CN103175805A - 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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- CN103175805A CN103175805A CN2013100760503A CN201310076050A CN103175805A CN 103175805 A CN103175805 A CN 103175805A CN 2013100760503 A CN2013100760503 A CN 2013100760503A CN 201310076050 A CN201310076050 A CN 201310076050A CN 103175805 A CN103175805 A CN 103175805A
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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
5The method of index.
Background technology
Organic Pollution is one of important pollutant of water pollution.In water quality monitoring, often adopt chemical oxygen demand (COD) (COD) and biochemical oxygen demand (BOD
5) estimate organic pollution level in water body as important overall target.The method of measuring at present the COD index both at home and abroad mainly contains potassium dichromate method, enclosed pasture method and colourimetry; Measure BOD
5The method of index mainly contains dilution and inocalation method, fluorescence method and biology sensor method.These assay methods need to carry out pre-service to sample usually, and complicated operation needs to use toxic reagent sometimes, not only endanger healthyly, 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 advantage such as on-line analysis, therefore be widely applied at numerous areas.Near infrared spectrum also has report in the application aspect water quality monitoring: directly set up rating model after the simple pre-service of near infrared spectrum to sewage sample; Adopt optimized algorithm that the near infrared spectrum of sewage sample is optimized, then set up rating model; By measuring variation and the combination of light path, the sensitivity that improves the near infrared ray model.But because the moisture in sewage has strong absorption in the near infrared spectrum zone, can cause to the spectral signature of index to be determined in sewage strong interference, cause the error of final testing index larger.
Summary of the invention
The objective 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
5The method of index.
The present invention for achieving the above object, the technical scheme that adopts is: COD and BOD in a kind of near infrared ray sewage
5The method of index comprises the steps:
(1) get sewage sample, first measure COD and the BOD of sewage sample with 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 the pure water sample, measure the near infrared spectrum of pure water sample under the condition identical with sewage sample, obtain the near infrared spectrum data of pure water sample;
(3) the original near infrared spectrum data of sewage sample is carried out pre-service after, with Kai Nade-stone algorithm, sewage sample is divided into calibration set and checking collection, deduct the near infrared spectrum of pure water in sewage sample by calculating, obtain the residue near infrared spectrum data of sewage sample;
(4) with the residue near infrared spectrum data of calibration set sewage sample respectively with the COD and the BOD that measure with conventional method
5Standard value carry out association, set up respectively COD and BOD in sewage with partial least square method
5The rating model of index;
(5) will verify that the rating model that the residue near infrared spectrum data substitution step (4) of collection sewage sample is set up obtains COD and BOD
5Measured value, and with the COD and the BOD that measure with conventional method
5Standard value relatively, rating model is verified, is estimated;
(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, the substitution rating model can record COD and BOD in unknown sewage sample
5Index.
COD and BOD in a kind of near infrared ray sewage of the present invention
5The method of index, in the deduction sewage sample described in step (3), the computing method of the near infrared spectrum of pure water are:
1. build the transition matrix Z with the near infrared spectrum data quadrature of pure water sample
,The 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, and W ' is the transposed matrix of 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, 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
5The method of index, the pre-service described in step (3) is for adopting smoothing filter to carry out filtering to the original near infrared spectrum data of sewage sample.
COD and BOD in a kind of near infrared ray sewage of the present invention
5The method of index, the spectral range of the near infrared spectrum that described rating model is corresponding comprises Three regions, is respectively: I is regional: 8800cm
-1～8500cm
-1, II zone: 7556cm
-1～7162cm
-1, III zone: 6329cm
-1～5470cm
-1
COD and BOD in a kind of near infrared ray sewage of the present invention
5The method of index adopts the Orthogonal Signal Correction Analyze method, and 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
OtherThe three add and, that is: S=
kW+S
Have+ S
OtherCan remove the impurity (S such as high frequency noise by the filter preprocessing to the sewage sample near infrared spectrum data
Other) to the interference of spectrum.After multiplying each other with the quadrature transition matrix of the near infrared spectrum data of sewage sample and pure water, can deduct the near infrared spectrum characteristic information of pure water from the near infrared spectrum characteristic information of sewage, with this eliminate water in the strong absorption of near infrared region to COD and BOD
5The interference that index determining causes has improved predictive ability and the degree of accuracy of the rating model of final foundation.
