CN109900694A - A kind of measuring method of vega soil alkaline hydrolysis nitrogen content - Google Patents
A kind of measuring method of vega soil alkaline hydrolysis nitrogen content Download PDFInfo
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- CN109900694A CN109900694A CN201910048823.4A CN201910048823A CN109900694A CN 109900694 A CN109900694 A CN 109900694A CN 201910048823 A CN201910048823 A CN 201910048823A CN 109900694 A CN109900694 A CN 109900694A
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Abstract
The invention belongs to vega soil nutrient detection field more particularly to a kind of measuring methods of vega soil alkaline hydrolysis nitrogen content.The present invention is greater than the characteristic of 150mg/kg for alkaline hydrolysis nitrogen content in vega soil, carries out research and development improvement on the basis of existing soil alkali-hydrolyzable nitrogen determination techniques, The present invention reduces H in the prior art first3BO3- indicator solution is adjusted in micro- aubergine, detection error caused by reducing because of artificial visual color.Secondly, the present invention in the determination step of high-content alkali-hydrolyzable nitrogen, has properly increased standardized titration acid H also in vega soil2SO4Concentration, reduce the volume of titrating solution, reduce workload, improve working efficiency.
Description
Technical field
The invention belongs to vega soil nutrient detection field more particularly to a kind of measurement sides of vega soil alkaline hydrolysis nitrogen content
Method.
Background technique
Vega soil nutrient is indispensable important ecological factors during leaf tobacco production, can be generated to quality of tobacco
A degree of influence.There are the processes such as the nitrogen cycle of tobacco leaf carbon and Physiology and biochemistry certain in studies have shown that difference tobacco-growing soil
Influence.Therefore selecting suitable soil is the important link of High Quality Tobacco production.The content of nitrogen is as soil fertility in soil
One of important behaviour, rationally the nitrogen in the assessment vega soil of science is most important to the production of tobacco leaf.
In view of the limitation of farming operation area, tobacco field continuous cropping becomes the universal phenomenon of tobacco leaf planting.Since tobacco is to nitrogenous fertilizer
Demand it is higher, tobacco grower be reach higher income, it is also higher to the amount of application of tobacco field chemical fertilizer, lead to cigarette over time
Nitrogen content in the soil of field is much higher than the nitrogen content in other crops soil.The nitrogen content of soil is excessively high, and it is greedy to will cause tobacco leaf
It is green late-maturing, and there is the quick-fried stalk cigarette of blue veins when baking modulation, lead to the reduction of quality of tobacco and purchasing price.So to tobacco field
The detection research of nitrogen content in soil is very necessary.
The method for detecting soil alkali-hydrolyzable nitrogen in the prior art is mainly the improvement carried out on the basis of Kelvin method, such as open
Number for CN104111256A the detection methods such as Patent Application Publication, these detection methods, to detecting general or slightly lower fertile soil
The result of available nitrogen (≤100mg/kg) in earth is reliable.But the alkali for the vega soil of higher fertility, in soil
It solves nitrogen content and is greater than 150mg/kg, the detection method of the prior art shows slightly cumbersome and complicated, reduces working efficiency, while to reduction
Error is without too big effect.It is mainly manifested in the detection method Plays acid H of the prior art3BO3The tune of-indicator mixed liquor is micro-
There are the serious artificial collimation errors for aubergine step, not only complex steps, but also the process mixed colours, the accuracy meeting to test
It affects.Therefore detection method in the prior art is insufficient for the measurement work compared with rich soil alkali-hydrolyzable nitrogen
Make.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of measuring method of vega soil alkaline hydrolysis nitrogen content.The present invention
For the characteristic of alkaline hydrolysis nitrogen content (150mg/kg) higher in vega soil, soil alkali-hydrolyzable nitrogen determination techniques in the prior art
On the basis of carry out research and development improvement, guarantee measurement result in allowable range of error on the basis of, simplify operating procedure, reduce
Human factor error caused by testing result.
