CN106885780A - A kind of method for determining soil nitrate-N - Google Patents

A kind of method for determining soil nitrate-N Download PDF

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Publication number
CN106885780A
CN106885780A CN201510944782.9A CN201510944782A CN106885780A CN 106885780 A CN106885780 A CN 106885780A CN 201510944782 A CN201510944782 A CN 201510944782A CN 106885780 A CN106885780 A CN 106885780A
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nitrate
absorbance
nitrate nitrogen
soil
solution
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周桦
马强
宇万太
姜春明
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Institute of Applied Ecology of CAS
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Institute of Applied Ecology of CAS
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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)
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Abstract

It is specifically a kind of method for determining soil nitrate-N and nitrite nitrogen summation the present invention relates to a kind of method for determining soil nitrate-N.Pedotheque is vibrated into extraction with 4 times of 2mol/L KCl solution of bulking value (g/ml), filtering, gained leaching liquor uses A in 220nm and 275nm absorbances are determined on ultraviolet-visible spectrophotometer220–2×A275Computational methods try to achieve absorbance, and establishing criteria curve, nitrate in inquiry leaching liquor.The concentration passes through formula:Y=1.021x-0.223 is corrected, and as a result determining ammonium nitrogen with the way of distillation is combined, and is set up complete set, efficient, the accurate way of distillation and is determined the inorganic nitrogen systems of soil available.The inventive method is reproducible, and reappearance is high, simple and easy to apply.

