CN101526468B - Method for detecting and extracting content of slowly available potassium in limy soil - Google Patents
Method for detecting and extracting content of slowly available potassium in limy soil Download PDFInfo
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- CN101526468B CN101526468B CN2009100588510A CN200910058851A CN101526468B CN 101526468 B CN101526468 B CN 101526468B CN 2009100588510 A CN2009100588510 A CN 2009100588510A CN 200910058851 A CN200910058851 A CN 200910058851A CN 101526468 B CN101526468 B CN 101526468B
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- available potassium
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Abstract
The present invention relates to a method for detecting and extracting the content of slowly available potassium in limy soil, comprising the following steps of: 1. weighing loftdried soil samples 2.5g which passes through 1 mm sieve meshes in large test tube; 2. dripping a drop of plant oil into the large test tube and dripping 1 mol L<-1> HNO3 25 ml; 3. putting the large test tube into an iron wire cage, putting the cage into an oil bath pan with 160 DEG C to be heated up and boiled for 11 min, filtering mixture in a 100 ml volumetric flask while the mixture is hot, washing the soil and the test tube for 4 times with the HNO3 solution with 15 ml at each time, defining volume after cooling; and 4. directly measuring by an atomic-absorption spectrophotometer. By dipping a drop of plant oil in to the soil sample, the invention avoids the overflow of extracting solution and the temperature of the extracting solution is much stable. By using hard test tube and heating up in a way of oil bath, the invention can extract about 60 soil samples at one time, has the advantage of convenient operation, greatly improves work efficiency, and is particularly suitable for measuring the slowly available potassium in the large quantities of soil during soil testing and formulated fertilization.
Description
Technical field
The present invention relates to a kind of detection method of soil chemistry element, concrete is a kind of method for detecting and extracting content of slowly available potassium in limy soil.
Background technology
The output of soil slowly available potassium and crops has better correlativity, be put into portion, economize that fertilization compositions based on earth measurement subsidy project soil detects must survey project.At present, adopt 1molL
-1HNO
3Boiling extracting method measures the method for calacareous soil slowly available potassium content and is: take by weighing air-dry soil sample 2.50g by the 1mm sieve aperture in the 100mL triangular flask, add 1molL
-1HNO
325ml adds a curved little funnel of neck at bottleneck, boils 10min on thermostatic electrothermal plate, and filtered while hot is used 0.1mol L in the 100mL volumetric flask
-1HNO
3Solution washing soil and test tube 4 times are used 15mL at every turn, cooling back constant volume.On the GBC933 atomic spectrophotometer, directly record the solubility in acid potassium of pedotheque, deduct the slowly available potassium that available potassium promptly gets this soil sample.The soil liquid of this method discharges a large amount of CO in boiling part
2Gas makes that boiling time is difficult to judge, and leaching liquor is easy to overflow bottleneck, influences the testing result accuracy.During mass detection, make container with triangular flask, it is big to take up space, and the sample 10-20 of every batch of lixiviate, limited amount has limited detection speed.As thermal source, it is slow to heat up with electric hot plate, and the about temperature difference is big, inconvenient operation.
Summary of the invention
In order to solve the existing the problems referred to above that exist in the leach extraction method that detect, the invention provides a kind of easy to operate, detection speed is fast, efficient is high, measure method for detecting and extracting content of slowly available potassium in limy soil accurately.
The present invention is achieved in that
A kind of method for detecting and extracting content of slowly available potassium in limy soil comprises the steps:
(1) weighing
Take by weighing air-dry soil sample 2.50g by the 1mm sieve aperture in 25 * 250mm Boiling tube;
(2) add preparation
In Boiling tube, splash into a vegetable oil, add 1molL again
-1HNO
325ml;
(3) disappear and boil
Do not add curved neck funnel at the Boiling tube mouth of pipe, Boiling tube is placed wire mesh cage simultaneously, put into 160 ℃ of oil bath pan heated and boiled 11min, filtered while hot is used 0.1mol L in the 100mL volumetric flask
-1HNO
3Solution washing soil and test tube 4 times are used 15mL at every turn, cooling back constant volume;
(4) measure
On atomic spectrophotometer, directly record the solubility in acid potassium of pedotheque, deduct the slowly available potassium that available potassium promptly gets this soil sample.
Wherein vegetable oil can be a soybean oil, rapeseed oil, a kind of in the peanut oil.