COD and BOD in a kind of near infrared ray sewage of the present invention
5The method of index after unknown sewage sample is measured its near infrared spectrum data and carried out the data processing, directly calculates COD and BOD in unknown sewage sample by the rating model of setting up
5Index.Minute is fast, need not any chemical reagent, has easy, rapid, accurate, easy-operating advantage.Monitor water quality with the inventive method, greatly improved the ageing of water quality early-warning, have stronger practicality.
Description of drawings
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
5The method of index comprises the steps:
(1) get sewage sample, first measure COD and the BOD of sewage sample with 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 the pure water sample, measure the near infrared spectrum of pure water sample under the condition identical with sewage sample, obtain the near infrared spectrum data of pure water sample;
(3) the original near infrared spectrum data of sewage sample is carried out pre-service after, with Kai Nade-stone algorithm, sewage sample is divided into calibration set and checking collection, deduct the near infrared spectrum of pure water in sewage sample by calculating, obtain the residue near infrared spectrum data of sewage sample;
(4) with the residue near infrared spectrum data of calibration set sewage sample respectively with the COD and the BOD that measure with conventional method
5Standard value carry out association, set up respectively COD and BOD in sewage with partial least square method
5The rating model of index;
(5) will verify that the rating model that the residue near infrared spectrum data substitution step (4) of collection sewage sample is set up obtains COD and BOD
5Measured value, and with the COD and the BOD that measure with conventional method
5Standard value relatively, rating model is verified, is estimated;
(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, the substitution rating model can record COD and BOD in unknown sewage sample
5Index.
In deduction sewage sample described in step (3), the computing method of the near infrared spectrum of pure water are:
1. build the transition matrix Z with the near infrared spectrum data quadrature of pure water sample
,The 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, and W ' is the transposed matrix of 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, S is the original near infrared light spectrum matrix of sewage sample.These computing method can effectively be eliminated the spectral absorption of water at COD and BOD
5The interference that causes in the index determining process, predictive ability and the degree of accuracy of raising rating model.
Pre-service described in step (3) is for adopting smoothing filter to carry out filtering to the original near infrared spectrum data of sewage sample.By eliminating the impurity such as high frequency noise to the filtering of spectroscopic data to the interference of sewage sample near infrared spectrum 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 is regional: 8800cm
-1～8500cm
-1, II zone: 7556cm
-1～7162cm
-1, III zone: 6329cm
-1～5470cm
-1Be down to minimumly by calculating the interference that the near infrared spectrum of water can be caused in described I, II, III zone, make the degree of accuracy of final rating model reach the highest.
The selected sewage sample quantity of the present invention is more, the rating model of setting up is more accurate, precision is higher, but the workload of setting up rating model is also larger, therefore, be the minimizing workload in practical operation, generally choose contain as far as possible might predicted value sample size, the preferred sewage sample quantity of the present invention is at 60-120.Between the different samples of pure water sample, without significant difference, preferred amount is 5-10.
The conventional method of the mensuration COD index described in step of the present invention (1) is with reference to the mensuration-dichromate titration of GB11914-89(water quality-chemical oxygen demand (COD)) measure; Described mensuration BOD
5The conventional method of index is with reference to GB7488-87(dilution and inocalation method) measure.
Sewage sample is divided into calibration set and verifies 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: selecting the sewage sample of the most representative distribution according to the maximum Euclidean distance between the different sewage sample is calibration set.According to Kai Nade-stone algorithm, i sewage sample to the computing formula of the Euclidean distance of j sewage sample is:
The ultimate principle that step of the present invention (4) is set up rating model with partial least square method following (take the COD index as example): the product that first the residue near infrared light spectrum matrix R of calibration set sewage sample is 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, be R=TP+A, Y=UQ+B, then U and T are carried out linear regression, U=TM, so relational expression between COD index and near infrared spectrum is arranged: Y=TMQ+C(A, B, C are the stochastic error matrix).Utilize the calibration set sample to determine P, adopt the leaving-one method validation-cross to determine number of principal components.For unknown sewage sample, can try to achieve according to relational expression Y=TMQ+C the COD index of unknown sewage sample.
