alkenyl C - H of 894.8 - 898.8 nm in spectrogram ; obtaining the coding figure as per above calculation ; obtaining property data of determined sample by comparing obtained coding figure to property figure stored in databank .
Description
Technical field
The present invention is the assay method of character data of gasoline, specifically, is the method that a kind of characteristic parameter of the near infrared spectrogram that utilizes gasoline sample is measured character data of gasoline, particularly octane value.
Background technology
Octane number is the index of the tolerance gasoline capability of antidetonance, and its size directly affects the performance of motor petrol.Increase octane number with the method for economical rationality and will produce huge economic benefit in oil refining process, people are from raw material, catalyzer, and aspects such as technology are constantly explored and are studied, and attempt to find the optimal path of raising octane number.Therefore, the measuring method of research octane number to the production of gasoline with use all with significant.
At present, octane value standard determination method ASTM D adopts ASTM-CFR octane number testing machine stand assay method, China adopts the standard method of test with ASTM D equivalence: GB/T 5487-1995 has stipulated the determination method of organon octane number, and GB/T 503-1995 has stipulated the determination method of motor method octane number.But, ASTM-CFR octane number testing machine stand assay method the production control of gasoline with use in be subjected to certain limitation: (1) test speed is slow, and an octane value is measured and needed more than 1 hour at least, can not in time feed back and carry out the production optimal control; (2) because the ASTM-CFR octane number testing machine is bulky, need special laboratory, be unfavorable for that on-the site analysis uses; (3) operation and maintenance expense height, the cost of equipment height needs continuous maintenance in the use; (4) feature of environmental protection is poor, and the sample consumption of test is big, needs the 500ml gasoline sample approximately, and measuring process exists volatilization loss and severe contamination.
Advantages such as it is fast that near-infrared spectral analytical method has speed, and precision height and expense are low have been widely used in measuring the octane value of gasoline, and have produced good social benefit and economic benefit thus.The spectrum of near-infrared spectral analysis technology by known sample is related with composition or character, sets up calibration model with the multivariate calibration methods in the Chemical Measurement, predicts the composition or the character of unknown sample then according to the spectrum of model and unknown sample.Disclose a kind of productive unit optimal control method as US5490085, this method is selected wave number 4800～4000cm
-1The near infrared absorption wave spectrum of scope working sample, by its spectral data by setting up multiple regression analysis, the near infrared spectral data of working sample is associated with its octane value, obtain the octane value of sample, and have the production run of predetermined octane value product by the sample octane value control of prediction.
But the broader applications of above-mentioned near-infrared spectral analysis technology are subjected to the restriction of modelling and maintenance.When this showed with near-infrared spectrum analysis mensuration octane number, owing to be subjected to the influence of raw material variation and processing technology, gasoline composition and variation thereof be complexity very.Form when differing greatly when gasoline, need set up different models respectively, set up the workload of model and very expensive it.At present, the method for also useful non-homing method prediction product property discloses a kind of prediction product property as US6070128, as the method for octane number, vapour pressure, gum level, sulfur content and other content of material.This method adopts the various character of contiguous index method prediction product.At first set up database by collecting a large amount of samples, each storehouse sample all has the various product property data of measuring with standard method, the ir data of the sample m that measures under similarity condition in the ir data of measuring at 600～2600nm place with sample and the storehouse calculates and is close to index then, and the minimal index used with determining the prediction product property in advance compared, choose the storehouse sample of the contiguous index of those correspondences less than minimal index, the average of the product property data that it is corresponding is the predicted value of the character data of unknown sample.This method is when the prediction octane number, and the characteristic measurement wavelength of choosing is more, reaches 17 wave bands, and each about 10～20nm in wave band wavelength interval.Therefore, calculating contiguous index, when choosing the storehouse sample and carrying out the product property prediction, the characteristic peak of near infrared spectrogram of determining sample seems complicated, loaded down with trivial details especially to determine calculating parameter.
Summary of the invention
The purpose of this invention is to provide a kind of by the near infrared ray character data of gasoline, the method of octane value particularly, this method need not be set up calibration model, and directly by the character data of near infrared wave spectrum characteristic absorption section parameter prediction gasoline sample, finding speed is fast, precision is high.
