CN109030449A - A kind of lubricating oil and mixture ratio of fuel to oil rapid detection method - Google Patents
A kind of lubricating oil and mixture ratio of fuel to oil rapid detection method Download PDFInfo
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Abstract
The present invention provides a kind of lubricating oil and mixture ratio of fuel to oil rapid detection method, belong to aero-engine field.This method comprises: step 1: obtaining test sample from suspecting to be mixed in the lubricating oil sample of fuel oil；Step 2: carrying out Raman spectrum test to test sample, the Raman spectrum curve of test sample is obtained；It is eliminated the Raman spectrum curve after back end step 3: carrying out processing to the Raman spectrum curve of test sample；Step 4: reading the peak value of characteristic peak on eliminating the Raman spectrum curve after back end；Step 5: obtaining the lubricating oil and mixture ratio of fuel to oil of test sample using the peak value of the characteristic peak.Lubricating oil and mixture ratio of fuel to oil can be quickly detected using the method for the present invention, 3-10 milliliters need to be only obtained and suspect the sample being mixed, test can be completed in 3-5 minutes, testing efficiency is substantially increased, has ensured flight safety.
Description
Technical field
The invention belongs to aero-engine fields, and in particular to a kind of lubricating oil and mixture ratio of fuel to oil rapid detection method,
Mixing ratio for rapid quantitative detection lubricating oil and aviation kerosine mixture.
Background technique
Aero-engine is mainly equipped with the Oil system of three types at present, is that Aviation Fuel (aviation kerosine) supplies respectively
To system, lubricating oil (lubricating oil) feed system and hydraulic oil feed system.It is simultaneously raising fuel efficiency, CFM56 engine etc.
It is provided with the heat-exchange system of lubricating oil and fuel oil on the outside of fan bulkhead, while cooling lubricating oil, improves the combustion for entering combustion chamber
Oil temperature improves efficiency of combustion.But due to heat-exchange system failure and other accidental situations or other reasons, lead to lubricating oil
It is mixed with fuel oil.When being mixed into lubricating oil in fuel system, lubricating oil enters combustion system, and harm is little.When fuel oil enters cunning
When oil system, since the molecular weight of fuel oil is smaller, mostly short chain molecule structure.Bearing, gear etc. need lubricating component to use
Lubricating oil, then mainly based on long-chain molecule.Fuel oil is mixed into the decaying and deterioration for leading to greasy property, causes localized hyperthermia,
Lead to engine bearing or gear locking, endangers flight safety.
Current aero-oil method for testing performance mainly has acidity detection method (the ASTM D664- based on electrometric titration
2017, national standard GB/T 7304-2014) (it can refer to document " Standard Test Method for Acid Number of
" petroleum produces for Petroleum Products By Potentiometric Tritration, ASTM D664-2017 " and document
The spotting titration of product acid value, national standard GB/T 7304-2014 ")；Water content test method based on Coulomb equation
(ASTM D6304-2016e, GB/T 11133-2015) (can refer to document " Standard Test Method for
Determination of Water in Petroleum Products,Lubricating Oils,and Additives
By Coulometric Karl Fischer Titration.ASTM D6304-2016e " and document " oil product, lubricating oil
With the measurement karl Fischer Coulomb equation of water content in additive, GB/T 11133-2015 ")；Based on energy dispersion X-ray
The petroleum of fluorescent spectrometry and the measuring method (ASTM D4294-2016e, GB/T 17040-2008) of oil product sulfur content；
Lubricate oil whip particular assay method (ASTM D892-2013, GB/T 12579-2002) and viscosity measurement method (ASTM
D2270-10).Being mixed into fuel oil in new lubricating oil is pole incident, consults other data, can not measure in lubricating oil rapidly
The method for being mixed into fuel ratio continues to use the lubricating oil, will lead to lubricating oil performance and decays rapidly, endangers flight safety.