Description

A kind of method for determining soil nitrate-N
Technical field
The present invention relates to the measure of nitrified nitrogen in soil, specifically a kind of measure side for improving soil nitrate-N Method.
Background technology
Inorganic nitrogen can be divided into water-soluble state, exchange state and stationary state etc. in soil.Determine ammonium state, the nitre state in soil And nitrite nitrogen element, typically determine both water-soluble state and exchange state total amount.Exchange state is can be by neutral salt solution Exchange the part extracted (neutral salt solution is potassium chloride or sodium chloride).Neutral salt solution mixes with soil, shakes Swing, the ammonium nitrogen of adsorption by soil is exchanged and is leached, wherein also including water-soluble state.This extract is through filtering, filtrate The measure of various form nitrogen is carried out again.Conventional measure ammonium nitrogen method has the way of distillation and indophenol blue colorimetry, so And the method for determining nitrate nitrogen has a lot, including the way of distillation, disulfonic acid phenol, cadmium reducing process and dual wavelength are purple Outer AAS (document 1:Lu Rukun, soil agrochemistry analysis method, Beijing:Chinese agriculture science and technology Publishing house, 2000:156-165).
It should be noted that nitrite nitrogen falls within exchange state nitrogen, in process of crop growth, as effective nitrogenous fertilizer For crop provides nutrient, even if its content and low, the 5% of not enough nitrate nitrogen.Said determination soil nitrate-N The value determined in method can contain nitrite nitrogen.Herein involved by us be determine soil nitrate-N and Asia The method of nitrate nitrogen summation.
Conventional measure nitrate nitrogen method has the disadvantage that:The way of distillation needs specific device, and energy resource consumption is big, and Determine nitrogen alloy and be difficult the mesh sieve of levigate mistake 100;Disulfonic acid phenol operating procedure is excessively cumbersome, soil extraction moisture Evaporation time is long, take the energy and many kinds of substance has interference;Although Cadmium reduction column is disturbed less, high precision, Cumbersome and cadmium is highly toxic heavy metal, easily pollutes environment;Ripple is determined in dual-wavelength ultraviolet spectrophotometry No unified standard (document 2 long:Evergreen, Wen Xinrong is applied, dual-wavelength ultraviolet spectrophotometry determines soil nitre State nitrogen, soil and fertilizer, 2006 (1):50-51).
The content of the invention
Simple to operate it is an object of the invention to provide one kind, reproducible without any reagent, reappearance is high Measure soil nitrate-N method.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of method for determining soil nitrate-N,
1) with 2mol/L KCl as solvent compound concentration be more than 6 in the range of 0.1-20mg N/L not With the nitrate nitrogen solution of concentration, respectively with ultraviolet-visible spectrophotometer at 220nm and 275nm wavelength Determine each and prepare solution absorbance A220And A275;Use A220–2×A275Computational methods try to achieve absorbance, With nitrate as abscissa, the absorbance of calculating is ordinate making standard curve;
2) prepared by soil extraction:By pedotheque with 4 times of 2mol/L KCl solution of bulking value (g/ml) Vibration extraction more than 1h, filtering obtains leaching liquor;
3) leaching liquor is placed directly within ultraviolet-visible spectrophotometer and determines 220nm and 270nm absorbances Value, uses A220–2×A275Computational methods try to achieve absorbance, by the absorbance tried to achieve in step 1) make Standard curve in inquire about obtain leaching liquor in nitrate;
4) correction of ultraviolet spectrophotometry method measured value is turned into way of distillation measured value, formula is Y=1.021x-0.223, wherein x are the soil nitrate-N concentration measurement of ultraviolet spectrophotometry, and y is distillation The soil nitrate-N concentration measurement of method.
The step 1) prepare nitrate nitrogen solution detailed process be:It is solvent compound concentration with 2mol/L KCl It is the nitrate nitrogen solution of more than 6 various concentrations in the range of 0.1-20mg N/L, including 0.1mg The nitrate nitrogen solution of bis- end value concentration of N/L and 20mg N/L, and more than 0.1mg N/L to less than 20 The nitrate nitrogen solution of more than 4 various concentrations of mg N/L.
The step 1) prepare nitrate nitrogen solution detailed process be:It is solvent compound concentration with 2mol/L KCl It is the nitrate nitrogen solution of more than 6 various concentrations in the range of 0.1-15mg N/L, including 0.1mg The nitrate nitrogen solution of bis- end value concentration of N/L and 15mg N/L, and more than 0.1mg N/L to being less than The nitrate nitrogen solution of more than 4 various concentrations of 15mg N/L.
