CN114910547A - Method for detecting ammonium nitrogen 15N and application thereof - Google Patents
Method for detecting ammonium nitrogen 15N and application thereof Download PDFInfo
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- CN114910547A CN114910547A CN202210829498.7A CN202210829498A CN114910547A CN 114910547 A CN114910547 A CN 114910547A CN 202210829498 A CN202210829498 A CN 202210829498A CN 114910547 A CN114910547 A CN 114910547A
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Abstract
The invention belongs to the technical field of ecological environment substance circulation and pollution control, and particularly relates to a method for detecting ammonium nitrogen 15N and application thereof. The method comprises the following steps: NH in a sample to be tested 4 + Oxidation to NO 2 ‑ Obtaining a treatment liquid, mixing the treatment liquid with denitrifying microorganisms to remove NO 2 ‑ Conversion to N 2 O, detecting N 2 Nitrogen isotope composition of O. The invention provides a method for detecting ammonium nitrogen by combining the characteristics of denitrifying microorganisms through a chemical method 15 Compared with the traditional method, the method saves the detection time, avoids using various highly toxic reducing agents, and is safer. The invention provides a method for detecting ammonium nitrogen 15 The N method has higher detection recovery rate, accuracy and precision, and is used for tracing ammonium nitrogen pollutionAnd nitrogen cycling processes provide important research tools.
Description
Technical Field
The invention belongs to the technical field of ecological environment substance circulation and pollution control, and particularly relates to a method for detecting ammonium nitrogen 15N and application thereof.
Background
Nitrogen is one of elements constituting earth life and is an important limiting factor for plant growth and crop yield increase. At present, the nitrogen content in the ecological environment is increased, and a series of environmental problems such as surface water eutrophication, aquatic organism toxicity generation, dust-haze weather and the like are caused. Ammonium nitrogen is one of the important existing forms of nitrogen in water, and the nitrogen isotope composition is an important means for identifying nitrogen sources and an effective way for researching the migration and transformation processes of nitrogen in land and aquatic ecosystems.
There are many methods for measuring the ammonium nitrogen isotopes in water and soil, and the common method is to adopt the pretreatment of distillation, diffusion and ion exchange to treat NH 4 + Conversion to N 2 Or a nitrogen containing ammonium salt, in combination with a mass spectrometer. The distillation method comprises heating and distilling NH by increasing pH value of the solution 4 + Conversion to NH 3 And measuring after absorbing the distillate by an acidic absorbent or acidic filter paper. The diffusion method comprises micro-diffusion method comprising directly placing water or soil leaching solution in a container, adding alkaline reagent, sealing, performing shaking culture at room temperature or under heating condition for several hours to more than ten days to obtain NH in the sample 4 + Conversion to NH 3 Added with an acid absorbent (such as H) 2 SO 4 、KHSO 4 Etc.), drying the filter paper or the filter membrane, wrapping the filter paper or the filter membrane by a tin cup, and measuring by an element analyzer-isotope mass spectrometer. The ion exchange chromatography is generally to enrich NH in water or soil leach liquor by passing through ion exchange resin 4 + Then the N isotope abundance is determined by combining the diffusion method. For lower NH concentrations 4 + In recent years, researchers have proposed a new analytical technique, chemical conversion, which uses hypobromite to begin with NH 4 + Oxidation to Nitrite (NO) 2 - ) Then NO is reduced by using reducing agent such as sodium azide-acetic acid buffer solution or hydroxylamine hydrochloride 2 - Reduction to N 2 O, and then measuring the delta by combining a Precon or TraceGas connecting isotope mass spectrometer 15 N-N 2 O, calculating delta in the original solution by using a calibration curve of the standard solution 15 N-NH 4 + The value is obtained.
