CN110672486A - Method for accurately measuring surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene - Google Patents
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- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 title claims abstract description 149
- 239000010802 sludge Substances 0.000 title claims abstract description 116
- 238000000034 method Methods 0.000 title claims abstract description 38
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000006228 supernatant Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 34
- 238000002835 absorbance Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000002798 spectrophotometry method Methods 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 abstract description 8
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 125000001792 phenanthrenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C=CC12)* 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method for accurately measuring the surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene. Centrifuging a collected sludge sample for three times by using a dimethyl sulfoxide solution, resuspending the centrifuged sludge sample by using the dimethyl sulfoxide solution, adding the suspended sludge sample into a phenanthrene solution, slightly mixing, and standing for a period of time; taking a sludge sample after light mixing to measure VSS, taking supernatant after standing for a period of time for centrifugation, taking a certain volume of supernatant after centrifugation to dilute the supernatant in dimethyl sulfoxide solution, and measuring the concentration of phenanthrene by using an ultraviolet spectrophotometer; and finally, the surface hydrophobicity of the aerobic granular sludge is equal to the ratio of the concentration difference of phenanthrene to VSS. The method can accurately measure the surface hydrophobicity of the sludge, and is an improved method for measuring the surface hydrophobicity of the aerobic granular sludge.
Description
Technical Field
The invention relates to a method for accurately measuring the surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene, belonging to the field of biological treatment of wastewater.
Background
With respect to surface hydrophobicity of aerobic granular sludge, according to the theory of thermodynamics, increased cell hydrophobicity promotes self-aggregation of cells by decreasing intracellular gibbs free energy. On the other hand, the increase of the cell hydrophobicity improves the sludge-water separation efficiency of the aerobic granular sludge, thereby reducing the occupied area and the operation cost. Thus, cell hydrophobicity is an important parameter in determining microbial interactions and is also a determining factor in affecting sludge structure.
The current methods for representing hydrophobicity mainly comprise three methods of contact angle measurement, an alkane distribution method and a phenanthrene adsorption method. Wherein, the contact angle measurement can only measure the contact angle of the sludge within a certain range, and has certain limitation; when the alkane distribution method is used for measuring, the sludge is crushed, and the hydrophobicity of the surface of the sludge cannot be measured; the specific operating steps for the adsorption of phenanthrene by granular sludge are still unclear. Therefore, it is necessary to develop a method for precisely measuring the surface hydrophobicity of the aerobic granular sludge adsorbing phenanthrene.
Disclosure of Invention
The invention aims to provide a method for accurately measuring the surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene, which accurately measures the hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene by the aerobic granular sludge and adopting an ultraviolet spectrophotometer.
The method for accurately measuring the surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene mainly comprises the following steps of (1) collecting and cleaning a sludge sample; (2) suspending; (3) and (3) adsorbing phenanthrene: the method comprises the steps of adding a suspended sludge sample into a phenanthrene solution with the volume fraction of 60%, wherein the solvent of the phenanthrene is dimethyl sulfoxide, lightly mixing and standing, so that the phenanthrene is adsorbed on the sludge sample, and subsequent determination is facilitated; (4) determination of VSS and phenanthrene concentrations; (5) the surface hydrophobicity was calculated.
The technical scheme adopted by the invention is as follows:
the method for accurately measuring the surface hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene comprises the following steps:
step 1: quantitatively transferring a sludge sample into a centrifugal tube, and performing centrifugal solid-liquid separation; then, continuously washing and centrifugally separating the separated sludge for multiple times by using a dimethyl sulfoxide solution;
step 2: quantitatively transferring the dimethyl sulfoxide solution, and completely suspending the sludge after centrifugal separation;
and step 3: quantitatively transferring the dimethyl sulfoxide solution of phenanthrene, adding the dimethyl sulfoxide solution into the suspended sludge sample, and uniformly mixing, wherein the initial phenanthrene concentration in the mixed solution is C0(ii) a Immediately taking the uniformly mixed sludge sample, and measuring the volatile suspended substance VSS of the sludge sample;
and 4, step 4: standing the residual sludge sample after mixing in the dark, quantitatively transferring supernatant into a centrifuge tube, centrifuging, quantitatively transferring supernatant, and determining the concentration of phenanthrene in the supernatant as C by an ultraviolet spectrophotometry;
and 5: calculating (C)0-C)/VSS for characterizing sludge surface hydrophobicity.
