CN111239274A - Method for measuring apparent yield coefficient of aerobic activated sludge - Google Patents

Method for measuring apparent yield coefficient of aerobic activated sludge Download PDF

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CN111239274A
CN111239274A CN202010075379.8A CN202010075379A CN111239274A CN 111239274 A CN111239274 A CN 111239274A CN 202010075379 A CN202010075379 A CN 202010075379A CN 111239274 A CN111239274 A CN 111239274A
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activated sludge
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aerobic activated
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headspace
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胡湛波
郑榆凯
李佩仪
吴凯
涂晓杰
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Guangxi University
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Abstract

The invention relates to the technical field of environmental monitoring analysis, and discloses a method for determining an apparent yield coefficient of aerobic activated sludge. The method comprises (1) sample pretreatment; (2) culturing a sample; (3) detecting the culture sample by adopting headspace gas chromatography; (4) and (6) calculating a result. The invention utilizes the headspace gas chromatography technology to measure the oxygen consumption and the carbon dioxide generation of an aerobic sludge sample cultured in a headspace bottle in a short time, and the apparent productivity coefficient of the aerobic activated sludge sample can be obtained through calculation. The method has good precision and accuracy, and the relative standard deviation of the apparent yield coefficient is less than 5.46 percent; compared with the prior art, the relative deviation of the two methods is within 9.23 percent. Compared with the traditional method, the method is simpler and more efficient, and is particularly suitable for research and application related to aerobic activated sludge in the environmental field.