The technical solution adopted by the invention is as follows:
A kind of measuring method of vega soil alkaline hydrolysis nitrogen content, steps are as follows:
1) prepared by pedotheque: soil to be measured and after natural drying is taken, grind and 40 meshes of mistake, obtained soil-like
Product；
2) the alkaline hydrolysis processing of pedotheque:
Pedotheque 2.0g is taken to be placed in diffusion boat mistress, rotation diffusion boat spreads out pedotheque uniformly, takes FeSO4
7H2O powder 0.2g is simultaneously uniformly layered on pedotheque, then takes saturation Ag2SO4Solution 0.1mL is placed on pedotheque, is finally taken
H3BO3- indicator solution 2mL is placed in diffusion boat interior room；
Alkaline glue is applied at diffusion boat mistress edge, frosted glass lid is covered and rotates for several times to diffusion boat edge and frosted glass
Lid bonding completely；Then turn on frosted glass lid make on one side diffusion boat mistress expose gap and inwardly addition 1.0mol/LNaOH it is molten
Frosted glass lid is covered tightly after liquid 10mL, rotation diffusion boat makes NaOH solution cover pedotheque；Frosted glass lid is fixed with rubber band
After lay flat in 40 DEG C of isoperibols and alkaline hydrolysis spreads 23.5-24.5h, take out diffusion boat, diffusion boat interior room becomes blue；
3) measurement of pedotheque:
Using the H of 0.01mol/L2SO4Titer titrates diffusion boat interior room blue solution, until interior room blue solution becomes
Yellowish red color, record consumption H2SO4The volume V of titer；
4) prepared by blank control sample:
Except not placing pedotheque, FeSO47H2O powder and saturation Ag2SO4Solution step, other operate same step
2) and step 3), record consume H2SO4The volume V of titer0；
5) alkaline hydrolysis nitrogen content in pedotheque is calculated:
According to formula:In calculation formula: alkali in W-pedotheque
Solve nitrogen content, unit mg/kg；
C—H2SO4The concentration of standard solution, unit 0.01mol/L；
V-pedotheque measurement consumption 0.01mol/LH2SO4The volume of titer, unit mL；
V0- blank control sample measurement consumption 0.01mol/LH2SO4The volume of titer, unit mL；
2—0.01mol/LH2SO4Hydrogen ion conversion coefficient in titer；
The molal weight of 14-nitrogen-atoms, unit g/mol；
M-pedotheque quality, unit g；
10^3-Units conversion factor.
Specifically, NaOH solution concentration is 1.0mol/L in step 2)；H3BO3- indicator solution concentration is 20g/L.
Specifically, the H3BO3The configuration method of-indicator solution is as follows: taking 10g H3BO3It is dissolved in 500mL water, adds
Enter 2.5mL methyl red-bromocresol green mixed indicator up to green-yellow, that is, is made into the H that pH theoretical value is 4.373BO3- instruction
Agent solution.
Preferably, the methyl red-bromocresol green mixed indicator configuration method is as follows: take 0.5g bromocresol green and
0.1g methyl red is dissolved in 100mL ethyl alcohol, ultrasonic vibration to abundant dissolution.
Specifically, the configuration method of the alkaline glue is as follows in step 2): Arabic gum 40g and water 50mL being taken to exist
It is cooling after stirring and dissolving 1h hot warm to 70-80 DEG C in beaker, add glycerol 20mL and saturation K2CO3Aqueous solution 20mL, stirring
Natural cooling afterwards to obtain the final product.
The present invention compares compared with prior art, has the advantages that
1) measuring method of the present invention increases the concentration of standard acid, and the less consumption of titrating solution volume improves
The working efficiency of detection, while in titration process since titrating solution concentration is larger, mixed liquor color change is obvious after titration,
Artificial titration end-point deviation is smaller, and preferably, the accuracy of testing result is higher for repeatability；
2) present invention omits H in the detection method of the prior art3BO3- indicator solution is adjusted to adjust in micro- aubergine
The step of pH value is to 4.8, reduce workload, improve work efficiency, while considerably reducing artificial visual color and causing
Detection error, improve the accuracy of testing result.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right below in conjunction with subordinate list and embodiment
The present invention is further elaborated.It should be appreciated that specific example described herein is only used to explain the present invention, not
For limiting the present invention.