Based on the scheme, the following preferred schemes can be adopted for parameters and materials in each step:
preferably, the step 1 specifically comprises the following steps: taking 20mL of sludge sample with the sludge concentration of 3000mg/L into a centrifugal tube, centrifuging at 20000rpm for 1min, and removing impurities in the sludge sample; then centrifuging the sludge for three times by using a dimethyl sulfoxide solution to remove the water in the sludge.
Preferably, in step 1, the volume fraction of the dimethyl sulfoxide solution used in each washing and centrifugation is 2/3, the volume is 10mL, the centrifugation speed is 20000rpm, and the centrifugation time is 1 min.
Preferably, in the step 2, the volume fraction of the dimethyl sulfoxide solution used for suspending the sludge is 2/3, and the volume is 100 mL. .
Preferably, in the step 3, the volume fraction of the solution of phenanthrene in dimethyl sulfoxide is 60%, and the volume is 20 mL.
Preferably, in step 3, the initial phenanthrene concentration in the mixture is also determined by ultraviolet spectrophotometry.
Preferably, in the step 3, the method for measuring the volatile suspended substance VSS comprises: filtering the sludge sample with the volume of V after being uniformly mixed, and drying the sludge sample to constant weight m0Drying the sludge sample and the filter paper again, and weighing the sludge sample and the filter paper as m1(ii) a Then putting the dried sludge sample and filter paper into the drying chamber to be dried to constant weight m2In the crucible, putting the crucible in a muffle furnace, firing the crucible, weighing the crucible as m3Then volatile suspended matter VSS ═ m (m)1+m2-m0-m3)/V。
Preferably, in the step 4, the sludge sample is allowed to stand in the dark for 10 min.
Preferably, in the step 4, the specific measurement process of the ultraviolet spectrophotometry is as follows: and diluting the removed 50 mu L of supernatant into 5mL of dimethylsulfoxide with volume fraction of 2/3, measuring the absorbance of the supernatant at the absorption wavelength by using an ultraviolet spectrophotometer, and calculating the concentration of phenanthrene in the supernatant according to the absorbance and a standard curve.
Preferably, in the step 4, the absorption wavelength in the ultraviolet spectrophotometer is set to 296 nm.
Preferably, the phenanthrene solution is measured by the ultraviolet spectrophotometry within the range of 0-5g/L, and if the phenanthrene solution exceeds the range, the phenanthrene solution needs to be diluted firstly.
The invention has the beneficial effects that:
according to the invention, on the basis of the traditional method for measuring the surface hydrophobicity of the sludge, the surface hydrophobicity of the aerobic granular sludge is accurately measured by adopting the content of phenanthrene adsorbed by the aerobic granular sludge, so that the follow-up effective research is facilitated.
Drawings
FIG. 1 is a flow chart of the method for accurately measuring the surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene.
FIG. 2 is a line marking of the phenanthrene solution measured in the example.
FIG. 3 is an infrared spectrum of a sludge sample after the addition of phenanthrene solution for 0min and 10 min.
Detailed Description
The invention is further illustrated by the following figures and specific examples.
As shown in figure 1, the method for accurately measuring the surface hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene generally comprises the following basic steps: (1) collecting and cleaning a sludge sample; (2) suspending; (3) adsorbing phenanthrene; (4) determination of VSS and phenanthrene concentrations; (5) the surface hydrophobicity was calculated.
The principle of hydrophobicity measurement according to the present invention is as follows:
the aerobic granular sludge is a microbial aggregate with a compact structure and excellent sedimentation, has both hydrophobic groups and hydrophilic groups, has a high hydrophobic group content, and has good adsorption capacity on nonpolar phenanthrene. The hydrophobicity of the surface of the aerobic granular sludge is in positive correlation with the adsorption capacity of the sludge on phenanthrene, and the phenanthrene can be completely dissolved in a dimethyl sulfoxide aqueous solution, so that the functional groups on the surface of the aerobic granular sludge are not affected. Therefore, the hydrophobicity of the sludge surface is represented by the ratio of the concentration difference of phenanthrene in the supernatant to VSS before and after phenanthrene is adsorbed on the surface of the aerobic granular sludge. And measuring absorbance A at 296nm by ultraviolet spectrophotometry296In this case, the phenanthrene concentration is proportional to the absorbance, and the phenanthrene concentration can be converted from the absorbance.