Description

Method for measuring apparent yield coefficient of aerobic activated sludge
Technical Field
The invention relates to the technical field of environmental monitoring analysis, in particular to a method for measuring an apparent yield coefficient of aerobic activated sludge.
Background
Apparent yield coefficient of aerobic activated sludge (The anaerobic produced coefficient, Y)obs) Refers to the ratio of biomass (Mixed liquid suspended solids, MLSS) to Biochemical Oxygen Demand (BOD) consumption synthesized over a period of time.
The apparent yield coefficient is one of the key parameters in the mathematical model of the sewage treatment system, and can calculate not only the aerobic sludge production and the oxygen demand, but also kinetic parameters, such as the maximum specific growth rate (mu) in the sewage treatment systemm) And the substrate half-saturation coefficient (K)S). Therefore, the method for effectively determining the apparent yield coefficient has important significance for the operation and management of the aerobic activated sludge sewage treatment system.
At present, the determination of the apparent yield coefficient of the aerobic activated sludge is mainly realized by measuring the MLSS increase amount and the BOD decrease amount of the aerobic activated sludge in a culture period (usually 0.5-2 h). The MLSS is generally determined by a gravimetric method, a sample needs to be filtered through 0.45-micron filter paper, the filter paper and substances collected on the filter paper are placed in an oven at 105 ℃ for 6-8 hours to completely remove moisture, the weight difference of the filter paper before and after drying is MLSS, and in order to determine the significant change of the MLSS, the detection limit of each weighed sample is required to be more than 25 mg. The consumption of Biochemical Oxygen Demand (BOD) is generally measured by iodometric titration, dissolved oxygen meters. To determine significant changes in BOD, the sample culture required 5 days. In short, the traditional method for determining the apparent yield coefficient of the aerobic activated sludge by measuring MLSS and BOD has poor detection limit, long measuring and culturing time and complex operation process.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for measuring the apparent yield coefficient of aerobic activated sludge.
The purpose of the invention is realized by the following technical scheme:
a method for measuring an apparent yield coefficient of aerobic activated sludge comprises the following steps:
step (1), sample pretreatment: after flushing an aerobic activated sludge sample by using normal saline, adding the normal saline for aeration; simultaneously, filtering and aerating the sewage;
step (2) sample culture: placing the washed sludge and the aerated wastewater into a headspace bottle, and placing the headspace bottle in a constant-temperature shaking table for culture;
step (3) sample determination: after different culture times, respectively taking out the headspace bottles from the incubator, and injecting 0.5-2 mL of hydrochloric acid into each headspace bottle to finish the metabolic activity of the microorganisms in the sample; then, the headspace bottle is placed in a headspace sample injector to measure the signal values of oxygen and carbon dioxide;
and (4) calculating a result: substituting the peak area obtained in the step (3) into the following formula to obtain the yield coefficient Y of the aerobic activated sludgeobs：
Figure BDA0002378362470000021
In the formula: k is a proportional constant of the variation of the carbon dioxide peak area in the headspace bottle and the microbial growth in the culture process; k is a proportional constant of the variation of the oxygen peak area in the headspace bottle and the oxygen consumption of the microorganism in the culture process; delta AcIs the variation of the peak area of carbon dioxide in the culture process; delta AOIs the amount of change in the oxygen peak area during the culture.
Preferably, in the step (1), the aerobic activated sludge sample is washed for 3 to 5 times, and the sewage is filtered by using 0.45 mu m filter paper, wherein the aeration time is 0.5 to 2.0 hours, so as to ensure that the dissolved oxygen concentration is 6.0 to 8.0 mg/L.
Preferably, the volume of the mixed sample in the step (2) is 5-20 mL; the volume of the headspace bottle in step (2) was 21.6 mL.
Preferably, the temperature of the constant-temperature shaking table in the step (3) is 20-30 ℃, and the rotating speed is 100-300 rpm; the concentration of the hydrochloric acid in the step (3) is 0.001-0.05 mol/L.
Preferably, the headspace sampler operating conditions in step (3) are: the balance temperature is 40-100 ℃, the sample balance time is 4-40 min, the air-carrying balance time in the headspace sample bottle is 10-20 s, the pipeline inflation time is 10-20 s, the pipeline balance time is 1-10 s, and the loop balance time is 10-20 s.
Preferably, the chromatograph operating conditions in step (3) are: the method comprises the following steps of preparing a GS-Q type capillary chromatographic column (30m multiplied by 0.53mm), wherein the temperature of the chromatographic column is 30-150 ℃, nitrogen is used as a carrier gas, the flow rate of the nitrogen is 2.0-6.0 mL/min, and the temperature of a Thermal Conductivity Detector (TCD) detector is 150-250 ℃.
Preferably, the determination of the scaling factor K:
measuring the growth amount of aerobic activated sludge MLSS by using a gravimetric method, and measuring the carbon dioxide signal value of the same sample according to the method of any one of claims 1 to 6;
the carbon dioxide signal value of the same sample and the MLSS growth amount of the aerobic activated sludge have a linear relation, namely:
ΔMLSS＝KΔAC(2)
in the formula: delta MLSS is the growth of activated sludge MLSS; delta AcIs the amount of change in the peak area of carbon dioxide during the culture.
Preferably, the determination of the scaling factor k:
the signal value of oxygen in the air is measured by setting a blank sample, and the proportionality coefficient k is calculated according to the following formula at the room temperature of 20 ℃:
Figure BDA0002378362470000031
in the formula: cbIs the molar concentration of oxygen in air, M is the molecular weight of oxygen, gamma is the volume fraction of oxygen in air, P0At atmospheric pressure, AbThe oxygen peak area was measured for a blank sample.
The method is only suitable for aerobic activated sludge, the apparent yield coefficient is a specific kinetic parameter of the aerobic activated sludge, and other types of sludge are not suitable for the parameter.
Compared with the prior art, the invention has the following technical effects:
according to the invention, the headspace gas chromatography technology is utilized to measure the carbon dioxide generation amount and the oxygen consumption amount in the aerobic activated sludge culture process, and the apparent productivity coefficient of the aerobic activated sludge sample is obtained after calculation, so that the measuring speed is high, the accuracy of an analysis result is high, and the operation is simple.
