CN111537420B - Method for online determination of pore complexity of particulate matter in water - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000011148 porous material Substances 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000013618 particulate matter Substances 0.000 title claims description 9
- 239000002245 particle Substances 0.000 claims abstract description 40
- 239000000725 suspension Substances 0.000 claims abstract description 26
- 239000000523 sample Substances 0.000 claims abstract description 16
- 238000012360 testing method Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 11
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- 230000003595 spectral effect Effects 0.000 claims description 13
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- 238000012546 transfer Methods 0.000 claims description 7
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- 238000004458 analytical method Methods 0.000 claims description 3
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- 238000005259 measurement Methods 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 2
- 238000000844 transformation Methods 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000012423 maintenance Methods 0.000 abstract description 2
- 238000010223 real-time analysis Methods 0.000 abstract description 2
- 239000010802 sludge Substances 0.000 description 17
- 238000003556 assay Methods 0.000 description 6
- 238000004364 calculation method Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 238000002591 computed tomography Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229920002401 polyacrylamide Polymers 0.000 description 3
- HJPIFBJPTYTSEX-UHFFFAOYSA-N 2h-tetracen-1-one Chemical compound C1=CC=C2C=C(C=C3C(=O)CC=CC3=C3)C3=CC2=C1 HJPIFBJPTYTSEX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- MSNWSDPPULHLDL-UHFFFAOYSA-K ferric hydroxide Chemical compound [OH-].[OH-].[OH-].[Fe+3] MSNWSDPPULHLDL-UHFFFAOYSA-K 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The invention discloses an on-line determination method for underwater particlesA method for determining the complexity of object pores belongs to the technical field of environmental protection and aims to solve the problems that the existing method is difficult to meet the actual online control requirement and the like. The invention utilizes an electrochemical impedance meter connected with a conductive electrode to carry out real-time frequency scanning on a particle suspension, and particle spectrum dimension d formed by impedance feedback signals in the scanning process s The complexity of the particle pores is represented, and the probability that the same electron appears at the same position and the spectrum dimension d of the particle impedance feedback signal are assumed to be random walking of the electron in the pores in the scanning process s And (4) directly associating. d s Larger means that the probability of electrons appearing at the same location in the pore is smaller, corresponding to a more complex pore structure. The invention does not need to specially process the sample during the test, only inserts the electrode probe into the particle suspension to be tested for frequency scanning, has relatively simple equipment maintenance, and can better meet the requirement of real-time analysis and control of the particles in the water.
Description
Technical Field
The invention relates to a method for online measuring the complexity of pores of particulate matters in water, belonging to the technical field of environmental protection.
Background
The complexity of the pores of particles (such as activated sludge) in water has a remarkable influence on the processes of adsorption, filtration and the like of the particles, and is also related to the migration and conversion of pollutants in water. Therefore, the real-time determination of the pore complexity of the particles in the water is of great significance to the control of these processes. The current methods for characterizing the particle pores in water mainly comprise a specific surface area measuring method, a microscopic image method, an electronic Computed Tomography (CT) scanning method and the like. The specific surface area measurement method is to observe a pore structure by pressing gas (such as nitrogen) or non-wetting liquid (such as mercury) into pores of particles, and obtain characteristic parameters such as specific surface area, pore size distribution and the like. Microscopy and CT scanning methods reflect characteristic parameters of pore structure by imaging. However, these methods are complicated in sample preparation process during measurement, difficult to realize on-line test, and expensive in instruments involved in the test process, which limits the practical industrial application.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for measuring the pore complexity of particulate matters in water on line, which aims to bypass the defects of the prior method, utilize electrical equipment connected with a probe to carry out real-time frequency scanning on the particulate matters in the water to obtain impedance feedback signals, and calculate the spectral dimension d of the impedance feedback signals of the particulate matters in the scanning process s Therefore, the pore complexity of the particulate matters is characterized.
The invention can be realized by the following technical approaches:
comprises real-time frequency scanning of the suspension of particles with a commercial electrochemical impedance meter connected with a conductive electrode, assuming that electrons randomly walk in the pores of the particles during the scanning process, and the probability of the same electron appearing at the same position and the spectral dimension d of the particle impedance feedback signal s And (4) directly associating. d s The larger the size, the more disordered the movement track of the electrons in the pores, the more complex the movement path, the smaller the probability of the electrons appearing at the same position of the pores, and the more complex the pore structure corresponding to the particles.
