CN102297861A - Determination method of soil alkaline hydrolyzable nitrogen - Google Patents
Determination method of soil alkaline hydrolyzable nitrogen Download PDFInfo
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- CN102297861A CN102297861A CN2011102010076A CN201110201007A CN102297861A CN 102297861 A CN102297861 A CN 102297861A CN 2011102010076 A CN2011102010076 A CN 2011102010076A CN 201110201007 A CN201110201007 A CN 201110201007A CN 102297861 A CN102297861 A CN 102297861A
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- frosted glass
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- sulfuric acid
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Abstract
The invention provides a determination method of soil alkaline hydrolyzable nitrogen, which solves shortages of present methods. According to the determination method, the subnormal result caused by the ammonia loss is avoided through flushing a frosted glass plate, and the above normal result caused by putting an alkaline Arabic gum into an inner chamber of a diffuser in flushing the frosted glass plate is avoided by replacing the Arabic gum with a gelatin, so the precision and the accuracy of data are guaranteed. Detection results of standard soil samples prove that data determined with the method are all in a standard range, but determined results of the present methods are lower than a standard value. Simultaneously the relative standard deviation of the method of the invention, which is 2.94%, is lower than the relative standard deviation of the present methods of 5.30%.
Description
Technical field
The present invention relates to a kind of assay method of soil alkaline hydrolysis nitrogen, be applicable to the mensuration of alkaline hydrolysis nitrogen in the soil.
Background technology
At present, soil alkaline hydrolysis nitrogen determination method: take by weighing wind desiceted soil, itself and ferrous sulphate powder are placed the diffusion boat mistress equably, get 2% boric acid-indicator solution and be put in the diffusion boat inner room, coat alkaline glue at diffusion boat mistress edge then, cover frosted glass, rotation makes ware limit and frosted glass bonding fully for several times.Gradually turn-off frosted glass makes the diffusion boat mistress expose a slit on one side again, adds sodium hydroxide solution rapidly, covers completely immediately, and is tight with the bungee circle again, and frosted glass is fixed, and shakes diffusion boat gently, and alkali lye is fully mixed with soil.Put into constant temperature oven subsequently and cultivate, take out then.With the ammonia in the sulfuric acid standard solution titration inner room absorption liquid.Have very big defective in this method, the ammonia that the absorption fraction volatilizes is adhered in moisture content volatilization meeting in the interior solution of diffusion boat on frosted glass plate on the one hand; Distilled water flushing frosted glass plate of no use on the other hand is incorporated in the diffusion boat inner room to washing fluid, causes the ammonia loss, thereby causes measurement result (the forestry industry standard LY/T 1229-1999 of the People's Republic of China (PRC)) on the low side.
Summary of the invention
For solving the problem that occurs in the soil alkaline hydrolysis nitrogen determination method, the assay method of a kind of soil alkaline hydrolysis nitrogen provided by the invention is a kind of earth of necromancer more accurately alkaline hydrolysis nitrogen determination method, and its step is as follows:
(1) took by weighing the wind desiceted soil 2.00g that 2mm sieves, and placed the diffusion boat mistress, and added 0.2g ferrous sulphate powder, mixing also paves soil equably;
(2) boric acid-indicator solution of getting the 20g/L of 2mL is put in the diffusion boat inner room, coats gelatin solution at diffusion boat mistress edge then, covers frosted glass, and rotation makes ware limit and frosted glass bonding fully; Turn-off frosted glass makes the diffusion boat mistress expose a slit on one side again, and adding 10.0mL concentration as early as possible is the 1mol/L sodium hydroxide solution, cover completely immediately, tight with the bungee circle again, frosted glass is fixed, shake diffusion boat, alkali lye is fully mixed with soil, note not making mistress's alkali lye sneak into inner room; Put into 40 ℃ ± 1 ℃ constant temperature oven subsequently, take out behind alkali silver diffusion 24h ± 0.5h, the centre is shaken twice above acceleration diffusion and is absorbed; Take off the frosted glass plate on the diffusion boat, with the hair side of distilled water flushing frosted glass plate, washing fluid is incorporated in the diffusion boat inner room; With the ammonia in the sulfuric acid standard solution titration inner room absorption liquid; It is titration end-point that solution becomes blush by blue look, the volume numerical value of record consumption acids;
(3) carry out blank test, calibration reagent and titration error simultaneously at sample determination; Blank test is not for adding pedotheque, and other step is consistent with above-mentioned steps;
The result calculates: ω (N)=(V-V
0) * c*M*1000/m
In the formula: ω (N) is alkaline hydrolysis nitrogen content/mg/kg in the sample;
V consumes the volume/mL of sulfuric acid standard solution during for sample determination;
V
0Consume the volume/mL of sulfuric acid standard solution during for blank determination;
C is the concentration/mol/L of sulfuric acid standard solution;
M is the amount of substance/g/moL of nitrogen;
M is sample sample weighting amount/g.