The specific implementation of each step in the method is described in detail below:
(1) step 1, sludge sample collection and cleaning
A20 mL sludge sample (with the sludge concentration of 3000mg/L) is weighed by using a measuring cylinder, centrifuged at 20000rpm in a 50mL centrifuge tube for 1min, and subjected to solid-liquid separation to remove impurities in the sludge sample. Then, a pipetting gun is used for measuring 10mL of dimethyl sulfoxide solution (the solvent is water, the same is applied below) with the volume fraction of 2/3 to be mixed with the precipitated sludge after the previous centrifugation, the mixture is centrifuged again at 20000rpm for 1min, and the mixing-centrifuging process is repeated for 3 times, so that the water in the sludge sample is further removed, and the subsequent suspension is facilitated.
(2) Step 2, suspending
100mL of dimethyl sulfoxide solution with the volume fraction of 2/3 is measured by a measuring cylinder, and the sludge after centrifugation in the step 1 is completely suspended into a 250mL conical flask. The dimethyl sulfoxide solution is selected as a universal solvent in the step, so that phenanthrene can be dissolved in the dimethyl sulfoxide solution when the dimethyl sulfoxide solution is mixed with water, and the phenanthrene can be better adsorbed by sludge. (3) Step 3, adsorption of phenanthrene
And (3) measuring 20mL of 60% phenanthrene solution (the solvent is 2/3 volume fraction aqueous solution of dimethyl sulfoxide) by using a measuring cylinder, and adding the solution into the sludge sample suspended in the step (2) to be lightly mixed uniformly.
(4) Step 4, determination of VSS and phenanthrene concentration
Immediately taking the uniformly mixed sludge sample, and measuring the phenanthrene concentration C of the sludge sample0(the phenanthrene concentration of the solution noted as standing for 0 min) and volatile suspension VSS.
And then, standing the residual sludge sample after mixing in the dark, quantitatively transferring the supernatant into a centrifuge tube, centrifuging, quantitatively transferring the supernatant, and measuring the phenanthrene concentration in the supernatant as C (recording as the phenanthrene concentration of the solution after light mixing for 10 min) by an ultraviolet spectrophotometry.
It was found by the infrared spectroscopy shown in fig. 3 that the phenanthrene solutions of 0min and 10min had little effect on the functional groups on the sludge surface, while the time for standing in the dark was set to 10min in order to prevent photolysis of the phenanthrene, allowing the sludge surface to better adsorb the phenanthrene.
In this step, the specific VSS measurement method is as follows: taking out a uniformly mixed sludge sample with the volume V of 5mL by using a liquid transfer gun, completely filtering the sludge sample, and drying the sludge sample until the weight m is constant0Drying the sludge sample and the filter paper again, and weighing the sludge sample and the filter paper as m1(ii) a Then putting the dried sludge sample and filter paper into the sludge sample and drying the sludge sample and the filter paper in advance to constant weight m2In the crucible, putting the crucible in a muffle furnace, firing the crucible, weighing the crucible as m3Then volatile suspended matter VSS ═ m (m)1+m2-m0-m3)/V。
In this step, the method for specifically determining the phenanthrene concentration is as follows: taking 1mL of the supernatant after 0min and standing for 10min respectively, centrifuging the supernatant in a 2mL centrifuge tube at 20000rpm for 1min, and removing turbidity in the supernatant. After centrifugation, 50. mu.L of the supernatant was taken out by a pipette and diluted in 5mL of 2/3 volume fraction dimethylsulfoxide solution. And (3) measuring the absorbance of the diluent under the absorption wavelength by adopting an ultraviolet spectrophotometer, and then substituting the absorbance into a standard curve for conversion to obtain the corresponding phenanthrene concentration. Wherein, after the full scan of the ultraviolet spectrophotometer, the absorption wavelength used for the measurement can be determined to be 296 nm. FIG. 2 is a marked line of the phenanthrene solution used for measurement in the invention, the working range of the marked line is 0-5g/L, and the marked line has good correlation.
(5) Calculation of surface hydrophobicity
Phenanthrene concentration C obtained as described above0C and VSS values, the ratio of the sludge sample can be calculated: (C)0-C)/VSS, which value is useful for characterizing the sludge surface hydrophobicity.
This example sets up A, B, C three sets of parallel tests, and the final calculated surface hydrophobicity results are as follows:
the surface hydrophobicity of the aerobic granular sludge is phenanthrene concentration difference/VSS.
The variance of the three sets of data is 4.74, which shows that the determination method has better accuracy and reproducibility. It should be noted that the sludge surface hydrophobicity refers to relative hydrophobicity, different samples can respectively calculate corresponding hydrophobicity values according to the method, and the relative size of the hydrophobicity of the sludge sample is determined by comparison.
