CN105300980A - Method for rapidly determining soil ammonium nitrogen - Google Patents
Method for rapidly determining soil ammonium nitrogen Download PDFInfo
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- CN105300980A CN105300980A CN201510799017.2A CN201510799017A CN105300980A CN 105300980 A CN105300980 A CN 105300980A CN 201510799017 A CN201510799017 A CN 201510799017A CN 105300980 A CN105300980 A CN 105300980A
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Abstract
The invention relates to a method for rapidly determining soil ammonium nitrogen, which comprises the following steps: 1) extraction: weighing a certain amount of a soil sample and placing the soil sample in a container, adding phosphorus-free active carbon, adding a NaHCO3 aqueous solution with concentration being 0.6 mol/L, oscillating for 3-5 minutes, and filtering to obtain a leaching liquor; 2) colorimetric reaction: respectively configuring a blank control liquid, an ammonium nitrogen standard solution and a liquid to-be-measured, respectively adding a soil ammonium nitrogen masking agent, a soil ammonium nitrogen assisting agent and an ammonium nitrogen developer, standing the solution for determining the solution; and 3) colorimetric determination: adjusting an optical path wavelength to 420nm, taking the soil leaching liquor as the blank control liquid, taking the ammonium nitrogen standard solution as a scale, then placing the liquid to-be-measured in an optical path, and calculating or reading the ammonium nitrogen content in a soil sample to-be-measured. On base of rapid determination, the usage reagent quantity is reduced, the reagents are merged, the process is simplified, the cost is reduced, and stability is obviously increased.
Description
Technical field
The invention belongs to agriculture quick test technique field, be specifically related to a kind of soil ammonium rapid assay methods being applicable to neutrality, calacareous soil.
Background technology
Rich the lacking of soil nutrient, not only directly affects growing and output of nursery stock, and is weigh fertilization effect and determine whether to need fertilising, is the foundation of fertilising.When formulating plan of fertilizer application, first soil nutritional diagnosis be should carry out, according to soil nutrient content and supply situation, kind and the quantity of fertilizer determined.
In soil, the content of available nitrogen is the deliverability of reflect soil nutrient and the key foundation of rational application of fertilizers; Ammonium nitrogen wherein directly can be absorbed by plant, good correlativity is had with plant nitrogen nutrition, the confession nitrogen level reflecting soil at no distant date that can be definite, so ammonium nitrogen content's index can provide good directive function for agricultural production, reduce due to the unreasonable Environmental and ecological problems caused that applies fertilizer.Therefore, necessary to the Fast Measurement of soil ammonium.
At present, the method measuring soil ammonium mainly contains the way of distillation and colourimetry.Wherein, need in the way of distillation to use distilling apparatus, and the use procedure of this device is comparatively complicated, and still-process has potential safety hazard, some simple organic nitrogen weakly hydrolyses still may be made when weak base distills to become ammonia to steam simultaneously, make result higher, therefore the ammonium nitrogen in conventional colorimetric method for determining soil.In experiment, the colourimetry of the most conventional employing is indophenol blue colorimetry, and the method is highly sensitive, and accuracy is also higher, but the reagent used is but comparatively dangerous.Therefore, in recent years in speed is surveyed (as NY/T1848-2010), adopt Na's colorimetry to measure ammonium nitrogen comparatively conventional, but the mercuric iodixde wherein will used is extremely toxic substance, and the nessler reagent be mixed with should not be preserved for a long time, its storage life mostly is one month most.
Comprehensive, prior art remains in following problem, can not get for a long time solving: the amount of reagent required for (1) existing fast determining method is too many, and a test gets off to need to drip at least 4 kinds of reagent, and program is comparatively complicated; (2) preservation condition of nessler reagent is comparatively harsh, and the pot-life is shorter; (3) reappearance of existing fast determining method is poor.
