CN1129001C - Method for analyzing water in gap between deposits - Google Patents
Method for analyzing water in gap between deposits Download PDFInfo
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- CN1129001C CN1129001C CN 00134364 CN00134364A CN1129001C CN 1129001 C CN1129001 C CN 1129001C CN 00134364 CN00134364 CN 00134364 CN 00134364 A CN00134364 A CN 00134364A CN 1129001 C CN1129001 C CN 1129001C
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Abstract
The present invention discloses a method for analyzing the gap between deposits, which comprises the steps that samples are collected and processed, the processed samples are added into an indoor simulation device which is arranged in an artificial weather case for shade culture, measuring the pH and Eh of deposits, collecting covering water and gap water, measuring the adsorption state NH4 <+> of substrate sludge, measuring the NH4 <+>-N of the substrate sludge by nesslerization, calculating the release flux of the calculate, etc. Since the present invention uses the specific indoor simulation device, the disadvantages of the poor time accuracy, the large volume and complicated sampling steps of a gap water balance sampler are overcome.
Description
Technical field
The invention belongs to the collection and the analysis and testing technology field of water sample, relate to a kind of method for analyzing water in gap between deposits.
Background technology
In lake, ocean water Environmental Studies, especially to the chemical quality of sediment-water termination shift, in the research of chemical substance early stage diagenetic process in the distribution characteristics of near interface and migration mechanism and sediment, the geochemistry of gap water is an important research contents.Use gap water balance sampling thief in the open air always and gather original position gap water or gather loam core or top layer bed mud, again through layering, centrifugal or pressure (taking out) filter acquisition gap water with special sediment sampler.
In lab simulation research, adopt the anaerobism centrifuge method to obtain gap water mostly.But anaerobism is centrifugal operating conditions is required harshness, in filling the environment of nitrogen, carry out to avoid the influence of oxygen in the air as need.Even so, the change of pressure, acidity and temperature also can influence the chemical equilibrium of gap water in the operation.The maximum deficiency of centrifuge method is that it belongs to destructive sampling, can not carry out long-term Position Research to sample.
Summary of the invention
The object of the present invention is to provide a kind of method for analyzing water in gap between deposits, to overcome existing weak point in the above-mentioned prior art.
Task of the present invention is finished in the following manner, and a kind of method for analyzing water in gap between deposits may further comprise the steps:
The collection of a, sample and processing: get the S ﹠ W sample of required layer position, filter water sample immediately after transporting the laboratory back, 0～4 ℃ of preservation of sediment and filtered water sample is standby;
B, the sample (being the S ﹠ W sample) after will handling add indoor simulation device: make the water layer thickness of sedimental mud layer thickness and water sample form certain altitude; Described indoor simulation device is a cylindrical container, it is drilled with aperture on base plate sidewall nearby, level is inserted rhizosphere soil solution sampling thief to the container middle part, be inserted with platinum electrode, Ag-AgCl electrode and pH combination electrode on the rubber plug of container upper cover plate, and be provided with air-vent (thermowell of holding concurrently);
C, jam-pack rubber plug insert in the bed mud electrode; Feed high-purity (99.99%) N by air-vent to head space
22～8 minutes, insert thermometer immediately and use the sealing of silicone glass cement; Indoor simulation device is put into growth cabinet carry out the shading cultivation;
The mensuration of d, sediment pH and Eh: every 3～5 days, with the SY-5 electricity lead, pH-Eh, temperature-indicating instrument measure sedimental pH and Eh;
The collection of e, overlying water and gap water: every 10～20 days once sampling, gather the gap water sample, open rubber plug and gather the overlying water sample, use filtering with microporous membrane, refrigeration immediately with syringe with rhizosphere soil solution sampling thief; In culture vessel, mend the water sample of equivalent carefully, take a breath, seal with quadrat method by recited above then, put into growth cabinet and continue to cultivate by step a gained.
