CN105259301A - Ammonium polyphosphate agricultural water soluble fertilizer polymerization degree detection method - Google Patents
Ammonium polyphosphate agricultural water soluble fertilizer polymerization degree detection method Download PDFInfo
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- CN105259301A CN105259301A CN201510771189.9A CN201510771189A CN105259301A CN 105259301 A CN105259301 A CN 105259301A CN 201510771189 A CN201510771189 A CN 201510771189A CN 105259301 A CN105259301 A CN 105259301A
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Abstract
The invention belongs to the technical field of fertilizer detection, and particularly relates to an ammonium polyphosphate agricultural water soluble fertilizer polymerization degree detection method. The PH of a sample solution is adjusted through a HCl solution to be 2, then, standard NaOH is sucked for back titration so that a titration curve can be drawn, and the distance between two jumping points is a weak acid function fw; the PH of the sample solution is adjusted through HCl to be 1, backflowing is performed at the temperature of 80 DEG C to 100 DEG C for 10-15 min, then, backflowing is performed at the temperature of 70-80 DEG C for 5-10 min, then the PH is adjusted through NaOH to be 2.5, then, standard NaOH is sucked for back titration so that a titration curve can be drawn, and the distance between two jumping points is a strong acid function fs; the average degree of polymerization n is equal to 2fs/fw. The ammonium polyphosphate agricultural water soluble fertilizer polymerization degree detection method has the advantages of being rapid, easy to operate, accurate, good in reproducibility, economical and high in operability.
Description
Technical field
The invention belongs to fertilizer detection technique field, be specifically related to a kind of ammonium polyphosphate agricultural water soluble fertilizer degree of polymerization detection method.
Background technology
APP (ammoniumpolyphosphate, hereinafter referred to as APP) has following general structure: (NH4)
n+2p
no
3n+1, be a kind of Quadrafos of nitrogenous, phosphorus, by its degree of polymerization size, can be divided into oligomeric, in poly-, high poly-3 kinds, its degree of polymerization is higher, water-soluble less.Can be divided into crystallization shape and amorphous by its structure, crystalline state APP is long-chain shape water-insoluble Quadrafos.
Recent APP has progressed into the production field of composite fertilizer and liquid fertilizer, is extensively utilized especially in developed country.Early 1970s U.S. TVA company develops the method with commodity phosphoric acid by wet process ammonification in tubular reactor, produces the molten mass containing APP, mainly for the preparation of suspension fertilizer, after again for the manufacture of granular compound fertilizer.The liquid fertilizer that the nineties in 20th century, the U.S. consumed every year accounts for more than 38% of fertilizer consumption total amount, but does not also have a kind of detection method of the ammonium fertilizer of the polyphosphoric acids effectively and rapidly degree of polymerization.
China not yet has the polymerization degree measurement method of professional APP fertilizer at present.It is generally acknowledged as fertilizer APP it should is that short chain is entirely water-soluble, comprise the multiple APPs such as ammonium phosphate, tripolyphosphate ammonium and four APPs, the APP that the degree of polymerization is higher, chain is longer only has a small amount of existence; Separately having data to introduce the usual degree of polymerization of agricultural APP is 2-8, and dissolubility is well the principal item of liquid fertilizer.The China that is determined at of the agricultural APP fertilizer degree of polymerization does not also have concrete method.
The assay method of the industry preparation APP degree of polymerization is a lot, and generally speaking the assay method operation of the degree of polymerization is more time-consuming.The assay method of the degree of polymerization common is at present (1) terminal group titration.Terminal group titration is the earliest for one of the method for Quadrafos polymerization degree measurement, and being considered to characterize the most useful method of the Quadrafos degree of polymerization, is also the most frequently used assay method; (2) nuclear magnetic resonance method.NMR (Nuclear Magnetic Resonance) analysis is quick and easy, accurate, and is applicable to the mensuration of arbitrary size degree of polymerization APP, is a kind of APP polymerization degree measurement method preferably, but due to apparatus expensive range of application less; (3) high-speed liquid chromatography; (4) chromatography of ions; (5) viscosimetry; (6) light scattering method etc.
Said method is not also applied in the production detecting low polymerization degree, highly-water-soluble polyphosphoric acids ammonium fertilizer, all there is the mensuration that the shortcomings such as this error is large, poor reproducibility are not suitable for low polymerization degree, the highly-water-soluble polyphosphoric acids ammonium fertilizer degree of polymerization due to said method, therefore the detection method of research and development novel, the quick polyphosphoric acids ammonium fertilizer degree of polymerization is problem in the urgent need to address.
Summary of the invention
The object of this invention is to provide a kind of ammonium polyphosphate agricultural water soluble fertilizer degree of polymerization detection method, simple, quick, accurate, favorable reproducibility.