Claims (10)
1. A method for accurately measuring the surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene is characterized by comprising the following steps:
step 1: quantitatively transferring a sludge sample into a centrifugal tube, and performing centrifugal solid-liquid separation; then, continuously washing and centrifugally separating the separated sludge for multiple times by using a dimethyl sulfoxide solution;
step 2: quantitatively transferring the dimethyl sulfoxide solution, and completely suspending the sludge after centrifugal separation;
and step 3: quantitatively transferring the dimethyl sulfoxide solution of phenanthrene, adding the dimethyl sulfoxide solution into the suspended sludge sample, and uniformly mixing;
and 4, step 4: immediately taking the uniformly mixed sludge sample, and determining the initial phenanthrene concentration to be C0And volatile suspended matter VSS; standing the residual sludge sample after mixing in the dark, quantitatively transferring supernatant into a centrifuge tube, centrifuging, quantitatively transferring supernatant, and determining the concentration of phenanthrene in the supernatant as C by an ultraviolet spectrophotometry;
and 5: calculating (C)0-C)/VSS for characterizing sludge surface hydrophobicity.
2. The method for accurately measuring the surface hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene as claimed in claim 1, wherein the step 1 is implemented by the following steps: taking 20mL of sludge sample with the sludge concentration of 3000mg/L into a centrifugal tube, centrifuging at 20000rpm for 1min, and removing impurities in the sludge sample; then centrifuging the sludge for three times by using a dimethyl sulfoxide solution to remove the water in the sludge.
3. The method for accurately measuring the surface hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene as claimed in claim 1, wherein in the step 1, the volume fraction of the dimethyl sulfoxide solution used for each cleaning and centrifugal separation is 2/3, the volume is 10mL, the centrifugal speed is 20000rpm, and the centrifugal time is 1 min.
4. The method for accurately measuring the surface hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene as claimed in claim 1, wherein in the step 2, the volume fraction of the dimethyl sulfoxide solution used for suspending the sludge is 2/3, and the volume is 100 mL. .
5. The method for accurately measuring the surface hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene as claimed in claim 1, wherein in the step 3, the volume fraction of the dimethyl sulfoxide solution of the phenanthrene is 60%, and the volume is 20 mL.
6. The method for accurately measuring the surface hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene as claimed in claim 1, wherein in the step 3, the initial phenanthrene concentration in the mixed solution is also measured by ultraviolet spectrophotometry.
7. The method for accurately measuring the surface hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene as claimed in claim 1, wherein in the step 3, the method for measuring the volatile suspended substance VSS comprises the following steps: filtering the sludge sample with the volume of V after being uniformly mixed, and drying the sludge sample to constant weight m0Drying the sludge sample and the filter paper again, and weighing the sludge sample and the filter paper as m1(ii) a Then putting the dried sludge sample and filter paper into the drying chamber to be dried to constant weight m2In the crucible, putting the crucible in a muffle furnace, firing the crucible, weighing the crucible as m3Then volatile suspended matter VSS ═ m (m)1+m2-m0-m3)/V。
8. The method for accurately measuring the surface hydrophobicity of the aerobic granular sludge by adsorbing phenanthrene as claimed in claim 1, wherein in the step 4, the sludge sample is kept standing in the dark for 10 min.
9. The method for accurately measuring the surface hydrophobicity of the aerobic granular sludge through adsorbing phenanthrene as claimed in claim 1 or 6, wherein in the step 4, the specific measurement process of the ultraviolet spectrophotometry is as follows: and diluting the removed 50 mu L of supernatant into 5mL of dimethylsulfoxide with volume fraction of 2/3, measuring the absorbance of the supernatant at the absorption wavelength by using an ultraviolet spectrophotometer, and calculating the concentration of phenanthrene in the supernatant according to the absorbance and a standard curve.
10. The method for accurately measuring the surface hydrophobicity of the aerobic granular sludge through adsorbing phenanthrene as claimed in claim 1, wherein in the step 4, the absorption wavelength in an ultraviolet spectrophotometer is set to 296 nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113504154A (en) * | 2021-04-30 | 2021-10-15 | 武汉理工大学 | Method, system, device and storage medium for determining hydrophilicity and hydrophobicity of metal sulfide ore |
| CN113504154B (en) * | 2021-04-30 | 2023-12-12 | 武汉理工大学 | Method, system, device and storage medium for determining hydrophilicity and hydrophobicity of metal sulfide ore |
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