Further, d s The determination comprises the following steps:
(1) During testing, a sample is not required to be specially processed, only the electrode probe is inserted into the suspension of the particles to be tested to carry out frequency scanning so as to obtain the real impedance part, the imaginary impedance part and the complex impedance modulus of the suspension, the complex impedance modulus is corrected, and the critical frequency of the sudden change of the corrected complex impedance modulus is calculated;
(2) Taking the critical frequency and the corrected complex impedance modulus corresponding to the critical frequency as an initial end point, and performing Fourier transform on a frequency-corrected complex impedance modulus curve to obtain a transformed time domain and the amplitude of an impedance signal;
(3) Performing inverse Fourier transform on the obtained time domain-impedance signal amplitude curve to obtain a frequency domain and the square of the impedance signal amplitude;
(4) The spectral dimension of the particulate matter is calculated from a scale-free model of the frequency squared with the amplitude of the impedance signal.
In particular, the concentration range of the particulate matter suspension sample in the substep (1) is 1mg/L-100g/L, the temperature is kept constant during measurement, the sinusoidal voltage applied by the electrochemical impedance meter ranges from 1 mV to 1000mV, and the scanning frequency ranges from 0.1Hz to 10MHz. The method for correcting the complex impedance modulus is that the corrected complex impedance modulus is equal to the complex impedance modulus corresponding to each scanning frequency minus the complex impedance modulus at the highest frequency. The critical frequency is a relative frequency point at which the logarithm value of the corrected complex impedance modulus is changed from approximately constant to decrease along with the increase of the logarithm value of the frequency, and the calculation formula is as follows:
in the formula (f) c Critical frequency for abrupt change of complex impedance modulus, R t And C p The values of the charge transfer resistance and the electric double layer capacitance of the suspension double layer interface can be determined by using R t And C p In series with a charge-transfer resistor R of the suspension c The equivalent circuit of (1) is fitted to the impedance real and imaginary data acquisition.
Further, the unscaled model of the frequency and the square of the impedance signal amplitude in substep (4) is:
in the formula, P is the square of the amplitude of the impedance signal, and f is the scanning frequency after fourier transform and inverse fourier transform. D is s The calculation method of (1) is to use the logarithm value of P as the Y axis and the logarithm value of f as the X axis to plot, and fit the plot by linear regression analysis, and the obtained slope is substituted into the scale-free model between P and f, so as to obtain the spectrum dimension of the particulate matter.
The invention has the beneficial effects that:
compared with the existing method, the method does not need to specially process the sample during testing, only inserts the electrode probe into the particle suspension to be tested to carry out frequency scanning, has relatively simple equipment maintenance, and can better meet the requirement of real-time analysis and control of the particles in the water.
Drawings
FIG. 1 is a schematic diagram of frequency scanning of an aqueous suspension of particulate matter according to the present invention.
In the figure: 1-thermostat, 2-conductive electrode, 3-particle suspension, 4-commercial electrochemical impedance meter, 5-electrochemical impedance meter and connecting wire between electrodes.
Fig. 2 is a schematic diagram of an equivalent circuit according to the present invention.
In the figure: r c Charge-transfer resistance, R, of the suspension t Charge transfer resistance of the electric double layer of the suspension, C p Is an electric double layer capacitor.
Fig. 3 is a schematic diagram of the critical frequency of the present invention.
In the figure: lgZ is the logarithmic value of the corrected complex impedance modulus, lgf is the logarithmic value of the scanning frequency, lgf c Is the logarithmic value of the critical frequency.
Detailed Description
The present invention will be described in detail with reference to the drawings and examples, which are only exemplary and should not be construed as limiting the scope of the present invention. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Frequency scanning test: a commercial electrochemical impedance analyzer with a frequency scanning function is firstly connected with a conductivity electrode as a tool for online testing. The impedance meter is preferably a daily IM3570, the performance parameters of which are described in Table 1. The electrically conductive electrode is preferably a Tetracon 325 electrode, the main performance parameters of which are described in table 2.
