CN103175805B - Method for determining indexes of COD and BOD5 in sewage through near infrared spectrometry - Google Patents
Method for determining indexes of COD and BOD5 in sewage through near infrared spectrometry Download PDFInfo
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- CN103175805B CN103175805B CN201310076050.3A CN201310076050A CN103175805B CN 103175805 B CN103175805 B CN 103175805B CN 201310076050 A CN201310076050 A CN 201310076050A CN 103175805 B CN103175805 B CN 103175805B
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Abstract
The invention provides a method for determining the indexes of COD and BOD5 in sewage through near infrared spectroscopy. The method concretely comprises the following steps: 1, taking a sewage sample, determining the standard values of COD and BOD5 through a routine way, and determining the near infrared spectrum of the sewage sample; 2, taking a pure water sample, and determining the near infrared spectrum of the pure water; 3, preprocessing the spectral data of the sewage sample, dividing the sewage sample into a correction set and a verification set, and calculating to obtain the residual near infrared spectral data of the sewage sample; 4, associating the residual near infrared spectral data of the correction set of the sewage sample with the standard values of COD and BOD5, and establishing a determining model; 5, verifying the determining model; and 6, taking an unknown sewage sample, determining the near infrared spectrum of the unknown sewage sample, repeating step 3, and substituting the residual near infrared spectral data into the determining model to obtain the indexes of COD and BOD5. The method has the advantages of simplicity, rapidness, accuracy and easy operation.
Description
Technical field
The invention belongs to sewage treatment area, especially relate to COD and BOD in a kind of near infrared ray sewage
5refer to calibration method.
Background technology
Organic Pollution is one of important pollutant of water pollutions.In water quality monitoring, often adopt chemical oxygen demand (COD) (COD) and biochemical oxygen demand (BOD
5) evaluate organic pollution level in water body as important overall target.Measure COD at present both at home and abroad and refer to that calibration method mainly contains potassium dichromate method, coulomb method and colourimetry; Measure BOD
5refer to that calibration method mainly contains dilution and inocalation method, fluorescence method and hexavalent chrome bio-removal.These assay methods need to carry out pre-service, complicated operation to sample usually, sometimes need to use toxic reagent, not only endanger healthy, and can cause secondary pollution.
In recent years, near-infrared spectral analysis technology develops rapidly.Utilize this technical Analysis sample to have rapidly and efficiently, do not destroy sample, do not consume chemical reagent, pollution-free, be convenient to the advantages such as on-line analysis, be therefore widely applied at numerous areas.The application of near infrared spectrum in water quality monitoring also has report: directly set up rating model to after the simple pre-service of the near infrared spectrum of sewage sample; Adopt the near infrared spectrum of optimized algorithm to sewage sample to be optimized, then set up rating model; By measuring change and the combination of light path, improve the sensitivity of near infrared ray model.But because the moisture in sewage has strong absorption near infrared spectrum region, strong interference can be caused to the spectral signature of index to be determined in sewage, cause the error of final testing index larger.
Summary of the invention
The object of the invention is for above-mentioned the deficiencies in the prior art, COD and BOD in a kind of near infrared ray sewage is provided
5refer to calibration method.
For achieving the above object, the technical scheme adopted is in the present invention: COD and BOD in a kind of near infrared ray sewage
5refer to calibration method, comprise the steps:
(1) get sewage sample, first measure COD and BOD of sewage sample by conventional method
5standard value, then measure the near infrared spectrum of sewage sample, obtain the original near infrared spectrum data of sewage sample;
(2) get pure water sample, under the condition identical with sewage sample, measure the near infrared spectrum of pure water sample, obtain the near infrared spectrum data of pure water sample;
(3) after pre-service being carried out to the original near infrared spectrum data of sewage sample, with Kai Nade-stone algorithm, sewage sample is divided into calibration set and checking collection, by calculating the near infrared spectrum of pure water in deduction sewage sample, obtain the residue near infrared spectrum data of sewage sample;
(4) by the residue near infrared spectrum data of calibration set sewage sample respectively with COD and BOD measured by conventional method
5standard value associate, set up COD and BOD in sewage respectively by partial least square method
5the rating model of index;
(5) rating model that residue near infrared spectrum data substitution step (4) of checking collection sewage sample is set up is obtained COD and BOD
5measured value, and with COD and BOD measured by conventional method
5standard value compare, rating model is verified, evaluates;
(6) get unknown sewage sample, measure its near infrared spectrum, after repeating step (3), obtain the residue near infrared spectrum data of unknown sewage sample, substitute into rating model, COD and BOD in unknown sewage sample can be recorded
5index.
