CN105891148A - Method for measuring VFA concentration in anaerobic wastewater treatment process by means of near infrared spectrum - Google Patents
Method for measuring VFA concentration in anaerobic wastewater treatment process by means of near infrared spectrum Download PDFInfo
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- CN105891148A CN105891148A CN201610196010.6A CN201610196010A CN105891148A CN 105891148 A CN105891148 A CN 105891148A CN 201610196010 A CN201610196010 A CN 201610196010A CN 105891148 A CN105891148 A CN 105891148A
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- near infrared
- water sample
- vfa
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- waste water
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- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 19
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 14
- 239000002351 wastewater Substances 0.000 claims abstract description 33
- 238000001228 spectrum Methods 0.000 claims abstract description 10
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 18
- 230000009466 transformation Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 239000010865 sewage Substances 0.000 claims description 5
- 238000004611 spectroscopical analysis Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 230000003595 spectral effect Effects 0.000 claims description 2
- 238000011156 evaluation Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 5
- 238000012544 monitoring process Methods 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
Abstract
A method for measuring the VFA concentration in the anaerobic wastewater treatment process by means of near infrared spectrum comprises the steps of 1, taking N wastewater samples in the anaerobic wastewater treatment process within the typical cycle, measuring the VFA concentration of the N wastewater samples with the gas chromatographic method, and measuring the original near infrared spectrum of the N wastewater samples by means of an near infrared spectrometer; 2, pretreating original near infrared spectrum data through wavelet transform; 3, establishing a calibration model based on the VFA concentration of the N wastewater samples and a pretreated spectrogram by means of interval partial least squares, calculating the correlation coefficient, adopting the calibration model when the correlation coefficient is larger than or equal to 0.945, and repeating step 1-3 and conducting modeling again and correlation evaluation otherwise; 4, measuring the original near infrared spectrum of a wastewater sample to be measured, conducting pretreatment, and substituting pretreated spectrum data into the calibration model to obtain a VFA concentration value. The method is convenient to operate, low in cost, environmentally friendly, and capable of obtaining a result quickly and effectively.
Description
Technical field
The present invention relates to waste water process and monitoring technical field, particularly relate to one and utilize near infrared spectrum
The method of VFA concentration during mensuration Anaerobic wastewater treatment.
Background technology
Anaerobic treatment is one of conventional means of waste water process, in order to realize anti-during anaerobic treatment
Answer the control of device stable operation, need intermediate product VFA (the volatile fatty in anaerobic reaction
Acid, i.e. volatile fatty acid) realize monitoring, and traditional chemical analysis method is time-consuming, effort, stagnant
After, and consumed medicament is easily generated secondary pollution.Therefore, this area urgently research and develop new right
The method that during Anaerobic wastewater treatment, VFA carries out detecting.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of easy and simple to handle, low cost, environmental protection, can
Rapidly and efficiently obtain the method for VFA concentration in Anaerobic wastewater treatment process water sample that measures of result, main
Near infrared spectrum scanning to be combined and chemometrics application.
For achieving the above object, the technical scheme that the present invention provides is as follows:
A kind of utilize the method for VFA concentration during near infrared ray Anaerobic wastewater treatment, bag
Include following steps:
(1) the waste water water sample chosen during Anaerobic wastewater treatment in typical cycle is N number of, uses gas
Phase chromatography measures the concentration of the VFA of this N number of water sample, then measures this N by near infrared spectrometer
The near-infrared original spectrum of individual water sample；
(2) utilize wavelet transformation that the near-infrared original spectral data obtained is carried out pretreatment, obtain
Pretreated spectrogram；
(3) use interval partial least square, utilize VFA concentration and this N of this N number of water sample
The pretreated spectrogram of individual water sample, sets up the calibration model of the near infrared spectrum data of sewage sample,
And computational theory value and the correlation coefficient of measured value, this straightening die is used when correlation coefficient >=0.945
Type, otherwise repeats the operation of step (1)-(3), again models and evaluate dependency；
(4) the reddest of waste water water sample to be measured is measured according to the method that step (1) is identical with in (2)
Outer original spectrum, and preprocessed obtain pretreated spectrogram, after the pretreatment that then will obtain
Spectroscopic data substitute into described calibration model, obtain the VFA concentration value of waste water water sample to be measured.
Wherein, described VFA (volatile fatty acid) i.e. volatile fatty acid, it is at waste water
Intermediate product during reason anaerobic reaction.
During described Anaerobic wastewater treatment, the waste water water sample in typical cycle is those skilled in the art
Content easy to understand, it i.e. refers to the waste water gathered in general anaerobic treatment process carries out the cycle
Water sample.
Wherein, it should be readily apparent to one skilled in the art that N is necessary for positive integer, it is preferable that N takes
Value scope is 50 ＜ N ＜ 80, most preferably N=60.
Equally, it should be readily apparent to one skilled in the art that heretofore described correlation coefficient≤1.