Firstly, the invention relates to the determination of the apparent yield coefficient of aerobic activated sludge, the traditional method needs to determine MLSS and BOD respectively to obtain the apparent yield coefficient of aerobic activated sludge, and the invention only needs to test the variable quantities of oxygen and carbon dioxide in a headspace bottle to obtain the apparent yield coefficient of aerobic activated sludge, wherein the quantities of oxygen and carbon dioxide can be synchronously determined in one headspace gas chromatography detection, thus greatly simplifying the determination operation steps.
The method has good precision and accuracy, and the relative standard deviation of the apparent yield coefficient is less than 5.46 percent; compared with the prior art, the relative deviation of the two methods is within 9.23 percent.
Secondly, the analysis time (90-120min) used by the method is much shorter than that (2-5d) of the traditional method, which shows that the method has higher efficiency for determining the apparent yield coefficient of the aerobic activated sludge.
Drawings
FIG. 1 is a graph showing changes in signal values of oxygen and carbon dioxide in the aerobic activated sludge culture process
FIG. 2 is a graph showing the relationship between the signal value of carbon dioxide in a flask and the increase amount of MLSS during the culture of aerobic activated sludge.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto.
Example 1
(1) Sample pretreatment: flushing aerobic activated sludge 1(MLSS 4238mg/L, pH 7.28) taken from an aerobic tank of a certain sewage treatment plant with physiological saline for 3-5 times, and then adding the physiological saline for aeration. At the same time, the wastewater was filtered (using 0.45 μm paper) and aerated for 1.0h to ensure a dissolved oxygen concentration of 8.0 mg/L.
(2) Sample culture: 15mL of the mixed sample (i.e., sludge and aerated wastewater) was placed in a 21.6mL headspace bottle and cultured in a constant temperature shaker at a temperature of 20 ℃ and a rotational speed of 150 rpm.
(3) And (3) sample determination: after the different incubation times, the headspace bottles were removed from the incubator, respectively, and 1.0mL of hydrochloric acid (0.005mol/L) was injected into each headspace bottle to terminate the metabolic activity of the microorganisms in the sample. The headspace vials were then placed in headspace injectors to measure the signal values for oxygen and carbon dioxide.
The headspace injector operating conditions were: the balance temperature is 75 ℃, the balance time is 6.0min, the balance time of the air-carrying in the headspace sample bottle is 12s, the pipeline inflation time is 12s, the pipeline balance time is 3s, and the loop balance time is 12 s;
the gas chromatograph was operated at a column temperature of 105 ℃ using a GS-Q type capillary chromatography column (30 m.times.0.53 mm, J & W Scientific Co.); nitrogen is taken as a carrier, and the flow rate of the nitrogen is 3.1 mL/min; the detector temperature of the Thermal Conductivity Detector (TCD) is 220 ℃.
The signal values of oxygen and carbon dioxide in the aerobic activated sludge culture process are shown in fig. 1.
(4) Determination of the proportionality factor K
The increase of the aerobic activated sludge MLSS was determined gravimetrically and the carbon dioxide signal value of the same sample was determined according to the detection method of the above example. As shown in fig. 2, there is a linear relationship between the carbon dioxide signal value measured by headspace gas chromatography and the MLSS increase amount of aerobic activated sludge, that is:
ΔMLSS＝8.65×10-4ΔAC(n＝11,R2＝0.9938) (1)
in the formula: delta MLSS is the growth of activated sludge MLSS; delta AcIs the variation of the peak area of carbon dioxide in the culture process;
(5) determination of the scaling factor k
Since the partial pressure of oxygen in the headspace bottle behaves very similar to that of an ideal gas, the signal value of oxygen in air can be determined by setting a blank sample, and the proportionality coefficient k is calculated according to the following formula at room temperature of 20 ℃:
Figure BDA0002378362470000041
in the formula: cbIs the molar concentration of oxygen in air, M is the molecular weight of oxygen, gamma is the volume fraction of oxygen in air, P0At atmospheric pressure, AbThe oxygen peak area was measured for a blank sample.
(6) And (4) calculating a result:
substituting the oxygen and carbon dioxide signal values of the sample in the oxygen and carbon dioxide linear change area in the step (3) into the following formula to obtain the yield coefficient Y of the aerobic activated sludge sampleobs：
Figure BDA0002378362470000051
Examples 2 to 4 examination of various samples
Examples 2 to 4 were conducted on aerobic activated sludge samples from several different sewage treatment plants of nanning, and the conditions of the respective parameters are shown in table 1, but the operation is the same as that of example 1 except that the other steps are not shown.
TABLE 1 detection conditions for each of the samples of examples 2 to 4
Figure BDA0002378362470000052
Comparative examples 1 to 3
The process conditions for comparative examples 1 to 3 are shown in Table 2, and the same operations as in example 1 are not shown.
TABLE 2 Process conditions for comparative examples 1 to 3
Figure BDA0002378362470000053
Figure BDA0002378362470000061
The accuracy and precision evaluation of the method of the invention
(1) Reproducibility test
4 different aerobic activated sludge samples were taken and 5 parallel samples were measured by headspace gas chromatography according to examples 1 to 4, respectively. The results are shown in Table 1. As can be seen from table 3, the relative standard deviation of the apparent yield coefficient obtained by headspace gas chromatography was less than 5.46%. Therefore, the method has better repeatability for detecting the yield coefficient. However, as can be seen from comparative example and table 4, if the operation detection parameter conditions are not within the range of the method, the method accuracy cannot be guaranteed, and the method cannot exert the detection advantages of the aerobic activated sludge sample, specifically, the standard deviation is more than 12.8%.
TABLE 3 example headspace gas chromatography repeatability test
Numbering Yobs,mg MLSS/mg BOD Relative standard deviation,%
Aerobic activated sludge 1 0.236±0.014 5.46
Aerobic activated sludge 2 0.435±0.021 3.95
Aerobic activated sludge 3 0.562±0.016 2.65
Aerobic activated sludge 4 0.643±0.012 2.51
Table 4 repeatability test for comparative example headspace gas chromatography
Figure BDA0002378362470000062
(2) Comparison of the methods
4 different aerobic activated sludge samples are taken, analyzed and detected by the headspace gas chromatography and the traditional method (namely, the national standards HJ 505-. The results are shown in Table 5.
TABLE 5 comparison of the results of determining yield coefficients for headspace gas chromatography with conventional methods
Figure BDA0002378362470000071
The relative deviation of the two methods is within 9.23 percent, which shows that the accuracy of the measurement result of the headspace gas chromatography is high. Meanwhile, the analysis time (90-120min) of the headspace gas chromatography is much shorter than that (2-5d) of the traditional method, which indicates that the headspace gas chromatography is more efficient.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.