TABLE 1 Main Performance parameters Table of impedance Analyzer
TABLE 2 conductivity electrode Primary Performance parameters
| Electrode type | Tetracon 325 |
| Manufacturer of the product | WTW, germany |
| Number of |
4 |
| Material of sensing electrode | Graphite |
| Electrode constant | 0.475cm -1 ±1.5％ |
| Temperature range | -5-100℃ |
As shown in fig. 1, the conductive electrode is used as a probe to be inserted into the suspension of the particles to be measured for frequency scanning, and the insertion depth of the probe is ensured to ensure that the sample is submerged in the contact wafer of the electrode. The concentration of the suspension is 1mg/L-100g/L. During scanning, the impedance instrument applies 1-1000mV sine voltage, the scanning frequency is 0.1Hz-10MHz, the real part, the imaginary part and the complex impedance modulus of the suspension impedance under different frequencies are recorded, and the number of acquisition points is 201.
Equivalent circuit fitting and critical frequency determination: fitting the real part and imaginary part of the obtained impedance by using an equivalent circuit shown in FIG. 2 to obtain the electric double layer charge transfer resistance R of the suspension t And an electric double layer capacitor C p Should comprise the critical frequency of the abrupt change of the complex impedance modulus, preferably 1Hz to 1MHz. The critical frequency of the abrupt change of the complex impedance modulus is the point of the relevant frequency at which the logarithmic value of the corrected complex impedance modulus changes from approximately constant to decreasing with increasing logarithmic value of the frequency, as shown in fig. 3. The calculation formula is as follows:
in the formula (f) c Is the critical frequency of the abrupt change of the complex impedance modulus. To reduce the effect of suspension conductivity, the corrected complex impedance modulus is equal to the corresponding complex impedance modulus at each scanning frequency minus the complex impedance modulus at the highest frequency.
Fourier transform and inverse Fourier transform processing: taking the critical frequency and the corrected complex impedance modulus corresponding to the critical frequency as starting endpoints, performing Fourier transform on a frequency-corrected complex impedance modulus curve to obtain the amplitude of a time domain and an impedance signal after transformation, and then performing inverse Fourier transform on the obtained time domain-impedance signal amplitude curve to obtain the square of the frequency domain and the impedance signal amplitude.
Calculation of spectral dimensions: assuming that the electrons randomly walk in the pores of the particles during the scanning process, the fourier transformed and inverse transformed frequencies and the square of the impedance signal amplitude conform to the following scale-free model:
where P is the square of the amplitude of the impedance signal and f is the scan frequency after fourier and inverse fourier transformation. Plotting the logarithm of P as Y axis and the logarithm of f as X axis, fitting the plot by linear regression analysis, substituting the slope into the scale-free model between P and f to obtain the spectral dimension d of the particulate matter s 。d s Larger means more complex pore structure of the particulate matter.
The steps of fitting of the equivalent circuit, determining the critical frequency, fourier transformation and inverse transformation, calculating the spectral dimension and the like can be realized through programming, so that the test probe is only required to be inserted into the suspension to be tested to obtain the real impedance part, the imaginary impedance part and the complex impedance modulus during frequency scanning in specific implementation, and the pore complexity of the particles in the water can be fed back on line through the designed program steps.
The invention is further illustrated by the following examples:
the first embodiment is as follows:
taking activated sludge (marked as sludge 1) as particles to be measured from a membrane bioreactor of which the daily treated water amount is 10 ten thousand tons in a certain regeneration water plant (marked as regeneration water plant 1) in Beijing. The sludge concentration was 17.9g/L. Other assay procedures were as described in the detailed description. The lgP and lgf obtained are shown in Table 3. The resulting spectral dimension of sludge 1 was 1.826.
Example two:
excess activated sludge (marked as sludge 2) is taken as particles to be detected from an anaerobic/anoxic/aerobic biological reaction process with daily treatment water amount of 20 ten thousand tons in a certain regeneration water plant (marked as regeneration water plant 2) in Beijing. The sludge concentration was 18.1g/L. Other assay procedures were as described in the detailed description. The lgP and lgf obtained are shown in Table 3. The spectral dimension of the obtained sludge 2 was 1.811.
Example three:
taking residual activated sludge (marked as sludge 3) as particles to be measured from an anaerobic/aerobic biological reaction process in which the daily treatment water amount of a certain reclaimed water plant (marked as reclaimed water plant 3) in Beijing is 100 ten thousand tons. The sludge concentration is 18g/L. Other assay procedures were as described in the detailed description. The lgP and lgf obtained are shown in Table 3. The resulting sludge 3 has a spectral dimension of 1.819.