Wherein, described pretreatment is preferably and uses the wavelet transformation original near infrared light to wastewater sample
Modal data carries out denoising.
The corresponding interval of the preferred VFA of described calibration model is 7394.15-7814.58cm-1。
Described waste water water sample the most all through filtration treatment, with remove the float in waste water water sample and
Impurity, more preferably carries out filtration treatment through 0.45 μm filter membrane.
The preferred BRUKER of near infrared spectrometer (originating from Germany, commercially available brand) used in the present invention
Fourier Transform Near Infrared instrument, wherein, more preferably instrument scanning wave-number range is 4000-12500
cm-1, resolution is 8cm-1, scanning times is 32 times.
The present invention also provide for above-mentioned utilize near infrared ray Anaerobic wastewater treatment during VFA dense
The application in water treatment field of the method for degree.
On the basis of meeting common sense in the field, above-mentioned each optimum condition, can combination in any, obtain this
Invent each preferred embodiments.
Agents useful for same of the present invention and raw material are the most commercially.
The most progressive effect of the present invention is:
The detection method of the present invention is quick, convenient, for the real-time monitoring of anaerobic reactor operation conditions
Significant with regulation and control.Monitor the operation conditions of anaerobic reactor by the method for the present invention, have
High efficiency, easy and simple to handle, the feature such as pollution-free, there is stronger practicality simultaneously.
The characteristic wave bands of the method for building up employing interval partial least square selection VFA of model, and
Carry out method of least square (PLS) in selected wave band interval to return, obtain the near infrared light of degree of precision
Spectrum detection model, the VFA correlation coefficient of calibration model is higher.The waste water water sample of unknown concentration value is surveyed
Its near infrared spectrum data fixed is gone forward side by side after line number Data preprocess, substitutes into calibration model, can directly obtain not
Know the concentration value of VFA in waste water water sample.Therefore, the method for the present invention has efficient, convenient, knot
Fruit service advantages accurately, and without other chemical reagent during detection, solve traditional detection
Time-consuming length, big energy-consuming, cost height and secondary pollution problems in method.
Accompanying drawing explanation
Fig. 1 is the near-infrared primary light spectrogram of water sample in embodiment 1；
Fig. 2 is the near infrared light spectrogram of Wavelet Denoising Method in embodiment 1；
Fig. 3 is VFA calibration model in embodiment 1；
Fig. 4 is VFA forecast model in embodiment 1.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with concrete real
Execute example, and referring to the drawings, the present invention is described in further detail.
Embodiment 1
The method of VFA concentration in anaerobic waste water biological treatment process that measures of the present embodiment includes as follows
Concrete steps:
(1) the waste water water sample chosen in anaerobic waste water biological treatment process in typical cycle 84.Its
In, 60 water samples, first with the concentration value of VFA in Water By Gas Chromatography sample, then gather water sample
Near infrared spectrum, obtain original near infrared spectrum data (as shown in Figure 1)；
(2) utilize wavelet transformation that original spectrum carries out pretreatment, remove a part in original spectrum
Noise and irrelevant information, obtain near infrared light spectrogram (as shown in Figure 2) after pretreatment；
(3) use interval partial least square, utilize the VFA concentration of these 60 water samples with this 60
The pretreated spectrogram of individual water sample, sets up the calibration model of the near infrared spectrum data of sewage sample,
Evaluating measured value and the dependency of theoretical value, obtaining correlation coefficient was 0.945 (as shown in Figure 3)；
(4) take and have neither part nor lot in the cycle water sample 24 of modeling, measure its near infrared spectrum, repeat step
(2) after, obtain spectroscopic data after the pretreatment of water sample, substitute into calibration model, obtain the dense of VFA
Degree.The true value relatedness that its value and chemical method record is as shown in Figure 4.
Wherein, in described calibration model, the corresponding interval of VFA is 7394.15-7814.58cm-1。
Described waste water water sample all carries out filtration treatment through 0.45 μm filter membrane, to remove waste water water sample
In float and impurity.
Described near infrared spectrometer is BRUKER Fourier Transform Near Infrared instrument；Wherein,
Instrument scanning wave-number range is 4000-12500cm-1, resolution is 8cm-1, scanning times is 32
Secondary.
By Fig. 3 and Fig. 4 it can be seen that the correlation coefficient (rc) of VFA timing is reached by institute's established model
0.9450, correction root-mean-square error (RMSECV) is respectively 0.5413；Correlation coefficient (rp ') during prediction
It is respectively 0.8888, it was predicted that root-mean-square error (RMSEP ') is respectively 0.1434.Result shows, correction
Model prediction excellent performance.