The step 1) detailed process be:Respectively draw concentration for 100mg N/L nitrate nitrogen solution 0.05, 0.25th, 0.5,2.5,5.0,7.5mL adds 2mol/L KCl to 50mL to carve in 50mL volumetric flasks Degree line, shake up, with ultraviolet-visible spectrophotometer at 220nm and 275nm wavelength mensuration absorbance; Use A220–2×A275Computational methods try to achieve absorbance, with nitrate as abscissa, the absorbance of calculating It is worth for ordinate makes standard curve, the standard curve range of linearity is 0.1-15mg N/L, standard curve one As be polynomial equation.
The solute that the preparation nitrate nitrogen solution is used is potassium nitrate.
Detailed process can be:A kind of method for determining soil nitrate-N,
1) standard curve is made:100mg N/L nitrate nitrogens solution (2mol/L KCl preparations) 0.05,0.25 are drawn, 0.5,2.5,5.0,7.5mL in 50mL volumetric flasks, add 2mol/L KCl constant volumes, shake up, With ultraviolet-visible spectrophotometer in 220nm and 275nm wavelength mensuration absorbances, A is used220–2×A275 Computational methods try to achieve absorbance, with nitrate as abscissa, the absorbance of calculating is ordinate Make standard curve;
2) prepared by soil extraction:Pedotheque is vibrated with 4 times of 2mol/L KCl solution of bulking value (g/ml) Extraction 1h, filtering obtains leaching liquor;
3) leaching liquor is placed directly within ultraviolet-visible spectrophotometer and determines 220nm and 270nm absorbances, Use A220–2×A275Computational methods try to achieve absorbance, query criteria curve calculates nitrate nitrogen in leaching liquor Concentration;
4) correction of ultraviolet spectrophotometry method measured value is turned into way of distillation measured value, formula is y=1.021x-0.223 (R2=0.9722, n=20), wherein x is ultraviolet spectrophotometry method measured value, and y is surveyed for the way of distillation Definite value.
Content of Nitrate-Nitrogen in Soil is determined using the method, is had the following advantages:
1. the method is easy to operate, and step is few, without adding any reagent, directly carries out the UV absorption of leaching liquor Determine, human error is small.
2. the method saves trouble.Original way of distillation or colorimetric method determine nitrate nitrogen for one day no more than 100, identical 1000 can be determined with the method in time, efficiency improves 9 times.
3. the soil nitrate nitrogen concentration and the fabulous (R of way of distillation measured value correlation for being determined using the method2=0.9722, N=20), therefore after can measured value be corrected determine ammonium nitrogen with the way of distillation to be combined, set up a set of complete Whole, efficient, the accurate inorganic nitrogen determination method system of soil available.
The inventive method is reproducible, and reappearance is high, simple and easy to apply.
Brief description of the drawings
Fig. 1 nitrate nitrogen bioassay standards curve -1;
Fig. 2 nitrate nitrogen bioassay standards curve -2;
Fig. 3 way of distillations and Soil by Spectrophotometry nitrate nitrogen result are compared;
Fig. 4 verifies the correlation of the way of distillation and determined by ultraviolet spectrophotometry nitrate nitrogen.
Specific embodiment
Embodiment 1
Set up determined by ultraviolet spectrophotometry nitrate nitrogen standard curve
Because nitrate is directly determined without any operation in soil extraction, therefore nitrate should Fully fall in the standard curve range of linearity, otherwise measurement result is inaccurate.It is computed, when nitre in the soil liquid When state nitrogen concentration is 15mg N/L, content of soil nitrate-N is about 66kg/mg, equivalent to amount of application of nitrogen fertilizer (the 0-20cm soil weight is 1.2g/cm to 158kg N/ha3), therefore nitrate nitrogen Cmax sets in standard curve 15m N g/L (if desired, it can also be provided that 20mg N/L) are set to, experiment need can be met completely Will.
After measured, there is stronger suction all at 220nm in determined by ultraviolet spectrophotometry nitrate nitrogen and nitrite nitrogen Receive peak, therefore the measurement result of the method contains nitrite nitrogen content, this nitrate nitrogen determined with the way of distillation and Nitrite nitrogen summation matches, as the experiment basis that the method and the way of distillation are mutually authenticated.In addition, soil is sub- Nitrate nitrogen is the pilot process of soil nitrification, and content is extremely low, is generally ignored in continuous mode, because This calibration curve solution is added without standard nitrite nitrogen, and its absorbance control nitrate nitrogen is calculated.
Detailed process is as follows:
1) nitrate nitrogen storing solution is prepared:It is accurate to weigh 7.216g drying potassium nitrate, add 2mol/L KCl molten Solution, is settled in 1L volumetric flasks, and this solution contains nitrate nitrogen 1000mg/L.This storing solution is pressed into 10 multiples Dilution, 2mol/L KCl constant volumes obtain the solution that concentration is 100mg N/L;