The present invention has avoided overflowing of extracting solution by splash into a vegetable oil in soil sample, and the temperature of leaching liquor is also more stable.After using hard Boiling tube and oil bath heating instead, but once about 60 soil samples of lixiviate, easy to operate, and improved work efficiency greatly, be specially adapted to the mensuration of the soil slowly available potassium of batch samples in the fertilization compositions based on earth measurement process.
Embodiment
For the relative merits of the existing method (hereinafter to be referred as existing method) mentioned in comparative illustration the inventive method (hereinafter to be referred as this method) and the background technology, do following comparing embodiment with regard to the different situations of each analysis phase appearance of this method and existing method.
Embodiment one
The Comparative Examples of two kinds of method leaching liquor temperature variation
When existing method is measured the calacareous soil slowly available potassium, reach boiling with leaching liquor in a collection of triangular flask and differ bigger around the heat time heating time, require the testing staff to write down boiling zero-time (table 1) respectively.In the boiling process,, be difficult to control to the area requirement strictness of electric hot plate heating-up temperature, leaching liquor is easy to overflow bottleneck, requires to note at any time leaching liquor boiling situation in the triangular flask, when boiling is violent, triangular flask is moved on on the limit of electric hot plate, in case leaching liquor overflows bottleneck.Therefore, though heating-up temperature can be controlled, the temperature of extract still has some variations, and variation range is between 100.8-102.5 ℃ (table 2).
In this method, oil bath heating 1min left and right sides leaching liquor all comes to life, and differs around time about the 5s clock, does not need to write down respectively the zero-time of boiling.This method adds a vegetable oil in leaching liquor after, vegetable oil has played the effect of froth breaking, and leaching liquor does not produce a large amount of foams, does not overflow the danger of the mouth of pipe, and the leaching liquor temperature stabilization changes by less (table 2) about 103.8 ℃.
Two kinds of method leaching liquors of table 1 reach the required heat time heating time of seething with excitement
Annotate: from triangular flask be placed on 160 ℃ of electric hot plates, Boiling tube puts into 160 ℃ oil bath and picks up counting, seethe with excitement to leaching liquor.
The leaching liquor temperature of two kinds of methods of table 2 is situation over time
Annotate: leaching liquor reaches boiling and picks up counting, and temperature shown in the table is the temperature variations of single sample.
Embodiment two
Two kinds of detection methods detect the Comparative Examples of precision
Choose 5 pedotheques, extract the soil sample slowly available potassium respectively with existing method and this method, 5 parallel, with a collection of lixiviate, checks the error of parallel of two kinds of methods, result such as table 3.
Precision comparison test (the mgkg of two kinds of methods of table 3
-1)
The coefficient of variation of the parallel sample testing result of this method is between 1.2-2.4, and all less than 5.0%, the coefficient of variation of the existing parallel sample testing result of method is between 2.5-6.2, and therefore, the existing method of the error ratio between the parallel sample of this method is little.
Embodiment three
Two kinds of detection methods detect reproducible Comparative Examples
Choose 5 pedotheques, extract the soil sample slowly available potassium respectively with existing method and this method, 5 repetitions divide 5 lixiviates, detect two kinds of detection method reappearances, result such as table 4.
Reappearance test (the mgkg of two kinds of methods of table 4
-1)
This method repeats the coefficient of variation of sample testing result between 1.2-3.3, all less than 5.0%, existing method repeats the coefficient of variation of sample testing result between 3.0-6.9, therefore, the existing method of error ratio that this method repeats between sample is little, illustrates that the reappearance of this method detection calacareous soil slowly available potassium is better than existing method.
Embodiment four
Two kinds of methods detect the Comparative Examples of different slowly available potassium content soil samples
In order to verify reliability, the adaptability of this method extraction soil slowly available potassium, choose slowly available potassium content at 600-1000mgkg
-1Between 20 of pedotheques, measure the content of soil slowly available potassium, result such as table 5 respectively with this method and existing method.
The comparison of two kinds of method measurement results of table 5
Two kinds of methods are measured the permission relative error of slowly available potassiums, being standard less than 5.0%.In 20 pedotheques, when measuring the content of soil slowly available potassium respectively with this method and existing method, have 3 groups of sample relative error 〉=5.0%, surpass the relative error scope, other 17 groups of samples met detect the requirement of relative error, as seen measure the calacareous soil slowly available potassium with this method and compare, 85% coincidence rate is arranged with existing method.
Embodiment five
Measure the slowly available potassium content that fertilization compositions based on earth measurement reference soil sample two is closed soil with this method, each 3 parallel, do 10 batches altogether, the relative error of comparative measurements mean value and the average definite value of reference soil sample.Result such as table 6.