Summary of the invention
For above problem, the invention provides a kind of soil ammonium rapid assay methods, on the basis of existing Fast Measurement, reduce the quantity using reagent, merge reagent, simplify processing step, reduce testing cost, and can stability be significantly improved, be particularly useful for the Fast Measurement of ammonium nitrogen in neutrality, calacareous soil.
For overcoming the above problems, the present invention is achieved through the following technical solutions:
Design a kind of soil ammonium rapid assay methods, comprise the following steps:
(1) lixiviate: take a certain amount of air-dry soil sample, or with its etc. the fresh soil sample of dry weight, be placed in container, non-phosphorus active carbon is added by 20 ~ 30wt% of described soil sample dry weight, universal soll digestion agent is added again by the solid-to-liquid ratio of 1g:18 ~ 25mL, temperature be 20 ~ 25 DEG C, rotating speed be the condition of 150 ~ 200r/min under concussion 3 ~ 5min after, filter, gained filtrate is the liquid to be measured of soil ammonium; Described universal soll digestion agent is the NaHCO of concentration 0.6 ~ 0.7mol/L
3aqueous solution;
Preferably, take the air-dry soil sample that 2.00g crosses 20 mesh sieves, be placed in 250mL triangular flask, add 0.5g non-phosphorus active carbon, then add the NaHCO of concentration 0.6mol/L of 40mL
3aqueous solution, then temperature be 20 ~ 25 DEG C, rotating speed be the condition of 180r/min under concussion 3 ~ 5min after, filter, gained filtrate is the liquid to be measured of soil ammonium.
Preferably, the preparation method of described non-phosphorus active carbon is: first by the hydrochloric acid soaked overnight of activated charcoal 2mol/L, then with after distilled water washing repeatedly, uses 0.5mol/LNaHCO
3aqueous solution soaking is spent the night, and after suction filtration, then washs repeatedly with distilled water, without phosphorus to cleansing solution, to obtain final product.
(2) chrominance response: get blank liquid, ammonium nitrogen standard solution and liquid to be measured respectively, and add soil ammonium screening agent respectively, soil ammonium helps and covers agent and ammonium nitrogen developer, leave standstill, in order to measuring;
Concrete steps are as follows: draw a certain amount of distilled water and do blank liquid in a container, draw isopyknic ammonium nitrogen standard solution in another container, draw isopyknic gained liquid to be measured again in the 3rd container, equivalent soil ammonium screening agent is added respectively in three containers, after shaking up, the soil ammonium adding equivalent respectively again helps the ammonium nitrogen developer covering agent and equivalent, then shakes up, leave standstill 10 minutes, in order to measuring.
Described soil ammonium screening agent, soil ammonium help covers agent and ammonium nitrogen developer consumption is 8 ~ 15% of described blank liquid accumulated amount.
The collocation method of described ammonium nitrogen standard solution: take 0.0113g(NH
4)
2sO
4(at 110 DEG C, drying 2h) is dissolved in 600mL water, adds the 10mL concentrated sulphuric acid, adds water and be settled to 1L, is ammonium nitrogen standard solution (ρ (NH
4-N)=2.40mg/L) (in subsequent measurements process, measurement of concetration shelves are adjusted with reference to scale value 48mg/kg with this ammonium nitrogen standard solution).
The collocation method of described soil ammonium screening agent: take the distilled water that 250 ~ 500g sodium potassium tartrate tetrahydrate is dissolved in 800mL, takes 200 ~ 400g NaOH in addition and is dissolved in 800mL distilled water, then mixed by two solution, add water and be settled to 2L.
Described soil ammonium helps the collocation method covering agent: take 35 ~ 60g Arabic gum and 25 ~ 45g sodium fluoride is dissolved in boiling water, and naturally cool, hold over night, gets supernatant, adds water and is settled to 1L.
The collocation method of described soil ammonium developer: take 40 ~ 65g potassium iodide and 150g NaOH is dissolved in 600mL water, adds saturated mercuric chloride solution while stirring, till there is orange precipitation, adds water and be settled to 1L, hold over night, get supernatant.