The method of the near infrared ray character data of gasoline that the inventive method provides comprises the steps:
(1) measures the near infrared spectrum of gasoline sample to be measured, calculate the spectrum peak area of following each absorption bands correspondence in the spectrogram: 1. phenyl ring C-H absorber portion, 872.8-879.8nm; 2. methyl C-H absorber portion, 904.8-907.8nm, 909.8-916.8nm; 3. methylene C-H absorber portion, 931.8-934.8nm; 4. thiazolinyl C-H absorber portion, 894.8-898.8nm; And calculate the coding numerical value of sample by each section peak area value,
(2) testing sample is encoded sample in numerical value and the sample data storehouse coding numerical value relatively, obtain the character data of testing sample by the character data of corresponding with it storehouse sample.
The present invention is the coding numerical value of Parameter Calculation sample with the characteristic peak area of four near infrared absorption wave bands of gasoline sample, and this numerical value is corresponding with the character data of this sample, sets up the database of standard model thus.When unknown sample is tested, only need to calculate its coding numerical value by the near-infrared spectra diagram data of this unknown sample, can be by the character data of the properties of samples data prediction unknown sample that has corresponding encoded numerical value in the database, thereby need not set up the standard model calibration curve, saved the workload of setting up forecast model.In addition,, have the sample of corresponding encoded numerical value fast in the searching database, make the properties of samples data prediction simple, quick, accurate according to the coding numerical value that four near infrared characteristic absorption wave band spectrum peak areas are set up.
Embodiment
The spectrum peak area value that the inventive method is extracted four characteristic absorption wave bands of sample near infrared spectrum is a characteristic parameter, calculate its coding numerical value by characteristic parameter by formula, set up the corresponding relation of coding numerical value and properties of samples data, and predict the character data of specimen thus.At first, collect gasoline sample that various processing technology produces several, decide on institute's database construction design capacity size.Be generally and make prediction accurately, need choose each 200～500 of the gasoline samples that various technologies produce, amount to about 200～1000 of gasoline sample data volume.Test the character data of each sample earlier with standard method, test its near infrared spectrogram again, calculate the coding numerical value of each sample by selected four characteristic peak areas, each coding numerical value is corresponding one by one with the SOME PROPERTIES data of this sample, thus, set up the topological database of sample encoded numerical value and its character data, measure the near infrared spectrum of unknown sample then, calculate the spectrum peak area value of four characteristic absorption wave bands, try to achieve its coding numerical value thus, by character data at the properties of samples data prediction unknown sample of database retrieval and unknown sample respective coding data.
In the inventive method, the formula of (1) described calculation sample coding numerical value of step (CODE) is:
CODE(i)=(α
i-1)×500
3+(Z
i-1)×500
2+(Y
i-1)×500+X
i
In the formula, X
i, Y
i, Z
i, α
iRespectively be sample i at 1.～4. spectrum peak area value of absorption bands.
When the coding numerical value of a certain sample in the sample data storehouse was identical with testing sample coding numerical value, then the character data of this sample was the character data of testing sample.
When not having the sample not identical in the sample data storehouse with testing sample coding numerical value, then getting search length is 1～3, retrieval and the contiguous sample of testing sample coding numerical value in the sample data storehouse, again by contiguous sample at 1.～4. spectrum peak area value of absorption bands, calculate the character data of testing sample by following formula:
Wherein
In the formula, n is the contiguous storehouse sample number that searches, P
iIt is the character data of i contiguous storehouse sample;
X
i, Y
i, Z
i, α
iBe i contiguous storehouse sample at 1.～4. spectrum peak area value of absorption bands, X
u, Y
u, Z
u, α
uFor testing sample at 1.～4. spectrum peak area value of absorption bands.
Described search length r is the contiguous storehouse sample chosen and the testing sample absolute value in the spectrum peak area difference of same absorbent wave band.Promptly
r＝|M
j-M
u|
In the formula, M
iFor contiguous storehouse sample j at 1.～4. spectrum peak area value of absorption bands, M
jBe X
j, Y
j, Z
jOr α
j, M
uBe the spectrum peak area value of testing sample at the absorption bands identical, M with j
uBe X
u, Y
u, Z
uOr α
u
The suitable gasoline sample of measuring of the inventive method is reformed gasoline or catalytically cracked gasoline, also can be the gasoline component that other technology produces, as gasoline alkylate, coker gasoline etc.