COD and BOD in a kind of near infrared ray sewage of the present invention
5refer to calibration method, in the deduction sewage sample described in step (3), the computing method of the near infrared spectrum of pure water are:
1. the transition matrix Z orthogonal with the near infrared spectrum data of pure water sample is built
,structure formula is as follows:
Z=I – W × (W ' × W)
-1× W ', wherein, W is the near infrared light spectrum matrix of pure water sample, and I is unit matrix, the transposed matrix that W ' is W;
2. according to transition matrix Z, calculate the residue near infrared spectrum data of sewage sample, computing formula is as follows:
R=Z × S, wherein, R is the residue near infrared light spectrum matrix of sewage sample, and S is the original near infrared light spectrum matrix of sewage sample.
COD and BOD in a kind of near infrared ray sewage of the present invention
5refer to calibration method, the pre-service described in step (3) is adopt the original near infrared spectrum data of smoothing filter to sewage sample to carry out filtering.
COD and BOD in a kind of near infrared ray sewage of the present invention
5refer to calibration method, the spectral range of the near infrared spectrum that described rating model is corresponding comprises three regions, is respectively: I region: 8800cm
-1~ 8500cm
-1, II region: 7556cm
-1~ 7162cm
-1, III region: 6329cm
-1~ 5470cm
-1.
COD and BOD in a kind of near infrared ray sewage of the present invention
5refer to calibration method, adopt Orthogonal Signal Correction Analyze method, the near infrared spectrum characteristic information S of sewage sample can be expressed as the spectral signature information S of organic contaminant in sewage sample
have, water the Impurity spectra characteristic information S such as spectral signature information W, sewage medium-high frequency noise
otherthree add and, that is: S=
kw+S
have+ S
other.By can the impurity (S such as high frequency noise be removed to the filter preprocessing of sewage sample near infrared spectrum data
other) interference to spectrum.After being multiplied with the orthogonal transition matrix of pure water by the near infrared spectrum data of sewage sample, the near infrared spectrum characteristic information of pure water can be deducted from the near infrared spectrum characteristic information of sewage, eliminate the strong absorption of water near infrared region to COD and BOD with this
5the interference that index determining causes, improves predictive ability and the degree of accuracy of the final rating model set up.
COD and BOD in a kind of near infrared ray sewage of the present invention
5refer to calibration method, its near infrared spectrum data is measured to unknown sewage sample and after carrying out data processing, directly calculates COD and BOD in unknown sewage sample by the rating model set up
5index.Minute is fast, without the need to any chemical reagent, have easy, rapid, accurate, easy-operating advantage.Monitor water quality by the inventive method, substantially increase the ageing of water quality early-warning, there is stronger practicality.
Accompanying drawing explanation
Fig. 1 is the original near infrared spectrum of sewage sample.
Fig. 2 is the near infrared spectrum of pure water sample.
Fig. 3 is the residue near infrared spectrum of sewage sample.
Fig. 4 is measured value and the standard value graph of a relation of the COD index of unknown sewage sample.
Fig. 5 is the BOD of unknown sewage sample
5the measured value of index and standard value graph of a relation.
