CN104198419B - Soil nitrate-N digestion agent and soil nitrate-N rapid assay methods - Google Patents
Soil nitrate-N digestion agent and soil nitrate-N rapid assay methods Download PDFInfo
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Abstract
The present invention relates to the rapid assay methods of a kind of soil nitrate-N digestion agent and Content of Nitrate-Nitrogen in Soil.The KCl aqueous solution of the soil nitrate-N digestion agent of the present invention for 0.5～0.8mol/L of concentration；Assay method of the present invention with which as digestion agent, with 5 ~ 10mL：The soil ratio extraction of 1g, reenacts calibration curve, colorimetric, calculating；, using the KCl aqueous solution of low concentration as soil nitrate-N digestion agent, extracting effect is good for the present invention, and testing result accurately, and greatlys save detection medicine, saved testing cost and reduced the harmful effect to environment.
Description
Technical field
The present invention relates to agrochemical analysis technical field, and in particular to a kind of soil nitrate-N digestion agent and nitrified nitrogen in soil
The rapid assay methods of content.
Background technology
In existing agricultural production, the decisive factor of soil nutrient balance is the Input Level of fertilizer.Generally, increase
Nitrogenous fertilizer puts into, and is conducive to Crop to assimilate more nitrogens, increases yield, be also beneficial to the improvement of cereal crops quality.But
It is, the absorption and assimilation amount change not synchronous with amount of nitrogen of crop nitrogen.The generally increase of amount of nitrogen, the Apparent Availability of nitrogen
Decline, pedo relict increases, and accumulation, in soil, and then environmentally safe threatens in the form of nitrate nitrogen.In soil
Nitrate nitrogen be always a study hotspot of agrology and environmental science.At present, soil nitrate-N is that plant directly can absorb
The quick-acting nitrogen for utilizing, its content height are not only one of important indicator of measurement soil fertility, and evaluation of subterranean water ring
The potential pollution index in border.It is therefore to be understood that the fertility state of soil and whether causing groundwater resources environmental pollution, soil
It is one of big event of agrochemical analysis that nitrate nitrogen content is determined.
Relevant nitrified nitrogen in soil method for measuring has various, and its conventional assay method mainly has disulfonic acid phenol, purple
Outer AAS, Flow Analyzer method etc..Disulfonic acid phenol past attempts are widely used（Bremner, 1965）, but this method
Analysis time is long, there is organic matter and Cl again-Interference, it is impossible to carry out batch sample analysis in a short time, use less.Continuously
Although Flow Analysis Technique can complete sample test at short notice accurately, quickly, in large quantity, there is instrument price high
High, sampling valve easily breaks down, and needs specialty analysis human users, the shortcomings of maintenance cost is high, is not suitable for general scientific research
Unit and personnel, cause to be commonly used not yet so far.Wherein, ultraviolet spectrophotometry device therefor it is conventional, easy to operate, change
Reagent contamination is little, obtain data in time, is the advanced method for extensively receiving promotion at present.But ultraviolet spectrophotometry for a long time
All be from higher concentration Klorvess Liquid as soil extractant extracting the nitrate nitrogen in soil, and think 2mol/L chlorine
Actual conditions of the nitrate that change potassium solution is extracted out closest to land for growing field crops, but be measured using the leach extraction method large quantities of
The sample of amount, not only needs to expend the potassium chloride reagent of the expensive pure level of analysis of substantial amounts of price, and used potassium chloride
Solution also can threaten to environment into soil or water bodies of rivers and lakes, this become restriction the method popularize it is main because
One of element；And the potassium chloride salt solution of high concentration easily causes corrosion when in use to detecting instrument equipment.
For a long time, agrochemical worker thirsts for improving the method that ultraviolet spectrophotometry surveys nitrate nitrogen, expects ensureing inspection
On the basis of surveying precision and accuracy, its testing cost is greatly reduced, but does not obtain substantially progress.
The content of the invention
To solve the above problems, the invention provides a kind of soil nitrate-N digestion agent and content of soil nitrate-N is quick
Assay method, the digestion agent and assay method extracting effect it is good, testing result accurately, and greatlys save detection medicine, section
About testing cost, reduce the harmful effect to environment.
The present invention is achieved through the following technical solutions：
Design a kind of soil nitrate-N digestion agent, the KCl aqueous solution of the digestion agent for 0.5～0.8mol/L of concentration.
Preferably, the KCl aqueous solution of the digestion agent for concentration 0.5mol/L.
