CN115684471A - Multi-level analysis method based on black and odorous sediment nitrogen and sulfur release device - Google Patents
Multi-level analysis method based on black and odorous sediment nitrogen and sulfur release device Download PDFInfo
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Abstract
The invention provides a multi-level analysis method based on a black and odorous sediment nitrogen and sulfur release device, which can detect and evaluate the change process of the release concentration of black and odorous sediment nitrogen and sulfur pollutants to different levels of an overlying water body so as to analyze the release rule and the dynamic load change of the black and odorous sediment nitrogen and sulfur pollutants. The experimental device comprises a water column container, a water delivery pipe and a water tank. The flow comprises the steps and contents of selection of a black and odorous sediment collection position, on-site collection of the sediment, preparation of a sediment sample, layered sampling of a water sample covering a water column, detection of physical and chemical indexes of the water sample, and the like. The invention can be used for researching the migration and conversion process of nitrogen and sulfur pollutants of black and odorous sediments to overlying water and the change process of indexes such as dissolved oxygen, pH, oxidation-reduction potential and the like in each level. Provides technical support for accurately treating black and odorous water and black and odorous sediment pollution.
Description
Technical Field
The invention belongs to the technical field of ecological environment models, and particularly relates to a multi-level analysis method based on a black and odorous sediment nitrogen and sulfur release device.
Background
Due to increased human activities and poor environmental regulation, a large number of nitrogen and sulfur pollutants are discharged into surface waters around the world, and these pollutants cause the formation of black and odorous water bodies peculiar to southern china.
The high nitrogen content in water is one of the key factors causing eutrophication, which has become a worldwide problem due to the negative effects on biodiversity, human health and climate caused by the severe breeding of algae, oxygen deficiency and deterioration of the fresh water ecosystem.
Sulfur ion (S) generated by reduction of black and odorous deposits 2- ) Has strong toxicity to aquatic organisms, and causes serious deterioration of the structure and diversity of aquatic animals and plants. Sulfide ions (S) in the deposit 2- ) Oxidation and subsequent recombination with iron and other metals (e.g., al, as, cu, mn, and Zn) threatens the survival or growth of local organisms due to the toxicity of these compounds. Municipal and aquaculture wastewater discharges contain large amounts of organic sulfur and sulfates. Sulfate is reduced by Sulfate Reducing Bacteria (SRB) in water and sediments, resulting in the production of large quantities of hydrogen sulfide (H) in anaerobic environments 2 S). SO thus produced 4 2- The generation of malodour and the near anaerobic conditions characteristic of some waters in the area, thus giving rise to the term "black odorous water". Unpleasant color and odor in black and odorous water are caused by excessive pollution, and imbalance of oxygen consumption and reoxygenation.
Understanding the release rate and release rate of different nitrogen and sulfur pollutants at different depths and the change rules of parameters such as DO, ORP, pH and the like at different depths can provide inspiration for improving the water quality of black and odorous water bodies and reduce the negative influence on human health. The invention provides a feasible method for researching the release characteristics of endogenous pollutants in black and odorous sediments and the migration and transformation of pollutants in overlying water bodies with different depths.
Disclosure of Invention
The invention aims to provide a research method capable of monitoring and evaluating the release rule of nitrogen and sulfur pollutants in black and odorous sediments to overlying water bodies with different depths and the dynamic load change process of the water bodies. The method can be used for researching the single-layer or multi-layer release process of nitrogen and sulfur pollutants, various heavy metals, various organic pollutants and the like in the black and odorous sediments to the overlying water body and the change process of indexes such as dissolved oxygen, pH, oxidation-reduction potential and the like in each layer. Provides technical support for accurately treating black and odorous water pollution.
The purpose of the invention is realized by the following technical scheme:
a multi-level analysis method based on a black and odorous sediment nitrogen and sulfur release device comprises the following steps:
s1: sampling the black and odorous sediments and the overlying water thereof, recording sampling information, and respectively detecting physical and chemical indexes of the black and odorous sediments and the overlying water;
s2: designing and building a nitrogen and sulfur release device for black and odorous sediments;
s3: removing the overlying water generated by natural sedimentation in the collected sample, and laying the black and odorous sediments at the bottom of a water column container of a black and odorous sediment nitrogen-sulfur release device; slowly inputting water into a water column container, and standing to obtain an overlying water body; the depth of the overlying water body and the thickness of the black and odorous sediments are consistent with the depth of the water body of the river at the sampling site and the thickness of the sediment;
s4: sampling at different levels of the overlying water body in the S3 at intervals, and detecting physical and chemical indexes of a detection sample and the concentration of pollutants;
s5: analyzing the physicochemical indexes and the pollutant concentration obtained in the step S4 to obtain the time-space variation process of the conversion rate, the release rate, the total release amount and the physicochemical indexes of various pollutants in the single-layer or multi-layer water body;
s6: by analyzing the results obtained in S5, the relationship between the indices and the microbial population change are obtained.
