CN101566536B - Measuring method for N content in soil microorganism - Google Patents
Measuring method for N content in soil microorganism Download PDFInfo
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- CN101566536B CN101566536B CN2008100111615A CN200810011161A CN101566536B CN 101566536 B CN101566536 B CN 101566536B CN 2008100111615 A CN2008100111615 A CN 2008100111615A CN 200810011161 A CN200810011161 A CN 200810011161A CN 101566536 B CN101566536 B CN 101566536B
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Abstract
The invention relates to a measuring method for N content in the soil microorganism, which belongs to the technical field of analysis test methods. The method can accurately and reliably measure the soil microorganism with N content being less than 10 mg/L and comprises the following steps: the soil fumigation and leaching step; the digestion step of soil leaching solution; and the distillation and determination step of digestion solution, wherein the digestion step of the soil leaching solution comprises two processes of low temperature digestion and high temperature digestion; the low temperature digestion is carried out for 1 h at the temperature of 260 DEG C and the high temperature digestion is carried out for 3 h at the temperature of 380 DEG C; 20 ml of concentrated sulfuric acid and 1.5-2.0 g of mixed catalyst are added in 20ml of leaching solution; and the mixture ratio of the mixed catalyst of K2SO4:CuSO4 is equal to 20:1 (mass ratio). The invention has the advantages of simple and convenient operation, easily obtained reagent, accurate measuring result, wide application range, security and no toxic action to the human body.
Description
Technical field
The present invention relates to the analysis test method technical field, specifically be meant the assay method of soil microorganism nitrogen content.
Background technology
The mensuration of soil microorganism nitrogen content is the basis of research soil microorganism.At the beginning of the eighties, Chinese scholars begins to adopt chloroform to fumigate extraction (FE) to measure soil microorganism material (comprising microbial biomass C, N, P and S).The stifling direct extraction method of chloroform has quick, easy and is suitable for wide and reappearance measurement result of soil scope and better adopted widely, has greatly promoted the research of Soil microbial biomass nitrogen.But the stifling direct extraction method of chloroform is measured the full nitrogen of leaching liquor with traditional Kjeldahl, and is not only loaded down with trivial details time-consuming, but also can be not accurate enough because of the low measurement result that makes of leaching liquor total nitrogen content, is difficult to use in the test of batch samples.Therefore, be badly in need of fairly simple, soil microorganism N assay method fast.In recent years, develop rapidly along with science and technology, many scholars begin to adopt the TOC analyser to measure soil microorganism C, N content, its principle also is by measuring full carbon, the total nitrogen content in the soil extraction, be converted to soil microorganism C, N content by coefficient again, easy and simple to handle because of it, be widely used fast.Test findings shows, when adopting the TOC analyser to carry out soil microorganism C assay, no matter full concentration of carbon is low still high in the soil extraction, its measurement result highly sensitive, accuracy height, good reproducibility; But for N content in soil microorganism, have only that total nitrogen content is higher than 15mg/L in soil extraction, its recovery just reaches more than 95%, and is lower than its recovery of this concentration less than 80%, and the repeat samples differences is very big.Therefore, its result reliability is poor when utilizing the TOC analyser that microorganism N content analysis in the low soil extraction of nitrogen concentration is measured, and exists than mistake.
In people's such as Chen Guochao document, put down in writing assay method, having comprised: the stifling and lixiviate step of soil about red soil microorganism N; Step is boiled in disappearing of soil extraction; The determination of distillation step that disappears and boil liquid.Because this method disappears and boils step and be not divided into two processes, and the addition of the concentrated sulphuric acid is too high, strong acid and highly basic reaction are more violent in the process that adding highly basic distills, not only dangerous, and, cause recovery reduction because vigorous reaction can cause in the automatic distilling apparatus boiling the position that pipe is connected nitrogen loss taking place with disappearing.Therefore be lower than 10mg/L for N content in soil microorganism, this method is just inapplicable.This method mixed catalyst contains selenium powder in addition, to the toxic effect of health.
Summary of the invention
For overcoming above-mentioned deficiency, the purpose of this invention is to provide and a kind ofly be lower than the soil of 10mg/L applicable to microorganism N content, and accurately, safety, to the N content assaying method of human body nonhazardous effect.
For realizing purpose of the present invention, the technical solution used in the present invention is:
A kind of assay method of N content in soil microorganism comprises the steps:
Stifling and the lixiviate step of soil:
Step is boiled in disappearing of soil extraction:
The determination of distillation step that disappears and boil liquid:
The disappearing of described soil extraction boiled step and is divided into low temperature and disappears that boiling disappears with high temperature boils two processes.
Described low temperature disappears to boil and is 260 ℃ and disappears and boil 1h, and described high temperature disappears to boil and is 380 ℃ and disappears and boil 3h.
Described disappearing boiled in the step, and 20ml leaching liquor concentrated sulphuric acid addition is 3～5ml, and the mixed catalyst consumption is 1.5～2.0g.
The proportioning of described mixed catalyst is: K
2SO
4: CuSO
4=20: 1 (mass ratio).
Advantage of the present invention is:
1. applicability is wide, owing to avoided in the still-process strong acid and highly basic course of reaction too violent, caused nitrogen loss, the nitrogen recovery reduction, so be not only applicable to the soil that microorganism N content is higher than 10mg/L, be applicable to that also microorganism N content is lower than the soil of 10mg/L.
2. simple, quick, security, accuracy height.
3. mixed catalyst does not contain selenium powder, safety, to human body nonhazardous effect.