A kind of measuring method of vega soil alkaline hydrolysis nitrogen content, steps are as follows:
1) prepared by pedotheque: soil to be measured and after natural drying is taken, grind and 40 meshes of mistake, obtained soil-like
Product；
2) the alkaline hydrolysis processing of pedotheque:
Pedotheque 2.0g is taken to be placed in diffusion boat mistress, rotation diffusion boat spreads out pedotheque uniformly, takes FeSO4
7H2O powder 0.2g is simultaneously uniformly layered on pedotheque, then takes saturation Ag2SO4Solution 0.1mL is placed on pedotheque, is finally taken
H3BO3- indicator solution 2mL is placed in diffusion boat interior room；
Alkaline glue is applied at diffusion boat mistress edge, frosted glass lid is covered and rotates for several times to diffusion boat edge and frosted glass
Lid bonding completely；Then turn on frosted glass lid make on one side diffusion boat mistress expose gap and inwardly addition NaOH solution 10mL after
Frosted glass lid is covered tightly, rotation diffusion boat makes NaOH solution cover pedotheque；It lays flat after fixed frosted glass lid to 40 DEG C of constant temperature
In environment and alkaline hydrolysis spreads 23.5-24.5h, takes out diffusion boat, and diffusion boat interior room becomes blue；It repeats aforesaid operations and obtains three
Part parallel sample；
3) measurement of pedotheque:
Using the H of 0.01mol/L2SO4Titer titrates diffusion boat interior room blue solution, until interior room blue solution becomes
Yellowish red color, record consumption H2SO4The volume V of titer；
4) prepared by blank control sample:
Except not placing pedotheque, FeSO47H2O powder and saturation Ag2SO4Solution step, other operate same step
2) and step 3), record consume H2SO4The volume V of titer0；
5) alkaline hydrolysis nitrogen content in pedotheque is calculated:
According to formula:In calculation formula: alkali in W-pedotheque
Solve nitrogen content, unit mg/kg；
C—H2SO4The concentration of standard solution, unit 0.01mol/L；
V-pedotheque measurement consumption 0.01mol/LH2SO4The volume of titer, unit mL；
V0- blank control sample measurement consumption 0.01mol/LH2SO4The volume of titer, unit mL；
2—0.01mol/LH2SO4Hydrogen ion conversion coefficient in titer.
The molal weight of 14-nitrogen-atoms, unit g/mol；
M-pedotheque quality, unit g；
10^3-Units conversion factor.
Wherein, the preparation method of reagent is as follows:
1) 1.0mol/L NaOH solution accurately weighs NaOH (chemistry is pure) 20.0g and is dissolved in pure water, is transferred to after cooling
500mL volumetric flask, is settled to graduation mark.
2)20g/L H3BO3- indicator solution, 10g H3BO3(chemistry is pure) is dissolved in 500mL water, and 2.5mL first is added
Base is red-bromocresol green mixed indicator (preparation of methyl red-bromocresol green mixed indicator: weigh 0.5g bromocresol green and
0.1g methyl red is dissolved in 100mL ethyl alcohol, and dissolution is sufficiently stirred in assisting ultrasonic concussion), the solution is in green-yellow, pH reason this moment
It is 4.37 by value.This solution is easily ready-to-use, should not put long.
3)0.01mol/L H2SO4Titer measures H2SO4(chemistry is pure) 267.9uL, adds pure water to be diluted to 500mL,
Then it is demarcated with standard base (SB) or boric acid, this is 0.01mol/LH2SO4Standard solution.
4) alkaline glue weighs Arabic gum 40g and water 50mL the heat temperature in beaker and stirs dissolution, about to 70~80 DEG C
It is let cool after 1h.Glycerol 20mL and saturation K is added2CO3
Aqueous solution 20mL, stirring cool.Clear liquid is stored in spare in plug vial.