A kind of soil nitrate-N rapid assay methods are designed, is comprised the following steps：
（1）Extract：Fresh soil sample to be detected is taken, with 5～10mL：The soil ratio of 1g adds above-mentioned soil nitrate-N extraction
After agent, vibration 1 ~ 1.5 hour, then stand 3 ~ 5min and filter to obtain soil extract liquid；
（2）Formulate calibration curve：Take nitrate nitrogen standard liquid be configured to respectively nitrate for 0.5,1,2,3,4,
The gradient solution of 5mg/L；And with above-mentioned soil nitrate-N digestion agent as blank, double wave is used under 220nm and 275nm wavelength
Regular way determines the absorbance difference of each strength solution, makes respectively with standard work that concentration, absorbance difference are longitudinal and transverse coordinate
Make curve, or corresponding linear equation is fitted according to corresponding concentration, absorbance difference data；
（3）Colorimetric：With above-mentioned soil nitrate-N digestion agent as control, by step（1）Gained extract in 220nm and
With its absorbance difference of double-wavelength method colorimetric estimation under 275nm wavelength, obtain further according to the standard working curve or linear equation
To extract nitrate C；
（4）Calculate：Content of soil nitrate-N=C × B/A to be measured, A are the drying soil sample weight being converted to, and B is step（1）
In water and soil ratio.
Preferably, the fresh soil sample particle diameter is not more than 2mm.
Preferably, step（1）Gained extract should be measured in time, as determined in time, should be stored in-
In 20 DEG C of refrigerators.
Preferably, the nitrate nitrogen standard liquid is dissolved in what distilled water was formulated by pure or top pure grade level potassium nitrate is analyzed
Certain density potassium nitrate solution.
The positive beneficial effect of the present invention：
Instant invention overcomes intrinsic technology prejudice, using the KCl aqueous solution of low concentration as soil nitrate-N digestion agent,
Field soil environment can effectively be simulated（Including substitutional ion situation, distribution of charges situation, pH value situation etc.）, to greatest extent
Displacement and extract the nitrate nitrogen nutrient in soil, it is applied widely（Suitable for acid soil in the south and north neutrality, lime
The extraction of available nitrogen in property soil）, achieve unexpected technique effect：Extracting effect is good, range of linearity width, accuracy of detection
High, result is accurate, and the KCl solution of low concentration can be prevented effectively from or reduce interfering ion leaching, be conducive to follow-up colorimetric
Determine；Additionally, using the soil extractant of low concentration, greatly save detection medicine, saved testing cost and reduce it is right
The harmful effect of environment.
Specific embodiment
The present invention is expanded on further below in conjunction with specific embodiment.Test method in following embodiments, such as nothing are especially said
It is bright, it is conventional method；In following embodiments, test material used and reagent, if no special instructions, are commercial.
Embodiment 1
The rapid assay methods of the present embodiment content of soil nitrate-N, comprise the following steps：
（1）Extract：The fresh soil sample that 2mm hole sizers, weight are 10g was taken, addition volume is 50 mL, concentration is 0.5mol/
In the KCl aqueous solution of L, after vibrating 1 ~ 1.5 hour, then the filtration of 3 ~ 5min quantitative filter papers is stood, obtain soil extract liquid；
（2）Formulate calibration curve：The nitrate nitrogen standard liquid 0.5,1,2,3,4,5ml for pipetting 50mg/L respectively holds in 50ml
In measuring bottle, then be settled to 50ml with the KCl solution of 0.5mol/L, respectively obtain nitrate for 0.5,1,2,3,4,5mg/L
Gradient solution；With the KCl solution of 0.5mol/L as control, double-wavelength method colorimetric estimation is used under 220nm and 275nm wavelength,
Make corresponding standard working curve；
（3）Colorimetric：With the KCl solution of 0.5mol/L as control, extract is used into double wave under 220nm and 275nm wavelength
Regular way colorimetric estimation, is obtained extract nitrate C according to standard working curve；
（4）Calculate：Soil sample nitrate nitrogen content=C × B/A to be measured, A are soil sample weight（Convert to dry soil weight, according to soil sample
Moisture content is converted）, B is step（1）Digestion agent volume number used.
Embodiment 2
In addition to being related to KCl solution and being 0.6mol/L, other steps and parameter are same as Example 1.
Embodiment 3
In addition to being related to KCl solution and being 0.8mol/L, other steps and parameter are same as Example 1.
Comparative example 1
In addition to being related to KCl solution and being 2mol/L, other steps and parameter are same as Example 1.
Comparative example 2
In addition to being related to KCl solution and being 0.4mol/L, other steps and parameter are same as Example 1.
Comparative example 3
H is changed to except KCl solution is related to2Outside O, other steps and parameter are same as Example 1.