When the gasoline of measuring is reformed gasoline or gasoline alkylate because wherein the content of alkene is few, during calculation sample coding numerical value, but the 4. the spectrum peak area assignment of wave band be zero, to simplify calculation procedure.
The sample size that is used to set up the sample data storehouse in the inventive method can be 100～10000, and preferred 200-1000, sample should comprise the gasoline sample that various technologies produce in the storehouse, and the quantity of every kind of gasoline sample needs 100～500 approximately.
Coding method of the present invention is applicable to the various character datas of measuring gasoline sample, as octane number, density, vapour pressure, sulfur content, gum level or arene content.
Below by example in detail the present invention, but the present invention is not limited to this.
Set up the sample data storehouse: adopt NIR-3000 near-infrared analyzer (production of the virtuous instrument of Beijing English Industrial Co., Ltd.), with the air is reference, under 22 ± 5 ℃ condition, measure the near infrared spectrum of 208 reformed oil samples and 476 catalytically cracked gasoline samples, again by the research octane number (RON) (RON) of GB/T 5487 method working samples, by the motor octane number of GB/T 503 method working samples.Calculating the coding numerical value of each sample by the inventive method by the spectrum peak area value of described four absorption bandses, is that record data are set up database by coding numerical value and its corresponding octane value, the octane value of unknown sample is predicted being used for.
Example 1
This example is predicted the octane value that generates oil samples of reforming by institute's database construction, measure the near infrared spectrum of each reformed oil sample to be measured earlier, wherein the 4. the peak area assignment of wave band be zero, by 1. described～3. the spectrum peak area value of absorption bands calculates the coding numerical value of each sample.Retrieval has the sample of corresponding encoded numerical value in database then, and search length is 3, and the octane value of the formula prediction testing sample that is provided by the present invention by the octane value of sample the results are shown in Table 1 again.
As shown in Table 1, t check numbers illustrated between the result that the inventive method and GB/T 5487-1995 actual measurement obtains does not have significant difference between the two, and the difference between the inventive method and standard testing method is better than the repeatability of GB/T 5487-1995 gasoline research method octane number determination law regulation.
Example 2
This example is predicted the octane value of catalytically cracked gasoline sample by institute's database construction.Measure earlier the near infrared spectrum of each catalytically cracked gasoline sample to be measured, by 1. described～4. the spectrum peak area value of absorption bands calculates the coding numerical value of each sample.Retrieval has the sample of corresponding encoded numerical value in database then, and search length is 3, and the octane value of the formula prediction testing sample that is provided by the present invention by the octane value of sample the results are shown in Table 2 again.
As shown in Table 2, do not have significant difference between the t check numerical value between the result that the inventive method and GB/T 5487-1995 and GB/T 503-1995 actual measurement obtain, and the difference between the inventive method and standard testing method is better than the repeatability of GB/T 5487-1995 gasoline research method knock rating method and GB/T 503-1995 gasoline motor octane number determination method regulation.
Example 3
Under the same measured condition, to catalytically cracked gasoline and reformed oil sample, METHOD FOR CONTINUOUS DETERMINATION is 6 times respectively, and by institute's database construction the octane value of sample is predicted, the results are shown in Table 3.
As known from Table 3, the sample octane value that gets of the inventive method forecasting institute has better repeatability.