The distillation method has a high nitrogen recovery rate, but is easily caused by decomposition of organic nitrogen due to heating 15 N cross contamination and requires professional equipment such as Kjeldahl apparatus, freeze dryer, etc., flowComplicated process and difficult outdoor operation; the diffusion method has low recovery rate and long culture time (generally 5-10 days), and condensed water is generated on the container wall in the culture process, so that isotope fractionation is generated; the ion exchange method is susceptible to strong ions, and when the diffusion method is combined with the ion exchange method, the defect of the diffusion method exists. In addition, the methods require large sample amount, and samples such as general rainwater, lake water, river water, well water and the like need to be collected by 500-2500mL on site, so that the difficulty of field sampling work is increased. Although the chemical conversion of hypobromite requires a small sample size, the first step is to remove NH 4 + By oxidation to NO 2 - Sodium arsenite (NaAsO) is required 2 ) To terminate the oxidation reaction and absorb the excess hypobromite, NaAsO 2 The arsenic is extremely toxic and easily dissolved in water to cause water body pollution, and the risk of lung cancer, bladder cancer, skin cancer and other cancers of people can be increased by taking arsenic into a human body; in the second reduction step, sodium azide-acetic acid buffer solution (azide and acetic acid buffer) or hydroxylamine hydrochloride (NH) is used 2 OH, HCl) and the like, wherein the hydrazoic acid is extremely toxic and is easy to explode, and the hydroxylamine hydrochloride is also extremely toxic, has irritation to the skin, is easy to cause harm to the human body and has certain danger. On the other hand, both of the hydrazoic acid and the hydroxylamine hydrochloride contain N, and N is easily produced 2 The exchange of nitrogen occurs to O, which in turn affects the accuracy of the test results.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for detecting ammonium nitrogen 15N and application thereof. Detection of ammonium nitrogen by a combined chemical-microbiological assay 15 And N, the method has higher accuracy and safety.
In a first aspect, the present invention provides a method for detecting ammonium nitrogen 15 N, comprising:
NH in a sample to be tested 4 + Oxidation to NO 2 - Obtaining a treatment liquid, mixing the treatment liquid with denitrifying microorganisms to obtain NO 2 - Conversion to N 2 O, detection of N 2 Nitrogen isotope composition of O.
The invention adopts a chemical method combined with a microbiological method to measure ammonium nitrogenδ 15 The N value can be simultaneously carried out with the oxidation process of ammonium nitrogen, the completion time is easy to be grasped, and the test time is greatly shortened compared with a diffusion method and an ion exchange chromatography. According to the method, concentration and isotope tests can be completed by adopting a small sample volume (at most 15 mL), and the workload of collecting samples in the field is obviously reduced. Meanwhile, the invention adopts a microbiological method to replace virulent reducing agents such as hydrazoic acid or hydroxylamine hydrochloride and the like in the reduction process, the reaction waste liquid is easy to treat, and the harmfulness to human bodies and the environment is reduced.
As the denitrifying microorganism used in the present invention, commercially available denitrifying microorganisms having the ability to convert NO can be used 2 - Conversion to N 2 The ability to O is preferably selected from the group consisting of nitrite-reducing stenotrophomonas (A)Stenotrophomonas nitritireducens）。
Further, the mixing of the treatment liquid and the denitrifying microorganisms to mix NO 2 - Conversion to N 2 O comprises:
culturing the denitrifying microorganism with the concentration of 8 x 10 8 cfu/ml~1.6×10 9 Between cfu/ml, obtaining denitrifying microorganism bacterial liquid; after the foam inhibitor is added, removing N in the denitrifying microorganism liquid by nitrogen 2 O。
Further, the mixing reaction time of the treatment liquid and the denitrifying microorganism lasts at least 1 hour.
Further, detecting N 2 After the nitrogen isotope composition of O, ammonium nitrogen can be obtained by international standard sample correction 15 Isotopic results for N.
Further, the culture medium adopted in the culture process is a TSB culture medium and/or an NB culture medium; and/or the culture condition in the culture process is that the temperature is 22-30 ℃ and the rotating speed is 160-180 rpm/min.
Further, the TSB culture medium comprises the following components in parts by weight: 100-200 parts of TSB, (NH) 4 ) 2 SO 4 1-5 parts of KH 2 PO 4 20-30 parts.
Further, it is characterized byNH in the sample to be measured 4 + Oxidation to NO 2 - Obtaining a treatment fluid comprising:
using BrO - NH in the sample to be detected 4 + Oxidation to NO 2 - After the reaction is finished, Na is adopted 2 S 2 O 3 The oxidation reaction is terminated.
Further, the adoption of BrO - NH in the sample to be detected 4 + Oxidation to NO 2 - The reaction is carried out at room temperature for 30-45 min.
