CN106706540A - Method for simply measuring dissolved organic nitrogen of soil - Google Patents

Method for simply measuring dissolved organic nitrogen of soil Download PDF

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Publication number
CN106706540A
CN106706540A CN201710137318.8A CN201710137318A CN106706540A CN 106706540 A CN106706540 A CN 106706540A CN 201710137318 A CN201710137318 A CN 201710137318A CN 106706540 A CN106706540 A CN 106706540A
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soil
nitrogen
organic nitrogen
dissolved organic
soluble organic
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梁斌
李俊良
董静
丁效东
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Qingdao Agricultural University
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Qingdao Agricultural University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light

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  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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Abstract

The invention relates to a method for simply measuring dissolved organic nitrogen of soil. The method comprises the following steps of (1) collecting fresh soil, and preparing 0.5mol/L potassium sulfate solution into a soil extracting liquid, wherein the mass ratio of potassium sulfate solution to soil is 5:1; oscillating for 25 to 35min in an oscillator, and setting the rotation speed to 180 to 220 revolutions per minute; after oscillating, filtering by filter paper to obtain a clear soil extracting liquid; (2) adjusting the pH (potential of hydrogen) value of the soil extracting liquid to 8 to 9; (3) adding 2g or above of Devardas alloy into each 100ml of soil extracting liquid to perform reduction reaction for 2h at the reaction temperature of 20 to 25 DEG C; (4) enabling an ultraviolet spectrophotometer to directly measure the content of dissolved organic nitrogen in the solution, and multiplying the measuring value with coefficient 1.19, so as to obtain the actual content of dissolved organic nitrogen. The method has the advantages that the operation is simple, the efficiency is high, the measuring error is little, the result is more accurate, the measuring value is obviously related with the traditional method, and the method is especially suitable for limited testing conditions or high content of mineralizing nitrogen.