Table 1
| Sample number into spectrum | Coding numerical value | Research octane number (RON) | ||
| Actual value | Predicted value | Difference | ||
| 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 | 5128635 44095058 7878150 14614599 8628659 20362093 19872582 10118640 29606577 17109107 9121172 9372628 1012366 14125065 17117612 37099555 13122117 7376648 7877644 21609091 24612088 7624163 1511262 14872624 8124142 3285208 6123122 6627655 3060456 3285259 1711151 8124142 | 100.5 101.1 102.4 100.9 102.8 103.0 101.3 100.8 101.6 101.8 101.6 102.7 103.0 102.7 101.7 102.0 102.1 103.3 101.9 102.7 101.4 101.7 101.3 101.3 102.6 102.0 101.3 100.9 102.4 102.8 101.8 101.0 | 100.8 100.7 102.4 101.2 102.5 102.2 101.9 101.6 101.1 101.6 101.3 103.2 102.8 102.7 102.7 101.5 102.2 103.1 101.2 102.3 101.6 101.6 101.0 100.8 101.8 102.5 101.9 100.8 101.8 102.3 102.1 101.4 | 0.3 -0.4 0.0 0.3 -0.3 -0.8 0.6 0.8 -0.5 -0.2 -0.3 0.5 -0.2 0.0 1.0 -0.5 0.1 -0.2 -0.7 -0.4 0.2 -0.1 -0.3 -0.5 -0.8 0.5 0.6 -0.1 -0.6 -0.5 0.3 0.4 |
| Standard deviation t t (0.05，31) | 0.48 0.66 2.04 | |||
Table 2
| Sample number into spectrum | Coding numerical value | Research octane number (RON) | Motor octane number | ||||
| Actual value | Predicted value | Difference | Actual value | Predicted value | Difference | ||
| 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 | 6426047047 5910792054 5904297533 6036550032 6550546048 6035299031 6680047547 6161800030 7428052115 7291799135 7033544157 7159044655 3757761776 5646295032 5272794032 6292047531 6422299531 6678551031 5906548028 6041049030 6419800028 5782048529 6675301527 6035298526 6533541566 | 94.3 94.2 91.0 94.1 93.0 92.0 91.8 90.8 92.0 91.4 91.0 91.8 91.8 91.9 92.0 91.8 91.6 92.0 92.0 92.1 91.3 91.9 97.7 95.4 95.4 | 95.1 95.1 91.7 94.0 93.1 91.9 91.8 91.3 91.7 91.5 91.4 91.6 91.9 91.7 91.9 91.6 91.9 91.9 91.9 92.4 91.3 91.2 97.5 94.7 94.8 | 0.8 0.9 0.7 -0.1 0.1 -0.1 0.0 0.5 -0.3 0.1 0.4 -0.2 0.1 -0.2 -0.1 -0.2 0.3 -0.1 -0.1 0.3 0.0 -0.7 -0.2 -0.7 -0.6 | 84.8 84.8 81.4 80.6 80.7 80.9 80.4 80.2 80.1 80.4 80.4 80.1 80.5 80.7 80.8 80.6 80.9 81.2 81.3 80.5 80.5 80.4 86.7 80.0 80.0 | 85.1 85.1 81.3 80.6 80.8 80.7 80.2 80.5 80.2 80.3 80.2 79.9 80.7 80.4 80.8 80.2 80.8 80.8 80.9 80.1 80.3 80.2 86.4 80.4 80.0 | 0.3 0.3 -0.1 0.0 0.1 -0.2 -0.2 0.3 0.1 -0.1 -0.2 -0.2 0.2 -0.3 0.0 -0.4 -0.1 -0.4 -0.4 -0.4 -0.2 -0.2 -0.3 0.4 0.0 |
| Standard deviation t t (0.05，24) | 0.42 0.29 | 2.06 | 0.25 1.76 | ||||
Table 3
Claims (8)
1, a kind of method by the near infrared ray character data of gasoline comprises the steps:
(1) measures the near infrared spectrum of gasoline sample to be measured, calculate the spectrum peak area of following each absorption bands correspondence in the spectrogram: 1. phenyl ring C-H absorber portion, 872.8-879.8nm; 2. methyl C-H absorber portion, 904.8-907.8nm, 909.8-916.8nm; 3. methylene C-H absorber portion, 931.8-934.8nm; 4. thiazolinyl C-H absorber portion, 894.8-898.8nm; And calculate the coding numerical value of sample by each section peak area value,
(2) testing sample is encoded sample in numerical value and the sample data storehouse coding numerical value relatively, obtain the character data of testing sample by the character data of corresponding with it storehouse sample.