F, bed mud ADSORPTION STATE NH
4 +Mensuration: get plastic centrifuge tube several, add fresh sediment and filtered water sample respectively through mixing, all the other disposal routes are with described in the step e; Get 3 centrifuge tube samples when gathering water sample at every turn; Inhale with syringe and to remove overlying water, centrifugally measure bed mud ADSORPTION STATE NH after removing gap water
4 +
G, mensuration, calculating: bed mud NH
4 +-N measures with Nesslerization, NH
4 +-N discharges the calculating of flux to be undertaken by " lake eutrophication investigation standard ".
The water sample that institute's suction filtration goes out among the step a is preferably by 0.45 μ m filter membrane (use earlier the filter paper coarse filtration in case of necessity, suction filtration is by 0.45 μ m filter membrane again).
Preferably have additional on the rubber plug of the container upper cover plate of the indoor simulation device described in the step b/venthole and gas sampling mouth.
The degree of depth that electrode described in the step c inserts bed mud can be controlled at 0～5cm, and the temperature that described shading is cultivated needs to decide according to open-air actual conditions, and scope can be from 0～35 ℃.
Step e can also comprise the collection of gas, and gaseous sample is gathered by the gas sampling mouth with microsyringe.
Below by specific embodiment the present invention is described in further detail.
Description of drawings
Fig. 1 represents that sediment is in neutral strong reducing environment substantially;
Fig. 2 has reflected overlying water and gap water NH between culture period
4 +The variation of-N concentration;
Fig. 3 has reflected under the anaerobic condition, sediment-water termination NH
4 +The accumulative total flux of-N and the relation of incubation time;
Fig. 4 is an indoor simulation device synoptic diagram used in the present invention.
Embodiment
The West Lake, Hangzhou is China famous scenery travelling lake, still belongs to the eutrophy lake at present.Utilize method provided by the present invention that the anaerobism that West Lake bed mud carried out 78 days is by a definite date cultivated, and adopt rhizosphere soil solution sampling thief that sedimental gap water between culture period is positioned the continuous sampling analysis.
1. materials and methods
1.1 material
1.1.1 S ﹠ W sample on October 18th, 1999 is at the middle of a lake, the West Lake, Hangzhou acquisition tables surface sediments and water sample.Filter water sample immediately after transporting the laboratory back, 4 ℃ of preservations of bed mud and filtered water sample are standby.
1.1.2 rhizosphere soil solution sampling thief mainly is made up of porous polyester pipe, pvc pipe and screw type raised type connector.Its feature is (1) small and exquisite (caliber 2.5mm), and is little to the system disturbance during installation.(2) (bleed part limpid can directly analysis of variable-length, filtrate) easy to use (3) dead volume little (＜0.1ml), adsorption desorption effect is little, can respond the variation of solution concentration to be measured fast, measures the spatial and temporal resolution height.
(φ l0cm * 11cm) sidewall is apart from the boring of base plate 5mm place, and level is inserted rhizosphere soil solution sampling thief to the container middle part 1.1.3 indoor simulation device is at cylindrical container.Be inserted with platinum electrode, Ag-AgCl electrode and pH combination electrode on the rubber plug of container upper plate, and be provided with air-vent (thermowell of holding concurrently).In container, add the fresh sediment (mud layer thick about 5cm) of 1675g, and carefully add the filtered lake water of 1250mL (the thick about 4cm of water layer) through mixing.The jam-pack rubber plug makes electrode insert the about lcm of bed mud.Feed high-purity (99.99%) N by air-vent to head space
2About 5 minutes, insert thermometer immediately and use the sealing of silicone glass cement.Culture vessel is put into growth cabinet (LRH-250-GS Guangdong Medical Apparatus and Instruments Factory), cultivate, establish 4 repetitions 25 ℃ of following shadings.