Beneficial effect: the assay method of a kind of soil alkaline hydrolysis nitrogen provided by the invention, solve the deficiency that exists in the existing method, avoided the loss of ammonia to cause that the result is on the low side by the flushing frosted glass plate, bring alkaline Arabic gum into the diffusion boat inner room when avoiding washing frosted glass plate by alkaline Arabic gum is replaced to gelatin, cause that the result is higher, guaranteed the precision and the accuracy of data.Testing result by the standard pedotheque proves, this method records data all within critical field, and that existing method records number is on the low side than standard value, and the relative standard deviation of this method is 2.94% simultaneously, less than existing methods relative standard deviation 5.30%.
Embodiment
Embodiment 1 a kind of soil alkaline hydrolysis nitrogen determination method provided by the invention, step and testing result are as follows:
(1) take by weighing parallel 5 of standard pedotheque (GBW07413), each 2.00g places the diffusion boat mistress respectively, adds 0.2g ferrous sulphate powder respectively, the rotation diffusion boat, and mixing also paves soil equably;
(2) 20g/L boric acid-indicator solution of getting 2mL is put in the diffusion boat inner room, coats gelatin solution at diffusion boat mistress edge then, covers frosted glass, and rotation makes ware limit and frosted glass bonding fully; Turn-off frosted glass makes the diffusion boat mistress expose a slit on one side again, adds 10.0mL 1mol/L sodium hydroxide solution as early as possible, cover completely immediately, tight with the bungee circle again, frosted glass is fixed, shake diffusion boat, alkali lye is fully mixed with soil, note not making mistress's alkali lye sneak into inner room; Put into 40 ℃ ± 1 ℃ constant temperature oven subsequently, take out behind alkali silver diffusion 24h ± 0.5h, the centre is shaken twice above acceleration diffusion and is absorbed; Take off the frosted glass plate on the diffusion boat, with the hair side of distilled water flushing frosted glass plate, washing fluid is incorporated in the diffusion boat inner room; With the ammonia in the sulfuric acid standard solution titration inner room absorption liquid; It is titration end-point that solution becomes blush by blue look, and record consumes the volume numerical value of sulfuric acid;
(3) carry out blank test, calibration reagent and titration error simultaneously at sample determination;
Blank test is not for adding pedotheque, and other step is consistent with above-mentioned steps.
The result calculates: ω (N)=(V-V
0) * c*M*1000/m
In the formula: ω (N) is alkaline hydrolysis nitrogen content/mg/kg in the sample;
V consumes the volume/mL of sulfuric acid standard solution during for sample determination;
V
0Consume the volume/mL of sulfuric acid standard solution during for blank determination;
C is the concentration/mol/L of sulfuric acid standard solution;
M is the amount of substance/g/moL of nitrogen;
M is sample sample weighting amount/g.
(4) testing result sees Table 1.
Table 1
The assay method of comparative example's 1 existing soil alkaline hydrolysis nitrogen, step and testing result are as follows:
(1) take by weighing parallel 5 of standard pedotheque (GBW07413), each 2.00g places the diffusion boat mistress, adds 0.2g ferrous sulphate powder, rotates diffusion boat lightly, and soil is paved equably.
(2) 2% boric acid-indicator solution of getting 2mL is put in the diffusion boat inner room, coats alkaline glue at diffusion boat mistress edge then, covers frosted glass, and rotation makes ware limit and frosted glass bonding fully for several times.Gradually turn-off frosted glass makes the diffusion boat mistress expose a slit on one side again, adds 10.0mL 1mol/L sodium hydroxide solution rapidly, cover completely immediately, tight with the bungee circle again, frosted glass is fixed, shake diffusion boat gently, alkali lye is fully mixed with soil, note not making mistress's alkali lye sneak into inner room.Put into 40 ℃ ± 1 ℃ constant temperature oven subsequently, take out behind alkali silver diffusion 24h ± 0.5h, the centre is shaken and is quickened the diffusion absorption for 3 times.With the NH in the sulfuric acid standard solution titration inner room absorption liquid
3, it is titration end-point that solution becomes blush by blue look, record consumes the volume numerical value of sulfuric acid;
(3) carry out blank test, calibration reagent and titration error simultaneously at sample determination; Blank test is not for adding pedotheque, and other step is consistent with above-mentioned steps;
The result calculates: ω (N)=(V-V
0) * c*M*1000/m
In the formula: ω (N) is alkaline hydrolysis nitrogen content/mg/kg in the sample;
V consumes the volume/mL of sulfuric acid standard solution during for sample determination;
V
0Consume the volume/mL of sulfuric acid standard solution during for blank determination;
C is the concentration/mol/L of sulfuric acid standard solution;
M is the amount of substance/g/moL of nitrogen;
M is sample sample weighting amount/g.
(4) testing result sees Table 2.