(3) colorimetric estimation: the light path wavelength of adjustment photometer or photolometer is to 420nm, with soil extract agent solution or distilled water for blank liquid, the absorbance of ammonium nitrogen standard solution and liquid to be measured is measured respectively at absorbance measuring shelves, or adjust with reference to scale value at measurement of concetration shelves with ammonium nitrogen standard solution, then liquid to be measured is placed in light path, the corresponding content calculating or read ammonium nitrogen in pedotheque to be measured.
The present invention has following positive beneficial effect:
(1) assay method of the present invention simplifies determination step, improves work efficiency, 10 minutes batch sample, and multiple sample can a batch of mensuration.
(2) compared with existing fast determining method (NY/T1848-2010), assay method of the present invention decreases the quantity of reagent, is only 3 kinds, can reduce testing cost.And in soil ammonium lixiviate process in early stage, have employed the general digestion agent of single component, this general digestion agent overcomes traditional technology prejudice, only lixiviate can go out the soil effective constituent such as ammonium nitrogen and soil available nitrogen, nitrate nitrogen, rapid available phosphorus with a kind of reagent, and this digestion agent does not introduce the ion component of interfere with subsequent colorimetric estimation, comparatively abundant to the lixiviate of soil ammonium, very close with conventional leaching results.
(3) assay method of the present invention configure classes of agents stable performance, storage life limit for length, at least one year.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with specific embodiment, the present invention is described in more detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.Raw material involved in following examples, be commercially available if no special instructions, involved detection method if no special instructions, is then conventional method.
embodiment 1
Design a kind of soil ammonium rapid assay methods, comprise the following steps:
(1) lixiviate: take the air-dry soil sample that 2.00g crosses 20 mesh sieves, be placed in 250mL triangular flask, add 0.5g non-phosphorus active carbon, then the NaHCO of concentration 0.6mol/L adding 40mL
3aqueous solution, then temperature be 20 ~ 25 DEG C, rotating speed be the condition of 180r/min under concussion 3 ~ 5min after, filter, gained filtrate is the liquid to be measured of soil ammonium.
The preparation method of described non-phosphorus active carbon is: first by the hydrochloric acid soaked overnight of activated charcoal 2mol/L, then with after distilled water washing repeatedly, uses 0.5mol/LNaHCO
3aqueous solution soaking is spent the night, and after suction filtration, then washs repeatedly with distilled water, without phosphorus to cleansing solution, to obtain final product.
(2) chrominance response: get blank liquid, ammonium nitrogen standard solution and liquid to be measured respectively, draw 2mL distilled water and do blank liquid in a container, draw the ammonium nitrogen standard solution of 2mL in another container, draw 2mL gained liquid to be measured again in the 3rd container, in three containers, add 0.2mL soil ammonium screening agent respectively, after shaking up, add 0.2mL soil ammonium respectively again to help and cover agent and 0.2mL ammonium nitrogen developer, shake up again, leave standstill 10 minutes, in order to measuring.
The collocation method of described ammonium nitrogen standard solution: take 0.0113g(NH
4)
2sO
4(at 110 DEG C, drying 2h) is dissolved in 600mL water, adds the 10mL concentrated sulphuric acid, adds water and be settled to 1L, is ammonium nitrogen standard solution (ρ (NH
4-N)=2.40mg/L).The collocation method of described soil ammonium screening agent: take the distilled water that 500g sodium potassium tartrate tetrahydrate is dissolved in 800mL, takes 400g NaOH in addition and is dissolved in 800mL distilled water, then mixed by two solution, add water and be settled to 2L.Described soil ammonium helps the collocation method covering agent: take 50g Arabic gum and 30g sodium fluoride is dissolved in boiling water, and naturally cool, hold over night, gets supernatant, adds water and is settled to 1L.The collocation method of described soil ammonium developer: take 50g potassium iodide and 150g NaOH is dissolved in 600mL water, adds saturated mercuric chloride solution while stirring, till there is orange precipitation, adds water and be settled to 1L, hold over night, get supernatant.