Content of soil nitrate-N determination test
（1）Using the inventive method respectively to Henan Province Shangshui County state farm, Fengqiu County Pan Dian townshiies, Zhengzhou City Mao Zhuan towns
Soil be measured test, per ground soil survey two at, under the variable concentrations KCl solution conditions of embodiment 1,3 and comparative example 1
The nitrate of measure is shown in Table 1.
Soil nitrate nitrogen concentration is measured under 1 different extraction agent concentrations of table（NO3 -- N, mg/kg）
Table 1 is illustrated：Extractant concentration under the conditions of 0.5,0.8mol/L compared with the conditions of 2mol/L, extraction effect and survey
The soil nitrate nitrogen concentration for obtaining is not significantly different from, and the inventive method saves detection medicine, saved testing cost, reduced
Harmful effect to environment.
（2）Depth determination test is carried out respectively to soil at Henan Province Fengqiu County two using the inventive method, in embodiment 1
Nitrate with different depth level loam is determined under comparative example variable concentrations KCl solution conditions, is shown in Table 2.
Soil nitrate nitrogen concentration is measured under 2 different digestion agents of table and depth level（NO3 -- N, mg/kg）
This result of the test and many experiments show：Extractant concentration under the conditions of 0.5mol/L with 2mol/L under the conditions of phase
Than, it is no matter at all levels in the 180cm depth boundses, extraction effect and measure soil nitrate nitrogen concentration and be not significantly different from；
It is but 0.5mol/L conditions are compared with 0.4mol/L Klorvess Liquids, no matter at all levels in the 180cm depth boundses, extract effect
Fruit and measure soil nitrate nitrogen concentration and be all significantly increased；And using pure water as soil nitrate-N digestion agent, then cannot filter and obtain
Settled solution is obtained, thus follow-up colorimetric estimation cannot be carried out.
（3）Test is measured respectively to typical acid soil at south China three using the inventive method, in embodiment
With the nitrate that different location acid ground is determined under comparative example variable concentrations KCl solution conditions, same place make 4 times it is heavy
It is multiple, it is shown in Table 3, table 4 and table 5.
3 variable concentrations KCl digestion agents of table measure mountain yellow soil nitrate（NO3 -- N, mg/kg）
Note：In row, after mean value, different lowercases represent difference and reachP=0.05 level of signifiance, similarly hereinafter.
4 variable concentrations KCl digestion agents of table measure red earth nitrate（NO3 -- N, mg/kg）
。
5 variable concentrations KCl digestion agents of table measure lithology yellow earth nitrate（NO3 -- N, mg/kg）
。
It is above-mentioned test result indicate that, to 3 kinds of acid grounds in the range of KCl concentration 0.4mol/L～2mol/L（Chong Qingshan
Ground yellow earth, Xiamen of Fujian Province red earth and Lishui of Zhejiang lithology yellow earth）Nitrate nitrogen content is determined can normal filtration acquisition clarification filter
Liquid, and preferable analysis result is obtained, and difference reaches the level of signifiance between the soil test result with distilled water as extractant.
Additionally, more experimental studies also find, although yellow in Xiamen red earth and Lishui of Zhejiang lithology as extractant with distilled water
Earth is obtained in that clear filtrate, but measurement result is substantially less than the measurement result of 0.4mol/L ~ 2mol/L KCl, shows with distillation
Soil nitrate-N can not be extracted level used by test by water, it is impossible to meet the needs of result of the test.
（4）Test is measured to Typical North calcareous meta-alkalescence soil using the inventive method, embodiment with it is right
The nitrate of basic soil is determined under ratio variable concentrations KCl solution conditions, same place is made 4 repetitions, is shown in Table 6.
6 variable concentrations KCl digestion agents of table measure alkaline moisture soil nitrate（NO3 -- N, mg/kg）
By can be seen that to Zhengzhou basic soil nitrate analysis result with variable concentrations KCl digestion agents（Table 6）,
Difference between the soil nitrate nitrogen concentration of soil test is extracted in 0.5mol/L ~ 2mol/L KCl concentration ranges not notable, but
Pure water and 0.4mol/LKCl extractions soil test result are higher compared with 0.5mol/L to 2mol/LKCl results, and difference reaches and shows
Work level, analysis reason think soil is extracted under≤0.4mol/L concentration and cannot get clarified solution and cause Colorimetric results higher.Enter
The analysis and research of one step show, can be only achieved in meta-alkalescence soil nitrate-N leaching liquor concentration >=0.50mol/L and preferably test
Analysis result.In view of the impact of cost and environment, KCl leaching liquors concentration should be selected between 0.5mol/L ~ 0.8mol/L more
Suitably.