5)FeSO4·7H2O powder, by FeSO47H2O (chemistry is pure) is levigate, is fitted into airtight bottle, is stored in shady place.
6)Ag2SO4Saturated solution weighs 0.530g Ag2SO4Solid is dissolved in 100mL pure water, and ultrasonic wave auxiliary is molten
Solution.
NaOH solution concentration is 1.0mol/L；H3BO3- indicator solution concentration is 20g/L.It is measured by the above method,
The alkaline hydrolysis nitrogen analysis of three parts of parallel tests the results are shown in Table 1
Table 1
Pedotheque is measured using the detection method of the prior art, measurement result is shown in Table 2.
Table 2
Note: the detection method of the prior art and the application the difference is that:
1) to H3BO3- indicator solution needs that pH is adjusted: being adjusted to micro- aubergine with diluted acid or diluted alkaline；
2) concentration of titrated sulfuric acid titer is 0.005mol/L；The same embodiment of the present invention of other steps.
Contrast table 1, table 2 are it is found that for same pedotheque, the relative error of the testing result of the present invention and the prior art
It is 7.0%, the result is in the range of detection error allows (according to " soil analysis technical specification " alkaline hydrolysis nitrogen determination precision
It is required that parallel determinations allowable error rate≤10%), show the feasibility of the invention detection method.Meanwhile it is of the present invention
Relative standard deviation (2.8%) between the group of detection method, relative standard deviation (5.24%) compared with the existing technology is lower, and
Relatively low, the table compared with relative standard deviation (4.52%) between the group in the Patent Application Publication of Publication No. CN104111256A
Preferably, precision is higher for bright inventive method repeatability.Meanwhile the volume of present invention titrimetric standard acid in measurement is few, substantially
Degree improves determination efficiency, these suffice to show that the superiority and exploitativeness of detection method of the present invention.
Claims (6)
1. a kind of measuring method of vega soil alkaline hydrolysis nitrogen content, which is characterized in that steps are as follows:
1) prepared by pedotheque: taking soil to be measured, after natural drying, is ground and crossed 40 meshes, pedotheque is made；
2) the alkaline hydrolysis processing of pedotheque:
Pedotheque 2.0g is taken to be placed in diffusion boat mistress, rotation diffusion boat spreads out pedotheque uniformly, takes FeSO4·7H2O
Powder 0.2g is simultaneously uniformly layered on pedotheque, then takes saturation Ag2SO4Solution 0.1mL is placed on pedotheque, is finally taken
H3BO3- indicator solution 2mL is placed in diffusion boat interior room；
Alkaline glue is applied at diffusion boat mistress edge, frosted glass lid is covered and rotates complete to diffusion boat edge and frosted glass lid for several times
Full bond；Then turn on frosted glass lid make on one side diffusion boat mistress expose gap and to mistress be added 1.0mol/L NaOH it is molten
Frosted glass lid is covered tightly after liquid 10mL, rotation diffusion boat makes NaOH solution cover pedotheque；Laid flat after fixed frosted glass lid to
In 40 DEG C of isoperibols and alkaline hydrolysis spreads 23.5-24.5h, takes out diffusion boat and diffusion boat interior room is blue；
3) measurement of pedotheque:
Using the H of 0.01mol/L2SO4Titer titrates diffusion boat interior room blue solution, until interior room blue solution becomes Huang Hong
Color, record consumption H2SO4The volume V of titer；
4) prepared by blank control sample:
Diffusion boat mistress does not place pedotheque, FeSO4·7H2O powder and saturation Ag2SO4Solution step, other operations synchronize
It is rapid 2) and step 3), record consumption H2SO4The volume V of titer0；
5) alkaline hydrolysis nitrogen content in pedotheque is calculated:
According to formula:It calculates；
In formula: alkaline hydrolysis nitrogen content in W-pedotheque, unit mg/kg；
C—H2SO4The concentration of standard solution, unit 0.01mol/L；
V-pedotheque measurement consumption 0.01mol/LH2SO4The volume of titer, unit mL；
V0- blank control sample measurement consumption 0.01mol/LH2SO4The volume of titer, unit mL；
2—0.01mol/LH2SO4Hydrogen ion conversion coefficient in titer；
The molal weight of 14-nitrogen-atoms, unit g/mol；
M-pedotheque quality, unit g；
10^3-Units conversion factor.