2) standard curve is made:Draw above-mentioned nitrate nitrogen solution 0.05,0.25,0.5,2.5,5.0,7.5mL In 50mL volumetric flasks, add 2mol/L KCl to graduation mark, shake up, use ultraviolet-visible spectrophotometer The mensuration absorbance at 220nm and 275nm wavelength.Use A220–2×A275Computational methods try to achieve absorbance, With nitrate as abscissa, the absorbance of calculating is ordinate making standard curve.Result such as Fig. 1 Shown, standard curve meets polynomial equation, R2=0.998 (n=7).
Embodiment 2
Ultraviolet spectrophotometry determines nitrate and compares with the way of distillation
Specific implementation process:
1) prepared by soil extraction:By pedotheque (common n=44 pedotheque) respectively with 4 times The 2mol/L KCl solution vibration extraction 1h of bulking value (g/ml), filtering obtains leaching liquor.This extraction sample It is divided into two parts, a part of (common n=20 pedotheque) is used for determining that two methods determine nitrate Correlation, remaining sample (common n=24 pedotheque) is used to verify the accuracy of the correlation;
2) standard curve is made:It is the nitrate nitrogen solution 0.05,0.25 of 100mg N/L to draw concentration, 0.5,2.5,5.0,7.5mL in 50mL volumetric flasks, add 2mol/L KCl to graduation mark, shake up, With ultraviolet-visible spectrophotometer at 220nm and 275nm wavelength mensuration absorbance.Use A220–2×A275 Computational methods try to achieve absorbance, with nitrate as abscissa, the absorbance of calculating is that ordinate makes Standard curve (Fig. 2);Standard curve is generally polynomial equation;
3) nitrate in determined by ultraviolet spectrophotometry leaching liquor:By step 1) in leaching liquor (altogether N=20 pedotheque) measure 220nm and 270nm in ultraviolet-visible spectrophotometer is placed directly within respectively Absorbance A220And A275, use A220–2×A275Computational methods try to achieve absorbance, inquiry above-mentioned standard is bent Nitrate in line computation leaching liquor;
4) way of distillation determines nitrate in leaching liquor:Said determination step 3 is taken respectively) same leaching Extract (common n=20 pedotheque) 50mL in cucurbit, while it is (interior to do blank group in a cucurbit Equipped with 50mL 2mol/L KCl solution) compareed, 1g magnesia is separately added into, it is placed in distilling apparatus In, heating distillation is carried out to being passed through water vapour in leaching liquor and blank group respectively immediately, received to condenser pipe lower end When distillate volume reaches 100mL in the triangular flask of distillate, terminate distillation, remove the triangle for receiving distillate Bottle, this step purpose is removal ammonium nitrogen.Change the triangular flask for receiving distillate into one and fill 15mL weight Concentration be 2% boric acid plus one drop (0.05mL) mixed indicator (0.066g methyl reds and 0.099g bromocresol greens Be settled to 100ml with the ethanol of volumetric concentration 95%) receiving bottle in condenser pipe lower end, continue respectively to cucurbit Middle addition 0.2g determines nitrogen alloy, and (alloy is constituted:Cu 50%, Al 45%, Zn 5%), continue respectively to distillation Water vapour is passed through in bottle to be distilled, when the distillate volume into receiving bottle reaches 100mL, terminate distillation, Remove receiving bottle.Use 0.003molL-1Sulfuric acid standard liquid is titrated, and red is manifested in solution is by grey When be titration end-point.Sulfuric acid amount according to sample consumption calculates nitrate nitrogen content (document 1:Lu Rukun, soil Earth agrochemistry analysis method, Beijing:Chinese agriculture Science Press, 2000:156-165);
Measurement result is shown in Fig. 3, and the variation of the soil extraction nitrate that randomly selects is larger, scope from 0.1-3.7mg/L is representative strong.Coefficient R=0.986 of two methods, illustrates the correlation of two methods Property preferably, ultraviolet spectrophotometry can be used to replace the cumbersome way of distillation, for determining content of soil nitrate-N.
5) remaining 24 soil extractions are taken, according to above-mentioned 3) -4) described in step, use two kinds of sides Method is measured to its nitrate, and by determined by ultraviolet spectrophotometry result according to formula y=1.021x- 0.223 correction, acquired results are compared with way of distillation measurement result, as a result as shown in Figure 4.Result shows Two methods correlation is fabulous, particularly the very low sample of concentration, and measurement result is still very identical, illustrates operation Simple ultraviolet spectrophotometry can replace the cumbersome way of distillation completely, as measure soil nitrate-N Important method.

