CN104792929A - Method for detecting ammonium polyphosphate polymerization degree of fertilizer - Google Patents
Method for detecting ammonium polyphosphate polymerization degree of fertilizer Download PDFInfo
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- CN104792929A CN104792929A CN201510204254.XA CN201510204254A CN104792929A CN 104792929 A CN104792929 A CN 104792929A CN 201510204254 A CN201510204254 A CN 201510204254A CN 104792929 A CN104792929 A CN 104792929A
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Abstract
The invention discloses a method for detecting the ammonium polyphosphate polymerization degree of a fertilizer. The method comprises the following steps: (1) dissolving fertilizer samples, adjusting the pH value to be alkaline, defining the volume of a solution subjected to ion exchange, and uniformly dividing the solution into two liquids to be detected; (2) adding acid in one liquid to be detected to adjust the pH value to 2-4, titrating with alkali, recording the volume of alkali consumed in the process of titrating when the pH value ranges from 4.5 to 9.5, and marking A; (3) adding acid in the other liquid to be detected for digestion, adding acid to adjust the pH value to 2-4, titrating with alkali, recording the volume of alkali consumed in the process of titrating when the pH value ranges from 4.5 to 9.5, and marking Ah; calculating the polymerization degree of the fertilizer containing ammonium polyphosphate according to the content of end group weak acid and the total phosphorus content in the solution. The method has the advantages of being small in error, and high in precision.
Description
Technical field
The present invention relates to a kind of detection method of the degree of polymerization, be specifically related to a kind of detection method of the APP degree of polymerization of fertilizer.
Background technology
APP is a kind of inorganic polymer of phosphorous, nitrogen, and because nutrient content is high, dissolubility is good, and not easily with the calcium in the soil liquid, magnesium, iron, aluminium plasma reaction and make phosphate radical lose efficacy, therefore, be widely used in fertilizer, production technology is very ripe.Can be divided into oligomer, middle polymers and superpolymer 3 kinds by its degree of polymerization, its degree of polymerization more highly-water-soluble is less, otherwise then water-soluble larger, and as polymerization degree n < 20, APP is water-soluble; As n > 20, APP is slightly solubility.And the degree of polymerization of APP is important chemistry, the physical parameter that determine its character, there is material impact to the water tolerance Sum decomposition temperature etc. of APP.Therefore, the Accurate Determining of the APP degree of polymerization has important directive significance to its production application.
Superpolymer Measuring Molecule Weight generally carries out in lean solution, and APP is no exception.But because high polymerization degree APP is insoluble in water and organic solvent when normal temperature, therefore dissolved solution effect is bad.Therefore conventional ion exchange process changes the APP of indissoluble into soluble polyphosphate solution.But because the ion exchange process time is long, easily cause Quadrafos side chain and crosslinking points hydrolysis.
Terminal group titration is one of detection method of the Quadrafos degree of polymerization the earliest, the assay method of the industry standard HG/T2770-2008 " industrial polyphosphate sodium " that the Ministry of Chemical Industry promulgates, but the method is only applicable to the APP that polymerization degree n is greater than 20, but for polymerization degree n be less than 20 water-soluble poly ammonium phosphate inapplicable.In addition, in the testing process of reality, sample solution is by after H type cation resin exchange, and after exchanging, the pH value of solution is highly acid, and water-soluble poly ammonium phosphate very easily decomposes, and causes detecting data on the low side.
Because APP end group phosphorus atoms and middle phosphorus atoms are in different chemical environments, in 31P NMR spectrogram, show different chemical shifts, compare the intensity of end group peak and middle crest, just can calculate the degree of polymerization of APP.It is quick and easy, accurate that the method is analyzed, be applicable to the mensuration of any degree of polymerization APP, but for the APP fertilizer of metal ion, because metallic ion has magnetic, the magnetic environment around part can be disturbed, cause spectrum peak wider, the phenomenons such as shimming difficulty, can there is relatively large deviation in the degree of polymerization.
Other is a kind of relative detection method as viscosity method, exclusion chromatography, the chromatography of ions, paper chromatography etc., due to APP facile hydrolysis, be difficult to find standard model, the reappearance of polymerization degree measurement is also bad, therefore usually should not use relative manner to the Accurate Determining of the degree of polymerization.
Above-mentioned several method containing all there is the problems such as inapplicable or error is too large in the APP fertilizer degree of polymerization, cannot meet actual requirement, so need the detection method that a kind of accuracy is high, precision is good in mensuration.