Preferably, the conversion rate, release rate and total release amount of each pollutant in the single layer or multiple layers in step S5 are calculated according to the following formulas:
in the formula (1)Said R is n,m Represents the average pollutant release rate of the black and odorous sediment between the mth layer and the (m & gt 1) th layer on the nth day, and the unit is mg/(L & d); c. C m Represents the concentration of the contaminant in the mth layer, mg/L;
d in formula (2) n,m Represents the conversion rate of the pollutants in the m layers from the 1 st day to the n th day, and has the unit of mg/(L.d); c. C n,m Concentration at the mth layer of the contaminant on the nth day, mg/L;
w in formula (3) n,m Represents the release rate of the pollutant concentration of the black and odorous sediment between the m layer and the m +1 layer on the n day, and the unit is mg/(m) 2 ·d)；C n,m The pollutant concentration of the experimental water column on the mth layer on the nth day is expressed in mg/L; t is time in units of d; v is the volume of the water body between the mth layer and the m +1 layer, L; a is the horizontal projection area of the sediment and water interface, m 2 ；
The release rate of the average pollutant concentration of the experimental water column at the mth layer and the (m + 1) th layer on the nth day is expressed in mg/(L.d);
q in formula (4) n,m Represents the release amount of black smelly sediment pollutant in the mth layer from day 1 to day n, and the unit is mg; a represents the horizontal projection area of the black and odorous sediment and water interface, m 2 ；
Represents the unit area of the m-th layer of black and odorous deposits from day 1 to day nThe total amount of change is in mg/m 2 ；
Q in formula (5) n Represents the total release amount of black and odorous sediment pollutants in the whole covering water from the 1 st to the n th days, and the unit is mg; a represents the horizontal projection area of the black and odorous sediment and water interface, m 2 ；
The amount of the black-smelling sediment released per unit area from day 1 to day n is expressed in mg/m 2 。
Preferably, the sampling time interval of the overlying water body in the step S4 is: sampling once daily from day 1 to day 7 and once 2 days from day 7 to day 33; if the concentration of the pollutants is not stable at the 33 rd day, the period is prolonged to 48 days, and the sampling interval is 3 days; if not stable at day 48, extend to 63 days, during which the sampling interval is 5 days; until the target concentration stabilizes.
Preferably, the black and odorous sediment nitrogen and sulfur release device in the step S2 comprises a water column container, a water delivery pipe and a water tank, wherein a plurality of sampling ports are vertically arranged on the side surface of the water column container, and the sampling ports are equal in distance and are 10-20cm.
Preferably, the accumulated water sampling amount of the experiment set in the step S4 is controlled in the volume of the raw water
Within, discarding the first 20mL of samples each time, and taking the rest as a detection sample; and after sampling, replenishing the water body to the original water level in time.
Preferably, the steps S2 to S6 are repeated under different initial physicochemical conditions, the change trend of the pollutants in the overlying water body under multiple conditions, single-layer or multi-layer is analyzed statistically, and the pollutant concentration release rate of the black and odorous sediments, the release amount among layers and the total release amount in the whole overlying water body are respectively calculated.
Preferably, the black and odorous sediments are taken out for analysis after the experiment is finished, and the analysis is compared with the physicochemical indexes obtained in the step S1 to obtain the influence result of the covering of the overlying water body on the black and odorous sediments.
Preferably, the physicochemical indexes of the black and odorous sediment sample in the step S1 include pH, total nitrogen, total phosphorus, ammonia nitrogen, available sulfur, five-day biochemical oxygen demand, chemical oxygen demand, and heavy metal concentration; the physicochemical indexes of the overlying water sample comprise dissolved oxygen, sulfur ions, pH, oxidation-reduction potential, ferrous ions, total iron, suspended solids, total nitrogen, total phosphorus, ammonia nitrogen, nitrate nitrogen, nitrite nitrogen, five-day biochemical oxygen demand, chemical oxygen demand and other heavy metals; the sampling information comprises information such as water depth, sediment thickness, sediment color, odor degree, sediment state, sediment temperature and the like of a sampling place.
A black and odorous sediment nitrogen and sulfur release device for operating the analysis method of any one of the preceding claims, comprising a water column container, a water conveying pipe and a water tank; the side surface of the water column container is vertically provided with a plurality of sampling ports with equal intervals and intervals of 10-20cm, the center of the top cover of the water column container is vertically fixed with a porous water inlet pipe, and a water pipe connecting the water column container and the water tank is connected with a peristaltic pump.
