CN101907565A - Spectral analysis method capable of measuring chemical oxygen demand and biochemical oxygen demand in waste water simultaneously - Google Patents
Spectral analysis method capable of measuring chemical oxygen demand and biochemical oxygen demand in waste water simultaneously Download PDFInfo
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Abstract
The invention relates to a method capable of measuring chemical oxygen demand (COD) and biochemical oxygen demand (BOD) in waste water simultaneously. The method is characterized by comprising the following steps of: sampling and measuring, namely, sampling the waste water, measuring a COD standard value and a BOD standard value of the water sample and acquiring near infrared spectrum data of the water sample at the same time; establishing models, namely, associating the COD standard value and the BOD standard value of the water sample with the near infrared spectrum data of the water sample by using software and then establishing PLS1 regression models of the COD and the BOD values respectively by using software; and measuring a COD value and a BOD value of unknown waste water at the same time, namely, retrieving the COD value and the BOD value of the unknown waste water through the established models. The method has the advantages of simultaneous measurement on the COD value and the BOD value of the waste water, convenient operation of detecting the COD value and the BOD value of the waste water by using the models established by the method, on-line detection, high detection speed, repeatability and precision, no secondary pollution and great improvement on the detection quality and the detection efficiency of the waste water.
Description
Technical field
The present invention relates to the method that a kind of waste water detects, relate in particular to a kind of method of measuring chemical oxygen demand (COD) in the waste water (COD) and biochemical oxygen demand (BOD) simultaneously.
Background technology
Chemical oxygen demand (COD) (hereinafter to be referred as, COD) be meant the amount of organism and oxygenant that inorganics consumes easily oxidized in the water body; Biochemical oxygen demand (is generally made the BOD that is of cultivation in five days
5, this paper is called for short BOD and is BOD
5) be under rated condition, the dissolved oxygen DO that organism and inorganics are consumed under biological oxidation in the water.COD and BOD value have all been reacted the pollution level of water body, all are the overall targets of organism relative content in the water body.Therefore, measuring COD and BOD value has great importance to water pollutant overall control and water environment protection.
At present, usually measure the COD value of waste water both at home and abroad with potassium dichromate method, this method is to add a certain amount of potassium dichromate and catalyst sulfuric acid silver in water sample, reflux is 2 hours in the highly acid medium, the part potassium dichromate is reduced by the oxidizable substance in the water sample, with the remaining potassium dichromate of iron protosulfide ammonium titration, calculate the value of COD according to the amount of the potassium dichromate that consumes; This method has the high advantage of favorable reproducibility, accuracy and precision, analytical cycle is long, efficient is low, equipment volume is big, the silver salt consumption is big but exist, the deficiency that analysis cost is high, and, therefore can produce secondary pollution for the interference of eliminating chlorion need add mercuric sulfate.The report that also has some spectrophotometry COD values, but these methods need be carried out pre-service; In addition, the instrument of many Rapid Determination of COD values is arranged also in the market, these instruments are to utilize the coulometry principle to measure the COD value, but utilize these instruments also to need degraded earlier could measure in about 30 minutes.
The method of measuring the BOD value at present both at home and abroad is mainly the standard dilution method, this method is that water sample is divided into two parts, a wherein content of dissolved oxygen DO of in time measuring, and another part is after cultivating 5 days under 20 ℃ ± 1 ℃, measure its dissolved oxygen content, the difference of both dissolved oxygen contents of front and back is the BOD value.This method is owing to carrying out pre-service to water sample, and is consuming time very long.
Summary of the invention
The object of the present invention is to provide a kind of simple and efficient, cost is low and can measure the spectroscopic analysis methods of COD and BOD in the waste water simultaneously.