Embodiment
COD and BOD in a kind of near infrared ray sewage of the present invention
5refer to calibration method, comprise the steps:
(1) get sewage sample, first measure COD and BOD of sewage sample by conventional method
5standard value, then measure the near infrared spectrum of sewage sample, obtain the original near infrared spectrum data of sewage sample;
(2) get pure water sample, under the condition identical with sewage sample, measure the near infrared spectrum of pure water sample, obtain the near infrared spectrum data of pure water sample;
(3) after pre-service being carried out to the original near infrared spectrum data of sewage sample, with Kai Nade-stone algorithm, sewage sample is divided into calibration set and checking collection, by calculating the near infrared spectrum of pure water in deduction sewage sample, obtain the residue near infrared spectrum data of sewage sample;
(4) by the residue near infrared spectrum data of calibration set sewage sample respectively with COD and BOD measured by conventional method
5standard value associate, set up COD and BOD in sewage respectively by partial least square method
5the rating model of index;
(5) rating model that residue near infrared spectrum data substitution step (4) of checking collection sewage sample is set up is obtained COD and BOD
5measured value, and with COD and BOD measured by conventional method
5standard value compare, rating model is verified, evaluates;
(6) get unknown sewage sample, measure its near infrared spectrum, after repeating step (3), obtain the residue near infrared spectrum data of unknown sewage sample, substitute into rating model, COD and BOD in unknown sewage sample can be recorded
5index.
In deduction sewage sample described in step (3), the computing method of the near infrared spectrum of pure water are:
1. the transition matrix Z orthogonal with the near infrared spectrum data of pure water sample is built
,structure formula is as follows:
Z=I – W × (W ' × W)
-1× W ', wherein, W is the near infrared light spectrum matrix of pure water sample, and I is unit matrix, the transposed matrix that W ' is W;
2. according to transition matrix Z, calculate the residue near infrared spectrum data of sewage sample, computing formula is as follows:
R=Z × S, wherein, R is the residue near infrared light spectrum matrix of sewage sample, and S is the original near infrared light spectrum matrix of sewage sample.These computing method effectively can eliminate the spectral absorption of water at COD and BOD
5the interference caused in index determining process, improves predictive ability and the degree of accuracy of rating model.
Pre-service described in step (3) is adopt the original near infrared spectrum data of smoothing filter to sewage sample to carry out filtering.By the interference of the impurity such as high frequency noise to sewage sample near infrared spectrum data can be eliminated to the filtering of spectroscopic data, improve the degree of accuracy of rating model.
The spectral range of the near infrared spectrum that described rating model is corresponding comprises three regions, is respectively: I region: 8800cm
-1~ 8500cm
-1, II region: 7556cm
-1~ 7162cm
-1, III region: 6329cm
-1~ 5470cm
-1.Described I, II, the interference that the near infrared spectrum of water causes can be down to minimum by calculating in III region, make the degree of accuracy of final rating model reach the highest.
Selected by the present invention, sewage sample quantity is more, the rating model set up is more accurate, precision is higher, but the workload setting up rating model is also larger, therefore, for reducing workload in practical operation, generally choose contain as far as possible the sample size of likely predicted value, the preferred sewage sample quantity of the present invention is at 60-120.Without significant difference between the different sample of pure water sample, preferred amount is 5-10.
Mensuration-the dichromate titration of the conventional method reference GB11914-89(water quality-chemical oxygen demand (COD) of the mensuration COD index described in step of the present invention (1)) measure; Described mensuration BOD
5the conventional method of index is with reference to GB7488-87(dilution and inocalation method) measure.
Sewage sample carried out be divided into calibration set and checking collection with Kai Nade-stone algorithm described in step of the present invention (3).The ultimate principle of triumphant Nader-stone algorithm (transliteration of kennard-stone algorithm) is: select the sewage sample of the representative distribution of most to be calibration set according to the maximum Euclidean distance between different sewage sample.According to Kai Nade-stone algorithm, i-th sewage sample to the computing formula of the Euclidean distance of a jth sewage sample is:
, wherein,
prepresent the variable number of near infrared spectrum.