Preferably, the highest sampling port of the sampling ports is arranged below the water level of the overlying water body by 2cm, and the lowest sampling port is arranged above the surface of the sediment by 2 cm;
the height of the water column container is 40-100 cm higher than the sum of the depth of the water body and the thickness of the black and odorous sediments, the height-diameter ratio is 4-6, and the wall thickness is 1-2 cm, and the water column container is wrapped by a shading heating belt;
the porous water inlet pipe is made of PP (polypropylene), the length of the porous water inlet pipe is equal to the distance from a top cover of the water column to a sediment, the height-diameter ratio of the porous water inlet pipe is 15-30, small holes with the diameter of about 2mm are uniformly drilled in the underwater part, the top of the porous water inlet pipe is 2cm higher than the top of the water column, and the bottom of the porous water inlet pipe is flush with the lowest sampling port;
the sample connection includes at the inside porous outlet pipe of water column container and the sample valve who links to each other with it, porous outlet pipe material is PP, and length equals the water column radius, and the pipe wall has evenly beaten diameter 2 mm's hole.
The invention has the following beneficial effects:
the invention can simulate the migration and transformation process of endogenous pollutants of black and odorous sediments to the overlying water. In the experiment, a multi-layer process of migration and conversion of nitrogen and sulfur pollutants in the black and odorous sediments to a water body is calculated through the release rate or the total release amount of the concentration of the pollutants in water or a middle or multi-layer pollutant, compared with a common single-point monitoring and releasing experiment, the method can reduce the migration and conversion process of the nitrogen and sulfur pollutants in the black and odorous sediments, and can obtain a more real and comprehensive result.
Drawings
FIG. 1 is a schematic diagram of the experimental process, wherein 1 is an experimental water column, 2 is an overlying water body, 3 is a sampling valve, 4 is a porous water outlet pipe, 5 is a sample collecting pipe, 6 is a black and odorous deposit, 7 is a water column base, 8 is a porous water inlet pipe, 9 is a peristaltic pump, 10 is a water conveying pipe, 11 is a water tank, 12 is a sample analyzer, 13 is a computer, and 14 is an analysis result;
FIG. 2 shows the SO of the overlying water in the water column at 35 deg.C 4 2- Graph of concentration versus time of (a);
FIG. 3 shows the NO of the overlying water in the water column at 35 deg.C 3 - Graph of concentration versus time of (a);
FIG. 4 shows NO at depth 2cm for the coated water in the pilot test and at depth 2cm for the coated water in the indoor test 3 - The change of the concentration change value with time.
Detailed Description
It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
(1) Preparation work
1) As shown in FIG. 1, the validated measurement instruments, field test equipment, sampling consumables and refrigerated storage are prepared for storage and transport; the experimental device comprises a heating belt for experiment, a water column, a water tank, a water delivery pipe, a peristaltic pump, a computer with software, other tools and consumables for experiment and the like, wherein the objects are cleaned and labeled to perform the experiment;
2) Prior to the experiment, the heating belt should be opened in advance and set to a predetermined operating temperature. Wrapped in a water column and required to be opened at least twenty-four hours in advance. Before the test is started, the heating belt is opened and connected with a temperature controller to monitor the actual working temperature of the heating belt, and at least one measurement is carried out within twenty-four hours;
3) Shading should be performed to ensure that the sediment sample is not exposed to external light sources during transport, storage and the entire test;
4) If deionized water (pure water) is used for replacing raw water in the lake as a medium for releasing black and odorous sediment pollution, enough deionized water also needs to be prepared; the deionized water must be maintained at the specified temperature for the experiment.
(2) Sample collection
The sample of experimental choice is a typical black smelly deposit from one representative location. To achieve this, water is typically pumped around a weir over an area of no more than 0.3 square meters, black and odorous deposits are collected to a depth of no more than 6cm, and the amount of overlying water sample should be at least 7L (corresponding to the amount of water column under experimental operating conditions).
On a representative black and odorous sediment site, a columnar sampler with the appropriate length and the diameter phi of 30c is driven into the black and odorous sediment for about 10cm, the upper water in the sampler can be drained after at least 4 hours of stability, and when the water level drops to expose the black and odorous sediment, the black and odorous sediment with the thickness of 6cm is stored in a low-temperature storage box in a vacuum sealing and shading way by using a stainless steel sampling spoon. And (4) taking enough water with the depth of 20cm from the overlying water sample, and storing the water in a low-temperature storage box in a vacuum sealing and dark manner.
And (3) recording the collected black and odorous sediment samples and the collected overlying water samples in detail according to the collected information of the sampler, the sampling time, the geographic position coordinates of the collection point, weather, air temperature, water body temperature, sediment color, odor grade (no odor, slight odor or obvious odor), state (solid, thick or fluid state), sediment temperature and the like.