1.2 method
1.2.1 sediment pH and Eh every 3～5 days with the SY-5 electricity lead, pH-Eh, temperature-indicating instrument (Chinese Academy of Sciences's Nanjing soil Research Institute) measure sedimental pH and Eh.
1.2.2 the collection of overlying water and gap water is every 2 all left and right sides once sampling: gather gap water sample 15mL with rhizosphere soil solution sampling thief, open rubber plug and gather overlying water sample 75mL, use immediately that miillpore filter (0.45 μ m) filters, refrigeration with syringe.In culture vessel, mend the filtered water sample of 90mL carefully, press the described method ventilation of preamble, sealing then, put into growth cabinet and continue to cultivate.
1.2.3 bed mud ADSORPTION STATE NH
4 +Mensuration get 30 of 100mL plastic centrifuge tubes, add fresh sediment and the 30mL filtered lake water of 35g respectively through mixing, all the other disposal routes are with described in the 1.2.2.Get 3 centrifuge tube samples when gathering water sample at every turn.Inhale with syringe and to remove overlying water, centrifugal (5500rpm 25min) measures bed mud ADSORPTION STATE NH after removing gap water
4 +
1.2.4 mensuration, computing method bed mud NH
4 +-N measures with Nesslerization, NH
4 +-N discharges the calculating of flux to be undertaken by " lake eutrophication investigation standard ".
2. result and discussion
2.1 sediment pH and Eh
The variation of sediment pH and Eh as shown in Figure 1 between culture period.Cultivating in initial 10 days pH nearly 0.3 the pH unit (dropping to pH6.87) that descends from pH7.16.The pH luffing is less, basicly stable about 6.86 ± 0.01 after 10 days.And Eh in an initial week, sharply descend (reduce to-447mV), slightly go up afterwards from-185mV, basicly stable after one month at-379 ± 5mV.The syndiagenesis (as organic matter decomposition, redox, resolution of precipitate reaction etc.) that takes place in the variation of sediment Eh-pH and the sediment is relevant.Fig. 1 shows: sediment is in neutral strong reducing environment substantially.Under reducing condition, the NH that the organic nitrogen mineralising produces
4 +-N is everlasting and accumulates in the reducing zone, most ofly exists with exchange state.
2.2 overlying water and gap water NH
4 +The exchange of-N
Fig. 2 has reflected overlying water and gap water NH between culture period
4 +The variation of-N concentration.As can be seen from Figure 2, in the training period, overlying water NH
4 +-N concentration constantly increases, and gap water NH
4 +-N concentration descends earlier, after be and increase trend gradually.During to 78 days, overlying water NH
4 +-N concentration has approached gap water NH
4 +-N concentration (be respectively 11.6 and 11.96mg/L).
It should be noted that overlying water NH in preceding 18 days
4 +-N concentration has increased nearly 3.6 times (increasing to 7.29mg/L from 2.05), and the same period gap water NH
4 +-N concentration the 1.1mg/L (dropping to 9.05mgN/L) that only descended from 10.15.In this research, overlying water NH
4 +The variation of-N concentration only may be because the decomposition of diffusion (2) surface deposit of (1) gap water discharges.In fact, because the concentration difference of overlying water and gap water (being initially 8.1mg/L, is 1.76mg/L in the time of 18 days) greatly, it is slower to add under the anaerobic condition organic nitrogen decomposition rate
[12,17], overlying water NH in preceding 18 days
4 +The increase of-N concentration should be mainly owing to the diffusion of gap water.
For verifying above-mentioned viewpoint, we adopt Fick first law:
Estimate NH in preceding 18 days
4 +The diffusing capacity of-N.Wherein, F is the diffusion flux by sediment-water termination,
0Be the factor of porosity of surface deposit, D
sBe the molecular diffusivity that comprises the buckling effect of sedimentary particle irregular arrangement, when ＞0.7, D
s=
2D
0(D
0Be the desirable coefficient of diffusion of ion in infinite dilution solution), last is the concentration gradient of sediment water termination, the concentration difference Δ C/ Δ x that generally can be similar to near interface replaces.
