CN106153561A - The many metal ion inspections of uv-vis spectra based on wavelength screening - Google Patents
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- 238000012216 screening Methods 0.000 title claims abstract description 33
- 229910021645 metal ion Inorganic materials 0.000 title claims abstract description 17
- 238000007689 inspection Methods 0.000 title claims abstract description 11
- 238000002371 ultraviolet--visible spectrum Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 50
- 238000002835 absorbance Methods 0.000 claims abstract description 17
- 150000002500 ions Chemical class 0.000 claims abstract description 13
- 238000001228 spectrum Methods 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 238000005070 sampling Methods 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 4
- 238000000342 Monte Carlo simulation Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 238000001514 detection method Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 238000012614 Monte-Carlo sampling Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010187 selection method Methods 0.000 description 2
- 230000003044 adaptive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000010238 partial least squares regression Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N21/3151—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths using two sources of radiation of different wavelengths
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N2021/3155—Measuring in two spectral ranges, e.g. UV and visible
Abstract
The present invention discloses a kind of many metal ion inspections of uv-vis spectra based on wavelength screening, can rapidly and efficiently reject redundancy and interference wavelength information, reduce wavelength screening time, and improve precision and the robustness of model.Described method includes: S1, obtains with UV, visible light spectra photometric method and comprises the solution of many kinds of metal ions in 400 700nm full wave mixing absorbance；The absorbance obtaining is sampled by S2, employing Multiple Cycle DSMC, uses decaying exponential function to carry out primary election to wavelength, and applies without the EWL point in information variable null method selection mixing absorbance；S3, setting up based on the concentration of PLS method and regression model mix between absorbance, separation is calculated the concentration value of each ion.
Description
Technical field
The present invention relates to uv-vis spectra analysis field, be specifically related to a kind of uv-vis spectra based on wavelength screening
Many metal ion inspections.
Background technology
Ultraviolet-visible spectral analysis technology is the new and high technology of a quick analysis, owing to its pretreatment is simple, detection side
The feature such as just, the analysis at metal ion measures field and is increasingly widely applied.But use the many metals of the method measurement
During ion concentration, general selection all band wavelength information, carry out PLS modeling.In theory, the absorbance in each wavelength points
It is all adding and and meeting lambert's beer's law, but due to experimental error, noise of instrument and each component of various materials absorbed light degree
Influencing each other between material, each wavelength points is different to the contribution degree of model, even has some wavelength points information to affect
The application effect of model.Therefore, traditional all band modeling method cannot be by big for experimental error or little to model contribution ripple
Long message point screens out, and causes that model error is big, precision is low, and many concentration of metal ions are analyzed inaccurate.
At present, Chinese scholars has carried out correlative study to EWL Variable Selection method, by filtering out to model
The big wavelength points of contribution degree models, thus obtains more preferable detection model, reduces the modeling time.Conventional feature variables selection
Method mainly has interval partial least square (iPLS), and the interval PLS (siPLS) of associating, Monte Carlo becomes without information
Amount removing method (MC-UVE), competitive adaptive weighted algorithm (CARS) etc..Spectrum range is mainly selected by the above two,
Not selected characteristic variable pointedly, MC-UVE and CARS method then can filter out to modeling contribution degree is high and error is less
Variable.But being found by analysis, MC-UVE method is mainly used in rejecting the noise wavelength's point in spectrum, removing to modeling contribution
Exist compared with big limitation when spending low non-noise point；CARS method is that the new in recent years a kind of Variable Selection proposing is theoretical, the party
Method decreases the impact on model for the synteny variable while being removed Invalided variable also as far as possible.But due to Meng Teka
Sieve sampling selects sample different, so regression coefficient is changing always, its size can not reflect the importance of variable completely.
Content of the invention
In view of this, the present invention provides a kind of many metal ion inspections of uv-vis spectra based on wavelength screening,
Can rapidly and efficiently reject redundancy and interference wavelength information, reduce wavelength screening time, and improve precision and the robustness of model.
The embodiment of the present invention proposes a kind of many metal ion inspections of uv-vis spectra based on wavelength screening, bag
Include:
S1, obtain with UV, visible light spectra photometric method that to comprise the solution of many kinds of metal ions full wave mixed at 400-700nm
Close absorbance；
The absorbance obtaining is sampled by S2, employing Multiple Cycle DSMC, uses decaying exponential function pair
Wavelength carries out primary election, and applies without the EWL point in information variable null method selection mixing absorbance；
S3, setting up based on the concentration of PLS method and regression model mix between absorbance, separation is calculated each ion
Concentration value.