Table 2
Claims (1)
1. the assay method of a soil alkaline hydrolysis nitrogen, its step is as follows: (1) took by weighing the wind desiceted soil 2.00g of 2mm sieve, placed the diffusion boat mistress, added 0.2g ferrous sulphate powder, and mixing also paves soil equably;
(2) boric acid-indicator solution of getting the 20g/L of 2mL is put in the diffusion boat inner room, coats gelatin solution at diffusion boat mistress edge then, covers frosted glass, and rotation makes ware limit and frosted glass bonding fully; Turn-off frosted glass makes the diffusion boat mistress expose a slit on one side again, and adding 10.0mL concentration as early as possible is the 1mol/L sodium hydroxide solution, cover completely immediately, tight with the bungee circle again, frosted glass is fixed, shake diffusion boat, alkali lye is fully mixed with soil, note not making mistress's alkali lye sneak into inner room; Put into 40 ℃ ± 1 ℃ constant temperature oven subsequently, take out behind alkali silver diffusion 24h ± 0.5h, the centre is shaken twice above acceleration diffusion and is absorbed; Take off the frosted glass plate on the diffusion boat, with the hair side of distilled water flushing frosted glass plate, washing fluid is incorporated in the diffusion boat inner room; With the ammonia in the sulfuric acid standard solution titration inner room absorption liquid; It is titration end-point that solution becomes blush by blue look, the volume numerical value of record consumption acids;
(3) carry out blank test, calibration reagent and titration error simultaneously at sample determination; Blank test is not for adding pedotheque, and other step is consistent with above-mentioned steps;
The result calculates: ω (N)=(V-V
0) * c*M*1000/m
In the formula: ω (N) is alkaline hydrolysis nitrogen content/mg/kg in the sample;
V consumes the volume/mL of sulfuric acid standard solution during for sample determination;
V
0Consume the volume/mL of sulfuric acid standard solution during for blank determination;
C is the concentration/mol/L of sulfuric acid standard solution;
M is the amount of substance/g/moL of nitrogen;
M is sample sample weighting amount/g.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103411805A (en) * | 2013-07-25 | 2013-11-27 | 中国科学院东北地理与农业生态研究所 | Glue spreading device used in soil alkali-hydrolyzable nitrogen content measuring process and use method thereof |
| 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 |
| CN109490508A (en) * | 2018-10-23 | 2019-03-19 | 中国科学院合肥物质科学研究院 | A kind of nitrogenous test expectation system of soil alkali-hydrolyzable nitrogen |
| CN109900694A (en) * | 2019-01-18 | 2019-06-18 | 河南省烟草公司平顶山市公司 | A kind of measuring method of vega soil alkaline hydrolysis nitrogen content |
| CN112505292A (en) * | 2020-11-17 | 2021-03-16 | 中国环境科学研究院 | Culture device and culture method for nitrogen hydrolysis experiment |
| CN113252843A (en) * | 2021-04-29 | 2021-08-13 | 扬州大学 | Method for measuring available nitrogen of facility soil |
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| CN201034879Y (en) * | 2007-04-14 | 2008-03-12 | 新疆农业科学院土壤肥料研究所 | Pervasion dish |
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2011
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Patent Citations (1)
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| CN201034879Y (en) * | 2007-04-14 | 2008-03-12 | 新疆农业科学院土壤肥料研究所 | Pervasion dish |
Non-Patent Citations (2)
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| 李金彦: "土壤水解性氮的测定（碱解扩散法）", 《农业科技与信息》, 31 May 2010 (2010-05-31), pages 15 * |
| 王晓岚等: "土壤碱解氮测定方法的比较", 《北京师范大学学报（自然科学版）》, 28 February 2010 (2010-02-28), pages 76 - 78 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103411805A (en) * | 2013-07-25 | 2013-11-27 | 中国科学院东北地理与农业生态研究所 | Glue spreading device used in soil alkali-hydrolyzable nitrogen content measuring process and use method thereof |
| 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 |
| CN109490508A (en) * | 2018-10-23 | 2019-03-19 | 中国科学院合肥物质科学研究院 | A kind of nitrogenous test expectation system of soil alkali-hydrolyzable nitrogen |
| CN109490508B (en) * | 2018-10-23 | 2021-10-29 | 中国科学院合肥物质科学研究院 | Soil alkaline hydrolysis nitrogen-containing test prediction system |
| CN109900694A (en) * | 2019-01-18 | 2019-06-18 | 河南省烟草公司平顶山市公司 | A kind of measuring method of vega soil alkaline hydrolysis nitrogen content |
| CN112505292A (en) * | 2020-11-17 | 2021-03-16 | 中国环境科学研究院 | Culture device and culture method for nitrogen hydrolysis experiment |
| CN112505292B (en) * | 2020-11-17 | 2022-02-18 | 中国环境科学研究院 | Culture device and culture method for nitrogen hydrolysis experiment |
| CN113252843A (en) * | 2021-04-29 | 2021-08-13 | 扬州大学 | Method for measuring available nitrogen of facility soil |
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Application publication date: 20111228 |