(3) Method for preserving sediment and overlying water
And (3) carrying out vacuum sealing on the black and odorous sediments and the covered water, keeping out of the sun, naming, photographing and storing the evidence, and storing and transporting at a low temperature (4 ℃). The detection is completed within 16h of the self-collected sample, and the sediment laying is completed within 36 hours.
(4) Sample preparation
After reaching the laboratory, the upper water generated by natural sedimentation in the storage box is removed, and the black and odorous sediments are retained. Taking out a proper amount of the black and odorous sediments, and cleaning the impurities such as fallen leaves, plastics and the like in the black and odorous sediments. After stirring, the top cover of the experimental water column was opened and the mixture was poured in from the top. The funnel is used when laying the black and odorous sediment to prevent the sediment from splashing on the wall of the water column, and the adding point can be positioned at the center of the water column until the thickness reaches 23cm.
After the black and odorous sediments are well placed, slowly inputting deionized water into a water column to enable the water depth to reach 44cm.
Detecting pH value, total Organic Matter (TOM), total Nitrogen (TN), total Phosphorus (TP) and ammonia Nitrogen (NH) in black and odorous sediment sample 4 + -N), five days Biochemical Oxygen Demand (BOD) 5 ) Chemical Oxygen Demand (COD) cr ) Concentrations of contaminants such As sulfides, available sulfur and heavy metal contaminants (Hg, cd, as, pb, cu, zn, ce, ni).
Detecting the overlying water Dissolved Oxygen (DO) and the sulfur ion (S) of each layer 2- ) pH, oxidation-reduction potential (ORP), ferrous ion (Fe) 2+ ) Suspended Solids (SS), total Nitrogen (TN), total Phosphorus (TP), ammonia Nitrogen (NH) 4 + -N), five days Biochemical Oxygen Demand (BOD) 5 ) Chemical Oxygen Demand (COD) cr ) And other heavy metals (Hg, cd, as, pb, cu, zn, ce, ni).
(5) Initial experiment
And starting the heating belt, wherein the temperature fluctuation of the heating belt needs to be controlled within 1 ℃.
The water sample is collected after reaching the specified temperature for 4 hours, and the site index is synchronously and timely determined during each collection. Samples 3, 23 and 43cm below the water surface were collected and measured, and each sample was filtered through a Polyethersulfone (PES) filter with a pore size of 0.45 μm and a diameter of 13mm, and about 100mL of the filtered water sample was taken (which can be adjusted according to the experimental requirements). The experimental procedures and data were recorded in detail for subsequent analysis.
The time of sampling from the experimental water column is generally day 1, day 2, day 3, day 4, day 5, day 6, day 7, day 9, day 11, day 13, day 15, day 17, day 19, day 21, day 23, day 25, day 27, day 29, day 31, day 33; if any pollutant concentration of the overburden water is not in a stable state at the 33 rd day, the experimental days are prolonged to 48 days, and the sampling interval is changed to 3 days; if the concentration of any pollutant in the overlying water body is not in a stable state at the 48 th day, the experimental days are prolonged to 63 days, and the sampling interval is changed to 5 days; until the concentration of all pollutants in the overlying water body is stable.
(7) Collecting and detecting overlying water sample
On-site indicators, e.g. DO, S, should be determined in time after three water samples have been collected 2- pH and ORP, simultaneously storing enough samples in a sampling tube, storing the samples in a vacuum seal mode at 4 ℃, and detecting Fe within 6h 2+ 、SS、TN、TP、NH 4 -N、NO 3 -N、NO 2 -N、BOD 5 、COD cr And heavy metals (Hg, cd, as, pb, cu, zn, ce, ni) to minimize sample residence time.
If no pollutant is detected or the concentration is lower than the detection limit after continuous sampling for 3 times in a water sample covering a certain layer of the black and odorous sediment, the sampling for detecting the pollutant is not needed in the later period, and the disturbance to the system is reduced.
(8) Final detection of black-odor deposits
After the final sampling of the test, the overlying water is evacuated at a low flow rate, then samples are collected on the surface of the black and odorous sediment at the bottom of the water column and in the depth of 3cm, and the same project detection as the original test is carried out again.
(9) Data processing
Independently analyzing the experimental data of the migration and transformation of the pollutants of the black and odorous sediments and the overlying water respectively; analyzing the release rate and total release amount of pollutants of different sediments/underwater, different levels and different experimental days, generating a formula of the migration and transformation process of the nitrogen and sulfur pollutants in the black and odorous sediments, and making a required chart and other results.
FIGS. 2 and 3 show SO in overlying water at various depths for black ozone deposits 4 2- And NO 3 - The process of conversion of the nitrogen sulfur contaminants in the black ozone sediments to the migration of the overlying water body is a function of time.