Description

Soil dissolved organic nitrogen simplifies assay method
Technical field
The present invention relates to a kind of assay method of soluble organic nitrogen in soil of simplification.
Background technology
Soil dissolved organic nitrogen refers to the organic nitrogen that can be dissolved in water or salting liquid, is most active group in soil nitrogen / mono-.On the one hand, it is one of source of the available nutrient of soil, can directly or through after conversion be crop absorb;It is another Aspect, its mobility is stronger, runoff or leaching loss can occur with Water Transport, causes environmental pollution.Research discovery, Contents of Soluble Organic Nitrogen is 2.9~12.3mgkg in farmland-1, account for soluble total nitrogen (soluble organic nitrogen and inorganic nitrogen it With) 13~82%.Found by summarizing the research of forefathers, Kessel etc., the loss of soluble organic nitrogen accounts for total molten in farmland The 26% of solution property nitrogen loss.In recent years, to explore its influence factor, composition, transport characteristics etc., increasing research around Soluble organic nitrogen launches.
At present determine soluble organic nitrogen method be minusing (such as Fig. 1), it is necessary to determine soluble total nitrogen content and The content of mineral nitrogen, both differences are the content of soluble organic nitrogen.The method complex steps;And the survey of mineral nitrogen Determine the result of calculation that result directly affects soluble organic nitrogen, especially in mineral nitrogen content soil high, mineral nitrogen Content influence of the error of measure on calculating soluble organic nitrogen is very big, or even is calculated as negative value in other instances;Due to can The measure of dissolubility total nitrogen is carried out using alkaline chitinase oxidizing process, and the ammonium nitrogen in solution is often sent out in continuous mode Raw loss, makes the measurement result of soluble organic nitrogen relatively low;In addition, using15When N tracer techniques are tested, it is impossible to directly Detection15Behaviors of the N in soluble organic nitrogen.
The content of the invention
For problem above, the present invention is intended to provide a kind of new method, makes the measure of soluble organic nitrogen easier, error It is smaller, it is as a result more accurate, it is more suitable for mineral nitrogen content soil high.
A kind of Soil dissolved organic nitrogen simplifies assay method, comprises the following steps:
(1) fresh soil is gathered, soil extraction, potassium sulfate solution and soil is made of 0.5mol/L potassium sulfate solutions Mass ratio is 5:1,25-35min is vibrated in vibrating machine, rotating speed is 180-220 revs/min, is filtered with filter paper after the completion of vibration Soil extraction must be clarified;
(2) pH of soil extraction is adjusted to pH=8~9;
(3) reduction reaction is carried out to the Devardasalloy of addition 2g and the above in every 100ml soil extractions, reaction temperature is 20-25 DEG C, the reaction time is 2 hours;
(4) ultraviolet spectrophotometer method directly determines the Contents of Soluble Organic Nitrogen in solution, and measured value is multiplied by into coefficient 1.19 obtain actual Contents of Soluble Organic Nitrogen.
Further, 2mm soil sieves are crossed after collection soil in the step (1), makes the nitrogen in soil be easier to be dissolved into In solution.
Further, extraction temperature is 20-25 DEG C in the step (1), makes the nitrogen in soil be easier to be dissolved into solution In.
Further, pH is 9 in the step (2).
Further, reaction temperature is 20 DEG C in the step (3).
Leaching liquor prepared by the step (1) includes nitrate nitrogen, ammonium nitrogen and soluble organic nitrogen.
It is for next step nitrate-nitrogen reduction is ammonium nitrogen and ammonium nitrogen that the step (2) adjusts to pH=8-9 pH Volatilization provides reaction condition.
It is that nitrate nitrogen is completely converted into ammonium state that the step (3) adds the purpose of 2g and above Devardasalloy (excess) Nitrogen;
Step (4) coefficient 1.19 is that a small amount of hydrolysis of soluble organic nitrogen is damaged effectively in supplement correction above-mentioned steps Lose.
Mineral nitrogen in solution (nitrate nitrogen and ammonium nitrogen) can be converted into ammonia discharge by the inventive method, and retain original Soluble organic nitrogen, the solubility in solution is then directly determined by ultraviolet spectrophotometer method (potassium persulfate oxidation method) Organic nitrogen content, the method is simple to operate, efficient, and evaluated error is smaller, as a result more accurate, determines numerical value notable with conventional method Correlation, a kind of method that can be directly determined as soluble organic nitrogen.The method is particularly well-suited to following two situations:One is examination Test that condition is limited, lack the situation of instrument needed for mineral nitrogen determination;Two is high in mineral nitrogen content, to soluble organic nitrogen knot Fruit influences big situation.This method can also pass through15N isotope marks are directly studied in soluble organic nitrogen15N abundance.
Brief description of the drawings
Fig. 1 prior arts soluble organic nitrogen determines general flow chart;
Fig. 2 soluble organic nitrogens of the present invention determine general flow chart;
Influence of Fig. 3 differential responses condition to the ammonium nitrogen rate of recovery;