Step of the present invention (4) partial least square method sets up the ultimate principle following (for COD index) of rating model: the product first the residue near infrared light spectrum matrix R of calibration set sewage sample being decomposed into spectrum score matrix T and spectrum loading matrix P, COD standard value matrix Y is decomposed into the product of COD score matrix U and COD loading matrix Q, i.e. R=TP+A, Y=UQ+B, then linear regression is carried out to U and T, U=TM, so there is the relational expression between COD index and near infrared spectrum: Y=TMQ+C(A, B, C are stochastic error matrix).Utilize calibration set sample to determine P, adopt leaving-one method validation-cross determination number of principal components.For unknown sewage sample, the COD index of unknown sewage sample can be tried to achieve according to relational expression Y=TMQ+C.
Rating model is verified described in step of the present invention (5), to evaluate, rating model evaluating and the standard of calculating as follows:
1. related coefficient (
r):
，
rmore close to 1, measured value and the standard value of expression rating model are more close;
requal 1, represent measured value and the complete matching of standard value of rating model.
2. calibration set root-mean-square error (RMSEC), checking collection root-mean-square error (RMSEP):
，
RMSEC and RMSEP value is less, represents that rating model estimating precision is higher.
COD and BOD in a kind of near infrared ray sewage of the present invention
5refer to calibration method, sewage sample carried out described in the calculating of the near infrared spectrum dividing and deduct pure water in sewage sample, step (4), set up COD of sewage and BOD by partial least square method with Kai Nade-stone algorithm described in step (3)
5the rating model of index, the checking to rating model described in step (5), evaluation, above-mentioned computation process all processes by spectrochemistry metrology class process software, and the embodiment of the present invention adopts matlab software.
COD and BOD in a kind of near infrared ray sewage of the present invention
5refer to calibration method, can be described further by following specific embodiment:
The near infrared spectrometer adopted in the present embodiment is Thermo scientific Fourier Transform Near Infrared instrument, adopts 4mm to adapt to cuvette and makes sample cell, InGaAs detecting device; Condition determination is: transmission spectrum method measures, and air is as reference, and spectral resolution is 4cm
-1, spectral scan interval is 10000cm
-1~ 4000cm
-1, scanning times is 32 times; Sewage sample takes from sewage treatment plant of Jinan City.Pure water sample gets distilled water.
Embodiment 1, COD and BOD in a kind of near infrared ray sewage
5refer to that the concrete steps of calibration method are:
(1) get sewage sample 88, first measure COD and BOD of sewage sample by conventional method
5standard value, then measure the near infrared spectrum of sewage sample, obtain the original near infrared spectrum data (as shown in Figure 1) of sewage sample;
(2) get pure water sample 8, under the condition identical with sewage sample, measure the near infrared spectrum of pure water sample, obtain the near infrared spectrum data (as shown in Figure 2) of pure water sample;
(3) the original near infrared spectrum data of Savitzky-Golay smoothing filter to sewage sample is adopted to carry out filtering, sewage sample is divided into calibration set sewage sample 52 and checking collection sewage sample 36, with matlab software according to formula with Kai Nade-stone algorithm: Z=I – W × (W ' × W)
-1× W ' and R=Z × S calculates
,in deduction sewage sample, the near infrared spectrum of pure water, obtains the residue near infrared spectrum data (as shown in Figure 3) of sewage sample;
(4) by the residue near infrared spectrum data of calibration set sewage sample respectively with COD and BOD recorded by conventional method
5standard value associate, based on SPECTRAL REGION I region: 8800 cm
-1~ 8500 cm
-1, II region: 7556 cm
-1~ 7162 cm
-1, III region: 6329 cm
-1~ 5470cm
-1, set up COD of sewage and BOD respectively by partial least square method
5the rating model of index;
(5) rating model that residue near infrared spectrum data substitution step (4) of checking collection sewage sample is set up is obtained COD and BOD
5measured value, and with COD and BOD measured by conventional method
5standard value compare, rating model is verified, evaluates;
Table 1, table 2 are respectively based on sewage sample residue near infrared spectrum and COD and BOD based on the filtered near infrared spectrum foundation of sewage sample
5the number of principal components contrast situation of the rating model of index and rating model evaluation contrast situation:
The rating model contrast of the COD index of table 1 sewage sample
Table 2 sewage sample BOD
5the rating model contrast of index
Above-mentioned contrast situation shows, COD and BOD set up afterwards by the interference of the near infrared spectrum calculating deduction water
5the rating model measured value of index is closer to standard value, and estimating precision is higher.