Further, Na 2 S 2 O 3 The concentration of (b) is 0.1-0.3 mol/L, and the dosage is 20-50 muL, preferably 0.2mol/L and 20 muL.
The invention adopts sodium thiosulfate to replace sodium arsenite to terminate the oxidation reaction, thereby further reducing the harmfulness to human bodies and environment.
Further, the BrO - The preparation method comprises the following steps:
using sodium bromate and sodium bromide as raw materials, mixing acid to generate Br 2 And mixing alkali after 5-10 minutes to obtain BrO - Preferably for 5 min.
Further, the BrO - The dosage of the test sample is 6-15%, preferably 10%.
Further, the mass ratio of the sodium bromate to the sodium bromide is (0.4-0.8): (4-6).
NH in the sample to be tested 4 + Oxidation to NO 2 - After the treatment liquid is obtained, the pH value of the treatment liquid is adjusted to 5-12.
The pH of the treatment liquid is preferably 8-11.
Further, determination of N by means of a trace gas preconcentration device-isotope ratio mass spectrometer 2 The nitrogen isotope composition of O can obtain ammonium nitrogen 15 The amount of N.
Further, for the sample to be detected, if the total NH in the sample to be detected 4 + The concentration is higher and the concentration is diluted to 1-20 mu mol/L, preferably 10-15 mu mol/L.
The invention further provides the method for preparing ammonium nitrogen in soil, rainwater, surface water, underground water, bottom mud, atmospheric aerosol or isotope tracing experiments 15 N in the detection of the compounds.
The invention has the following beneficial effects:
the invention provides a method for measuring ammonium nitrogen delta by combining a chemical method with a microbiological method 15 Method for the N value, NO by denitrifying microorganisms 2 - Conversion to N 2 Compared with other existing methods, the O flow avoids using a highly toxic reducing agent and has higher safety; the used instruments and reagents are more conventional, and the detection cost is reduced; meanwhile, the method still has high recovery rate and accuracy, has the advantages of scientificity, simplicity and strong operability, and has a wide popularization prospect.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents, bacteria and the like used in the following examples are commercially available unless otherwise specified. Four standard substances USGS25, USGS26, USGS-N1 and RSIL-N7373 were purchased from USGS/Reston Stable Isotope Laboratory.
Example 1
The present embodiment provides an ammonium nitrogen δ 15 A chemical-microbiological combined assay method for N, comprising the steps of:
(1) enrichment of microbial colonies
3g tryptone Soy Broth agar (TSB), 0.05g (NH) was weighed 4 ) 2 SO 4 ，0.49g KH 2 PO 4 Dissolving 200mL deionized water, mixing, packaging 120mL into 250mL glass bottle with air-permeable plug, and autoclaving at 121 deg.C for 30min to obtain microbial colonyStenotrophomonas nitritireducensATCC number BAA-12, purchased from ATCC) enriched TSB broth; will be provided withStenotrophomonas nitritireducensInoculating single bacterial colony of microbial bacteria to a bottle TCulturing in SB culture solution on a shaker (30 deg.C, 180 rpm/min) for 1-2 days;
(2) determination of NH in a sample 4 + Concentration and sample application volume
Determination of NH in a rainwater sample by a flow injection analyser 4 + The concentration is 165.71 mu mol/L, the dilution is 15 times, 2mL is taken for subsequent reaction;
(3) oxidation reaction-NH in sample 4 + Oxidation to NO 2 -
First, BrO is prepared - Storage liquid: BrO - Storage liquid: 0.6g sodium bromate (sodium bromide) and 5g sodium bromide (sodium bromide) were dissolved in 250mL deionized water; 0.2mL of stock solution was added to 10mL of deionized water, followed by 0.6mL of 6M HCl to generate Br 2 After 5 minutes of dark reaction, 10mL 10M NaOH was added quickly to generate BrO - Form BrO - A working solution.