Summary of the invention
It is an object of the invention to solve above-mentioned problem existing in the prior art, a kind of lubricating oil and fuel oil mixing are provided
Both than rapid detection method, by the optic spectrum line of Raman spectrum rapid survey fuel oil and lubricating oil mixture, and calculate rapidly
Content ratio.
The present invention is achieved by the following technical solutions:
A kind of lubricating oil and mixture ratio of fuel to oil rapid detection method, comprising:
Step 1: obtaining test sample from suspecting to be mixed in the lubricating oil sample of fuel oil；
Step 2: carrying out Raman spectrum test to test sample, the Raman spectrum curve of test sample is obtained；
It is eliminated the Raman spectrum curve after back end step 3: carrying out processing to the Raman spectrum curve of test sample；
Step 4: reading the peak value of characteristic peak on eliminating the Raman spectrum curve after back end；
Step 5: obtaining the lubricating oil and mixture ratio of fuel to oil of test sample using the peak value of the characteristic peak.
The operation of the first step includes:
3-10ml sample is taken out as test sample from suspecting to be mixed in the lubricating oil sample of fuel oil.
The operation of the second step includes:
The test sample is transferred in the liquid sample pool of Raman spectrometer, starting Raman spectrometer is tested；
After test, the Raman spectrum curve of test sample is read from Raman spectrometer.
The operation of the third step includes:
Ambient noise is removed using Raman spectrum curve of the adaptive iteration least square method to test sample to handle,
Raman spectrum curve after the back end that is eliminated.
The operation of 4th step includes:
The spectrum peak at the position 1750cm-1 is found on eliminating the Raman spectrum curve after back end, using the spectrum peak as
Characteristic peak；
The peak value of the characteristic peak is read, the peak value refers to peak value or peak area value.
The operation of 5th step includes:
The peak value that will test the characteristic peak of sample is updated in mixing ratio mathematical model, obtains the lubrication of test sample
Oil and mixture ratio of fuel to oil；
What the mixing ratio mathematical model was obtained by:
(A) lubricating oil and fuel oil mixture of the different mixing ratios of n group are prepared；The n is more than or equal to 3；
(B) Raman spectrum test is carried out to every group of mixture respectively, obtains the Raman spectrum curve of every group of mixture；
(C) handled to obtain the Raman after the elimination back end of every group of mixture to the Raman spectrum curve of every group of mixture
The curve of spectrum；
(D) peak value that characteristic peak is read on the Raman spectrum curve after the elimination back end of every group of mixture, by n group feature
The peak value at peak is as n data point；
(E) the n data point is fitted to obtain mixing ratio mathematical model.
Preferably, the n is 7 to 10.
The operation of (C) step includes:
It is removed at ambient noise using Raman spectrum curve of the adaptive iteration least square method to every group of mixture
Reason, the Raman spectrum curve after obtaining the elimination back end of every group of mixture.
It is set a song to music in the third step and (C) step using Raman light of the adaptive iteration least square method to test sample
Raman spectrum curve when being handled of line, every group of mixture, solved using identical control the smoothness of back end parameter,
The identical parameter for solving back end order.
The operation of the step (D) includes:
The spectrum peak at the position 1750cm-1 is found on the Raman spectrum curve after the elimination back end of every group of mixture, it will
Characteristic peak of the spectrum peak as this group of mixture；
The peak value of the characteristic peak of every group of mixture is read, the peak value refers to peak value or peak area value；
Using the peak value of n group characteristic peak as n data point.
The operation of the step (E) includes:
p1=f (n1)；
p2=f (n2)；
…
pn=f (nn)；
Wherein, n1,n2…nnFor the mixing ratio of each group mixture, P1,P2…PnFor the corresponding characteristic peak of each group mixture
Peak value；
Above-mentioned n data point is fitted to obtain mixing ratio mathematical model:
nx=f-1(px)；
Wherein, nxFor the mixing ratio of test sample, PxFor the peak value of the corresponding characteristic peak of test sample.