2,, it is characterized in that (1) step formula of described calculation sample coding numerical value is according to the described method of claim l:
CODE(i)＝(α
i-1)×500
3+(Z
i-1)×500
2+(Y
i-1)×500+X
i
In the formula, X
i, Y
i, Z
i, α
iRespectively be sample i at 1.～4. spectrum peak area value of absorption bands.
3,, it is characterized in that then the character data of this sample is the character data of testing sample when the coding numerical value of a certain sample in the sample data storehouse is identical with testing sample coding numerical value according to the described method of claim l.
4, in accordance with the method for claim 1, it is characterized in that when not having the sample not identical in the sample data storehouse with testing sample coding numerical value, then getting search length is 1～3, retrieval and the contiguous sample of testing sample coding numerical value in the sample data storehouse, again by contiguous sample at 1.～4. spectrum peak area value of absorption bands, calculate the octane value of testing sample by following formula:
Wherein
In the formula, n is the contiguous storehouse sample number that searches, P
iIt is the character data of i contiguous storehouse sample;
X
i, Y
i, Z
i, α
iRespectively be i contiguous storehouse sample at 1.～4. spectrum peak area value of absorption bands, X
u, Y
u, Z
u, α
uRespectively be testing sample at 1.～4. spectrum peak area value of absorption bands.
5, in accordance with the method for claim 1, it is characterized in that described gasoline sample is reformed gasoline or catalytically cracked gasoline.
6, in accordance with the method for claim 1, when it is characterized in that described gasoline is reformed gasoline, during calculation sample coding numerical value, the 4. wave band spectrum peak area assignment be zero.
7, in accordance with the method for claim 1, the quantity that it is characterized in that sample in the described sample data storehouse is 100～10000.
8, in accordance with the method for claim 1, it is characterized in that described character data of gasoline is octane value, density, vapour pressure, sulfur content, gum level or the arene content of gasoline.
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| CN1727877A true CN1727877A (en) | 2006-02-01 |
| CN100425975C CN100425975C (en) | 2008-10-15 |
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| CN101893560A (en) * | 2010-07-13 | 2010-11-24 | 中国人民解放军总后勤部油料研究所 | Method for quickly determining manganese content in gasoline |
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| CN101995389B (en) * | 2009-08-27 | 2012-07-18 | 中国石油化工股份有限公司 | Method for fast recognition of crude oil variety through near infrared spectrum |
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| US5572030A (en) * | 1994-04-22 | 1996-11-05 | Intevep, S.A. | Method for determining parameter of hydrocarbon |
| EP0706049A1 (en) * | 1994-10-07 | 1996-04-10 | Bp Chemicals S.N.C. | Cracking property determination |
| WO1996018881A1 (en) * | 1994-12-13 | 1996-06-20 | Exxon Research & Engineering Company | Non linear multivariate infrared analysis method |
| US5512751A (en) * | 1994-12-19 | 1996-04-30 | Uop | Calibration of NIR spectra in measuring properties of petroleum products |
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| CN102998276A (en) * | 2011-09-15 | 2013-03-27 | 中国石油化工股份有限公司 | Method for determining crude oil true boiling point distillation curve by using infrared spectroscopy |
| CN102998276B (en) * | 2011-09-15 | 2015-09-23 | 中国石油化工股份有限公司 | By the method for infrared spectrum measurement true boiling point curve of crude oil |
| CN103033592A (en) * | 2012-12-13 | 2013-04-10 | 清华大学 | Measuring method and device for measuring detonation resistance property of fuel |
| CN103033592B (en) * | 2012-12-13 | 2014-12-31 | 清华大学 | Measuring method and device for measuring detonation resistance property of fuel |
| CN103237078A (en) * | 2013-04-27 | 2013-08-07 | 翁整 | Near-infrared food safety identification system |
| CN103760131A (en) * | 2014-01-17 | 2014-04-30 | 华东理工大学 | Real-time gasoline product attribute prediction method based on near infrared spectrum detection |
| CN109073541A (en) * | 2018-08-01 | 2018-12-21 | 深圳达闼科技控股有限公司 | A kind of data adding method, device and the detection device of substance Test database |
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