The object of the present invention is achieved like this:
A kind of spectroscopic analysis methods of measuring COD and BOD in the waste water simultaneously, it is characterized in that: this method may further comprise the steps:
A. take a sample and measure: get the waste water sample, measure the COD standard value and the BOD standard value of described waste water sample, gather its near infrared spectrum data simultaneously with standard method;
B. modeling: it is related to utilize software that the COD standard value of above-mentioned waste water sample and the BOD standard value and the near infrared spectrum data of above-mentioned waste water sample are carried out, and adopts software to set up the PLS1 regression model of this COD, BOD respectively then;
C. measure COD value, the BOD value of unknown waste water simultaneously: COD value, the BOD value of utilizing the unknown waste water of model index of above-mentioned foundation; The COD of described unknown waste water and BOD value will be in above-mentioned sampling and determination steps in the COD and BOD standard value range of the water sample that detects.
It is spectrochemistry metrology class process software that above-mentioned modeling process carries out related used software with the COD standard value of waste water sample with BOD standard value and its near infrared spectrum data, preferably adopts The Unscrambler 9.7 softwares.
Association in the above-mentioned modeling process is at first the near infrared spectrum data that records to be converted into the JCAMP-DX form, again with described data importing in The Unscrambler 9.7 softwares, then the COD of the above-mentioned waste water sample that records and BOD standard value are copied to carry out in the software related.
Because the spectral signal that collects is except that sample message, the noise that also comprises each side, for the elimination noise, optimize spectral signal, lay a solid foundation for Optimization Model, after in the above-mentioned modeling process near infrared spectrum data being imported The Unscrambler9.7 software this near infrared spectrum data is carried out pre-service, described pre-service is that convolution smoothing processing, first order derivative (9 level and smooth) are handled and second derivative (9 level and smooth) processing; Adopt the convolution smoothing processing through optimizing screening.
Owing to have abnormity point usually in the near infrared spectrum of waste water, in order to make model accuracy higher, above-mentioned employing PLS1 algorithm also is optimized processing when setting up model, reject described abnormity point, described optimization process is for adopting the method verification model of cross validation (Cross-validation), preferred " picking one " the cross validation method that adopts, reject exceptional value in exceptional value in the near infrared spectrum and COD standard value, the BOD standard value, the PLS1 regression model that is optimized respectively according to lever value and chemical score error.
Above-mentioned waste water sample COD standard value is with reference to GB11914-89 (water quality-chemical oxygen demand
Mensuration-the dichromate titration of amount) measures;
The near infrared spectrum of above-mentioned this water sample of collection, use the 1cm quartz sample pool, with the air is blank, near infrared region interscan wastewater sample at wavelength 800～1800nm, wavelength interval 2nm, it is 2nm that slit is set, choosing PbS gain is 2, sweep velocity is 1500nm/s, and each sample scanning is averaged for 3 times and is the near infrared spectrum of waste water.
More particularly, a kind of method of measuring COD and BOD in the waste water simultaneously,
A. take a sample and measure: get the waste water sample respectively as calibration set waste water sample and forecast set waste water sample, wherein calibration set waste water sample is at least 70 parts; Measure the COD standard value of described calibration set waste water sample and measure its BOD standard value with reference to GB11914-89 (mensuration-dichromate titration of water quality-chemical oxygen demand (COD)) then with reference to standard GB 7488-87 (mensuration-dilution and the inocalation method of water quality-five-day BOD (BOD5)); Gather the near infrared spectrum data of this calibration set waste water sample simultaneously;
B. modeling: above-mentioned near infrared spectrum data is converted into the JCAMP-DX form, again with described data importing in The Unscrambler 9.7 softwares, again the data of described importing software are carried out the convolution smoothing processing, then the COD of the above-mentioned waste water sample that records and BOD standard value are copied to carry out in the described software related; Adopt the PLS1 algorithm then, and adopt " picking one " cross validation method to obtain the PLS1 regression model of COD and BOD simultaneously;
C. forecast model: the near infrared light spectrogram that scans the unknown waste water sample of above-mentioned forecast set, utilize the PLS1 regression model match retrieval of above-mentioned foundation to obtain COD value, the BOD value of the unknown waste water sample of forecast set, the value that records with standard method compares predicts qualified i.e. use;
D. measure COD value, the BOD value of unknown waste water simultaneously: utilize after the above-mentioned prediction COD value, the BOD value of the unknown waste water of model index; In the COD and BOD standard value range of the COD of described unknown waste water and the BOD value water sample that detects in above-mentioned sampling and determination step.