2. the measuring method of vega soil alkaline hydrolysis nitrogen content as described in claim 1, which is characterized in that in step 2),
H3BO3- indicator solution concentration is 20.0g/L.
3. the measuring method of vega soil alkaline hydrolysis nitrogen content as claimed in claim 2, which is characterized in that the H3BO3- instruction
The configuration method of agent solution is as follows: taking 10.0g H3BO3It is dissolved in 500mL water, 2.5mL methyl red-bromocresol green mixing is added
Indicator is up to green-yellow, the H that pH is 4.373BO3- indicator solution.
4. the measuring method of vega soil alkaline hydrolysis nitrogen content as claimed in claim 3, which is characterized in that the methyl red-bromine
The configuration method of the green mixed indicator of cresols is as follows: taking 0.5g bromocresol green and 0.1g methyl red to be dissolved in 100mL ethyl alcohol, ultrasound
Concussion is dissolved to abundant.
5. the measuring method of vega soil alkaline hydrolysis nitrogen content as described in claim 1, which is characterized in that described in step 2)
Alkaline glue configuration method it is as follows: taking Arabic gum 40g and water 50mL, heat temperature is to 70-80 DEG C in beaker, stirring and dissolving
It is cooling after 1h, add glycerol 20mL and saturation K2CO3Aqueous solution 20mL, natural cooling after stirring to obtain the final product.
6. the measuring method of vega soil alkaline hydrolysis nitrogen content as described in claim 1, which is characterized in that in the pedotheque
Alkaline hydrolysis nitrogen content is greater than 150mg/kg.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102297861A (en) * | 2011-07-19 | 2011-12-28 | 中国科学院东北地理与农业生态研究所 | Determination method of soil alkaline hydrolyzable nitrogen |
| CN203231964U (en) * | 2012-12-21 | 2013-10-09 | 中国科学院东北地理与农业生态研究所 | Diffusion vessel for soil alkaline hydrolysis nitrogen |
| CN104111256A (en) * | 2014-07-04 | 2014-10-22 | 中国科学院东北地理与农业生态研究所 | Method for detecting content of soil alkali-hydrolyzable nitrogen |
| CN104991036A (en) * | 2015-08-03 | 2015-10-21 | 河南广电计量检测有限公司 | Determination method for soil alkali-hydrolyzable nitrogen |
| CN105806837A (en) * | 2016-03-08 | 2016-07-27 | 中国农业科学院农业资源与农业区划研究所 | Device and method for determining soil alkali-hydrolyzable nitrogen |
-
2019
- 2019-01-18 CN CN201910048823.4A patent/CN109900694A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102297861A (en) * | 2011-07-19 | 2011-12-28 | 中国科学院东北地理与农业生态研究所 | Determination method of soil alkaline hydrolyzable nitrogen |
| CN203231964U (en) * | 2012-12-21 | 2013-10-09 | 中国科学院东北地理与农业生态研究所 | Diffusion vessel for soil alkaline hydrolysis nitrogen |
| CN104111256A (en) * | 2014-07-04 | 2014-10-22 | 中国科学院东北地理与农业生态研究所 | Method for detecting content of soil alkali-hydrolyzable nitrogen |
| CN104991036A (en) * | 2015-08-03 | 2015-10-21 | 河南广电计量检测有限公司 | Determination method for soil alkali-hydrolyzable nitrogen |
| CN105806837A (en) * | 2016-03-08 | 2016-07-27 | 中国农业科学院农业资源与农业区划研究所 | Device and method for determining soil alkali-hydrolyzable nitrogen |
Non-Patent Citations (2)
| Title |
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| 彭正萍等: "《肥料科学施用技术》", 31 March 2013 * |
| 谢卫国: "《测土配方施肥理论与实践》", 31 May 2006 * |
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