(3) colorimetric estimation: three groups of liquid are transferred in 10mm cuvette respectively, OK-Q3 clay fertilizer tacheometer (production of Zhengzhou Ou Keqi instrument manufacturing company limited) is used to measure, adjust its light path wavelength to 420nm, with blank liquid adjustment zero point, adjust with reference to scale value 48mg/kg at measurement of concetration shelves with ammonium nitrogen standard solution, then liquid to be measured is placed in light path, the corresponding content reading ammonium nitrogen in pedotheque to be measured.
comparative example 1
A kind of soil ammonium rapid assay methods, except following content, substantially the same manner as Example 1: (1) lixiviate: NaHCO used
3the concentration of aqueous solution is 0.5mol/L.
comparative example 2
A kind of soil ammonium rapid assay methods, except following content, substantially the same manner as Example 1: (1) lixiviate: NaHCO used
3the concentration of aqueous solution is 0.7mol/L.
embodiment 2
A kind of soil ammonium rapid assay methods, except following content, substantially the same manner as Example 1: (2) chrominance response: described soil ammonium helps the collocation method covering agent: to take 55g Arabic gum and 30g sodium fluoride is dissolved in boiling water, naturally cool, hold over night, get supernatant, add water and be settled to 1L.
embodiment 3
A kind of soil ammonium rapid assay methods, except following content, substantially the same manner as Example 1: (2) chrominance response: the collocation method of described soil ammonium developer: to take 45g potassium iodide and 150g NaOH is dissolved in 600mL water, add saturated mercuric chloride solution while stirring, till there is orange precipitation, add water and be settled to 1L, hold over night, get supernatant.
Comparative test result is in table 1,2:
In table, soil ammonium conventional value adopts indophenol blue colorimetry to record; Speed measured value (rower) adopts NY/T1848-2010 lixiviate and measures; Speed measured value (embodiment 1), fast measured value (comparative example 1), fast measured value (comparative example 2), fast measured value (embodiment 2), fast measured value (embodiment 3) adopt above embodiment lixiviate respectively and measure.Each test method surveys 10 groups of samples.
Soil ammonium measurement result shows, the error range about 20% of rower and conventional value, and least error is 9%; Error between embodiment 1 and conventional value is about 7%, and least error is 2%; Error between comparative example 1 and conventional value is about 30%, and wherein minimum error values is 8%; Error between comparative example 2 and conventional value is about 25%, and minimum error values is 13%; Error between embodiment 2 and conventional value is about 15%, and wherein minimum error values is 7%; Error between embodiment 3 and conventional value is about 15%, and minimum error values is 2%
In sum, the difference between the result of embodiment 1 and conventional value is minimum, and closest to conventional determining result, embodiment 2,3 is taken second place.
Table 1 soil ammonium comparative test result one
。
Table 2 soil ammonium comparative test result two
。
Claims (9)
1. a soil ammonium rapid assay methods, is characterized in that, comprises the following steps:
(1) lixiviate: take a certain amount of air-dry soil sample, or with its etc. the fresh soil sample of dry weight, be placed in container, non-phosphorus active carbon is added by 20 ~ 30wt% of described soil sample dry weight, universal soll digestion agent is added again by the solid-to-liquid ratio of 1g:18 ~ 25mL, temperature be 20 ~ 25 DEG C, rotating speed be the condition of 150 ~ 200r/min under concussion 3 ~ 5min after, filter, gained filtrate is the liquid to be measured of soil ammonium; Described universal soll digestion agent is the NaHCO of concentration 0.6mol/L
3aqueous solution;
(2) chrominance response: get blank liquid, ammonium nitrogen standard solution and liquid to be measured respectively, and add soil ammonium screening agent respectively, soil ammonium helps and covers agent and ammonium nitrogen developer, leave standstill, in order to measuring;
(3) colorimetric estimation: the light path wavelength of adjustment photometer or photolometer is to 420nm, with universal soll lixiviant solution or distilled water for blank liquid, the absorbance of ammonium nitrogen standard solution and liquid to be measured is measured respectively at absorbance measuring shelves, or adjust with reference to scale value at measurement of concetration shelves with ammonium nitrogen standard solution, then liquid to be measured is placed in light path, the corresponding content calculating or read ammonium nitrogen in pedotheque to be measured.