Certainly, the waste water sample that the inventive method is gathered in modeling process is many more, and its COD and BOD standard value scope of statistics are wide more, and the unknown waste water scope that is suitable for after the modeling is many more, and it is just wide more to be applicability; The present invention is specially adapted to monitor the situation of change of its waste water COD of same sewage draining exit and BOD value.
The present invention has following beneficial effect:
When having realized the COD of waste water and BOD value, the inventive method measures, the COD and the BOD Value Operations of the model detection waste water that employing the inventive method is set up are easy, can realize that real-time online detects, detection speed is fast, favorable reproducibility, precision height, and do not produce secondary pollution, increased substantially quality and efficient that waste water detects.
Description of drawings
Fig. 1: the near infrared light spectrogram that is 120 wastewater samples; Horizontal ordinate: λ/nm, ordinate: A.
Fig. 2: be the standard value of COD and the scatter diagram of model predication value.
Fig. 3: be the standard value of BOD and the scatter diagram of model predication value.
Fig. 4: COD number of principal components and equal graphs of a relation of square residual error.
Fig. 5: BOD number of principal components and equal graphs of a relation of square residual error.
Embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in art can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
Embodiment 1
A kind of method of measuring COD and BOD in the waste water simultaneously,
A. gather water sample
The waste water water sampling utilizes 120 of glassware water samplings at 10 different dry points respectively from sanitary sewage place, Fuling, Chongqing.Method for fetching water according to environmental monitoring (Shen Xue is excellent for Wu Zhongbiao, Wu Zucheng. " environmental monitoring ", Beijing: Chemical Industry Press, 2003:96-97) method is carried out.
B. measure the COD and the BOD standard value of waste water water sample
The individual water sample of gathering in 120 (wherein the calibration set sample 110,10 in forecast set sample) is divided into 3 groups behind the 15min quiescent setting, measure its COD chemical score for first group, measures its BOD value for second group, gathers its near infrared spectrum for the 3rd group.The COD chemical score is measured with reference to GB11914-89 (mensuration-dichromate titration of water quality-chemical oxygen demand (COD)).The mensuration of BOD chemical score is measured with reference to standard GB 7488-87 (mensuration-dilution and the inocalation method of water quality-five-day BOD (BOD5)).The scope of COD that records and BOD standard value is respectively: 28.4～528.0mg.L
-1With 16.0～305.2mg.L
-1
C. scan water sample near infrared light spectrogram
Use the 1cm quartz sample pool, with the air is blank, near infrared region interscan water sample at wavelength 800～1800nm, wavelength interval 2nm, it is 2nm that slit is set, and choosing PbS gain is 2, and sweep velocity is 1500nm/s, each sample scanning is averaged to the near infrared light spectrogram of water sample for 3 times, sees Fig. 1.
D. the foundation of mathematical model
(1) spectrum pre-service
The near infrared spectrum intensity data of above-mentioned scanning gained is converted into the JCAMP-DX form by UV Wavelength Scan file layout, again with this data importing in The Unscrambler 9.7 softwares, spectrum is carried out convolution level and smooth (S.Goly Smoothing) handle (seeing Table 1), with the elimination noise, optimize spectral signal, for further calibration model lays the first stone.Certainly here also
Can take the preprocess method of first order derivative (level and smooth), second derivative (level and smooth) at 9 at 9.
(2) foundation of model and optimization
The above-mentioned COD that records and BOD standard value copied to from the Excel form carry out relatedly above-mentioned The Unscrambler 9.7 softwares, adopt PLS1 algorithm and cross validation (Cross-validation) method to set up the PLS1 regression model of measuring COD and BOD; The cross validation method of present embodiment is to adopt lever value (Leverage) and these 2 parameters of chemical score error (Residual) to reject the exceptional value of spectrum and chemical score respectively, obtain the PLS1 regression model, this model related coefficient adopts 0.9542 and 0.9652 respectively, and the prediction relative deviation (RMSEP) of model is respectively 25.24mg.L
-1And 12.13mg.L
-1(opinion) as the level and smooth pre-service of convolution in the table 1.The scatter diagram of the standard value of this model (measured) and model predication value (predicted) and their corresponding number of principal components (PCs) are seen accompanying drawing 2,3,4 and accompanying drawing 5 respectively with equal relations of square residual error.