In sum, the present invention institute using the Extractant concentration of 0.5mol/L both save detect medicine, saved detection
Cost（As having 5000 pedotheques to need to determine soil nitrate nitrogen concentration in each Wheat and maize rotation cycle according to,
The extract 50ml of each sample, if analyzing pure level according to every bottle of 500g of current Shanghai Chinese medicines group or Nanjing chemical reagent factory
20 yuan of calculating of potassium chloride, need 1500 yuan of 75 bottles of potassium chloride using 2mol/L KCl extracts, and adopt 0.5M KCl extracts
380 yuan of 19 bottles of potassium chloride are needed only, only testing chemical reagent cost directly reduces by 74.7%）, reduce the bad shadow to environment
Ring, Detection results and the degree of accuracy can be taken into account again.
Above-mentioned specific embodiment is the invention is not limited in, those skilled in the art can also make various changes accordingly,
But it is any all to cover within the scope of the claims with equivalent of the invention or similar change.
Claims (5)
1. a kind of soil nitrate-N rapid assay methods, it is characterised in that comprise the following steps：
（1）Extract：Fresh soil sample to be detected is taken, with 5～10mL：The soil ratio of 1g adds soil nitrate-N digestion agent, vibration 1
After ~ 1.5 hours, then stand 3 ~ 5min and filter to obtain soil extract liquid；The soil nitrate-N digestion agent be concentration 0.5～
The KCl aqueous solution of 0.8mol/L；
（2）Formulate calibration curve：Take nitrate nitrogen standard liquid be configured to respectively nitrate be 0.5,1,2,3,4,5mg/L
Gradient solution；And with described soil nitrate-N digestion agent as blank, double-wavelength method is used under 220nm and 275nm wavelength
The absorbance difference of each strength solution is determined, is made and is worked bent with the standard that concentration, absorbance difference are longitudinal and transverse coordinate respectively
Line, or corresponding linear equation is fitted according to corresponding concentration, absorbance difference data；
（3）Colorimetric：With described soil nitrate-N digestion agent as control, by step（1）Gained extract is in 220nm and 275nm
With its absorbance difference of double-wavelength method colorimetric estimation under wavelength, extracted further according to the standard working curve or linear equation
Liquid nitrate C；
（4）Calculate：Content of soil nitrate-N=C × B/A to be measured, A are the drying soil sample weight being converted to, and B is step（1）In
Water and soil ratio.
2. soil nitrate-N rapid assay methods according to claim 1, it is characterised in that：The digestion agent is concentration
The KCl aqueous solution of 0.5mol/L.
3. soil nitrate-N rapid assay methods according to claim 1, it is characterised in that：The fresh soil sample particle diameter is not
More than 2mm.
4. soil nitrate-N rapid assay methods according to claim 1, it is characterised in that：Step（1）Gained extract
It is stored in -20 DEG C of refrigerators.
5. soil nitrate-N rapid assay methods according to claim 1, it is characterised in that：The nitrate nitrogen standard liquid
The certain density potassium nitrate solution that distilled water is formulated is dissolved in by pure or top pure grade level potassium nitrate is analyzed.
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| CN106885780A (en) * | 2015-12-16 | 2017-06-23 | 中国科学院沈阳应用生态研究所 | A kind of method for determining soil nitrate-N |
| CN107192754B (en) * | 2016-03-15 | 2019-11-08 | 中国农业大学 | Farmland nitrate nitrogen detection method and system based on ion selective electrode |
| CN106198425A (en) * | 2016-06-24 | 2016-12-07 | 中国林业科学研究院热带林业实验中心 | A kind of soil nitrate-N detection method |
| CN107607484A (en) * | 2017-10-25 | 2018-01-19 | 天津市环境保护科学研究院 | The method of thimet content in quick measure soil |
| CN107884384B (en) * | 2017-11-13 | 2020-07-24 | 山东深海海洋科技有限公司 | Nitrate nitrogen Raman detection analysis method based on nitrate enhanced nano silver |
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| CN102435560A (en) * | 2011-09-06 | 2012-05-02 | 深圳市喜耕田生物科技股份有限公司 | Method for testing nitrification inhibition rate of stabilized fertilizer |
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| CN102435560A (en) * | 2011-09-06 | 2012-05-02 | 深圳市喜耕田生物科技股份有限公司 | Method for testing nitrification inhibition rate of stabilized fertilizer |
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| 氯化钾浸提法测定土壤中铵态氮含量条件研究;于向华等;《农业科技与装备》;20130331;第11页至第12页 * |
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