Compared with prior art, the beneficial effects of the present invention are:
Lubricating oil and mixture ratio of fuel to oil can be quickly detected using the method for the present invention, need to only obtain 3-10 milliliters of suspection hairs
Raw mixed sample can complete test in 3-5 minutes, substantially increase testing efficiency, ensure flight safety.
Detailed description of the invention
Raman spectrum containing 1% fuel oil in Fig. 1 lubricating oil
Fig. 2 initial data removes back end process schematic
The Raman spectrum curve for the different proportion mixture that Fig. 3 is successively obtained
Fig. 4 obtains the algorithm of label fuel oil content using exponential function fitting measurement data curve
The schematic diagram of Fig. 5 the method for the present invention.
Specific embodiment
Present invention is further described in detail with reference to the accompanying drawing:
The present invention is detected rapidly by the method for design using Raman spectrum detection device and calibrates lubricating oil and boat
Mixed proportion when empty kerosene is mixed.
Raman spectrum is a kind of scattering spectrum technology, is that the scattering spectrum different to incident light frequency is analyzed, with
The vibration information of nonpolar symmetrical structure into molecular structure, to be applied to the research of molecular structure.Due to Raman spectrum
The high efficiency of optical analysis, simultaneously because same sample, the displacement of Raman line and the wavelength of incident light are unrelated, only and sample
Vibration-rotation energy level is related, therefore the universality of Raman spectrum is preferable.Raman spectroscopy is gradually applied to safe prison in recent years
Survey intermediate item.
The method of the present invention obtains different proportion sample standard sample firstly the need of using the mixture for having determining ratio
Raman map establishes different proportion pair using peak height data or peak area data then using the characteristic peak of ingredient in lubricating oil
Algorithm (the characteristic peak height or face according to the image-forming principle of Raman spectrum, when light path is identical, in different proportion sample answered
Long-pending and mixing ratio existence function relationship, the algorithm are to solve for the process of this functional relation).It is finally solved and is appointed using the algorithm
In meaning sample, the ratio value of blended fuel oil.As shown in figure 5, mainly having following steps and algorithm.
1, sample link
Detection method of the present invention only needs in suspecting the lubricating oil sample for being mixed with fuel oil, takes out 3-10ml sample
Sample is transferred to a kind of liquid sample pool (appearance for liquid testing of Raman spectrometer as test sample by product after sampling
Device, capacity are about 3ml) in.
2. detection
According to the program of Raman spectrometer proper testing fluid sample, carry out test job.After the completion of test, from Raman light
The data read in spectrometer are as shown in Figure 1, due to the influence by fluorescence back end, which cannot be directly used to solve, therefore
It is a curve to be treated.
3. spectral filtering algorithm
Fig. 1 is that the common lubricating oil of aero-engine (Mobil Jet oil II) has been mixed into the aviation kerosine of 1% content
The Raman spectrum curve of mixture.The left end of curve is gradually weakened to right end back end peak, accurate to calculate, and should eliminate back first
Influence of the bottom to peak value.Here using adaptive iteration least square method, (this method is a kind of typical number for removing ambient noise
According to Processing Algorithm, it is to find mean square deviation by the curvature feature of the automatic accommodation curve of continuous alternative manner in solution procedure
The method of the smallest back end curve, to acquire the truthful data after eliminating noise or interference.) remove back end, the thick song in Fig. 2
Line is initial data, and fine line is the back end for needing to remove, and medium curve is the Raman spectrum data eliminated after back end.This method
The middle algorithm for eliminating back end is that one of source for introducing error (selects different parameters that can also introduce error, but selects identical
After parameter, then curve matching is done, fractional error can be eliminated.), adaptive iteration least square method is more commonly used (can also to adopt
With polynomial regression algorithm eliminate back end, but the experimental results showed that, polynomial regression algorithm be not so good as adaptive iteration least square
The effect of method is good, and it is advantageous to the solutions of adaptive iteration least square method), but parameter therein should be consistent, adaptively
When interative least square method solves, there are two parameter in algorithm, one is the parameter for controlling the smoothness for solving back end, and one is
The parameter for solving back end order should use unified parameter (i.e. to multiple groups when carrying out data processing to multicomponent sample
When sample being divided to be handled, same control is used to solve the parameter of the smoothness of back end, the ginseng of same solution back end order
Number), different back ends solves parameter and (solves the parameter of the smoothness of back end including control and solve the parameter of back end order) meeting
The curve obtained is caused to have a certain range of difference, to have certain influence to the peak height of Raman spectrum and peak area.