Rating model is verified, is estimated described in step of the present invention (5), rating model evaluating and calculating standard are as follows:
1. related coefficient (
r):
rMore near 1, measured value and the standard value of expression rating model are more approaching;
rEqual 1, measured value and the complete match of standard value of expression rating model.
2. calibration set root-mean-square error (RMSEC), checking collection root-mean-square error (RMSEP):
RMSEC and RMSEP value are less, and it is higher that the expression rating model is measured precision.
COD and BOD in a kind of near infrared ray sewage of the present invention
5The method of index, described in step (3) with Kai Nade-stone algorithm sewage sample is divided and is deducted the near infrared spectrum of pure water in sewage sample calculating, step (4) is described sets up COD of sewage and BOD with partial least square method
5The rating model of index, the described checking to rating model of step (5), evaluation, above-mentioned computation process all can be processed 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
5The method of index can be described further by following specific embodiment:
The near infrared spectrometer that adopts in the present embodiment is Thermo scientific Fourier Transform Near Infrared instrument, adopts 4mm to adapt to cuvette and makes sample cell, the InGaAs detecting device; Condition determination is: transmission spectrum method is measured, and air is as reference, and spectral resolution is 4cm
-1, the spectral scan interval is 10000cm
-1~ 4000cm
-1, scanning times is 32 times; Sewage sample is taken from Jinan City sewage treatment plant.The pure water sample is got distilled water.
Embodiment 1, COD and BOD in a kind of near infrared ray sewage
5The concrete steps of the method for index are:
(1) get 88 of sewage samples, first measure COD and the BOD of sewage sample with 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 8, pure water sample, measure the near infrared spectrum of pure water sample under the condition identical with sewage sample, obtain the near infrared spectrum data (as shown in Figure 2) of pure water sample;
(3) adopt the Savitzky-Golay smoothing filter to carry out filtering to the original near infrared spectrum data of sewage sample, with Kai Nade-stone algorithm, sewage sample is divided into 36 of 52 of calibration set sewage samples and checking collection sewage samples, with matlab software according to formula: Z=I – W * (W ' * W)
-1* W ' and R=Z * S calculate
,Deduct the near infrared spectrum of pure water in sewage sample, obtain the residue near infrared spectrum data (as shown in Figure 3) of sewage sample;
(4) with the residue near infrared spectrum data of calibration set sewage sample respectively with the COD that records with conventional method and BOD
5Standard value carry out association, based on SPECTRAL REGION I zone: 8800 cm
-1～8500 cm
-1, II zone: 7556 cm
-1～7162 cm
-1, III zone: 6329 cm
-1～5470cm
-1, set up respectively COD of sewage and BOD with partial least square method
5The rating model of index;
(5) will verify that the rating model that the residue near infrared spectrum data substitution step (4) of collection sewage sample is set up obtains COD and BOD
5Measured value, and with the COD and the BOD that measure with conventional method
5Standard value relatively, rating model is verified, is estimated;
Table 1, table 2 are respectively COD and the BOD that remains near infrared spectrum and set up based on the filtered near infrared spectrum of sewage sample based on 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, deducts by calculating COD and the BOD that the interference of the near infrared spectrum of water is set up afterwards
5The rating model measured value of index is the value of being near the mark more, measures precision higher.
(6) get 35 of unknown sewage samples, measure its near infrared spectrum, after the near infrared spectrum data repeating step (3) to unknown sewage sample, obtain the residue near infrared spectrum data of unknown sewage sample, the substitution rating model records COD and BOD in unknown sewage sample
5Index.COD and the BOD of the unknown sewage sample that records according to rating model
5The relation of the measured value of index and the standard value that records with conventional method is seen Fig. 4, Fig. 5.