Embodiment
Embodiment 1
For feasibility of the present invention is described, at first choose antifebrin and verify the recovery and the accuracy of this assay method as standard reagent, this reagent stable in properties, nitrogen content is determined, and it is the reductibility nitrogen, to microorganism N in the soil extraction exist form more similar.Antifebrin is configured to the standard solution of variable concentrations, disappears and boil determination of distillation, concrete steps are as follows:
(1) with the pure antifebrin of top grade as standard reagent, at first prepare 100mg/L antifebrin standard solution, dilute in proportion then and prepare 5,10,20 and 50mg/L antifebrin standard solution respectively.
(2) draw each 3 parts of the antifebrin standard solution of 20ml variable concentrations respectively, put into 200ml Kai Shi and disappear and boil pipe, add the 0.5ml concentrated sulphuric acid to prevent the loss of ammonium.
(3) disappearing of standard solution will be housed and boil pipe and put into to disappear and boil stove, 150 ℃ down about the about 1h of heating to liquid volume minimizing 2-3ml.
(4) will disappear and boil pipe and take out, (mass ratio is K to add the 2.0g mixed catalyst
2SO
4: CuSO
4=20: 1) and the 5ml concentrated sulphuric acid, shake up, 260 ℃ down the about 1h low temperature of heating disappear and boil and catch up with moisture in the solution, 380 ℃ then, the sulfuric acid high temperature of being fuming disappears and boils 3h.
(5) wait to disappear boil liquid and cool off fully after, Kai Shi disappeared boils pipe and receive automatically and decide on the nitrogen distiller, in distillation cascade, add 10mol/L sodium hydroxide solution 25ml, receive liquid with standard sulfuric acid titration boric acid.Do blank simultaneously.
(6) total nitrogen content that passes through to be measured calculates N content in soil microorganism.
Embodiment 2
Choose field original position soil sample, disappear and boil determination of distillation:
(1) take by weighing the bright soil sample of 50g in double dish, be full of in the vacuum dryer of chloroform, smoked kill 24h under 25 ℃ of dark conditions places double dish another clean vacuum dryer then, with the pump Ex-all residue chloroform of bleeding.
(2) soil sample in the transfer double dish adds the K of 150ml 0.5mol/L in the 250ml triangular flask
2SO
4Solution, the 25 ℃ of 200r/min lixiviate 30min that vibrates on vibrating machine gets clear liquid with filter paper filtering, does not fumigating soil leaching liquor simultaneously.
(3) pipette the 20ml leaching liquor and disappear in 200ml Kai Shi and boil in the pipe, add the 0.5ml concentrated sulphuric acid to prevent the loss of ammonium.
(4) disappearing of leaching liquor will be housed and boil pipe and put into to disappear and boil stove, 150 ℃ down about the about 1h of heating to liquid volume minimizing 2-3ml.
(5) will disappear and boil pipe and take out, (mass ratio is K to add the 1.5g mixed catalyst
2SO
4: CuSO
4=20: 1) and the 3ml concentrated sulphuric acid, shake up, 260 ℃ down the about 1h low temperature of heating disappear and boil and catch up with moisture in the solution, 380 ℃ then, the sulfuric acid high temperature of being fuming disappears and boils 3h.Do blank simultaneously.
(6) wait to disappear boil liquid and cool off fully after, Kai Shi disappeared boils pipe and receive automatically and decide on the nitrogen distiller, in distillation cascade, add 10mol/L sodium hydroxide solution 25ml, receive liquid with standard sulfuric acid titration boric acid.
(7) calculate N content in soil microorganism by total nitrogen content.
Table 1 is the determination of recovery rates result of antifebrin standard solution.
Table 1
Above-listed detailed description is at the specifying of possible embodiments of the present invention, and this embodiment is not in order to limiting claim of the present invention, does not allly break away from the equivalence that skill spirit of the present invention does and implements or change, all should be contained in the claim of the present invention.
Claims (1)
1. the assay method of a N content in soil microorganism comprises the steps:
Stifling and the lixiviate step of soil:
Step is boiled in disappearing of soil extraction:
The determination of distillation step that disappears and boil liquid:
It is characterized in that: the disappearing of described soil extraction boiled step and is divided into low temperature and disappears that boiling disappears with high temperature boils two processes;
Described low temperature disappears to boil and is 260 ℃ and disappears and boil 1h, and described high temperature disappears to boil and is 380 ℃ and disappears and boil 3h;
20ml leaching liquor concentrated sulphuric acid addition is 3-5ml, and the mixed catalyst consumption is 1.5-2.0g;
The proportioning of mixed catalyst is: K
2SO
4: CuSO
4=20: 1 (mass ratio).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100111615A CN101566536B (en) | 2008-04-23 | 2008-04-23 | Measuring method for N content in soil microorganism |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100111615A CN101566536B (en) | 2008-04-23 | 2008-04-23 | Measuring method for N content in soil microorganism |
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| CN101566536A CN101566536A (en) | 2009-10-28 |
| CN101566536B true CN101566536B (en) | 2010-12-08 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091353A (en) * | 2011-11-01 | 2013-05-08 | 中国科学院沈阳应用生态研究所 | Determination method of carbon and nitrogen contents in soil |
| CN105277404B (en) * | 2015-10-08 | 2018-01-23 | 浙江省农业科学院 | Determine soil microbes biomass carbon nitrogen chloroform device for fumigation and fumigating method |
| CN111751185A (en) * | 2020-07-07 | 2020-10-09 | 盐城工学院 | Soil microorganism fumigation device |
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2008
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Non-Patent Citations (1)
| Title |
|---|
| 候正仿等.土壤全氮分析方法探讨.《天津农林科技》.2008,(第5期),9-11. * |
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