To being simply described below for adaptive iteration least square method:
Assuming that x is the n dimensional vector that former spectrum is constituted, z is fitting vector.Generalized variable Q by z to the fidelity of z and z from
The Background roughness of body determines that expression formula is as follows:
Q=F+ λ R=| x-z |2+λ|Dz|2 (1)
Wherein, fidelity F is the difference of two squares of z and x；Background roughness R is first derivative (D) quadratic sum of z；λ is balance
Coefficient, value is bigger, and fitting vector is more smooth.Diagonal matrix W is introduced in fidelity, the value on diagonal line is weight wi, and
Seek the least effective solution of equation (1), that is, Q differentiates null solution to z:
Z=(W+ λ DTD)-1Wx (2)
W is set by the corresponding weight of characteristic peak in equation (2)k=0, z are baseline back end vector.Weight vectors w can
Logical iteration obtains, and presetting primary iteration is w0=1, the weight expression formula of the t times iteration are as follows:
dtFor vector (w-zT-1) in the sum of negative value element.By the fitting vector z of (t-1) secondary iterationT-1As candidate base
Line.When iteration result meets following discriminate, iteration ends export baseline results.
Wherein, xiFor each element in former spectral vector.
Fig. 3 is the Raman spectrogram for concentrating the mixture of 7 kinds of different proportions, curve from top to bottom are as follows: pr1, pr5,
Pr10, pr15, pr20 and pr50 are respectively the samples of lubricant oil for containing 1%, 5%, 10%, 15%, 20% and 50% aviation kerosine
The Raman curve of product；Pr100 is the Raman curve of 100% aviation kerosine.The peak value in picture is compared it can be found that 1750cm-1
There is the spectrum peak gradually decreased in position (i.e. the position marked in Fig. 4 with ellipse).The peak corresponds to hydroxyl C=in lipid material
The stretching vibration peak of O.The substance is not present in aviation kerosine.And it is based on Raman image principle, the substance in light path
Concentration is bigger, and the intensity at peak is higher.
4, establish mixing ratio algorithm
Using the spectrum peak of the position 1750cm-1 as labelled amount, peak value or peak area value can be taken.It is calculated using mathematics
Method, choosing the peak value, (peak height is usually the maximum value for passing through function and solving in a certain range curve (near 1750cm-1), peak face
Product is to solve for the integrated value of the curve of spectrum in a certain range.), (what is listed in Fig. 4 is that peak height solves as shown in data point in Fig. 4
Process, if it is about the same for solving curve using peak area value.).
The acquisition process of mathematical model is as follows:
Artificially preparing n group first, (n should be greater than the number for solving parameter in generation in data fitting, be generally higher than equal to 3 and be
Can, preferably 7-10 has 7 groups of data in the present embodiment, then n=7) mixture of different proportion, Raman spectrum test is then carried out,
The result of test is carried out respectively to eliminate back end processing (it is recommended that using adaptive iteration least square method), all spectrum test knots
The method (mainly parameter) that fruit eliminates back end is consistent.Then peak near characteristic spectrum information, that is, 1750cm-1 is extracted
Peak height or peak area information, Pn,
p1=f (n1)；
p2=f (n2)；
…
pn=f (nn)；
Wherein, n1,n2…nnFor the mixing ratio of each group mixture, P1,P2…PnFor the corresponding characteristic peak of each group mixture
Peak value；
Using above-mentioned truthful data, after obtaining function f (x) by fitting, in the sample for encountering non-principal component, with same
Method carries out Raman spectrum test, then carries out identical elimination back end to test result and handles, finally obtains characteristic peak, bring into
Following formula solves the content n of mixturex。
nx=f-1(px)；
In upper formula, nxFor unknown mixed proportion, PxThe spectrum peak obtained for test.