Ammonium polyphosphate of the present invention agricultural water soluble fertilizer degree of polymerization detection method, step is as follows:
(1) take ammonium polyphosphate fertilizer sample, join and fill in the beaker of distilled water, be adjusted to PH=12 with NaOH, heating, cooling, for subsequent use;
(2) get the solution that step (1) obtains, be adjusted to PH=2 with HCl solution, then draw standard NaOH and carry out back titration, record each caustic dosage and corresponding pH value, draw titration curve, the distance between two hop points is weak acid function f w;
(3) get the solution that step (1) obtains and be placed in round-bottomed flask, PH=1 is adjusted to HCl, 80-100 DEG C of backflow 10-15 minute, then 70-80 DEG C of backflow 5-10 minute, regulate PH=2.5 with NaOH again, then draw standard NaOH and carry out back titration, record each caustic dosage and corresponding pH value, draw titration curve, the spacing of two hop points is strong acid function f s;
(4) average degree of polymerization n=2fs/fw.
The quality of the ammonium polyphosphate fertilizer sample described in step (1) is 1-5g.
The addition of the distilled water described in step (1) is 500mL.
Heating-up temperature described in step (1) is 80-100 DEG C, and the heat time is 10-15 minute.
The solution usage that step (1) described in step (2) obtains is 200mL.
The concentration of the standard NaOH described in step (2) is 0.1240mol/L.
The solution usage that step (1) described in step (3) obtains is 200mL.
The concentration of the standard NaOH described in step (3) is 0.1240mol/L.
The present invention compared with prior art, has following beneficial effect:
The detection method of the ammonium polyphosphate water soluble fertilizer degree of polymerization of the present invention has quick, simple to operate, accurate, favorable reproducibility, economy, workable advantage.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
(1) take No. 1,2g ammonium polyphosphate fertilizer sample, join in the beaker filling 500mL distilled water, be adjusted to PH=12 with NaOH, 80 DEG C are heated 10 minutes, and cooling is for subsequent use.
(2) (1) solution 200mL is got, PH=2 is adjusted to HCl solution, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, observe the change of PH meter, record each caustic dosage and corresponding pH value, draw titration curve, the distance between two hop points is weak acid function f w.
(3) get (1) solution 200mL and be placed in round-bottomed flask, PH=1 is adjusted to HCl, 100 DEG C are refluxed 10 minutes, reflux again at 80 DEG C 5 minutes, PH=2.5 is regulated again with NaOH, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, record each caustic dosage and corresponding pH value, draw titration curve.The spacing of two hop points is strong acid function f s.
(4) average degree of polymerization n=2fs/fw.
Concrete test data is in table 1.
Embodiment 2
(1) take No. 2,3g ammonium polyphosphate fertilizer sample, join in the beaker filling 500mL distilled water, be adjusted to PH=12 with NaOH, 90 DEG C are heated 12 minutes, and cooling is for subsequent use.
(2) (1) solution 200mL is got, PH=2 is adjusted to HCl solution, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, observe the change of PH meter, record each caustic dosage and corresponding pH value, draw titration curve, the distance between two hop points is weak acid function f w.
(3) get (1) solution 200mL and be placed in round-bottomed flask, PH=1 is adjusted to HCl, 80 DEG C are refluxed 10 minutes, reflux again at 70 DEG C 5 minutes, PH=2.5 is regulated again with NaOH, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, record each caustic dosage and corresponding pH value, draw titration curve.The spacing of two hop points is strong acid function f s.
(4) average degree of polymerization n=2fs/fw.
Concrete test data is in table 1.
Embodiment 3
(1) take No. 3,4g ammonium polyphosphate fertilizer sample, join in the beaker filling 500mL distilled water, be adjusted to PH=12 with NaOH, 100 DEG C are heated 15 minutes, and cooling is for subsequent use.
(2) (1) solution 200mL is got, PH=2 is adjusted to HCl solution, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, observe the change of PH meter, record each caustic dosage and corresponding pH value, draw titration curve, the distance between two hop points is weak acid function f w.
(3) get (1) solution 200mL and be placed in round-bottomed flask, PH=1 is adjusted to HCl, 90 DEG C are refluxed 15 minutes, reflux again at 75 DEG C 8 minutes, PH=2.5 is regulated again with NaOH, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, record each caustic dosage and corresponding pH value, draw titration curve.The spacing of two hop points is strong acid function f s.
(4) average degree of polymerization n=2fs/fw.
Concrete test data is in table 1.
Embodiment 4
(1) take No. 4,4.5g ammonium polyphosphate fertilizer sample, join in the beaker filling 500mL distilled water, be adjusted to PH=12 with NaOH, 85 DEG C are heated 10 minutes, and cooling is for subsequent use.
(2) (1) solution 200mL is got, PH=2 is adjusted to HCl solution, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, observe the change of PH meter, record each caustic dosage and corresponding pH value, draw titration curve, the distance between two hop points is weak acid function f w.
(3) get (1) solution 200mL and be placed in round-bottomed flask, PH=1 is adjusted to HCl, 100 DEG C are refluxed 12 minutes, reflux again at 80 DEG C 10 minutes, PH=2.5 is regulated again with NaOH, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, record each caustic dosage and corresponding pH value, draw titration curve.The spacing of two hop points is strong acid function f s.