Because the biochemical effect in the black and odorous sediments and the water quality index of the overlying water system have great influence, the release rate and the total release amount of nitrogen and sulfur pollutants in the black and odorous sediments obtained by analyzing the water quality of the overlying water are often different from the data obtained by analyzing the physical property of the black and odorous sediments. Therefore, the above water-cover analysis results should be used as the standard.
The method for analyzing the data of the nitrogen-sulfur pollutant migration and conversion experiment in the black and odorous sediment is further illustrated by combining the examples.
Example 1 a multi-level analysis method based on a black and odorous deposit nitrogen and sulfur release device is as follows:
in a black-odor river, because pollutants such as organic matters, sulfate, nitrate and the like exceed standards, dissolved oxygen in water is greatly consumed, anaerobic microorganisms are greatly propagated and enriched in sediments, sulfate reduction reaction and iron reduction reaction occur in the sediments, and H generating odor is generated 2 S and black FeS, the deposits turned into black smelly deposits. Under the action of osmotic pressure, pollutants in the black and odorous sediments migrate to a plurality of layers of the overlying water to cause the water body to generate black and odorous substances; the levels of different depths have correlation with the content of dissolved oxygen, the illumination intensity, the pressure and the distance of a pollution source (black and odorous sediments), so the pollution degrees at different depths are different; under the influence of the action of microorganisms in the water, the pollutants are transformed to a certain extent. The method for analyzing the migration and transformation process of nitrogen and sulfur pollutants in the black and odorous sediments to the upper water body in multiple layers can provide revelation for improving the water quality of the black and odorous water body and reduce the negative influence on human health.
A column-shaped sampler with the appropriate length and the diameter phi of 30cm is driven into the black and odorous sediment from a representative black and odorous sediment site, about 5kg of the black and odorous sediment with the thickness of 6cm is collected, and the black and odorous sediment is stored in a low-temperature storage box at 4 ℃ in a vacuum sealing and shading manner. And (4) taking enough water at the depth of 20cm from the overlying water sample, and storing the water in a low-temperature storage box at 4 ℃ in a dark place in a vacuum sealing manner. Naming, taking a picture and storing the certificate, recording the sampling information in detail, finishing detection of black and odorous sediments within 16h, and finishing paving in the device within 36 h.
Uniformly placing the black and odorous sediments at the bottom of the water column, wherein the thickness of the black and odorous sediments is 23cm; slowly inputting deionized water into the water column to enable the water depth to reach 44cm. Detecting TOM, pH value and NH in black and odorous sediment sample 4 + -N、TN、TP、COD cr 、BOD 5 And heavy metals (Hg, cd, as, pb, cu, zn, ce, ni), sampling from three sampling ports covered with water, and measuring DO, pH, ORP, and S 2- 、Fe、Fe 2+ 、SS、TN、TP、NH 4 + -N、NO 3 -N、NO 2 -N、BOD 5 、COD cr And other indexes such as heavy metal.
The experiment adopts a water column with the outer diameter of 16cm, the inner diameter of 14cm and the height of 80cm, and the water column is tightly wrapped by a heating belt at the temperature of 35 ℃ to achieve the effects of heat preservation and light avoidance. 3 stainless steel valve sampling ports with the height interval of 20cm are arranged on the side wall of the water column, and water samples taken out from different sampling ports can be used for analyzing the water quality conditions of different levels.
After the sample is collected, black and odorous sediments and water samples need to be detected within 16h, so that the sample is prevented from deteriorating. A black and odorous sediment sample needs to be laid at the bottom of a water column within 36h, and then overlying water is input to reach a designated height. This experiment uses deionized water as the water column overhead.
Software is used for sorting and analyzing the release rate and the total release amount of various pollutants in a single layer or multiple layers and the time-space change process of physicochemical indexes in the overlying water body, namely, the multi-layer analysis of the migration of the nitrogen and sulfur pollutants in the black and odorous sediments to the overlying water body is carried out; calculating the average pollutant release rate of the black and odorous sediments in the current day between two adjacent layers, the average release amount of the black and odorous sediments in multiple days between two adjacent layers and the total release amount of the black and odorous sediments in the whole overlying water body according to the formulas (1), (2) and (3); and (5) calculating the conversion rate of the pollutants released by each layer of the overlying water body on the same day and the average conversion rate of each layer for multiple days according to the formulas (4) and (5). The experiment was run at a summer simulated temperature of 35 ℃ with the set sampling times being day 1, day 2, day 3, day 4, day 5, day 6, day 7, day 9, day 11, day 13, day 15, day 17, day 19, day 21, day 23, day 25, day 27, day 29, day 31, day 33; because the concentration of any pollutant of the overlying water is not in a stable state at the 33 rd day, the experimental days are prolonged to 48 days, and the sampling interval is changed to 3 days; and because the concentration of any pollutant in the overlying water body is not in a stable state at the 48 th day, the sampling time is prolonged to 63 days, and the sampling interval is changed to 5 days.