Summary of the invention:
Be not suitable for containing the APP fertilizer degree of polymerization or the large technical matters of testing result error for solving existing detection method, the present invention proposes the method for a kind of accurate detection containing the APP fertilizer degree of polymerization.
The invention provides a kind of detection method of the APP degree of polymerization of fertilizer, comprise the following steps: fertilizer sample is dissolved by (1), and adjust ph is to alkalescence, through the solution constant volume of ion-exchange, divide equally and obtain two parts of liquid to be measured, (2) a liquid to be measured adds acid for adjusting pH to 2 ~ 4, uses alkalimetric titration, the volume of the alkali that record pH value consumes from 4.5 to 9.5 titration, mark A; (3) after another part of liquid acid adding to be measured is cleared up, add acid for adjusting pH to 2 ~ 4, use alkalimetric titration, the volume of the alkali that record pH value consumes from 4.5 to 9.5 titration, mark Ah;
Computing formula: n=2*Ah/A,
In formula: the n------degree of polymerization;
A------end group phosphorus consumes the volume of alkali, mL;
Ah------total phosphorus consumes the volume of alkali, mL.
Preferably, comprise the following steps:
(1) 2 ~ 100g fertilizer sample is taken, be dissolved in water, regulate solution ph to alkalescence, filter insolubles, by filtrate constant volume in the volumetric flask of 100 ~ 1000ml, shift out 25 ~ 100ml solution with transfer pipet and carry out ion-exchange, be surely dissolved in 100 ~ 250ml volumetric flask, divide equally and obtain two parts of liquid to be measured;
(2) a liquid to be measured adds acid for adjusting pH to 2 ~ 4, uses aqueous slkali titration, the volume of the alkali that record pH value consumes from 4.5 to 9.5 titration, mark A, the i.e. content of sample end group phosphorus;
(3) another part of liquid deionized water to be measured is diluted to 100 ~ 250ml, after acid adding clears up 2 ~ 8 hours, regulates solution ph to 2 ~ 4, use aqueous slkali titration, the volume of alkali that record pH value consumes from 4.5 to 9.5 titration, is labeled as Ah, i.e. the content of total phosphorus in sample;
Computing formula: n=2*Ah/A
In formula: the n------degree of polymerization;
A------end group phosphorus consumes the volume of alkali, mL;
Ah------total phosphorus consumes the volume of alkali, mL.
Preferably, described fertilizer sample is the fertilizer containing APP, and APP is chain structure.
Preferably, step (1) described dissolving is at 0 ~ 20 DEG C.
Preferably, described ion-exchange uses Zeo-karb.
Be more preferably, described Zeo-karb is the polystyrene Na type resin of sulfuric acid sulfonation.
Preferably, step (2) described acid is inorganic acid.
Be more preferably, step (2) described acid is the concentrated sulphuric acid, red fuming nitric acid (RFNA), concentrated hydrochloric acid.
Preferably, the addition of step (2) described acid is 5 ~ 20ml, and concentration is 4 ~ 10mol/L.
The inventive method can also comprise the step of fertilizer sample Parallel testing 3 times.
The advantage that the present invention has relative to prior art and beneficial effect.
(1) the present invention carries out ion-exchange in the basic conditions, solves the ion exchange process time long, easily causes the problem of Quadrafos side chain and crosslinking points hydrolysis when sour environment;
(2) titration process is simple to operate, and error is little, can avoid the experiment impact that in titration process, hop does not significantly bring;
(3) the present invention is for water-soluble poly ammonium phosphate in fertilizer, and testing result error is little, and degree of accuracy is high, reproducible.
Embodiment
By the following examples the present invention is described
Embodiment 1: a kind of containing APP fertilizer degree of polymerization detection method, step is as follows:
(1) 3g sample is taken, add deionized water dissolving, regulate solution ph to alkalescence (specifically pH=8) by NaOH solution, insolubles in solution is fallen with Filter paper filtering, by filtrate constant volume in the volumetric flask of 100ml, shift out 50ml solution with transfer pipet and carry out ion-exchange, be surely dissolved in 250ml volumetric flask, after measuring pH value, equal portions are to be measured;
(2) solution to be measured adds enough HCl solution adjustment pH to 3, vs replaces with NaOH standard solution, and titration sample solution is to terminal near pH=9.5, the volume of the alkali that record pH value consumes from 4.5 to 9.5 titration, mark A, is namely equal to the content of sample end group phosphorus;
(3) choosing above-mentioned equal portions liquid to be measured in round-bottomed flask is diluted to 150ml with deionized water, add 10ml, HCl solution that concentration is 6mol/L, condensing reflux 6h, solution ph is regulated to be 3 places, titration is carried out according to the method for step (2), the volume of the alkali this time consumed, is labeled as Ah, is namely equal to the content of total phosphorus in sample.