(4) average degree of polymerization n=2fs/fw.
Concrete test data is in table 1.
Embodiment 5
(1) take No. 5,4.5g ammonium polyphosphate fertilizer sample, join in the beaker filling 500mL distilled water, be adjusted to PH=12 with NaOH, 95 DEG C are heated 10 minutes, and cooling is for subsequent use.
(2) (1) solution 200mL is got, PH=2 is adjusted to HCl solution, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, observe the change of PH meter, record each caustic dosage and corresponding pH value, draw titration curve, the distance between two hop points is weak acid function f w.
(3) get (1) solution 200mL and be placed in round-bottomed flask, PH=1 is adjusted to HCl, 100 DEG C are refluxed 10 minutes, reflux again at 80 DEG C 5 minutes, PH=2.5 is regulated again with NaOH, then draw 0.1240mol/L standard NaOH with 1ml liquid-transfering gun and carry out back titration, record each caustic dosage and corresponding pH value, draw titration curve.The spacing of two hop points is strong acid function f s.
(4) average degree of polymerization n=2fs/fw.
Concrete test data is in table 1.
No. 1-5, polyphosphoric acids ammonium fertilizer is that the Tai Baojin that Tai Bao biotech inc of Shandong Province produces gathers moral a great number of elements Water soluble fertilizer and buys 5 samples obtained for 5 times.
Table 1 embodiment 1-5 test data
Claims (8)
1. an ammonium polyphosphate agricultural water soluble fertilizer degree of polymerization detection method, is characterized in that step is as follows:
(1) take ammonium polyphosphate fertilizer sample, join and fill in the beaker of distilled water, be adjusted to PH=12 with NaOH, heating, cooling, for subsequent use;
(2) get the solution that step (1) obtains, be adjusted to PH=2 with HCl solution, then draw standard NaOH and carry out back titration, record each caustic dosage and corresponding pH value, draw titration curve, the distance between two hop points is weak acid function f w;
(3) get the solution that step (1) obtains and be placed in round-bottomed flask, PH=1 is adjusted to HCl, 80-100 DEG C of backflow 10-15 minute, then 70-80 DEG C of backflow 5-10 minute, regulate PH=2.5 with NaOH again, then draw standard NaOH and carry out back titration, record each caustic dosage and corresponding pH value, draw titration curve, the spacing of two hop points is strong acid function f s;
(4) average degree of polymerization n=2fs/fw.
2. ammonium polyphosphate according to claim 1 agricultural water soluble fertilizer degree of polymerization detection method, is characterized in that the quality of the ammonium polyphosphate fertilizer sample described in step (1) is 1-5g.
3. ammonium polyphosphate according to claim 1 agricultural water soluble fertilizer degree of polymerization detection method, is characterized in that the addition of the distilled water described in step (1) is 500mL.
4. ammonium polyphosphate according to claim 1 agricultural water soluble fertilizer degree of polymerization detection method, it is characterized in that the heating-up temperature described in step (1) is 80-100 DEG C, the heat time is 10-15 minute.
5. ammonium polyphosphate according to claim 1 agricultural water soluble fertilizer degree of polymerization detection method, is characterized in that the solution usage that the step (1) described in step (2) obtains is 200mL.
6. ammonium polyphosphate according to claim 1 agricultural water soluble fertilizer degree of polymerization detection method, is characterized in that the concentration of the standard NaOH described in step (2) is 0.1240mol/L.
7. ammonium polyphosphate according to claim 1 agricultural water soluble fertilizer degree of polymerization detection method, is characterized in that the solution usage that the step (1) described in step (3) obtains is 200mL.
8. ammonium polyphosphate according to claim 1 agricultural water soluble fertilizer degree of polymerization detection method, is characterized in that the concentration of the standard NaOH described in step (3) is 0.1240mol/L.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104155389A (en) * | 2013-05-14 | 2014-11-19 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for measuring average polymerization degree of galactooligosaccharide |
| CN104792929A (en) * | 2015-04-27 | 2015-07-22 | 深圳市芭田生态工程股份有限公司 | Method for detecting ammonium polyphosphate polymerization degree of fertilizer |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104155389A (en) * | 2013-05-14 | 2014-11-19 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for measuring average polymerization degree of galactooligosaccharide |
| CN104792929A (en) * | 2015-04-27 | 2015-07-22 | 深圳市芭田生态工程股份有限公司 | Method for detecting ammonium polyphosphate polymerization degree of fertilizer |
Non-Patent Citations (3)
| Title |
|---|
| 刘丽霞等: "聚磷酸铵聚合度分析方法综述", 《贵州化工》 * |
| 叶文淳等: ""聚磷酸铵聚合度分析方法综述"", 《云南化工》 * |
| 陈平初等: ""长链聚磷酸铵聚合度的快速测定方法"", 《分析化学》 * |
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Application publication date: 20160120 |