Influence of Fig. 4 differential responses condition to the nitrate nitrogen rate of recovery;
The influence that Fig. 5 differential responses condition is decomposed to soluble organic nitrogen;
Influence of Fig. 6 differential responses temperature and time to nitrate-nitrogen reduction efficiency;
Influence of Fig. 7 differential responses temperature and time to soluble organic nitrogen resolution ratio
Fig. 8 conventional methods and the inventive method soluble organic nitrogen determination data correlation analysis.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only used to explain the present invention, not For limiting the present invention.
The determination of each reaction condition of the inventive method of embodiment 1
(1) influence of different reducing agents and reaction pH to nitrate-nitrogen reduction
Ammonium nitrogen solution, nitrate nitrogen solution and the solubility of 10mg/L are prepared with ammonium sulfate, potassium nitrate and glycine respectively Organic nitrogen solution.
Choose two kinds of reducing agents to be tested, respectively:Zn-FeSO4And Devardasalloy.The different pH value of selection, determines The reduction efficiency of nitrate nitrogen, speed and the influence to Contents of Soluble Organic Nitrogen in solution.PH gradient selection is as follows:
Reducing agent species and pH value test process
Reducing agent species Solution and reducing agent volume mass ratio PH value test process
Zn-FeSO4 50:1 PH=7, pH=9, pH=14, COH -=2mol/L, COH -=5mol/L
Devardasalloy 50:1 PH=7, pH=9, pH=14, COH -=2mol/L, COH -=5mol/L
Nitrate nitrogen and ammonium nitrogen content in respectively processing above are determined with traditional Flow Analyzer method, potassium persulfate oxidation is used Minusing (Fig. 1) determines the content of soluble organic nitrogen, calculates the volatilization rate of recovery of ammonium nitrogen (with the volatilization discharge of ammonia form Ammonium nitrogen accounts for the percentage of ammonium nitrogen total amount in original solution in solution), the reduction rate of recovery of nitrate nitrogen (is reduced to the nitre of ammonium nitrogen State nitrogen accounts for the percentage of nitrate nitrogen total amount in original solution), clearly difference reducing agents and pH are to the shadow of soluble organic nitrogen in solution Ring.
Influence of the reaction condition to the ammonium nitrogen rate of recovery:From figure 3, it can be seen that when pH is 7, the rate of recovery of ammonium nitrogen Less than 15%;When pH is 9, Zn-FeSO4Under two kinds of reduction systems of Devardasalloy, the rate of recovery of ammonium nitrogen is respectively 93% With 96%;In pH14, Zn-FeSO4The rate of recovery with ammonium nitrogen under two kinds of reduction systems of Devardasalloy is 95%;In hydrogen-oxygen Root (OH-) when reaching 2mol/L, the rate of recovery of ammonium nitrogen has declined concentration, when hydroxyl concentration is 4mol/L, the rate of recovery is small In 85% (Fig. 3).
Influence of the reaction condition to the nitrate nitrogen rate of recovery:Nitrate nitrogen in solution is converted into ammonium state in the presence of reducing agent Nitrogen, ammonium nitrogen is converted into and its rate of recovery is determined after ammonia volatilizees in the basic conditions.Figure 4, it is seen that because pH7 is unfavorable In the volatilization of generation ammonium nitrogen, cause under conditions of pH7, the rate of recovery of nitrate nitrogen is less than 12%.PH value more than 9 (including 9) when, the rate of recovery of nitrate nitrogen all more than 70%, and Devardasalloy as reducing agent when nitrate nitrogen the rate of recovery it is obvious More than the situation that Zn-FeSO4 makees reducing agent, it is seen that in the basic conditions, Devardasalloy is more beneficial for the reduction of nitrate nitrogen.With When Devardasalloy makees reducing agent, the rate of recovery of nitrate nitrogen is respectively 89% and 91% under the conditions of pH9 and pH14, substantially conforms to survey Provisioning request.
Influence of the reaction condition to soluble organic nitrogen resolution ratio:The present invention, will be molten by selecting suitable reaction condition Ammonium nitrogen and nitrate nitrogen discharge in liquid, remaining soluble organic nitrogen is directly determined by ultraviolet spectrophotometer method, Therefore it is required that in preceding treatment, the decomposition loss of soluble organic nitrogen is reduced as far as possible.Fig. 5 shows, in pH7, substantially can not Dissolubility organic nitrogen is decomposed, and with the rising of pH value, the resolution ratio of soluble organic nitrogen gradually rises, and is illustrated in the strong condition of alkalescence Under, soluble organic nitrogen is hydrolyzed to ammonium nitrogen.Therefore suitable pH value is selected, should ensures that nitrate nitrogen and ammonium nitrogen are arranged completely Go out, reduce the decomposition loss of soluble organic nitrogen as far as possible again.Although the decomposition without soluble organic nitrogen in neutral conditions Loss, but now the rate of recovery of nitrate nitrogen and ammonium nitrogen is extremely low (Fig. 3, Fig. 4), does not meet test requirements document.When pH is 9, can The resolution ratio of dissolubility organic nitrogen is 10~12%, substantially conforms to require (Fig. 5).
By above test result analysis, pH9 is selected, it is optimal reaction condition that Devardasalloy makees reducing agent.