Claims (5)

1. it is a kind of determine soil nitrate-N method, it is characterised in that:
1) with 2mol/L KCl as solvent compound concentration be more than 6 in the range of 0.1-20mg N/L not With the nitrate nitrogen solution of concentration, respectively with ultraviolet-visible spectrophotometer at 220nm and 275nm wavelength Determine each and prepare solution absorbance A220And A275;Use A220–2×A275Computational methods try to achieve absorbance, With nitrate as abscissa, the absorbance of calculating is ordinate making standard curve;
2) prepared by soil extraction:By pedotheque with 4 times of 2mol/L KCl solution of bulking value (g/ml) Vibration extraction more than 1h, filtering obtains leaching liquor;
3) leaching liquor is placed directly within ultraviolet-visible spectrophotometer and determines 220nm and 270nm absorbances Value, uses A220–2×A275Computational methods try to achieve absorbance, by the absorbance tried to achieve in step 1) make Standard curve in inquire about obtain leaching liquor in nitrate;
4) correction of ultraviolet spectrophotometry method measured value is turned into way of distillation measured value, formula is Y=1.021x-0.223, wherein x are the soil nitrate-N concentration measurement of ultraviolet spectrophotometry, and y is distillation The soil nitrate-N concentration measurement of method.
2. in accordance with the method for claim 1, it is characterised in that:
The step 1) prepare nitrate nitrogen solution detailed process be:It is solvent compound concentration with 2mol/L KCl It is the nitrate nitrogen solution of more than 6 various concentrations in the range of 0.1-20mg N/L, including 0.1mg The nitrate nitrogen solution of bis- end value concentration of N/L and 20mg N/L, and more than 0.1mg N/L to less than 20 The nitrate nitrogen solution of more than 4 various concentrations of mg N/L.
3. in accordance with the method for claim 1, it is characterised in that:
The step 1) prepare nitrate nitrogen solution detailed process be:It is solvent compound concentration with 2mol/L KCl It is the nitrate nitrogen solution of more than 6 various concentrations in the range of 0.1-15mg N/L, including 0.1mg The nitrate nitrogen solution of bis- end value concentration of N/L and 15mg N/L, and more than 0.1mg N/L to being less than The nitrate nitrogen solution of more than 4 various concentrations of 15mg N/L.
4. according to the method described in claim 1 or 3, it is characterised in that:
The step 1) detailed process be:Respectively draw concentration for 100mg N/L nitrate nitrogen solution 0.05, 0.25th, 0.5,2.5,5.0,7.5mL adds 2mol/L KCl to 50mL to carve in 50mL volumetric flasks Degree line, shake up, with ultraviolet-visible spectrophotometer at 220nm and 275nm wavelength mensuration absorbance; Use A220–2×A275Computational methods try to achieve absorbance, with nitrate as abscissa, the absorbance of calculating It is worth for ordinate makes standard curve, the standard curve range of linearity is 0.1-15mg N/L, standard curve one As be polynomial equation.
5. according to any described methods of claim 1-4, it is characterised in that:The preparation nitrate nitrogen is molten The solute that liquid is used is potassium nitrate.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109085322A (en) * 2018-08-09 2018-12-25 中国科学院植物研究所 A method of measurement soil microbial biomass nitrogen
CN112082965A (en) * 2020-09-18 2020-12-15 武汉工程大学 Method for determining occurrence state of residual ammonium salt in weathered crust elution-deposited rare earth ore
CN113252843A (en) * 2021-04-29 2021-08-13 扬州大学 Method for measuring available nitrogen of facility soil
CN114112614A (en) * 2021-12-01 2022-03-01 浙江大学 Method for determining ammonia nitrogen in soil by using water quality ammonia nitrogen rapid detection kit

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CN104198419A (en) * 2014-08-14 2014-12-10 河南农业大学 Soil nitrate nitrogen extracting agent and method for rapid determination of soil nitrate nitrogen

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109085322A (en) * 2018-08-09 2018-12-25 中国科学院植物研究所 A method of measurement soil microbial biomass nitrogen
CN112082965A (en) * 2020-09-18 2020-12-15 武汉工程大学 Method for determining occurrence state of residual ammonium salt in weathered crust elution-deposited rare earth ore
CN113252843A (en) * 2021-04-29 2021-08-13 扬州大学 Method for measuring available nitrogen of facility soil
CN114112614A (en) * 2021-12-01 2022-03-01 浙江大学 Method for determining ammonia nitrogen in soil by using water quality ammonia nitrogen rapid detection kit

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Application publication date: 20170623