Embodiment 2
The method of VFA concentration in anaerobic waste water biological treatment process that measures of the present embodiment includes as follows
Concrete steps:
(1) the waste water water sample chosen in anaerobic waste water biological treatment process in typical cycle 84.Its
In, 60 water samples, first with the concentration value of VFA in Water By Gas Chromatography sample, then gather water sample
Near infrared spectrum, obtain original near infrared spectrum data；
(2) utilize wavelet transformation that original spectrum carries out pretreatment, remove a part in original spectrum
Noise and irrelevant information, obtain near infrared light spectrogram after pretreatment；
(3) use interval partial least square, utilize the VFA concentration of these 60 water samples with this 60
The pretreated spectrogram of individual water sample, sets up the calibration model of the near infrared spectrum data of sewage sample,
Evaluating measured value and the dependency of theoretical value, obtaining correlation coefficient is 0.95；
(4) take and have neither part nor lot in the cycle water sample 24 of modeling, measure its near infrared spectrum, repeat step
(2) after, obtain spectroscopic data after the pretreatment of water sample, substitute into calibration model, obtain the dense of VFA
Degree.The true value relatedness that its value and chemical method record is good, and correlation coefficient is high.
As can be seen from the above-described embodiment, the method for the present invention is applied to the sewage water of water treatment field
Sample detects, and obtains result quick, convenient, monitoring in real time and adjusting for anaerobic reactor operation conditions
Control significant.
The method of the present invention has efficient, convenient, result service advantages accurately, and detects process
In without other chemical reagent, solve the time-consuming length in traditional detection method, big energy-consuming, cost high
And secondary pollution problems.
Particular embodiments described above, is carried out the purpose of the present invention, technical scheme and beneficial effect
Further describe it should be understood that the foregoing is only the specific embodiment of the present invention,
Be not limited to the present invention, all within the spirit and principles in the present invention, any amendment of being made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. utilize a method for VFA concentration during near infrared ray Anaerobic wastewater treatment,
It is characterized in that: comprise the steps:
(1) the waste water water sample chosen during Anaerobic wastewater treatment in typical cycle is N number of, uses gas
Phase chromatography measures the concentration of the VFA of this N number of water sample, then measures this N by near infrared spectrometer
The near-infrared original spectrum of individual water sample；
(2) utilize wavelet transformation that the near-infrared original spectral data obtained is carried out pretreatment, obtain
Pretreated spectrogram；
(3) use interval partial least square, utilize VFA concentration and this N of this N number of water sample
The pretreated spectrogram of individual water sample, sets up the calibration model of the near infrared spectrum data of sewage sample,
And computational theory value and the correlation coefficient of measured value, this straightening die is used when correlation coefficient >=0.945
Type, otherwise repeats the operation of step (1)-(3), again models and evaluate dependency；
(4) the reddest of waste water water sample to be measured is measured according to the method that step (1) is identical with in (2)
Outer original spectrum, and preprocessed obtain pretreated spectrogram, after the pretreatment that then will obtain
Spectroscopic data substitute into described calibration model, obtain the VFA concentration value of waste water water sample to be measured.
Method the most according to claim 1, it is characterised in that: wherein, the span of N
It is 50 ＜ N ＜ 80.
Method the most according to claim 2, it is characterised in that: N=60.
Method the most according to claim 1, it is characterised in that: described pretreatment is for using
Wavelet transformation carries out denoising to the original near infrared spectrum data of wastewater sample.
Method the most according to claim 1, it is characterised in that: VFA in described calibration model
Corresponding interval be 7394.15-7814.58cm-1。
Method the most according to claim 1, it is characterised in that: the described equal warp of waste water water sample
Cross filtration treatment, to remove the float in waste water water sample and impurity.
Method the most according to claim 6, it is characterised in that: the described equal warp of waste water water sample
Cross 0.45 μm filter membrane and carry out filtration treatment.
Method the most according to claim 1, it is characterised in that: described near infrared spectrometer
For BRUKER Fourier Transform Near Infrared instrument.
Method the most according to claim 8, it is characterised in that: wherein, instrument scanning wave number
Scope is 4000-12500cm-1, resolution is 8cm-1, scanning times is 32 times.
10. utilize near infrared ray Anaerobic wastewater treatment mistake described in any one of claim 1～9
The method of VFA concentration application in water treatment field in journey.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108872144A (en) * | 2018-09-13 | 2018-11-23 | 中国农业大学 | A kind of on-Line Monitor Device for anaerobic digestion process |
| CN109136083A (en) * | 2018-09-13 | 2019-01-04 | 中国农业大学 | A kind of anaerobic digestion process on-line monitoring system |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872144A (en) * | 2018-09-13 | 2018-11-23 | 中国农业大学 | A kind of on-Line Monitor Device for anaerobic digestion process |
| CN109136083A (en) * | 2018-09-13 | 2019-01-04 | 中国农业大学 | A kind of anaerobic digestion process on-line monitoring system |
| CN109136083B (en) * | 2018-09-13 | 2021-08-27 | 中国农业大学 | Anaerobic digestion process on-line monitoring system |
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