During estimation, gets 0.88, and Δ x gets 5cm (being this research measured value), D
0Get 19.8 * 10
-6Cm
2s
-1[9], and suppose that overlying water and gap water concentration all are linear change, the F definite integral is tried to achieve NH in 18 days
4 +The diffusing capacity of-N.The estimation result is: the contribution rate of diffusion is about 99%, and the contribution rate that the top layer decomposition discharges only is about 1%.In addition, the bed mud ADSORPTION STATE NH that measures the same period
4 +The result of-N also shows: bed mud ADSORPTION STATE NH in initial 18 days
4 +-N has significantly and to reduce (reducing to 88 μ g/g dry weights from 115 μ g/g dry weights), and the ammonium that this explanation has part exchange state desorb from the bed mud gets off to enter gap water.Above rough estimation confirms: overlying water NH in preceding 18 days
4 +-N concentration increases main diffusion from gap water.
In late stage of culture, the gap water concentration has the trend of rising, and this explanation bed mud organic matter decomposition discharges into the NH of gap water
4 +The amount of-N has surpassed the NH that gap water reduces because of diffusion
4 +The amount of-N.
2.3 NH under the anaerobic condition
4 +The release flux of-N
Under the anaerobic condition, sediment-water termination NH
4 +The accumulative total flux of-N and the relation of incubation time are as shown in Figure 3.As can be seen from Figure 3, accumulative total flux vs incubation time curve presents three phases.In preceding 18 days, NH
4 +-N rate of release is very fast.This mainly shifts owing to the chemical quality of sediment-water termination, i.e. diffusion.During 18～39 days, along with constantly the dwindling of gap water and overlying water concentration difference (referring to Fig. 2), rate of diffusion descends, NH
4 +-N flux gathers way and slows down.After 39 days, NH
4 +The accumulative total flux of-N almost is linear to be increased, but the speed that increases is much smaller than first stage.This moment overlying water NH
4 +The increase of-N concentration has two approach probably: the organic decomposition product in (1) sediment top layer directly enters overlying water; (2) NH of the inner organic matter decomposition release of sediment
4 +-N partly enters gap water, enters overlying water via diffusion again.
According to two NH that linear stage calculates among Fig. 3
4 +The rate of release of-N is respectively 11.60 and 5.12mg m
-2d
-1Song Jing (1999) adopts manual shift overlying water pH to 8.5 every day, and intermittently feeds N to water layer
2Obtain West Lake bed mud NH under the condition
4 +The rate of release of-N is 1.99mg m
-2d
-1[18]Because differences such as research object, method, condition have bigger difference between the result of study.For example, Luijn etc. (1999) is to Nuldernauw lake (Holland) bed mud NH under the anaerobic condition
4 +The result of study that-N discharges flux is: 19.49～81.65mg m
-2d
-1(mud matter bed mud); 17.47～50.40mg m
-2d
-1(chiltern bed mud)
1
3. conclusion
Under the anaerobic condition, sediment-water termination NH
4 +Accumulative total flux and the time curve of-N present three phases, and the diffusion of different phase gap water discharges the contribution of overlying water concentration increase different with sedimental decomposition.According to two NH that linear stage calculates in accumulative total flux-incubation time curve
4 +The rate of release of-N is respectively 11.60 and 5.12mgm
-2d
-1
Soil liquid micro-scale sampler overcome traditional centrifuge method, take out that (pressure) filter method can't be carried out the shortcoming of original position METHOD FOR CONTINUOUS DETERMINATION and gap water balance sampling thief volume is big, sampling step is loaded down with trivial details, the weakness of time resolution rate variance.It has characteristics such as small and exquisite, easy to use, temporal resolution height, is a strong instrument of gap water geochemistry research.