Then there are: water volume between two adjacent layers of water column =12 × (1.4 ÷ 2) 2 ×π＝3.079L；
Total overlying water volume within the water column =2 x 3.079=6.158l;
horizontal projection area of sediment and water interface = (0.14 ÷ 2) 2 ×π＝0.01539m 2 ；
During sampling, about 100mL of water samples are respectively taken out from 3 sampling ports of a water column (only the minimum value meeting the experimental consumption is taken), and after three layers of water samples are collected, site indexes such as DO and S should be measured in time 2- pH value and ORP, simultaneously storing enough samples in a sampling tube, storing the samples in a vacuum seal mode at 4 ℃, and detecting Fe within 6h 2+ 、SS、TN、TP、NH 4 + -N、NO 3 -N、NO 2 -N、BOD 5 、COD cr And heavy metals (Hg, cd, as, pb, cu, zn, ce, ni), minimizing sample residence time. SO coated with water at each level 4 2- The change in concentration is shown in table 1, and the average conversion rate of the contaminants between the m-th layer and the m + 1-th layer of the black odorous sediments at day n of day 63, the release amount of the black odorous sediments between the m-th layer and the m + 1-th layer from day 1 to day n, the total release amount of the black odorous sediments in the whole overlying water body from day 1 to day n, the conversion rate of the contaminants at the m-th layer at day n, and the average conversion rate of the contaminants at the m-th layer from day 1 to day n were calculated. By using SO 4 2- And NO 3 - The data for the concentration calculations are also listed in tables 1 and 2. The black and odorous sediment SO can be obtained by calculation for 63 days 4 2- The total release amount is 7027.41mg, NO 3 - The cumulative total release was-502.58 mg.Under the condition that the heating zone is wrapped and maintained at 35 ℃, substances in the black and odorous sediments in the experiment migrate and convert to upper-layer water under the action of osmotic pressure, and SO at each layer 4 2- The line graph of the concentration with time is shown in FIG. 2, and NO is shown in each layer 3 - The line graph of the concentration with time is shown in fig. 3.
Wherein: Δ t n The time interval between this sampling and the last sampling; a-1, a-2 and a-3 are respectively upper covering water samples taken out from a first upper sampling port, a first middle sampling port and a first lower sampling port; a is the horizontal projection area of the interface of the overlying water and the sediment; d n,1 ，D n,2 ，D n,3 Average conversion rates of the contaminants in layers 1, 2 and 3 from day 1 to day n, respectively; r n,1 ，R n,2 ，R n,3 Average conversion rates of the pollutants in the 1 st, 2 nd and 3 rd layers on the nth day respectively; w n,1 ，W n,2 Average release rates of pollutants of the black and odorous sediments between the 1 st layer and the 2 nd layer and between the 2 nd layer and the 3 rd layer on the nth day are respectively; q n,1 ，Q n,2 The release amounts of the black smelly deposits between the 1 st layer and the 2 nd layer and between the 2 nd layer and the 3 rd layer from day 1 to day n, respectively; q n The total release amount of the black and odorous sediments in the whole overlying water body from day 1 to day n.
Calculated from the data in table 1:
average conversion rate of black odor sediment contaminants in layer 1 from day 1 to day 7:
average conversion rate of black odor sediment contaminants in layer 2 from day 1 to day 7:
average conversion rate of black odor sediment contaminants in layer 3 from day 1 to day 7:
average conversion rate of black odor sediment contaminants in layer 1 from day 1 to day 33:
average conversion rate of black odor deposit contaminants in layer 2 from day 1 to day 33:
average conversion rate of black odor sediment contaminants in layer 3 from day 1 to day 33:
average conversion rate of black odor sediment contaminants in layer 1 from day 1 to day 63:
average conversion rate of black odor deposit contaminants in layer 2 from day 1 to day 63:
average conversion rate of black odor deposit contaminants in layer 3 from day 1 to day 63:
black odor deposit contaminant layer 1 release rate: maximum value of 1.50mg/m 2 ·d；
Black odor deposit contaminant layer 2 release rate: maximum value of 1.62mg/m 2 ·d；
Black odor deposit contaminant layer 3 release rate: the maximum value is 6.99mg/m 2 ·d；
Black smelly deposit 63 days SO 4 2- The cumulative total release is
The above experimental results demonstrate that the closer the layer is to the sediment, the more the overlying water body is affected by the sediment; it has also been demonstrated that the more sediment, the greater the maximum released concentration of contaminants in the overlying water body.