The many metal ion inspections of uv-vis spectra based on wavelength screening that the embodiment of the present invention provides, sampling
During, the deviation of sampling process is evaded by the Monte Carlo sampling mode of Multiple Cycle, quick removal is mingled with the ripple of noise
Long variable, and remove in a large number not high to model contribution degree non-noise wavelength variable, solves tradition Monte Carlo EGS4 method right
During sampling, randomness is big, causes variable stability indicator to calculate inaccurate problem.In addition, for further speeding up
The speed of wavelength Variable Selection process, introduces decaying exponential function (EDF), the too low useless wavelength of quick superseded importance index
Variable, greatly reduces wavelength screening time.
Brief description
Fig. 1 is the flow process of uv-vis spectra many metal ion inspections one embodiment that the present invention screens based on wavelength
Schematic diagram；
Fig. 2 is Cu2+The relation of the number of wavelengths of screening, RMSECV and algorithm cycle-index；
Fig. 3 is Cu2+Result by modified MC-UVE algorithms selection wavelength；
Fig. 4 is Co2+The relation of the number of wavelengths of screening, RMSECV and algorithm cycle-index；
Fig. 5 is Co2+Result by modified MC-UVE algorithms selection wavelength；
Fig. 6 is Zn2+The relation of the variable number of screening, RMSECV and algorithm cycle-index；
Fig. 7 is Zn2+Result by modified MC-UVE algorithms selection wavelength；
Fig. 8 is Cu2+Model testing result after the screening of MC-UVE method wavelength；
Fig. 9 is Co2+Model testing result after the screening of MC-UVE method wavelength；
Figure 10 is Zn2+Model testing result after the screening of MC-UVE method wavelength.
Detailed description of the invention
Purpose, technical scheme and advantage for making the embodiment of the present invention are clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is explicitly described, it is clear that described embodiment is the present invention
A part of embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having
The every other embodiment being obtained under the premise of making creative work, broadly falls into the scope of protection of the invention.
Referring to Fig. 1, in order to rapidly and efficiently remove the wavelength variable being mingled with noise and not high to model contribution degree in a large number
Non-noise wavelength variable, improves model accuracy further, and the present embodiment discloses a kind of uv-vis spectra based on wavelength screening
Many metal ion inspections, comprising:
S1, obtain with UV, visible light spectra photometric method that to comprise the solution of many kinds of metal ions full wave mixed at 400-700nm
Close absorbance；
The absorbance obtaining is sampled by S2, employing Multiple Cycle DSMC, uses decaying exponential function pair
Wavelength carries out primary election, and applies without the EWL point in information variable null method selection mixing absorbance；
S3, setting up based on the concentration of PLS method and regression model mix between absorbance, separation is calculated each ion
Concentration value.
During wavelength sampling, evade the deviation of sampling process by the Monte Carlo sampling mode of Multiple Cycle,
The quick wavelength variable being mingled with noise of removing, and remove non-noise wavelength variable not high to model contribution degree in a large number, solve
Tradition Monte Carlo EGS4 method randomness during to sampling is big, causes wavelength variable stability indicator to calculate inaccurate
Problem.In addition, be the speed further speeding up wavelength Variable Selection process, introduce decaying exponential function (EDF), quickly eliminate
The too low useless wavelength variable of importance index, greatly reduces wavelength screening time.
Monte Carlo is a kind of variable choosing method based on PLS regression coefficient without information variable null method (MC-UVE),
The importance index of variable is formula (1):
In formula, h is the importance of wavelength variable, and me is the mean value of the regression coefficient of wavelength variable, and s is wavelength variable
The standard deviation of regression coefficient.Calculate the importance index of adopted wavelength variable by formula (1).By decaying exponential function (EDF)
Preliminary screening is carried out to wavelength, the wavelength variable after primary election is arranged from high to low according to importance, then use UVE method logarithm
According to screening further, draw minimum wavelength variable subset SETi of RMSECV after being modeled by PLS, be so circulated.Specifically
Algorithmic procedure comprise the steps:
A. by monte carlo method to sample stochastical sampling, according to the oversampling ratio of Nt, sampling number is M.After sampling
Employing formula (1) calculates the importance of each wavelength variable.
B. carrying out Preliminary screening by decaying exponential function (EDF) to wavelength, decaying exponential function can retain surely by force
The bigger wavelength variable of qualitative value, variable retention rate is calculated by formula (2):
ri=ae-ki (2)
Wherein, i is current cycle time, a and k is for concentrating modeling number with sample during n-th circulation for the first time, for traveling through
All wavelengths variable, n-th is set to 2 variablees, so r1=P；rN=2/P, thus can calculate
Wherein P is original wavelength number, and N is the global cycle number of times setting.
C. the wavelength variable after primary election is arranged from high to low according to importance, then use UVE method further to data
Screening, draws minimum wavelength variable subset SETi of RMSECV by PLS after being modeled, carry out next step circulation.