With reference to Fig. 4, employed indoor simulation device has measuring cell 1 in the method for analyzing water in gap between deposits disclosed by the invention, measuring cell top board 11, sensor 2 and soil liquid micro-scale sampler 4, measuring cell 1 is a cylindrical container, measuring cell top board 11 is in the top of measuring cell 1, be inserted with sensor 2 on the rubber plug 3 of measuring cell top board 11, sensor 2 in Fig. 4 includes platinum electrode 21, Ag- AgCl electrode 22,23 and pH combination electrode 24, the information acquisition end of sensor 2 is positioned at measuring cell 1 inside, and its information output stretches out the measuring cell outside, measuring cell 1 offers aperture near on the sidewall 12 of base plate, and soil liquid micro-scale sampler 4 is fixed in this aperture via rubber plug.From Fig. 4, it can also be seen that, be provided with simultaneously on the measuring cell top board 11/venthole 5 and gas sampling mouth 6.
And above-mentioned soil liquid micro-scale sampler is made of connector, pvc pipe and micropore polyester tube, one end closure of micropore polyester tube, the other end passes through the pvc pipe continued access on connector, the periphery of the binding site of pvc pipe and micropore polyester tube has additional a gum sleeve, have additional a reinforced wire in the inside of connector, pvc pipe and micropore polyester tube, in order to increase its intensity.
The present invention is owing to adopted a kind of specific indoor simulation device, both possessed gap water balance sampling thief and can position the advantage that non-destructive is sampled, spatial resolution is high, overcome the shortcoming that gap water balance sampling thief time precision is poor, volume is big, sampling step is loaded down with trivial details again, thereby the dynamically variation of continuous monitoring sediment pH and Eh, the variation of gap water and overlying water chemical composition and headspace gas composition, can be used to study the migration conversion process of water sludge interface material, calculate the transport flux of various materials at the interface.
Claims (8)
1, a kind of method for analyzing water in gap between deposits may further comprise the steps:
The collection of a, sample and processing: get the S ﹠ W sample of required layer position, filter water sample immediately after transporting the laboratory back, 0～4 ℃ of preservation of sediment and filtered water sample is standby;
B, the sample after will handling add indoor simulation device: make the water layer thickness of sedimental mud layer thickness and water sample form certain altitude; Described indoor simulation device is a cylindrical container, it is drilled with aperture on base plate sidewall nearby, level is inserted rhizosphere soil solution sampling thief to the container middle part, is inserted with platinum electrode, Ag-AgCl electrode and pH combination electrode on the rubber plug of container upper cover plate, and is provided with air-vent;
C, jam-pack rubber plug insert in the bed mud electrode; Feed high-purity N by air-vent to head space
22～8 minutes, insert thermometer immediately and use the sealing of silicone glass cement; Indoor simulation device is put into growth cabinet carry out the shading cultivation;
The mensuration of d, sediment pH and Eh: every 3～5 days, electricity consumption was led, pH-Eh, temperature-indicating instrument measure sedimental pH and Eh;
The collection of e, overlying water and gap water: every 10～20 days once sampling, gather the gap water sample, open rubber plug and gather the overlying water sample, use filtering with microporous membrane, refrigeration immediately with syringe with rhizosphere soil solution sampling thief; In culture vessel, mend the water sample of equivalent carefully, take a breath, seal with quadrat method by recited above then, put into growth cabinet and continue to cultivate by step a gained;
F, bed mud ADSORPTION STATE NH
4 +Mensuration: get plastic centrifuge tube several, add fresh sediment and filtered water sample respectively through mixing, all the other disposal routes are with described in the step e; Get 3 centrifuge tube samples when gathering water sample at every turn; Inhale with syringe and to remove overlying water, centrifugally measure bed mud ADSORPTION STATE NH after removing gap water
4 +
G, mensuration, calculating: bed mud NH
4 +-N measures with Nesslerization, according to NH in the overlying water
4 +The change calculations NH of-N concentration
4 +-N discharges flux.