Example 2 determination and analysis of overburden water contamination of outdoor pilot scale black and odorous sediments
In order to verify the accuracy of example 1, a pilot test was conducted, and an artificial wetland was constructed, which was divided into 3 river channels on average. From the same black and odorous river in example 1, a shovel is used for collecting about 100kg of black and odorous sediments with the thickness of 6cm, and the black and odorous sediments are evenly paved into a river channel until the thickness is 23cm; then, tap water is injected as an overlying water body until the water depth is 44cm. Selecting 3 point positions with average intervals in the river channel, sampling at the position 2cm below the water surface, and measuring DO, pH, ORP and S 2- 、Fe、Fe 2+ 、SS、TN、TP、NH 4 + -N、NO 3 -N、NO 2 -N、BOD 5 、COD cr And the migration and transformation conditions of indexes such as other heavy metals and the like are averaged and analyzed.
The pilot platform was 11000 x 3500 x 1000cm constructed from reinforced concrete. The silica gel hose was fixed to the concrete, and 3 sampling points were fixed.
Software is used for sorting and analyzing the release rate and the total release amount of various pollutants and the change process of physicochemical indexes in the overlying water body, namely the analysis of the migration of the nitrogen and sulfur pollutants in the black and odorous sediments to the overlying water body; the experiment was started at the same time as in example 1, and the sampling times were set to day 1, day 2, day 3, day 4, day 5, day 6, day 7, day 9, day 11, day 13, day 15, day 17, day 19, day 21, day 26, day 31, day 36, day 41, and day 46.
During sampling, about 100mL of water samples are respectively taken out from 3 sampling ports (only the minimum value meeting the experimental consumption is taken), and after three layers of water samples are collected, site indexes such as DO and S should be measured in time 2- pH value and ORP, simultaneously storing enough samples in a sampling tube, storing the samples in a vacuum seal mode at 4 ℃, and detecting Fe within 6h 2+ 、SS、TN、TP、NH 4 + -N、NO 3 -N、NO 2 -N、BOD 5 、COD cr And heavy metals (Hg, cd, as, pb, cu, zn, ce, ni), minimizing the sample residence time. NO at the position of 2cm deep covered by water in pilot test and at the position of 2cm deep covered by water in indoor test 3 - The change situation of the concentration change value along with time is shown in figure 4, the result of the indoor test is almost consistent with the result of the pilot test, and the method has reproducibility and accuracy.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A multi-level analysis method based on a black and odorous sediment nitrogen and sulfur release device is characterized by comprising the following steps:
s1: sampling the black and odorous sediments and the overlying water thereof, recording sampling information, and respectively detecting physical and chemical indexes of the black and odorous sediments and the overlying water;
s2: designing and building a nitrogen and sulfur release device for black and odorous sediments;
s3: removing the overlying water generated by natural sedimentation in the collected sample, and laying the black and odorous sediments at the bottom of a water column container of a black and odorous sediment nitrogen-sulfur release device; slowly inputting water into a water column container, and standing to obtain an overlying water body; the depth of the overlying water body and the thickness of the black and odorous sediments are consistent with the depth of the water body of the river at the sampling site and the thickness of the sediment;
s4: sampling at different levels of the overlying water body in the step S3 at intervals, and detecting the physical and chemical indexes of a detected sample and the concentration of pollutants;
s5: analyzing the physicochemical indexes and the pollutant concentration obtained in the step S4 to obtain the time-space variation process of the conversion rate, the release rate, the total release amount and the physicochemical indexes of various pollutants in the single-layer or multi-layer water body;
s6: by analyzing the results obtained in S5, the relationship between the indices and the microbial population change are obtained.