D. when cycle-index reaches designated value N, circulation terminates, and relatively more N number of wavelength variable subset, wherein RMSECV value is
Little subset is optimal subset, and wavelength screening process completes.
E. the most optimum wavelengths subset filtering out is carried out PLS modeling, calculate and separate each ion concentration.
With Cu2+、Co2+And Zn2+As a example by three component mixed ion solutions detect simultaneously.Experimental design according to uniform Design
Method, specific design scheme such as table 1.Obtain experimental data to be modeled, 20 groups three kinds in employing 0.1～1ppm concentration range
The biased sample of ion is used for verifying model accuracy as unknown sample.
Table 1 uniform design table
By the method for modified MC-UVE to Cu2+、Co2+And Zn2+602 wavelength of the full spectroscopic data of three kinds of ions become
Amount (400nm～700nm, resolution ratio is 0.5nm) selects, and method is as introduced above.
Step one: by monte carlo method to sample stochastical sampling.According to the oversampling ratio of Nt=60% to calibration set
Sample carries out stochastical sampling, and cycle-index is N=50, and sampling number is M=100.Formula (1) is used to calculate each wavelength after sampling
Importance.
Step 2: carrying out Preliminary screening by decaying exponential function (EDF) to wavelength, decaying exponential function can be protected by force
Staying the wavelength variable that stability value is bigger, variable retention rate is calculated by formula (2), as N=50, can be calculated a=through formula (3)
1.35, k=0.3.
Step 3: the wavelength after primary election is arranged from high to low according to importance, then use UVE method further to data
Screening, draws minimum wavelength variable subset SETi of RMSECV by PLS after being modeled, carry out next step circulation.
Step 4: when cycle-index reaches designated value 50, circulation terminates, relatively more N number of wavelength subset, wherein RMSEP value
Minimum subset is optimal subset.Wavelength screening process completes, result such as Fig. 2-7.
Step 5: the most optimum wavelengths subset filtering out carries out PLS modeling, calculates and separates each ion concentration.
Figure (2)～(7) are respectively three kinds of ions under such an approach with the increase of cycle-index, wavelength screening situation and mould
The RMSECV situation of change of type.Wherein (2), (4), abscissa is the cycle-index of modified MC-UVE method in (6) figure, dotted line
Represent that solid line is the model of surplus variable modeling after circulation each time with the increase of cycle-index, the situation of change of number of wavelengths
RMSECV value situation of change.As seen from the figure, wavelength screening process presents a process first quick and back slow, and this is primarily due to
EDF function is forced to eliminate the relatively low wavelength variable of a large amount of stability indicator in early stage.When RMSECV value reach minimum after, with
The continuation of circulation, RMSECV value fast lifting, this is owing to now the pressure screening function of EDF function starts to reject to model
Important wavelength variable, thus have impact on model inspection precision.Figure (2) is Cu2+Wavelength screening situation, when N=9, its
RMSECV value reaches minimum, and now obtain is exactly model optimal subset, totally 32 variablees.Similarly, (4) and figure (6) point are schemed
Wei Zn2+、Co2+Wavelength the selection result, respectively obtain 39 and 48 wavelength variablees.
Figure (3), (5), (7) show that modified MC-UVE method is respectively Cu2+, Co2+, Zn2+Three kinds of ion-selective ripples
Long result, wherein in figure, abscissa is wavelength, and ordinate is absorbance, and vertical bars is the wavelength points chosen.From selection
The position of wavelength points is it was found that in addition to selecting maximum absorption wavelength, it is only that the method also more can highlight from one-component
Vertical characteristic absorption peak selects.And 600～700nm is interval, due to low to PLS model contribution rate, so not having interval at this
Choose variable.
Carry out the selection of wavelength by above-mentioned improved algorithm, and PLS model has been established to the wavelength after screening, with tradition
MC-UVE algorithm compare, the wavelength variable quantity of Cu is reduced to 32 by 112 by this algorithm, and the wavelength variable number of Co is by 78
Individual being reduced to 39, the wavelength variable number of Zn is reduced to 48 by 95.
Prepare 20 groups of even concentration and be distributed in the mixing sample of 0.1～1ppm as detection sample set, to the mould set up
Type is verified, the result of Cu, Co, Zn is respectively as shown in figure (8), (9), (10).Through statistical analysis, and traditional
MC-UVE compares, this model by the RMSECV of Cu, Co, Zn respectively by the 0.841st, the 0.681st, 1.212 being reduced to the 0.532nd, the 0.515th,
1.083, accuracy of detection is improved；Meanwhile, in 20 groups of detection collection samples, the average relative error of Cu, Co, Zn is respectively
6.27%th, the 6.77%th, 6.36%, relative error is all within 10%, and accuracy of detection meets site technique requirement.