The number reason index of table 1 biochemical oxygen demand and chemical oxygen demand (COD) calibration model
Table?1?Mathematical?statistics?results?for?calibration?models?of?BOD?and?COD
E. measure in the time of unknown COD value of waste water and BOD value and checking
(1) biochemical oxygen demand (BOD) in 10 wastewater samples that have neither part nor lot in modeling and chemical oxygen demand (COD) (COD) are detected: the near infrared light spectrogram that scans unknown wastewater sample, the near infrared spectrum data of gained is imported in above-mentioned The Unscrambler 9.7 softwares, on the PLS1 of above-mentioned foundation regression model basis, utilize the automatic match retrieval of described software, obtain COD value, BOD value in the waste water, further, to 10 samples predict the outcome and the bilateral t of pairing check has been carried out in standard method, finished by origin 6.0 softwares, assay shows t
COD=0.6437, t
BOD=0.5297, p
COD=0.6092, p
BOD=0.6092, P wherein
CODAnd p
BODAll be far longer than 0.05, thus when level of significance greater than 0.05 the time, there is not significant difference in two kinds of assay methods, show that there is not systematic error in two kinds of methods, detailed results is shown in Table 2.
Table 2 mathematical model predicts the outcome to forecast set
Table2?Predicted?results?of?the?prediction?samples
(2) precision checking
Same sample is carried out 10 scanning, obtain 10 near infrared light spectrograms, utilize the above-mentioned model of having set up that 10 spectrograms are predicted that the result is as shown in table 3.Prediction COD and BOD relative standard deviation (RSD) are respectively 1.48% and 1.66% (n=10), visible precision is good, the sample determination result repeated fine.
Table 3 precision experiment (n=10)
Table?3?The?precision?test(n＝10)
Claims (10)
1. method of measuring COD and BOD in the waste water simultaneously is characterized in that: said method comprising the steps of:
A. take a sample and measure: get the waste water sample, measure the COD standard value and the BOD standard value of described waste water sample, gather its near infrared spectrum data simultaneously with standard method;
B. modeling: it is related to utilize software that the COD standard value of described waste water sample and the BOD standard value and the near infrared spectrum data of described waste water sample are carried out, and adopts software to set up the PLS1 regression model of this COD, BOD respectively then;
C. measure COD value, the BOD value of unknown waste water simultaneously: COD value, the BOD value of utilizing the unknown waste water of model index of described foundation; In the COD and BOD standard value range of the COD of described unknown waste water and the BOD value water sample that detects in described sampling and determination step.
2. the method for claim 1, it is characterized in that: it is spectrochemistry metrology class process software that described modeling process carries out related used software with the COD standard value of waste water sample with BOD standard value and its near infrared spectrum data.
3. method as claimed in claim 2 is characterized in that: described software is The Unscrambler 9.7 softwares.
4. as claim 1,2 or 3 described methods, it is characterized in that: the association in the described modeling process is at first the near infrared spectrum data that records to be converted into the JCAMP-DX form, again with described data importing in The Unscrambler 9.7 softwares, then the COD of the described waste water sample that records and BOD standard value are copied to carry out in the software related.
5. method as claimed in claim 4, it is characterized in that: also described near infrared spectrum data is carried out pre-service after in the described modeling process near infrared spectrum data being imported TheUnscrambler 9.7 softwares, convolution smoothing processing or 9 smoothing processing of first order derivative or 9 smoothing processing of second derivative are adopted in described pre-service.
6. method as claimed in claim 4 is characterized in that: also described near infrared spectrum data is carried out pre-service after in the described modeling process near infrared spectrum data being imported TheUnscrambler 9.7 softwares, the convolution smoothing processing is adopted in described pre-service.
7. method as claimed in claim 6 is characterized in that: described modeling process also is optimized processing simultaneously, and described optimization process is for adopting the method verification model of cross validation.