2. The method of claim 1, wherein the conversion rate, release rate, and total release of each contaminant in the single layer or multiple layers in step S5 are calculated according to the following equations:
r in the formula (1) n,m Represents the average pollutant release rate of the black and odorous sediment between the mth layer and the (m & gt 1) th layer on the nth day, and the unit is mg/(L & d); c. C m Represents the concentration of the contaminant in the mth layer, mg/L;
d in formula (2) n,m Represents the conversion rate of the pollutants in the m layers from the 1 st day to the n th day, and has the unit of mg/(L.d); c. C n,m Concentration at the mth layer on day n of the contamination, mg/L;
w in formula (3) n,m Represents the release rate of the pollutant concentration of the black and odorous sediment between the m layer and the m +1 layer on the n day, and the unit is mg/(m) 2 ·d)；C n,m The pollutant concentration of the experimental water column on the mth layer on the nth day is shown in the unit of mg/L; t is time in units of d; v is the volume of the water body between the mth layer and the m +1 layer, L; a is the horizontal projection area of the sediment and water interface, m 2 ；
The release rate of the average pollutant concentration of the experimental water column at the mth layer and the (m + 1) th layer on the nth day is expressed in mg/(L.d);
q in formula (4) n,m Represents the release amount of black odor sediment pollutants on the mth layer from the 1 st to the nth days, and the unit is mg; a represents the horizontal projection area of the black and odorous sediment and water interface, m 2 ；
The total amount of change in unit area of the m-th layer of black and odorous deposits from day 1 to day n is expressed in mg/m 2 ；
Q in formula (5) n The total release amount of the black odor sediment pollutants in the whole covering water from the 1 st day to the nth day is expressed in mg; a represents the horizontal projection area of the black and odorous sediment and water interface, m 2 ；
Representing black smelly deposits from day 1 to day nThe unit area release amount is mg/m 2 。
3. The multilevel analysis method according to claim 2, wherein the sampling time interval of the overlying water body in step S4 is: sampling once daily from day 1 to day 7 and once 2 days from day 7 to day 33; if the concentration of the pollutants is not stable at the 33 rd day, the period is prolonged to 48 days, and the sampling interval is 3 days; if not stable at day 48, extend to 63 days, during which the sampling interval is 5 days; until the target concentration stabilizes.
4. The multi-level analysis method according to claim 3, wherein the accumulated water sampling amount of the experiment set in step S4 is controlled to be equal to the volume of raw water
Within, the first 20mL of each sampling is discarded, and the rest is a detection sample; and after sampling, replenishing the water body to the original water level in time.
5. The multi-level analysis method as claimed in claim 4, wherein the black and odorous sediment nitrogen and sulfur release device in step S2 comprises a water column container, a water pipe and a water tank, wherein a plurality of sampling ports are vertically installed on the side surface of the water column container, and the sampling ports are equally spaced and are 10-20cm apart from each other.
6. The multi-level analysis method according to claim 5, wherein the steps S2 to S6 are repeated under different initial physicochemical conditions, the variation trend of the pollutants in the overlying water body of a single level or a plurality of levels under multiple conditions is statistically analyzed, and the pollutant concentration release rate of the black and odorous sediments, the release amount between each level and the total release amount in the whole overlying water body are respectively calculated.
7. The multilevel analysis method according to claim 1, wherein the black and odorous sediments are taken out for analysis after the experiment is finished, and compared with the physicochemical indexes obtained in the step S1, the influence result of the covering of the overlying water body on the black and odorous sediments is obtained.
8. The multi-level analysis method according to any one of claims 2-7, wherein the physicochemical indexes of the black and odorous sediment sample in step S1 include pH, total nitrogen, total phosphorus, ammonia nitrogen, available sulfur, five-day biochemical oxygen demand, chemical oxygen demand, and heavy metal concentration;
the physicochemical indexes of the overlying water sample in the step S1 comprise dissolved oxygen, sulfur ions, pH, oxidation-reduction potential, ferrous ions, total iron, suspended solids, total nitrogen, total phosphorus, ammonia nitrogen, nitrate nitrogen, nitrite nitrogen, five-day biochemical oxygen demand, chemical oxygen demand and other heavy metals;
the sampling information in the step S1 comprises information such as water depth, sediment thickness, sediment color, stink degree, sediment state and sediment temperature of a sampling place.
9. A black and odorous sediment nitrogen and sulfur release device for operating the analysis method of any one of the preceding claims, characterized by comprising a water column container, a water conveying pipe and a water tank; the side surface of the water column container is vertically provided with a plurality of sampling ports with equal intervals and intervals of 10-20cm, the center of the top cover of the water column container is vertically fixed with a porous water inlet pipe, and a water pipe connecting the water column container and the water tank is connected with a peristaltic pump.
10. The device of claim 9, wherein the highest sampling port of the sampling ports is arranged below the water level of the overlying water body by 2cm, and the lowest sampling port is arranged above the sediment surface by 2 cm;
the height of the water column container is 40-100 cm higher than the sum of the depth of the water body and the thickness of the black and odorous sediments, the height-diameter ratio is 4-6, and the wall thickness is 1-2 cm, and the water column container is wrapped by a shading heating belt;
the porous water inlet pipe is made of PP (polypropylene), the length of the porous water inlet pipe is equal to the distance from a top cover of the water column to a sediment, the height-diameter ratio of the porous water inlet pipe is 15-30, small holes with the diameter of about 2mm are uniformly drilled in the underwater part, the top of the porous water inlet pipe is 2cm higher than the top of the water column, and the bottom of the porous water inlet pipe is flush with the lowest sampling port;
the sample connection includes at the inside porous outlet pipe of water column container and the sample valve who links to each other with it, porous outlet pipe material is PP, and length equals the water column radius, and the pipe wall has evenly beaten diameter 2 mm's hole.
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