Next, 2mL of the rainwater sample tested in step (2) and 2mL of the USGS25, USGS26 and IAEA-N1 standard samples of 10. mu. mol/L were added to 20mL of a headspace bottle baked at 450 ℃ for 4 hours, respectively, followed by addition of 0.2mL of hypobromous acid (BrO) - ) The working solution is shaken on a shaker at 200rpm/min for reaction for 30min, and 20 mu L of 0.2mol/L Na is added after the reaction is finished 2 S 2 O 3 Terminating the oxidation reaction;
(4) NH in the sample 4 + Oxidation to NO 2 - Post pH adjustment
Adding a few drops of 6M HCl into the sample and the standard after the reaction in the step (3) is ended to adjust the pH value to be about 11, and sealing by using a sealing film for later use;
(5) adding cell culture into the headspace bottle, purifying the upper space and removing N in the microbial solution 2 O
Adding a few drops of antifoaming agent into the microorganism culture bottle in the step (1) after enrichment culture, subpackaging 4mL into 20mL headspace bottles, sealing, purging by adopting a nitrogen purging instrument, inserting the headspace bottles on a nitrogen needle in an inverted manner, inserting a 6 cm-long 25gauge needle on a bottleneck silica gel pad at the flow rate of 20-40 mL/min, and introducing air in the headspace bottles and N in bacterial liquid 2 Replacement of O with high-purity nitrogenDischarging, purging for 30min, and taking down the headspace bottle for later use;
(6) the microorganisms convert NO 2 - Conversion to N 2 O
Respectively adding 2mL of the sample and the standard substance obtained in the step (4) into the bacteria liquid headspace bottle purged in the step (5) by using an airtight syringe (the total ammonium nitrogen content is about 0.2 mu g), simultaneously sucking 2mL of gas, fully and uniformly mixing the sample and the bacteria liquid, carrying out inverted culture for 1 hour, adding 0.20 mL of NaOH with the concentration of 10mol/L after the reaction is finished, and stopping the reaction and absorbing the generated CO 2 ；
Meanwhile, 0.10mL (total nitrogen content is 0.2 mu g) of 2mg/L RSIL-N7373 standard sample is taken by an air-tight syringe to react with the bacterial liquid;
（7）N 2 o-nitrogen isotope assay
N generated by the headspace bottle obtained in the step (6) 2 The O gas is measured by a TraceGas trace gas analyzer-Isotope Ratio Mass Spectrometer (IRMS) to obtain N 2 A measurement of the composition of the O nitrogen isotope;
（8）NH 4 + -δ 15 n test result correction
The results obtained in step (7) are shown in Table 1, measured by an instrument:
TABLE 1 Standard and rainwater NH 4 + Delta of 15 True, measured and corrected values of N
Note: a is NaNO 2 Is a nitrite standard, and the value represents delta 15 N -NO 2 -
As can be seen from the results in Table 1, the value of RSIL-N7373 measured was delta 15 N = -80.26 +/-0.23 permillage, which is very close to the true value-79.6 permillage, which indicates that the microbial thallus reduces nitrite into N 2 The results for O are reliable. And performing linear regression on the measured value and the actual value of the ammonium nitrogen standard sample to obtain a correction equation of T = 1.0948M +2.7744, wherein T is the actual value, M is the measured value, and R =0.9999, so that the linear relation is better. According to a correction equation and rainwater NH 4 + -δ 15 N measured value, obtaining rainwater NH 4 + -δ 15 The true value of N is-7.12 per mill, and according to the literature, the value is traced to the source and shows NH in rainwater 4 + Mainly from ammonia released from animal excreta.
It can be seen that the method of the present invention is completely feasible to test the composition of the rainwater ammonium nitrogen isotopes.
Example 2
This example provides an ammonium nitrogen δ 15 The chemical-microorganism combined determination method of N comprises the following specific operation steps:
(1) 3g tryptone Soy Broth agar (TSB), 0.05g (NH) was weighed 4 ) 2 SO 4 ，0.49g KH 2 PO 4 Dissolving and uniformly mixing 200mL of deionized water, subpackaging 35mL of deionized water into a 50mL centrifuge tube, and carrying out autoclaving at 121 ℃ for 30min to form a microbial colony enriched TSB culture solution; respectively will be respectively provided withStenotrophomonas nitritireducensInoculating single colony into TSB culture solution, and culturing on shaker (26 deg.C, 160 rpm/min) for 2-3 days;
(2) determination of NH in a sample 4 + Concentration and sample application volume
Determination of NH in 2M KCl soil leach liquor by flow injection analyzer 4 + The concentration is 22.5 mu mol/L, the solution is diluted by 2 times, and 2mL of the solution is taken for subsequent reaction;
steps (3) to (4) were the same as in example 1.