8. method as claimed in claim 7 is characterized in that: described cross validation is " picking one " cross validation method, rejects exceptional value in exceptional value in the near infrared spectrum and COD standard value, the BOD standard value respectively according to lever value and chemical score error.
9. method as claimed in claim 8 is characterized in that: described waste water sample COD standard value is for to measure with reference to GB11914-89; The near infrared spectrum of described this water sample of collection, use the 1cm quartz sample pool, with the air is blank, near infrared region interscan wastewater sample at wavelength 800～1800nm, wavelength interval 2nm, it is 2nm that slit is set, choosing PbSgain is 2, sweep velocity is 1500nm/s, and each sample scanning is averaged for 3 times and is the near infrared spectrum of waste water.
10. the method for claim 1 is characterized in that:
A. take a sample and measure: get the waste water sample respectively as calibration set waste water sample and forecast set waste water sample; Measure the COD standard value of described calibration set waste water sample and measure its BOD standard value with reference to GB11914-89 then with reference to standard GB 7488-87; Gather the near infrared spectrum data of described calibration set waste water sample simultaneously;
B. modeling: described near infrared spectrum data is converted into the JCAMP-DX form, again with described data importing in TheUnscrambler 9.7 softwares, again the data of described importing software are carried out the convolution smoothing processing, the COD of the described calibration set waste water sample that will record then and BOD standard value copy to carry out in described The Unscrambler 9.7 softwares related; Adopt the PLS1 algorithm then, and adopt " picking one " cross validation method to obtain the PLS1 regression model of COD and BOD simultaneously;
C. forecast model: the near infrared light spectrogram that scans the unknown waste water sample of described forecast set, utilize the PLS1 regression model match retrieval of described foundation to obtain COD value, the BOD value of the unknown waste water sample of forecast set, the value that records with standard method compares predicts qualified i.e. use;
D. measure COD value, the BOD value of unknown waste water simultaneously: utilize after the described prediction COD value, the BOD value of the unknown waste water of model index; The COD of described unknown waste water and BOD value will be in above-mentioned sampling and determination steps in the COD and BOD standard value range of the water sample that detects.
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| CN102128808A (en) * | 2010-12-31 | 2011-07-20 | 上海衡伟信息技术有限公司 | Method for quickly identifying potassium hydrogen phthalate in surface water |
| CN102586503A (en) * | 2012-01-18 | 2012-07-18 | 朗盛（无锡）化工有限公司 | Method for treating leather by using tannery wastewater and method for producing leather |
| CN103175805A (en) * | 2013-03-11 | 2013-06-26 | 楚广诣 | Method for determining indexes of COD and BOD5 in sewage through near infrared spectrometry |
| 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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| CN102128808A (en) * | 2010-12-31 | 2011-07-20 | 上海衡伟信息技术有限公司 | Method for quickly identifying potassium hydrogen phthalate in surface water |
| CN102128808B (en) * | 2010-12-31 | 2012-12-05 | 上海衡伟信息技术有限公司 | Method for quickly identifying potassium hydrogen phthalate in surface water |
| CN102586503A (en) * | 2012-01-18 | 2012-07-18 | 朗盛（无锡）化工有限公司 | Method for treating leather by using tannery wastewater and method for producing leather |
| WO2013107293A1 (en) * | 2012-01-18 | 2013-07-25 | 朗盛（常州）有限公司 | Method for treating leather by using leather production wastewater and method for producing leather |
| CN102586503B (en) * | 2012-01-18 | 2014-02-26 | 朗盛（常州）有限公司 | Method for treating leather by using tannery wastewater and method for producing leather |
| CN103175805A (en) * | 2013-03-11 | 2013-06-26 | 楚广诣 | Method for determining indexes of COD and BOD5 in sewage through near infrared spectrometry |
| CN103175805B (en) * | 2013-03-11 | 2015-04-29 | 楚广诣 | Method for determining indexes of COD and BOD5 in sewage through near infrared spectrometry |
| 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 |
| CN104034660A (en) * | 2014-06-13 | 2014-09-10 | 长沙理工大学 | Method for testing photocatalytic degradation effect on oil leakage-polluted pavement surface |
| 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 |
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Application publication date: 20101208 |