There are 7 groups of data in Fig. 4, is the peak value of 7 groups of component ratios and character pair peak respectively.The method of fitting data point has
It is a variety of, such as can be using exponential function come fitting data point:
Y=e(ax)+b (5)
Wherein a and b is the parameter to be solved, and x is mixed proportion, and y is characterized peak value.Here there are 7 groups of (x, y) data.
It can also be using quadratic equation with one unknown come fitting data point:
Y=ax2+bx+c
Wherein a, b and c are the parameter to be solved, and x is mixed proportion, and y is characterized peak value.Here there are 7 groups of (x, y) data.
The curve obtained by fitting data point is as shown in figure 4, the peak height that the data point markers in Fig. 4 are test measurement
Value；Curve is the change curve of the peak value and content after fitting.Functional relation corresponding to the curve, as calculating lubricating oil fuel oil
The mathematical model of mixed proportion.
When mixed crude sample type determines, it is only necessary to prepare one group of sample in advance, finds out the mathematical model,
It is directly solved later using this mathematical model.The ingredient of Aviation Fuel and lubricating oil is relatively fixed, and variation is little.
5 subsequent measurements
When needing to measure mixture (mixture of lubricating oil and fuel oil) of unknown concentration, using step 1-3, measurement mixing
The Raman spectrum curve of object, after filtering out back end, read near the position 1750cm-1 (this range is not unique, as long as across
All can be in the hope of arriving on the both sides of 1750cm-1) peak heights.Then peak value is brought into mathematical model, obtains the peak height
Corresponding concentration is spent, the concentration of mixed fuel oil as in mixture.
Using the mixture of universal aeroengine oil (Mobil Jet oil II) and aviation kerosine, Fig. 1-Fig. 4 is to adopt
The process of founding mathematical models is realized with the method for the present invention, the error of the mathematical model is within 5%.In numerical analysis method
In, when obtaining functional relation using multicomponent given data, calculation procedure can obtain the error of the data, the i.e. mistake of mathematical model
Difference.Because n can obtain best (the i.e. total error of 7 groups of data when carrying out numerical analysis much larger than unknown parameter
It is minimum) a, then b value is brought into n group data, can obtain worst error.Known component data are more, and the value is smaller, but
It will not continue to reduce after reaching certain numerical value.
Above-mentioned technical proposal is one embodiment of the present invention, for those skilled in the art, at this
On the basis of disclosure of the invention application method and principle, it is easy to make various types of improvement or deformation, be not limited solely to this
Invent method described in above-mentioned specific embodiment, therefore previously described mode is only preferred, and and do not have limitation
The meaning of property.
Claims (10)
1. a kind of lubricating oil and mixture ratio of fuel to oil rapid detection method, it is characterised in that: the lubricating oil and mixture ratio of fuel to oil are fast
Fast detection method includes:
Step 1: obtaining test sample from suspecting to be mixed in the lubricating oil sample of fuel oil；
Step 2: carrying out Raman spectrum test to test sample, the Raman spectrum curve of test sample is obtained；
It is eliminated the Raman spectrum curve after back end step 3: carrying out processing to the Raman spectrum curve of test sample；
Step 4: reading the peak value of characteristic peak on eliminating the Raman spectrum curve after back end；
Step 5: obtaining the lubricating oil and mixture ratio of fuel to oil of test sample using the peak value of the characteristic peak.
2. lubricating oil according to claim 1 and mixture ratio of fuel to oil rapid detection method, it is characterised in that: the first step
Operation include:
3-10ml sample is taken out as test sample from suspecting to be mixed in the lubricating oil sample of fuel oil；
The operation of the second step includes:
The test sample is transferred in the liquid sample pool of Raman spectrometer, starting Raman spectrometer is tested；
After test, the Raman spectrum curve of test sample is read from Raman spectrometer.