(5) Adding cell culture into the headspace bottle, purifying the upper space and removing N in the microbial solution 2 O
Step (1) of completing a plurality of enrichment culturesStenotrophomonas nitritireducensPouring the culture tube into a sterilized triangular flask, mixing uniformly, adding a few drops of antifoaming agent, subpackaging 4mL into 20mL headspace bottles, sealing, purging with a nitrogen purging instrument, inserting the headspace bottles into a nitrogen needle in an inverted manner, inserting a 6cm needle with a length of 25gauge into a bottle mouth silica gel pad at a flow rate of 20-40 mL/min, and introducing air in the headspace bottles and N in the bacterial liquid 2 Replacing O with high-purity nitrogen, purging for 30min, and taking down the headspace bottle for later use;
steps (6) to (7) were the same as in example 1.
（8）NH 4 + -δ 15 N test result correction
The results obtained in step (7) are shown in Table 2, as measured by an instrument:
TABLE 2 Standard and soil leach liquor NH 4 + Delta of 15 True, measured and corrected values of N
Note: a is NaNO 2 Is a nitrite standard, the value represents delta 15 N -NO 2 -
As can be seen from the results in Table 2, the value of RSIL-N7373 determined is delta 15 N = -79.2 +/-0.11 permillage, which is very close to the true value-79.6 permillage, which indicates that the microbial thallus reduces nitrite into N 2 The results for O are reliable. And performing linear regression on the measured value and the actual value of the ammonium nitrogen standard sample to obtain a correction equation of T = 1.1116M +2.153, wherein T is the actual value, M is the measured value, and R =0.9998, so that the linear relation is better. According to a correction equation and soil leaching liquor NH 4 + -δ 15 The measured value of N is obtained to obtain soil leaching liquor NH 4 + -δ 15 The true value of N is-0.55 per mill, and according to the literature, the value is traced to the source and shows NH in the soil 4 + Mainly ammonia released by fertilizers.
Therefore, the method for testing the composition of the ammonium nitrogen isotopes in the soil leaching solution is completely feasible and has higher accuracy.
Example 3
Ammonium nitrogen delta 15 The chemical-microorganism combined determination method of N comprises the following specific operation steps:
step (1) was the same as in example 2.
(2) Determination of NH in a sample 4 + Concentration and sample application volume
Determination of river NH by flow injection Analyzer 4 + The concentration is 5.5 mu mol/L, 5 is takenmL, carrying out subsequent reaction;
steps (3) to (5) were the same as in example 2.
Step (4) requires taking 5mL of the river sample tested in step (2) and then adding 0.5mL of hypobromous acid (BrO) - ) Carrying out oxidation reaction on the working solution;
(6) the microorganisms convert NO 2 - Conversion to N 2 O
Respectively taking 5mL of the sample in the step (4) by using an airtight injector, adding 2mL of each standard sample into the bacteria liquid headspace bottle purged in the step (5) (the total ammonium nitrogen amount is about 0.2 mu g), simultaneously sucking out corresponding volume of gas, fully and uniformly mixing the sample and the bacteria liquid, carrying out inverted culture overnight, adding 0.20 mL of NaOH with the concentration of 10mol/L after the reaction is finished, and stopping reaction and absorbing generated CO 2 (ii) a Meanwhile, 0.10mL of 2mg/L RSIL-N7373 standard sample (total nitrogen content 0.2. mu.g) was taken out with a gas-tight syringe;
steps (7) to (8) were the same as in example 2.
As a result, NH of the river water is obtained 4 + -δ 15 The true value of N is-9.59 per mill, which indicates NH in the river water 4 + Mainly from ammonia released from animal excreta from surrounding farms.
Thus, it can be seen that the method of the present invention is used to test NH in a body of water 4 + -δ 15 The N value is completely feasible and has higher accuracy.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method for detecting ammonium nitrogen 15N, comprising:
NH in a sample to be tested 4 + Oxidation to NO 2 - Obtaining a treatment liquid, mixing the treatment liquid with denitrifying microorganismsNO 2 - Conversion to N 2 O, detecting N 2 Nitrogen isotope composition of O.