2. soil ammonium rapid assay methods according to claim 1, is characterized in that, described lixiviate step is specially:
Take the air-dry soil sample that 2.00g crosses 20 mesh sieves, be placed in 250mL triangular flask, add 0.5g non-phosphorus active carbon, then add the NaHCO of concentration 0.6mol/L of 40mL
3aqueous solution, then temperature be 20 ~ 25 DEG C, rotating speed be the condition of 180r/min under concussion 3 ~ 5min after, filter, gained filtrate is the liquid to be measured of soil ammonium.
3. soil ammonium rapid assay methods according to claim 1, is characterized in that, described chrominance response step is specially:
Draw a certain amount of distilled water and do blank liquid in a container, draw with the isopyknic ammonium nitrogen standard solution of blank liquid in another container, draw isopyknic gained liquid to be measured again in the 3rd container, equivalent soil ammonium screening agent is added respectively in three containers, after shaking up, the soil ammonium adding equivalent respectively again helps the ammonium nitrogen developer covering agent and equivalent, then shakes up, leave standstill 10 minutes, in order to measuring.
4. soil ammonium rapid assay methods according to claim 1, is characterized in that, the collocation method of described ammonium nitrogen standard solution: take 0.0113g(NH
4)
2sO
4be dissolved in 600mL water, add the 10mL concentrated sulphuric acid, add water and be settled to 1L, be ammonium nitrogen standard solution.
5. soil ammonium rapid assay methods according to claim 1, it is characterized in that, the collocation method of described soil ammonium screening agent: take the distilled water that 250 ~ 500g sodium potassium tartrate tetrahydrate is dissolved in 800mL, taking 200 ~ 400g NaOH is in addition dissolved in 800mL distilled water, then two solution are mixed, add water and be settled to 2L.
6. soil ammonium rapid assay methods according to claim 5, is characterized in that: described soil ammonium screening agent, soil ammonium help covers agent and ammonium nitrogen developer consumption is 8 ~ 15% of described blank liquid accumulated amount.
7. soil ammonium rapid assay methods according to claim 1, is characterized in that, described soil ammonium helps the collocation method covering agent: take 35 ~ 60g Arabic gum and 25 ~ 45g sodium fluoride is dissolved in boiling water, naturally cool, hold over night, gets supernatant, adds water and is settled to 1L.
8. soil ammonium rapid assay methods according to claim 1, it is characterized in that, the collocation method of described soil ammonium developer: take 40 ~ 65g potassium iodide and 150g NaOH is dissolved in 600mL water, add saturated mercuric chloride solution while stirring, till there is orange precipitation, add water and be settled to 1L, hold over night, get supernatant.
9. soil ammonium rapid assay methods according to claim 4, is characterized in that, described colorimetric estimation step is specially:
Blank liquid, ammonium nitrogen standard solution and liquid to be measured after carrying out chromogenic reaction are transferred in corresponding cuvette respectively, the light path wavelength of adjustment photometer or photolometer is to 420nm, with blank liquid adjustment zero point, adjust with reference to scale value 48mg/kg at measurement of concetration shelves with ammonium nitrogen standard solution, then liquid to be measured is placed in light path, the corresponding content calculating or read ammonium nitrogen in pedotheque to be measured.
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Cited By (4)
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| CN109001196A (en) * | 2018-10-10 | 2018-12-14 | 闫宏涛 | A kind of solid powder detection agent measuring ammonium nitrogen content |
| 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 |
| CN114354594A (en) * | 2019-08-23 | 2022-04-15 | 中国科学院沈阳应用生态研究所 | Method for measuring ammonium nitrogen, nitrate nitrogen, nitrite nitrogen and total dissolved nitrogen in sample |
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