Claims (4)
1. COD and BOD in a near infrared ray sewage
5The method of index is characterized in that: comprise the steps:
(1) get sewage sample, first measure COD and the BOD of sewage sample with 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 the pure water sample, measure the near infrared spectrum of pure water sample under the condition identical with sewage sample, obtain the near infrared spectrum data of pure water sample;
(3) the original near infrared spectrum data of sewage sample is carried out pre-service after, with Kai Nade-stone algorithm, sewage sample is divided into calibration set and checking collection, deduct the near infrared spectrum of pure water in sewage sample by calculating, obtain the residue near infrared spectrum data of sewage sample;
(4) with the residue near infrared spectrum data of calibration set sewage sample respectively with the COD and the BOD that measure with conventional method
5Standard value carry out association, set up respectively COD and BOD in sewage with partial least square method
5The rating model of index;
(5) will verify that the rating model that the residue near infrared spectrum data substitution step (4) of collection sewage sample is set up obtains COD and BOD
5Measured value, and with the COD and the BOD that measure with conventional method
5Standard value relatively, rating model is verified, is estimated;
(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, the substitution rating model can record COD and BOD in unknown sewage sample
5Index.
2. COD and BOD in a kind of near infrared ray sewage according to claim 1
5The method of index is characterized in that: in the deduction sewage sample described in step (3), the computing method of the near infrared spectrum of pure water are:
1. build the transition matrix Z with the near infrared spectrum data quadrature of pure water sample
,The 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, and W ' is the transposed matrix of 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, S is the original near infrared light spectrum matrix of sewage sample.
3. COD and BOD in a kind of near infrared ray sewage according to claim 1
5The method of index is characterized in that: the pre-service described in step (3) is for adopting smoothing filter to carry out filtering to the original near infrared spectrum data of sewage sample.
4. COD and BOD in a kind of near infrared ray sewage according to claim 1
5The method of index is characterized in that: the spectral range of the near infrared spectrum that described rating model is corresponding comprises Three regions, is respectively: I is regional: 8800cm
-1～8500cm
-1, II zone: 7556cm
-1～7162cm
-1, III zone: 6329cm
-1～5470cm
-1
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| CN104034684A (en) * | 2014-06-05 | 2014-09-10 | 北京金达清创环境科技有限公司 | Water quality multi-index detection method on basis of ultraviolet-visible absorption spectrum |
| CN104990889A (en) * | 2015-05-20 | 2015-10-21 | 安徽建筑大学 | Method for rapidly determining concentration of inorganic salt nitrogen in shortcut nitrification-denitrification through near infrared spectroscopy |
| CN105891143A (en) * | 2016-03-30 | 2016-08-24 | 安徽建筑大学 | Method for measuring total phosphorus concentration in denitrifying phosphorus removal system by means of near infrared spectrum |
| CN105891148A (en) * | 2016-03-30 | 2016-08-24 | 安徽建筑大学 | Method for measuring VFA concentration in anaerobic wastewater treatment process by means of near infrared spectrum |
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| 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 |
| CN117074361A (en) * | 2023-08-29 | 2023-11-17 | 无锡迅杰光远科技有限公司 | Calibration method, device, cleaning machine and storage medium |
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Cited By (9)
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|---|---|---|---|---|
| CN104034684A (en) * | 2014-06-05 | 2014-09-10 | 北京金达清创环境科技有限公司 | Water quality multi-index detection method on basis of ultraviolet-visible absorption spectrum |
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| CN105891148A (en) * | 2016-03-30 | 2016-08-24 | 安徽建筑大学 | Method for measuring VFA concentration in anaerobic wastewater treatment process by means of near infrared spectrum |
| 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 |
| CN117074361A (en) * | 2023-08-29 | 2023-11-17 | 无锡迅杰光远科技有限公司 | Calibration method, device, cleaning machine and storage medium |
| 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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