2. The method of claim 1, wherein the denitrifying microorganism is stenotrophomonas nitrite-reducing.
3. The method of claim 1, wherein the mixing of the treatment fluid and the denitrifying microorganisms mixes the NO with the treatment fluid 2 - Conversion to N 2 O comprises:
culturing the denitrifying microorganism with the concentration of 8 x 10 8 cfu/ml~1.6×10 9 Between cfu/ml, obtaining denitrifying microorganism bacterial liquid; after the foam inhibitor is added, removing N in the denitrifying microorganism liquid by nitrogen 2 O。
4. The method according to claim 3, wherein the culture medium used in the culture process is TSB medium and/or NB medium; and/or the culture condition in the culture process is that the temperature is 22-30 ℃ and the rotating speed is 160-180 rpm/min.
5. The method of claim 1, wherein the NH in the sample to be tested is 4 + Oxidation to NO 2 - Obtaining a treatment fluid comprising:
using BrO - NH in the sample to be detected 4 + Oxidation to NO 2 - After the reaction is finished, Na is adopted 2 S 2 O 3 The oxidation reaction is terminated.
6. The method of claim 5, wherein the BrO - The preparation method comprises the following steps:
using sodium bromate and sodium bromide as raw materials, mixing acid to generate Br 2 And mixing alkali after 5-10 minutes to obtain BrO - 。
7. The method of claim 5, wherein the BrO - The amount of the reagent is 6-15% of the sample to be detected.
8. The method according to claim 5, wherein Na is added to the mixture 2 S 2 O 3 After the oxidation reaction is terminated, adjusting the pH of the treatment liquid to 5-12; the Na is 2 S 2 O 3 The concentration of (b) is 0.1 to 0.3 mol/L.
9. The method of claim 1, wherein the determination of N is performed by a trace gas preconcentration device-isotope ratio mass spectrometer 2 The nitrogen isotope composition of O can obtain ammonium nitrogen 15 The amount of N.
10. Ammonium nitrogen for use in soil, rain, surface water, ground water, sediment, atmospheric aerosol or isotope tracer experiments according to the method of any one of claims 1 to 9 15 N in the detection of the compounds.
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007090148A (en) * | 2005-09-27 | 2007-04-12 | Hitachi Plant Technologies Ltd | Method and apparatus for measuring reaction ratio |
| US20080245730A1 (en) * | 2004-09-30 | 2008-10-09 | Takaaki Tokutomi | Process and Apparatus for Treating Nitrogeneous Liquor |
| CN105601820A (en) * | 2015-12-31 | 2016-05-25 | 四川大学 | Hydrophilic modification method of methyl cellulose |
| CN106483294A (en) * | 2015-08-27 | 2017-03-08 | 中国科学院大连化学物理研究所 | A kind of selective enrichment and the method for identification N- connection glycopeptide |
| CN108680697A (en) * | 2018-06-28 | 2018-10-19 | 南京信息工程大学 | Ammonium nitrogen isotope ratio values determination method in a kind of atmospheric aerosol based on chemical conversion |
| CN109593838A (en) * | 2018-12-28 | 2019-04-09 | 江苏大学 | A kind of screening technique of the heterotrophic nitrification of saline-alkali tolerant-anaerobic denitrifying bacterial strain |
| CN110988106A (en) * | 2020-03-04 | 2020-04-10 | 中国农业科学院农业环境与可持续发展研究所 | Nitrous oxide isotope delta15N correction method |
| CN111111422A (en) * | 2019-12-05 | 2020-05-08 | 中国科学院生态环境研究中心 | Method for cooperatively treating volatile organic compounds and nitrogen-sulfur-containing malodorous substances |
| CN111167302A (en) * | 2019-12-05 | 2020-05-19 | 中国科学院生态环境研究中心 | Plug flow combined biological-electrochemical co-processing equipment and application thereof |