(2) influence of different temperatures and reaction time to nitrate-nitrogen reduction
On the basis of the optimal reducing agent and pH value in reaction chosen in step (1), using the potassium nitrate solution of 10mol/L Influence of the research differential responses temperature and time to reduction efficiency (nitrate-nitrogen reduction is the percentage of ammonium nitrogen efficiency).Experiment because Element and level are as follows, constitute completely randomized experiment, are repeated 3 times.
Experimental factor Reaction temperature Reaction time
Test level 20 DEG C of ebuillition of heated, room temperature 0.5h、1h、2h、5h
The content of nitrate nitrogen, ammonium nitrogen in respectively processing above is determined with the method in step (1), the reduction of ammonium nitrogen is calculated Efficiency.
Temperature and time influences on the reduction efficiency of nitrate nitrogen:Either room temperature or ebuillition of heated, prolonging over time Long, nitrate-nitrogen reduction rate is raised, and is 2 hours in the reaction time, and the nitrate nitrogen rate of recovery reaches respectively under the conditions of room temperature and ebuillition of heated 95% and 97% (Fig. 6) is respectively during by 92% and 94%, 5 hour.
The influence that temperature and time is decomposed to soluble organic nitrogen:On the whole, ebuillition of heated promotes soluble organic nitrogen Decomposition, this is unfavorable for test objective.As shown in fig. 7, at ambient temperature, the reaction time is 0.5,1,2,5 small When soluble organic nitrogen resolution ratio be respectively 5%, 8.7%, 10.2% and 9.8%.
Consider raising nitrate-nitrogen reduction efficiency, reduce soluble organic nitrogen resolution ratio, while test efficiency is improved, Selected in the present invention under room temperature condition, reaction be advisable within 2 hours.
2 pairs of detections of actual soil of embodiment
Drawn by embodiment 1, selection Devardasalloy does reducing agent, pH9, and reaction temperature is room temperature, 2 hours reaction time It is optimum reaction condition.At this point in the reaction, determine Contents of Soluble Organic Nitrogen in Soil, and carried out with conventional method it is right Than verifying the reliability of the method.
Collection pedotheque totally 102, soil types includes moisture soil (54), cinnamon soil (32) and loessal soil (16) three Kind, Land-Use includes three kinds of farmland (45), orchard (34) and vegetable plot (23).Use 0.5mol/L potassium sulfate solutions 102 pedotheques are made soil extraction respectively, extraction temperature is 23 DEG C, and potassium sulfate solution is 5 with the mass ratio of soil: 1,30min is vibrated in vibrating machine, rotating speed is 180 revs/min, and being filtered with filter paper after the completion of vibration must clarify leaching liquor, will soak Extract is divided into two parts, and for the measure of the inventive method (Fig. 2), another is determined portion for conventional method (Fig. 1).
The inventive method is followed the steps below:
(1) pH of each soil extraction is adjusted to pH=9 with NaOH solution.
(2) reduction reaction is carried out to the Devardasalloy of addition 2g in every 100ml soil extractions, reaction temperature is 20 DEG C, Reaction time is 2 hours.
(3) ultraviolet spectrophotometer method directly determines the Contents of Soluble Organic Nitrogen in solution.
Conventional method is followed the steps below:
(1) 5ml soil extractions and 5ml oxidants, oxidant NaOH containing 0.15mol/L are added in tool plug test tube With 30g/L potassium peroxydisulfates;
(2) it is the wrapping of tool plug test tube stopper is tight, heating in pressure cooker is put into, maintain 121 DEG C of 30min;
(3) take out tool plug test tube and be cooled to room temperature;
(4) total nitrogen content in solution (C is determined with ultraviolet specrophotometer1);
(5) 5ml soil extractions are taken in addition, and wherein mineral nitrogen content C is determined with Flow Analyzer2
(6) Contents of Soluble Organic Nitrogen is C1And C2Difference.
The correlation of the control present invention and conventional method, as shown in figure 8, the soil that the inventive method is determined with conventional method Contents of Soluble Organic Nitrogen is in extremely notable positive correlation, and numerical value is less than normal compared with conventional method, and relational expression is y=1.1896x, Data of the present invention are multiplied by the ≈ 1.19 of correction coefficient 1.1896 and can obtain conventional method determination data.
Come from 23 pedotheques in vegetable plot in the present embodiment more due to applying fertilizer, thus wherein mineral nitrogen content compared with Height, is remained to accurately determine very much its organic nitrogen content with the present invention.Therefore, the inventive method is particularly well-suited to mineral nitrogen Content situation high, because conventional method is minusing, therefore the error that mineral nitrogen is determined is to calculating soluble organic nitrogen Content influence is very big, or even is calculated as negative value in other instances.And the inventive method is by excluding the mineral nitrogen in soil, Directly organic nitrogen is measured, then will not be influenceed by mineral nitrogen content, therefore measurement result is more accurate.
It should be appreciated that for those of ordinary skills, can according to the above description be improved or converted, And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.