Example four:
taking residual activated sludge (marked as sludge 4) as particles to be measured from an oxidation ditch biological reaction process of which the daily treatment water amount of a certain reclaimed water plant (marked as reclaimed water plant 4) in Beijing is 20 ten thousand tons. The sludge concentration is 18.5g/L. Other assay procedures were as described in the detailed description. The lgP and lgf obtained are shown in Table 3. The resulting sludge 4 has a spectral dimension of 1.831.
Example five:
preparing a suspension of polyacrylamide cross-linked ferric hydroxide gel (FHG-PAM) particles as the particles to be measured. The particle concentration was 3.25g/L. Other assay procedures were as described in the detailed description. The lgP and lgf obtained are shown in Table 3. The spectral dimension of the obtained FHG-PAM is 1.969.
Example six:
a suspension of Cationic Hydrogel (CH) particles was prepared as the particulate material to be tested. The particle concentration was 0.2g/L. Other assay procedures were as described in the detailed description. The lgP and lgf obtained are shown in Table 3. The resulting spectral dimension of CH is 1.916.
Table 3 lgP and lgf obtained by testing in examples
Claims (6)
1. A method for on-line measuring the complexity of the pores of particles in water includes such steps as using a commercial electrochemical impedance meter connected with electric conducting electrodes to test the suspension of particles, and features that the spectrum dimension d of particles is formed by the impedance feedback signals during electric frequency scan s The complexity of the particle pores is represented, and if electrons randomly walk in the particle pores in the scanning process, the same electron appears at the same positionProbability of and d s Direct association, d s Larger means that the electron moves in the pore with a disordered track, the more complex the movement path, the lower the probability of the electron appearing in the same position of the pore, and the more complex the pore structure corresponding to the particle, wherein the spectrum dimension d s The test of (2) comprises the following steps:
(1) During testing, a sample is not required to be specially processed, only the electrode probe is inserted into the particle suspension to be tested to carry out frequency scanning so as to obtain the real part and imaginary part of the impedance of the suspension and the complex impedance modulus, the complex impedance modulus is corrected, and the critical frequency f of the sudden change of the corrected complex impedance modulus is calculated c ；
(2) At a critical frequency f c Taking the corrected complex impedance modulus as an initial end point, and performing Fourier transform on the frequency-corrected complex impedance modulus curve to obtain a transformed time domain and the amplitude of the impedance signal;
(3) Performing inverse Fourier transform on the obtained time domain-impedance signal amplitude curve to obtain a frequency domain f and a square P of the impedance signal amplitude;
(4) The spectral dimension ds of the particulate matter is calculated from a scale-free model of the frequency f and the square P of the amplitude of the impedance signal.
2. The method of claim 1, wherein the sample of the suspension of particles has a concentration ranging from 1mg/L to 100g/L, the temperature is kept constant during the measurement, the sinusoidal voltage applied by the electrochemical impedance meter ranges from 1 mV to 1000mV, and the scanning frequency ranges from 0.1Hz to 10MHz.
3. The method of claim 1, wherein the complex impedance modulus is corrected by subtracting the complex impedance modulus at the highest frequency from the corresponding complex impedance modulus at each scanning frequency.
4. The method of claim 1, wherein the critical frequency is a point at which the logarithm of the complex impedance modulus changes from approximately constant to decreasing with increasing logarithm of the frequency, and is calculated as:
in the formula (f) c Critical frequency, R, for the abrupt change of complex impedance modulus t And C p Charge transfer resistance and electric double layer capacitance of the suspension double layer interface respectively, the value of which is determined by using R t And C p In series with a charge-transfer resistor R of the suspension c The equivalent circuit of (1) is fitted to the impedance real and imaginary data acquisition.
5. The method of claim 1, wherein the frequency and impedance signal amplitude squared unscaled model is:
in the formula, P is the square of the amplitude of the impedance signal, and f is the scanning frequency after fourier transform and inverse fourier transform.
6. The method of claim 1, wherein the particle spectrum dimension is calculated by plotting the logarithm of the square of the impedance signal amplitude, P, on the Y-axis and the logarithm of the scan frequency, f, after fourier and inverse fourier transformations, on the X-axis, fitting the plot using linear regression analysis, and substituting the resulting slope into a scale-free model between P and f.
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