| US20200223716A1 (en) * | 2018-02-01 | 2020-07-16 | University Of Central Florida Research Foundation, Inc. | Iron filings-based green environmental media for nutrient removal and methods of use |
| WO2021008617A1 (en) * | 2019-07-18 | 2021-01-21 | 中国环境科学研究院 | Pretreatment method for nitrogen and oxygen isotope measurement with chemical conversion method and measurement method |
| CN114591119A (en) * | 2022-04-08 | 2022-06-07 | 天津农学院 | Degradable resin coated slow-release fertilizer and preparation method thereof |
-
2022
- 2022-07-15 CN CN202210829498.7A patent/CN114910547A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080245730A1 (en) * | 2004-09-30 | 2008-10-09 | Takaaki Tokutomi | Process and Apparatus for Treating Nitrogeneous Liquor |
| JP2007090148A (en) * | 2005-09-27 | 2007-04-12 | Hitachi Plant Technologies Ltd | Method and apparatus for measuring reaction ratio |
| CN106483294A (en) * | 2015-08-27 | 2017-03-08 | 中国科学院大连化学物理研究所 | A kind of selective enrichment and the method for identification N- connection glycopeptide |
| CN105601820A (en) * | 2015-12-31 | 2016-05-25 | 四川大学 | Hydrophilic modification method of methyl cellulose |
| US20200223716A1 (en) * | 2018-02-01 | 2020-07-16 | University Of Central Florida Research Foundation, Inc. | Iron filings-based green environmental media for nutrient removal and methods of use |
| CN108680697A (en) * | 2018-06-28 | 2018-10-19 | 南京信息工程大学 | Ammonium nitrogen isotope ratio values determination method in a kind of atmospheric aerosol based on chemical conversion |
| CN109593838A (en) * | 2018-12-28 | 2019-04-09 | 江苏大学 | A kind of screening technique of the heterotrophic nitrification of saline-alkali tolerant-anaerobic denitrifying bacterial strain |
| WO2021008617A1 (en) * | 2019-07-18 | 2021-01-21 | 中国环境科学研究院 | Pretreatment method for nitrogen and oxygen isotope measurement with chemical conversion method and measurement method |
| CN111111422A (en) * | 2019-12-05 | 2020-05-08 | 中国科学院生态环境研究中心 | Method for cooperatively treating volatile organic compounds and nitrogen-sulfur-containing malodorous substances |
| CN111167302A (en) * | 2019-12-05 | 2020-05-19 | 中国科学院生态环境研究中心 | Plug flow combined biological-electrochemical co-processing equipment and application thereof |
| CN110988106A (en) * | 2020-03-04 | 2020-04-10 | 中国农业科学院农业环境与可持续发展研究所 | Nitrous oxide isotope delta15N correction method |
| CN114591119A (en) * | 2022-04-08 | 2022-06-07 | 天津农学院 | Degradable resin coated slow-release fertilizer and preparation method thereof |
Non-Patent Citations (7)
| Title |
|---|
| JOHN KARL BO1HLKE 等: "《Isotopic analysis of N and O in nitrite and nitrate by sequential selective bacterial reduction to N2O》", 《ANALYTICAL CHEMISTRY》 * |
| RICHARD L. SMITH 等: "《Occurrence and Turnover of Nitric Oxide in a Nitrogen-Impacted Sand and Gravel Aquifer》", 《ENVIRONMENTAL SCIENCE & TECHNOLOGY》 * |
| RICHARD L. SMITH 等: "《Role of Anaerobic Ammonium Oxidation (Anammox) in NitrogenRemoval from a Freshwater Aquifer》", 《ENVIRONMENTAL SCIENCE & TECHNOLOGY》 * |
| SOPHIE WERTZ 等: "《Processes contributing to nitrite accumulation and concomitant N2O emissions in frozen soils》", 《SOIL BIOLOGY AND BIOCHEMISTRY》 * |
| WEI LIN 等: "《Evaluation of N2O sources after fertilizers application in vegetable soil by dual isotopocule plots approach》", 《ENVIRONMENTAL RESEARCH》 * |
| 郑欠 等: "《土壤含水量对硝化和反硝化过程 N2O 排放及同位素特征值的影响》", 《中国农业科学》 * |
| 陈功 等: "《泡菜榨菜亚硝酸盐含量及其N2-NH4+转化机理的研究》", 《食品与发酵科技》 * |
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