Claims (8)

1. A method for measuring an apparent yield coefficient of aerobic activated sludge is characterized by comprising the following steps:
step (1), sample pretreatment: after flushing an aerobic activated sludge sample by using normal saline, adding the normal saline for aeration; simultaneously, filtering and aerating the sewage;
step (2) sample culture: placing the washed sludge and the aerated wastewater into a headspace bottle, and placing the headspace bottle in a constant-temperature shaking table for culture;
step (3) sample determination: after different culture times, respectively taking out the headspace bottles from the incubator, and injecting 0.5-2 mL of hydrochloric acid into each headspace bottle to finish the metabolic activity of the microorganisms in the sample; then, the headspace bottle is placed in a headspace sample injector to measure the signal values of oxygen and carbon dioxide;
and (4) calculating a result: substituting the peak area obtained in the step (3) into the following formula to obtain the yield coefficient Y of the aerobic activated sludgeobs：
Figure FDA0002378362460000011
In the formula: k is a proportional constant of the variation of the carbon dioxide peak area in the headspace bottle and the microbial growth in the culture process; k is a proportional constant of the variation of the oxygen peak area in the headspace bottle and the oxygen consumption of the microorganism in the culture process; delta AcIs the variation of the peak area of carbon dioxide in the culture process; delta AOIs the amount of change in the oxygen peak area during the culture.
2. The method for determining the apparent yield coefficient of the aerobic activated sludge as claimed in claim 1, wherein the aerobic activated sludge sample is washed 3 to 5 times in step (1), and the sewage is filtered by using 0.45 μm filter paper, and the aeration time is 0.5 to 2.0h, so as to ensure that the dissolved oxygen concentration is 6.0 to 8.0 mg/L.
3. The method for determining the apparent yield coefficient of the aerobic activated sludge according to claim 1, wherein the volume of the mixed sample in the step (2) is 5-20 mL; the volume of the headspace bottle in step (2) was 21.6 mL.
4. The method for determining the apparent yield coefficient of the aerobic activated sludge according to claim 1, wherein the temperature of the constant temperature shaking table in the step (3) is 20 to 30 ℃, and the rotation speed is 100 to 300 rpm; the concentration of the hydrochloric acid in the step (3) is 0.001-0.05 mol/L.
5. The method of claim 1, wherein the headspace sampler operating conditions in step (3) are: the balance temperature is 40-100 ℃, the sample balance time is 4-40 min, the air-carrying balance time in the headspace sample bottle is 10-20 s, the pipeline inflation time is 10-20 s, the pipeline balance time is 1-10 s, and the loop balance time is 10-20 s.
6. The method for determining the apparent yield coefficient of the aerobic activated sludge according to claim 1, wherein the operating conditions of the chromatograph in the step (3) are as follows: GS-Q type capillary chromatographic column (30m is multiplied by 0.53mm), the temperature of the chromatographic column is 30-150 ℃, nitrogen is used as carrier gas, the flow rate of the nitrogen is 2.0-6.0 mL/min, and the temperature of the detector of the thermal conductivity detector is 150-250 ℃.
7. The method for determining the apparent yield coefficient of the aerobic activated sludge according to claim 1, wherein the determination of the proportionality coefficient K:
measuring the growth amount of aerobic activated sludge MLSS by using a gravimetric method, and measuring the carbon dioxide signal value of the same sample according to the method of any one of claims 1 to 6;
the carbon dioxide signal value of the same sample and the MLSS growth amount of the aerobic activated sludge have a linear relation, namely:
ΔMLSS＝KΔAC(2)
in the formula: delta MLSS is the growth of activated sludge MLSS; delta AcIs the amount of change in the peak area of carbon dioxide during the culture.
8. The method for determining the apparent yield coefficient of the aerobic activated sludge according to claim 1, wherein the determination of the proportionality coefficient k:
the signal value of oxygen in the air is measured by setting a blank sample, and the proportionality coefficient k is calculated according to the following formula at the room temperature of 20 ℃:
Figure FDA0002378362460000021
in the formula: cbIs the molar concentration of oxygen in air, M is the molecular weight of oxygen, gamma is the volume fraction of oxygen in air, P0At atmospheric pressure, AbThe oxygen peak area was measured for a blank sample.
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