Although being described in conjunction with the accompanying embodiments of the present invention, but those skilled in the art can be without departing from this
Making various modifications and variations in the case of bright spirit and scope, such modification and modification each fall within by claims
Within limited range.
Claims (3)
1. the many metal ion inspections of uv-vis spectra based on wavelength screening, it is characterised in that include:
S1, obtain with UV, visible light spectra photometric method and comprise the solution of many kinds of metal ions and inhale in the full wave mixing of 400-700nm
Luminosity；
The absorbance obtaining is sampled by S2, employing Multiple Cycle DSMC, uses decaying exponential function to wavelength
Carry out primary election, and apply without the EWL point in information variable null method selection mixing absorbance；
S3, setting up based on the concentration of PLS method and regression model mix between absorbance, separation is calculated the dense of each ion
Angle value.
2. method according to claim 1, it is characterised in that described S2, comprising:
S20, according to default oversampling ratio Nt and sampling number M, use monte carlo method to sample stochastical sampling, in sampling
The importance of rear each wavelength variable of calculating, computing formula isWherein, h is the importance of wavelength variable, and me is wavelength
The mean value of the regression coefficient of variable, s is the standard deviation of the regression coefficient of wavelength variable；
S21, carried out Preliminary screening, wherein, the variable retention rate r of decaying exponential function to wavelength by decaying exponential functioniMeter
Calculating formula is
ri=ae-ki,
Wherein,P is original wavelength number, and N is the global cycle number of times setting, and i is previous cycle
Number；
S22, the wavelength variable after primary election is arranged from high to low according to importance, then use UVE method to sieve data further
Choosing, draws minimum wavelength variable subset SETi of RMSECV by PLS after being modeled, it is judged that whether current cycle time reaches to specify
Value N, if so, step S23, otherwise, then step S20, enter and circulate next time；
S23, comparison N number of wavelength variable subset, select the minimum subset of RMSECV value as optimal subset；
S24, the most optimum wavelengths subset filtering out is carried out PLS modeling, calculate and separate each ion concentration.
3. method according to claim 2, it is characterised in that the many kinds of metal ions that described solution comprises is Cu2+、Co2+
And Zn2+, Nt=60%, M=100, N=50.
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| CN109100315A (en) * | 2018-08-21 | 2018-12-28 | 暨南大学 | A kind of Wavelength selecting method based on jamtosignal |
| CN109115704A (en) * | 2018-08-29 | 2019-01-01 | 中南大学 | The more metal ion detection Spectroscopy differential preprocess methods of trace under a kind of high zinc background |
| CN109187392A (en) * | 2018-09-26 | 2019-01-11 | 中南大学 | A kind of zinc liquid trace metal ion concentration prediction method based on two-zone model |
| CN109270022A (en) * | 2018-09-14 | 2019-01-25 | 山东大学 | A kind of band selection method and model building method of near-infrared spectroscopy |
| CN109781721A (en) * | 2019-03-15 | 2019-05-21 | 中南大学 | Test system optimization method that is a kind of while measuring copper cobalt ferronickel content in zinc electrolyte |
| CN110873694A (en) * | 2018-08-31 | 2020-03-10 | 中国科学院物理研究所 | Device and method for detecting ion content in secondary battery electrolyte |
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Cited By (9)
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| CN109115704A (en) * | 2018-08-29 | 2019-01-01 | 中南大学 | The more metal ion detection Spectroscopy differential preprocess methods of trace under a kind of high zinc background |
| CN110873694A (en) * | 2018-08-31 | 2020-03-10 | 中国科学院物理研究所 | Device and method for detecting ion content in secondary battery electrolyte |
| CN109270022A (en) * | 2018-09-14 | 2019-01-25 | 山东大学 | A kind of band selection method and model building method of near-infrared spectroscopy |
| CN109270022B (en) * | 2018-09-14 | 2020-03-10 | 山东大学 | Waveband selection method of near-infrared spectrum model and model construction method |
| CN109187392A (en) * | 2018-09-26 | 2019-01-11 | 中南大学 | A kind of zinc liquid trace metal ion concentration prediction method based on two-zone model |
| CN109781721A (en) * | 2019-03-15 | 2019-05-21 | 中南大学 | Test system optimization method that is a kind of while measuring copper cobalt ferronickel content in zinc electrolyte |
| CN109781721B (en) * | 2019-03-15 | 2020-04-14 | 中南大学 | Test system optimization method for determining content of copper, cobalt and nickel and iron in zinc electrolyte |
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Application publication date: 20161123 |