Claims (5)

1. a kind of Soil dissolved organic nitrogen simplifies assay method, it is characterised in that comprise the following steps:
(1) fresh soil is gathered, the quality of soil extraction, potassium sulfate solution and soil is made of 0.5mol/L potassium sulfate solutions Than being 5:1,25-35min is vibrated in vibrating machine, rotating speed is 180-220 revs/min, filters clear with filter paper after the completion of vibration Clear soil extraction;
(2) pH of soil extraction is adjusted to pH=8~9;
(3) reduction reaction is carried out to the Devardasalloy of addition 2g and the above in every 100ml soil extractions, reaction temperature is 20- 25 DEG C, the reaction time is 2 hours;
(4) ultraviolet spectrophotometer method directly determines the Contents of Soluble Organic Nitrogen in solution, and measured value is multiplied by into coefficient 1.19 Obtain actual Contents of Soluble Organic Nitrogen.
2. Soil dissolved organic nitrogen according to claim 1 simplifies assay method, it is characterised in that the step (1) 2mm soil sieves are crossed after middle collection soil.
3. Soil dissolved organic nitrogen according to claim 1 and 2 simplifies assay method, it is characterised in that the step (1) extraction temperature is 20-25 DEG C in.
4. Soil dissolved organic nitrogen according to claim 1 simplifies assay method, it is characterised in that the step (2) Middle pH is 9.
5. Soil dissolved organic nitrogen according to claim 1 simplifies assay method, it is characterised in that the step (3) Middle reaction temperature is 20 DEG C.
CN201710137318.8A 2017-03-09 2017-03-09 Method for simply measuring dissolved organic nitrogen of soil Pending CN106706540A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107102023A (en) * 2017-06-27 2017-08-29 伊犁师范学院 A kind of method of testing of Land-Use
CN107505274A (en) * 2017-09-01 2017-12-22 湖北大学 A kind of method system of visible spectrophotometry measure content of soil nitrate-N

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101545866A (en) * 2009-05-06 2009-09-30 北京市农林科学院 Method for measuring content of inorganic nitrogen in soil

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101545866A (en) * 2009-05-06 2009-09-30 北京市农林科学院 Method for measuring content of inorganic nitrogen in soil

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
贾勇: "影响水中氮测量准确性因素的研究", <散文百家-教育百家> *
闫颖等: "总有机碳分析仪测定土壤中微生物量方法的改进", <理化检验-化学分册> *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107102023A (en) * 2017-06-27 2017-08-29 伊犁师范学院 A kind of method of testing of Land-Use
CN107505274A (en) * 2017-09-01 2017-12-22 湖北大学 A kind of method system of visible spectrophotometry measure content of soil nitrate-N

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