The comparison of two kinds of method measured values of table 6
The result shows that the relative error of this method measured value and the average definite value of reference soil sample is between 0.1-3.5%, and all less than 5%, measurement result and reference coincide, and illustrate that this method can replace the conventional sense method fully.
Claims (2)
1. a method for detecting and extracting content of slowly available potassium in limy soil is characterized in that comprising the steps:
(1) weighing
Take by weighing air-dry soil sample 2.50g by the 1mm sieve aperture in 25 * 250mm Boiling tube;
(2) add preparation
In Boiling tube, splash into a vegetable oil, add 1molL again
-1HNO
325ml;
(3) disappear and boil
Do not add curved neck funnel at the Boiling tube mouth of pipe, Boiling tube is placed wire mesh cage simultaneously, put into 160 ℃ of oil bath pan heated and boiled 11min, filtered while hot is used 0.1mol L in the 100mL volumetric flask
-1HNO
3Solution washing soil sample and test tube 4 times are used 15mL at every turn, cooling back constant volume;
(4) measure
On atomic spectrophotometer, directly record the solubility in acid potassium of pedotheque, deduct the slowly available potassium that available potassium promptly gets this soil sample.
2. a kind of method for detecting and extracting content of slowly available potassium in limy soil according to claim 1 is characterized in that: the vegetable oil that adds in the step (two) is a kind of in soybean oil, rapeseed oil, the peanut oil.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100588510A CN101526468B (en) | 2009-04-03 | 2009-04-03 | Method for detecting and extracting content of slowly available potassium in limy soil |
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| CN2009100588510A CN101526468B (en) | 2009-04-03 | 2009-04-03 | Method for detecting and extracting content of slowly available potassium in limy soil |
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| CN101526468A CN101526468A (en) | 2009-09-09 |
| CN101526468B true CN101526468B (en) | 2011-12-07 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207164B (en) * | 2013-04-09 | 2015-05-20 | 青岛农业大学 | Method for measuring ith potassium of moisture soil and clay coil mineral crystal lattice |
| CN105300989A (en) * | 2015-11-17 | 2016-02-03 | 郑州欧柯奇仪器制造有限公司 | Rapid measurement method of soil available potassium |
| CN109470689A (en) * | 2019-01-07 | 2019-03-15 | 青海省核工业地质局核地质研究所（（青海省核工业地质局检测试验中心）） | The measuring method of slowly available potassium and available potassium in a kind of soil |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1218119A (en) * | 1967-05-26 | 1971-01-06 | Siemens Ag | Monitoring the concentration of potassium hydroxide solutions |
| CN1270309A (en) * | 2000-06-02 | 2000-10-18 | 中国科学院生态环境研究中心 | Method for high-speed measurement of quick-acting N, P and K in soil |
| JP2004251670A (en) * | 2003-02-18 | 2004-09-09 | Gifu Prefecture | Excreted urinary potassium quantity determining method and quantity determining device |
| KR20050074187A (en) * | 2004-01-13 | 2005-07-18 | 플래닛팔이 주식회사 | Potassium analysis method using chromoionophore |
| CN1677086A (en) * | 2004-04-02 | 2005-10-05 | 中国科学院生态环境研究中心 | Biological effective phosphor determining method |
-
2009
- 2009-04-03 CN CN2009100588510A patent/CN101526468B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1218119A (en) * | 1967-05-26 | 1971-01-06 | Siemens Ag | Monitoring the concentration of potassium hydroxide solutions |
| CN1270309A (en) * | 2000-06-02 | 2000-10-18 | 中国科学院生态环境研究中心 | Method for high-speed measurement of quick-acting N, P and K in soil |
| JP2004251670A (en) * | 2003-02-18 | 2004-09-09 | Gifu Prefecture | Excreted urinary potassium quantity determining method and quantity determining device |
| KR20050074187A (en) * | 2004-01-13 | 2005-07-18 | 플래닛팔이 주식회사 | Potassium analysis method using chromoionophore |
| CN1677086A (en) * | 2004-04-02 | 2005-10-05 | 中国科学院生态环境研究中心 | Biological effective phosphor determining method |
Non-Patent Citations (2)
| Title |
|---|
| 刑世和，潘敏芳 等.耕作土壤缓效钾释放特性及其评定方法.《福建农业学报》.1999,第14卷(第3期),47-52. * |
| 罗家贤, 蒋梅茵.土壤中含钾矿物的研究II湖南省一些土壤的含钾矿物含量及其与缓效钾的关系.《土壤学报》.1981,第18卷(第1期),87-95. * |
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