(6) unknown sewage sample 35 is got, measure its near infrared spectrum, after step (3) is repeated to the near infrared spectrum data of unknown sewage sample, obtain the residue near infrared spectrum data of unknown sewage sample, substitute into rating model, record COD and BOD in unknown sewage sample
5index.According to COD and BOD of the unknown sewage sample that rating model records
5the measured value of index and the relation of standard value recorded by conventional method are shown in Fig. 4, Fig. 5.
Claims (1)
1. COD and BOD in a near infrared ray sewage
5refer to calibration method, it is characterized in that: concrete steps are as follows:
(1) get sewage sample, first measure COD and BOD of sewage sample by conventional method
5standard value, then measure the near infrared spectrum of sewage sample, obtain the original near infrared spectrum data of sewage sample, sewage sample is divided into calibration set and checking collection with Kai Nade-stone algorithm;
(2) get pure water sample, under the condition identical with sewage sample, measure the near infrared spectrum of pure water sample, obtain the near infrared spectrum data of pure water sample;
(3), after pre-service being carried out to the original near infrared spectrum data of sewage sample, by calculating the near infrared spectrum of pure water in deduction sewage sample, the residue near infrared spectrum data of sewage sample is obtained;
(4) by the residue near infrared spectrum data of calibration set sewage sample respectively with COD and BOD measured by conventional method
5standard value associate, set up COD and BOD in sewage respectively by partial least square method
5the rating model of index;
(5) the residue near infrared spectrum data of checking collection sewage sample and COD and BOD measured by conventional method is utilized
5standard value rating model is verified, evaluates;
(6) get unknown sewage sample, measure its near infrared spectrum, after repeating step (3), obtain the residue near infrared spectrum data of unknown sewage sample, substitute into rating model, COD and BOD in unknown sewage sample can be recorded
5index;
In deduction sewage sample described in step (3), the computing method of the near infrared spectrum of pure water are:
1. the transition matrix Z orthogonal with the near infrared spectrum data of pure water sample is built
,structure formula is as follows:
Z=I–W×(W’×W)
-1×W’，
Wherein, W is the near infrared light spectrum matrix of pure water sample, and I is unit matrix, the transposed matrix that W ' is W;
2. according to transition matrix Z, calculate the residue near infrared spectrum data of sewage sample, computing formula is as follows:
R=Z×S
Wherein, R is the residue near infrared light spectrum matrix of sewage sample, and S is the original near infrared light spectrum matrix of sewage sample;
Pre-service described in step (3) is adopt the original near infrared spectrum data of smoothing filter to sewage sample to carry out filtering;
The spectral range of the near infrared spectrum that described rating model is corresponding comprises three regions, is respectively: I region: 8800cm
-1~ 8500cm
-1, II region: 7556cm
-1~ 7162cm
-1, III region: 6329cm
-1~ 5470cm
-1.
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| CN106018359A (en) * | 2016-05-12 | 2016-10-12 | 常州市排水管理处 | Sewage plant water-quality monitoring early-warning method and system |
| CN109975262A (en) * | 2019-04-15 | 2019-07-05 | 上海交通大学 | One kind optimizing full spectrum monitoring COD method based on three-dimensional fluorescence domain integral method |
| CN117074361B (en) * | 2023-08-29 | 2024-02-09 | 无锡迅杰光远科技有限公司 | Calibration method, device, cleaning machine and storage medium |
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