3. lubricating oil according to claim 2 and mixture ratio of fuel to oil rapid detection method, it is characterised in that: the third step
Operation include:
Ambient noise is removed using Raman spectrum curve of the adaptive iteration least square method to test sample to handle, and is obtained
Raman spectrum curve after eliminating back end.
4. lubricating oil according to claim 3 and mixture ratio of fuel to oil rapid detection method, it is characterised in that: the 4th step
Operation include:
The spectrum peak at the position 1750cm-1 is found on eliminating the Raman spectrum curve after back end, using the spectrum peak as feature
Peak；
The peak value of the characteristic peak is read, the peak value refers to peak value or peak area value.
5. lubricating oil according to claim 4 and mixture ratio of fuel to oil rapid detection method, it is characterised in that: the 5th step
Operation include:
The peak value that will test the characteristic peak of sample is updated in mixing ratio mathematical model, obtain test sample lubricating oil and
Mixture ratio of fuel to oil；
What the mixing ratio mathematical model was obtained by:
(A) lubricating oil and fuel oil mixture of the different mixing ratios of n group are prepared；The n is more than or equal to 3；
(B) Raman spectrum test is carried out to every group of mixture respectively, obtains the Raman spectrum curve of every group of mixture；
(C) handled to obtain the Raman spectrum after the elimination back end of every group of mixture to the Raman spectrum curve of every group of mixture
Curve；
(D) peak value that characteristic peak is read on the Raman spectrum curve after the elimination back end of every group of mixture, by n group characteristic peak
Peak value is as n data point；
(E) the n data point is fitted to obtain mixing ratio mathematical model.
6. lubricating oil according to claim 5 and mixture ratio of fuel to oil rapid detection method, it is characterised in that: the n arrives for 7
10。
7. lubricating oil according to claim 5 and mixture ratio of fuel to oil rapid detection method, it is characterised in that: (C)
The operation of step includes:
Ambient noise is removed using Raman spectrum curve of the adaptive iteration least square method to every group of mixture to handle, and is obtained
Raman spectrum curve to after the elimination back end of every group of mixture.
8. lubricating oil according to claim 7 and mixture ratio of fuel to oil rapid detection method, it is characterised in that: in the third
Drawing in step and (C) step using adaptive iteration least square method to the Raman spectrum curve of test sample, every group of mixture
When the graceful curve of spectrum is handled, using the parameter of the smoothness of identical control solution back end, identical solution back end rank
Several parameters.
9. lubricating oil according to claim 5 and mixture ratio of fuel to oil rapid detection method, it is characterised in that: the step
(D) operation includes:
The spectrum peak at the position 1750cm-1 is found on the Raman spectrum curve after the elimination back end of every group of mixture, by the light
Characteristic peak of the spectral peak as this group of mixture；
Read the peak value of the characteristic peak of every group of mixture；
Using the peak value of n group characteristic peak as n data point.
10. lubricating oil according to claim 5 and mixture ratio of fuel to oil rapid detection method, it is characterised in that: the step
(E) operation includes:
p1=f (n1)；
p2=f (n2)；
…
pn=f (nn)；
Wherein, n1,n2…nnFor the mixing ratio of each group mixture, P1,P2…PnFor the peak value of the corresponding characteristic peak of each group mixture；
Above-mentioned n data point is fitted to obtain mixing ratio mathematical model:
nx=f-1(px)；
Wherein, nxFor the mixing ratio of test sample, PxFor the peak value of the corresponding characteristic peak of test sample.
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| CN113655050A (en) * | 2021-08-17 | 2021-11-16 | 南京富岛信息工程有限公司 | Method for improving Raman spectrum detection limit of trace crude oil in light oil |
| CN113655050B (en) * | 2021-08-17 | 2024-04-26 | 南京富岛信息工程有限公司 | Method for improving Raman spectrum detection limit of trace crude oil in light oil |
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