2, method for analyzing water in gap between deposits as claimed in claim 1 is characterized in that the water sample that institute's suction filtration goes out among the step a passes through 0.45 μ m filter membrane suction filtration.
3, method for analyzing water in gap between deposits as claimed in claim 1 or 2 is characterized in that having additional into/venthole and gas sampling mouth on the rubber plug of container upper cover plate of the indoor simulation device described in the step b.
4, method for analyzing water in gap between deposits as claimed in claim 1 or 2 is characterized in that the degree of depth of the electrode insertion bed mud described in the step c is 0～5cm, and the temperature that described shading is cultivated is controlled at 0～35 ℃.
5, method for analyzing water in gap between deposits as claimed in claim 3 is characterized in that the degree of depth of the electrode insertion bed mud described in the step c is 0～5cm, and the temperature that described shading is cultivated is controlled at 0～35 ℃.
6, as claim 1,2 or 5 described method for analyzing water in gap between deposits, it is characterized in that step e also comprises the collection of gas, gaseous sample is gathered by the gas sampling mouth with microsyringe.
7, method for analyzing water in gap between deposits as claimed in claim 3 is characterized in that step e also comprises the collection of gas, and gaseous sample is gathered by the gas sampling mouth with microsyringe.
8, method for analyzing water in gap between deposits as claimed in claim 4 is characterized in that step e also comprises the collection of gas, and gaseous sample is gathered by the gas sampling mouth with microsyringe.
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| CN 00134364 CN1129001C (en) | 2000-12-07 | 2000-12-07 | Method for analyzing water in gap between deposits |
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| CN 00134364 CN1129001C (en) | 2000-12-07 | 2000-12-07 | Method for analyzing water in gap between deposits |
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| CN1129001C true CN1129001C (en) | 2003-11-26 |
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| MY159740A (en) * | 2005-10-17 | 2017-01-31 | Univ Putra Malaysia | Starter kit for the production of pure and high quality microalgae |
| CN101131383B (en) * | 2006-08-25 | 2011-06-08 | 中国科学院沈阳应用生态研究所 | Method and apparatus for analyzing pollutant movement in different media |
| CN100548894C (en) * | 2007-10-19 | 2009-10-14 | 中国科学院南京地理与湖泊研究所 | Be applied to the indoor simulation device of lake sediment-water interface process research |
| CN102608164A (en) * | 2012-02-16 | 2012-07-25 | 北京师范大学 | Simulation device for measuring microbial action of river sediment-water micro-interface |
| CN102914634B (en) * | 2012-10-17 | 2015-07-01 | 中国水产科学研究院南海水产研究所 | Determining system for flux of bottom mud nutritive salt under condition of simulating natural environment |
| CN105758687B (en) * | 2016-04-13 | 2018-09-07 | 杭州电子科技大学 | A kind of cultivation of halmeic deposit original position and sealing sampling mechanism |
| CN107449638A (en) * | 2017-08-29 | 2017-12-08 | 天津大学 | The device of sediment water interface Nutrients Fluxes under the influence of a kind of research oxygen |
| CN111766181B (en) * | 2020-06-29 | 2023-05-12 | 东北电力大学 | In-situ aquatic ecological nutrient salt sediment-overlying water interface migration and transformation simulation system |
| CN113406031A (en) * | 2021-06-16 | 2021-09-17 | 南京工业大学 | Quantitative calculation method for nitrogen migration and conversion in pipeline sediment-water system |
| CN113406027B (en) * | 2021-06-16 | 2022-06-14 | 南京工业大学 | Quantitative calculation method for phosphorus migration and conversion in pipeline sediment-water system |
| CN116499803B (en) * | 2023-06-29 | 2023-08-25 | 云南省生态环境科学研究院 | Mining area waste rock river sediment sampling method and sampling device |
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