Computing formula: n=2*Ah/A
In formula: the n------degree of polymerization;
A------end group phosphorus consumes the volume of alkali, mL;
Ah------total phosphorus consumes the volume of alkali, mL;
Same sample Parallel testing 3 times, the relative error of measurement result should within 10%.
Concrete test data is in table 1
Embodiment 2: a kind of containing APP fertilizer degree of polymerization detection method, step is as follows:
(1) 5g sample is taken, add deionized water dissolving, regulate solution ph to alkalescence (specifically pH=8) by NaOH solution, insolubles in solution is fallen with Filter paper filtering, by filtrate constant volume in the volumetric flask of 100ml, shift out 50ml solution with transfer pipet and carry out ion-exchange, be surely dissolved in 250ml volumetric flask, after measuring pH value, equal portions are to be measured;
(2) solution to be measured adds enough HCl solution adjustment pH to 3, vs replaces with NaOH standard solution, and titration sample solution is to terminal near pH=9.5, the volume of the alkali that record pH value consumes from 4.5 to 9.5 titration, mark A, is namely equal to the content of sample end group phosphorus;
(3) choosing above-mentioned equal portions liquid to be measured in round-bottomed flask is diluted to 100ml with deionized water, add 10ml, HCl solution that concentration is 6mol/L, condensing reflux 6h, solution ph is regulated to be 3 places, titration is carried out according to the method for step (2), the volume of the alkali this time consumed, is labeled as Ah, is namely equal to the content of total phosphorus in sample.
Computing formula: n=2*Ah/A
In formula: the n------degree of polymerization;
A------end group phosphorus consumes the volume of alkali, mL;
Ah------total phosphorus consumes the volume of alkali, mL;
Same sample Parallel testing 3 times, the relative error of measurement result should within 10%.
Concrete test data is in table 1
Embodiment 3: a kind of containing APP fertilizer degree of polymerization detection method, step is as follows:
(1) 4g sample is taken, add deionized water dissolving, regulate solution ph to alkalescence (specifically pH=8) by NaOH solution, insolubles in solution is fallen with Filter paper filtering, by filtrate constant volume in the volumetric flask of 100ml, shift out 50ml solution with transfer pipet and carry out ion-exchange, be surely dissolved in 250ml volumetric flask, after measuring pH value, equal portions are to be measured;
(2) solution to be measured adds enough HCl solution adjustment pH to 3, vs replaces with NaOH standard solution, and titration sample solution is to terminal near pH=9.5, the volume of the alkali that record pH value consumes from 4.5 to 9.5 titration, mark A, is namely equal to the content of sample end group phosphorus;
(3) choosing above-mentioned equal portions liquid to be measured in round-bottomed flask is diluted to 150ml with deionized water, add 10ml, HCl solution that concentration is 6mol/L, condensing reflux 6h, solution ph is regulated to be 3 places, titration is carried out according to the method for step (2), the volume of the alkali this time consumed, is labeled as Ah, is namely equal to the content of total phosphorus in sample.
Computing formula: n=2*Ah/A
In formula: the n------degree of polymerization;
A------end group phosphorus consumes the volume of alkali, mL;
Ah------total phosphorus consumes the volume of alkali, mL;
Same sample Parallel testing 3 times, the relative error of measurement result should within 10%.
Concrete test data is in table 1
Table 1
This detection method is that the research and development containing APP fertilizer provide force data, instruct the cycle of technological parameter formula, APP fertilizer fertilizer efficiency release in soil, the calcium with the soil liquid, magnesium, iron, aluminium plasma reaction thus promote fertilizer efficiency utilization factor, the main functionality of APP in fertilizer can be given prominence to, additive method on year-on-year basis, the method is stable, reliable, and result is more accurate.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change above-mentioned embodiment and revise.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this instructions, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (10)
1. the detection method of the APP degree of polymerization of a fertilizer, it is characterized in that, comprise the following steps: fertilizer sample is dissolved by (1), and adjust ph is to alkalescence, through the solution constant volume of ion-exchange, divides equally and obtains two parts of liquid to be measured, (2) a liquid to be measured adds acid for adjusting pH to 2 ~ 4, use alkalimetric titration, the volume of the alkali that record pH value consumes from 4.5 to 9.5 titration, mark A; (3) after another part of liquid acid adding to be measured is cleared up, add acid for adjusting pH to 2 ~ 4, use alkalimetric titration, the volume of the alkali that record pH value consumes from 4.5 to 9.5 titration, mark Ah;
Computing formula: n=2*Ah/A,
In formula: the n------degree of polymerization;
A------end group phosphorus consumes the volume of alkali, mL;
Ah------total phosphorus consumes the volume of alkali, mL.
2. detection method according to claim 1, is characterized in that, comprises the following steps:
(1) 2 ~ 100g fertilizer sample is taken, be dissolved in water, regulate solution ph to alkalescence, filter insolubles, by filtrate constant volume in the volumetric flask of 100 ~ 1000ml, shift out 25 ~ 100ml solution with transfer pipet and carry out ion-exchange, be surely dissolved in 100 ~ 250ml volumetric flask, divide equally and obtain two parts of liquid to be measured;
(2) a liquid to be measured adds acid for adjusting pH to 2 ~ 4, uses aqueous slkali titration, the volume of the alkali that record pH value consumes from 4.5 to 9.5 titration, mark A, the i.e. content of sample end group phosphorus;
(3) another part of liquid deionized water to be measured is diluted to 100 ~ 250ml, after acid adding clears up 2 ~ 8 hours, regulates solution ph to 2 ~ 4, use aqueous slkali titration, the volume of alkali that record pH value consumes from 4.5 to 9.5 titration, is labeled as Ah, i.e. the content of total phosphorus in sample;
Computing formula: n=2*Ah/A
In formula: the n------degree of polymerization;
A------end group phosphorus consumes the volume of alkali, mL;
Ah------total phosphorus consumes the volume of alkali, mL.
3. detection method according to claim 1 and 2, is characterized in that, described fertilizer sample is for containing APP fertilizer, and APP is chain structure.
4. detection method according to claim 1 and 2, is characterized in that, step (1) described dissolving is at 0 ~ 20 DEG C.
5. detection method according to claim 1 and 2, is characterized in that, described ion-exchange uses Zeo-karb.
6. detection method according to claim 5, is characterized in that, described Zeo-karb is the polystyrene Na type resin of sulfuric acid sulfonation.
7. detection method according to claim 1 and 2, is characterized in that, step (2) described acid is inorganic acid.
8. detection method according to claim 7, is characterized in that, step (2) described acid is the concentrated sulphuric acid, red fuming nitric acid (RFNA), concentrated hydrochloric acid.
9. detection method according to claim 1 and 2, is characterized in that, the addition of step (2) described acid is 5 ~ 20ml, and concentration is 4 ~ 10mol/L.
10. detection method according to claim 1 and 2, is characterized in that, also comprises the step of fertilizer sample Parallel testing 3 times.
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Cited By (4)
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| CN105259301A (en) * | 2015-11-12 | 2016-01-20 | 山东泰宝生物科技股份有限公司 | Ammonium polyphosphate agricultural water soluble fertilizer polymerization degree detection method |
| CN105259070A (en) * | 2015-11-12 | 2016-01-20 | 山东泰宝生物科技股份有限公司 | Ammonium polyphosphate agricultural water soluble fertilizer polymerization degree detection method |
| CN105572120A (en) * | 2015-12-16 | 2016-05-11 | 贵州省化工研究院 | Method for detecting phosphorus content of compound fertilizer |
| CN111044670A (en) * | 2019-12-25 | 2020-04-21 | 西安热工研究院有限公司 | Cation exchange capacity test method for ammonium type and ammonium type mixed powder ion exchange resin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105259301A (en) * | 2015-11-12 | 2016-01-20 | 山东泰宝生物科技股份有限公司 | Ammonium polyphosphate agricultural water soluble fertilizer polymerization degree detection method |
| CN105259070A (en) * | 2015-11-12 | 2016-01-20 | 山东泰宝生物科技股份有限公司 | Ammonium polyphosphate agricultural water soluble fertilizer polymerization degree detection method |
| CN105259070B (en) * | 2015-11-12 | 2017-12-15 | 山东泰宝生物科技股份有限公司 | The agricultural water soluble fertilizer aggregate rate detection method of ammonium polyphosphate |
| CN105572120A (en) * | 2015-12-16 | 2016-05-11 | 贵州省化工研究院 | Method for detecting phosphorus content of compound fertilizer |
| CN111044670A (en) * | 2019-12-25 | 2020-04-21 | 西安热工研究院有限公司 | Cation exchange capacity test method for ammonium type and ammonium type mixed powder ion exchange resin |
| CN111044670B (en) * | 2019-12-25 | 2022-06-10 | 西安热工研究院有限公司 | Cation exchange capacity test method for ammonium type and ammonium type mixed powder ion exchange resin |
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